#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/83/4108346.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_4108346
loop_
_publ_author_name
'Suzanne C. Bart'
'Christian Anthon'
'Frank W. Heinemann'
'Eckhard Bill'
'Norman M. Edelstein'
'Karsten Meyer'
_publ_section_title
;
 Carbon Dioxide Activation with Sterically Pressured Mid- and High-Valent
 Uranium Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12536
_journal_page_last               12546
_journal_paper_doi               10.1021/ja804263w
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C51 H78 N3 O4 U, 3(C5 H12)'
_chemical_formula_sum            'C66 H114 N3 O4 U'
_chemical_formula_weight         1251.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           173
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c'
_symmetry_space_group_name_H-M   'P 63'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   14.841(2)
_cell_length_b                   14.841(2)
_cell_length_c                   15.8111(8)
_cell_measurement_reflns_used    210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     3015.9(6)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
 ω-rotations with 2.00 ° and 192 sec per frame
;
_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  0.1023
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48237
_diffrn_reflns_theta_full        27.09
_diffrn_reflns_theta_max         27.09
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    2.740
_exptl_absorpt_correction_T_max  0.900
_exptl_absorpt_correction_T_min  0.716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       needle
_exptl_crystal_F_000             1310
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack H D (1983), Acta Cryst. A39, 876-881
 2139 Friedel pairs used in the refinement of Flack parameter
;
_refine_ls_abs_structure_Flack   0.190(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4439
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0325P)²+13.3406P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                2863
_reflns_number_total             4439
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja804263w_si_003.cif
_cod_data_source_block           sd0728
_cod_original_sg_symbol_Hall     P6c
_cod_database_code               4108346
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, 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
U1 U 0.0000 1.0000 -0.02769(9) 0.01194(10) Uani 1 3 d S . .
O1 O -0.0287(4) 0.8397(4) -0.0382(5) 0.0210(13) Uani 1 1 d . . .
N1 N 0.0830(5) 0.9572(5) 0.1059(4) 0.0156(13) Uani 1 1 d . . .
C1 C 0.0077(6) 0.8866(6) 0.1722(5) 0.0156(15) Uani 1 1 d . . .
H1A H 0.0171 0.9272 0.2245 0.019 Uiso 1 1 calc R . .
H1B H 0.0235 0.8309 0.1858 0.019 Uiso 1 1 calc R . .
C2 C -0.1041(6) 0.8379(6) 0.1437(5) 0.0175(16) Uani 1 1 d . . .
H2A H -0.1188 0.7830 0.1014 0.021 Uiso 1 1 calc R . .
H2B H -0.1508 0.8049 0.1927 0.021 Uiso 1 1 calc R . .
C3 C 0.1406(6) 0.9074(6) 0.0686(5) 0.0186(16) Uani 1 1 d . . .
H3A H 0.1782 0.9474 0.0177 0.022 Uiso 1 1 calc R . .
H3B H 0.1934 0.9137 0.1100 0.022 Uiso 1 1 calc R . .
C4 C 0.0766(6) 0.7964(6) 0.0443(5) 0.0203(16) Uani 1 1 d . . .
C5 C -0.0077(5) 0.7663(6) -0.0119(5) 0.0168(19) Uani 1 1 d . . .
C6 C -0.0648(6) 0.6602(6) -0.0378(8) 0.026(2) Uani 1 1 d . . .
C7 C -0.0378(8) 0.5921(7) -0.0033(6) 0.037(3) Uani 1 1 d . . .
H7A H -0.0765 0.5212 -0.0199 0.044 Uiso 1 1 calc R . .
C8 C 0.0436(9) 0.6206(7) 0.0551(6) 0.041(3) Uani 1 1 d . . .
C9 C 0.0974(7) 0.7228(7) 0.0757(6) 0.0283(19) Uani 1 1 d . . .
H9A H 0.1534 0.7449 0.1145 0.034 Uiso 1 1 calc R . .
C10 C -0.1513(7) 0.6237(6) -0.1055(5) 0.0231(18) Uani 1 1 d . . .
C11 C -0.1052(8) 0.6860(7) -0.1879(6) 0.033(2) Uani 1 1 d . . .
H11A H -0.0506 0.6731 -0.2091 0.050 Uiso 1 1 calc R . .
H11B H -0.0755 0.7604 -0.1764 0.050 Uiso 1 1 calc R . .
H11C H -0.1603 0.6639 -0.2305 0.050 Uiso 1 1 calc R . .
C12 C -0.2387(8) 0.6432(9) -0.0765(8) 0.055(3) Uani 1 1 d . . .
H12A H -0.2659 0.6088 -0.0219 0.082 Uiso 1 1 calc R . .
H12B H -0.2947 0.6149 -0.1185 0.082 Uiso 1 1 calc R . .
H12C H -0.2112 0.7181 -0.0704 0.082 Uiso 1 1 calc R . .
C13 C -0.2017(8) 0.5083(7) -0.1270(6) 0.039(2) Uani 1 1 d . . .
H13A H -0.2268 0.4671 -0.0750 0.058 Uiso 1 1 calc R . .
H13B H -0.1503 0.4947 -0.1542 0.058 Uiso 1 1 calc R . .
H13C H -0.2603 0.4889 -0.1656 0.058 Uiso 1 1 calc R . .
C14 C 0.0685(11) 0.5376(9) 0.0840(8) 0.060(4) Uani 1 1 d . . .
C15 C 0.1039(15) 0.4985(11) 0.0152(9) 0.088(5) Uani 1 1 d . . .
H15A H 0.1680 0.5556 -0.0087 0.132 Uiso 1 1 calc R . .
H15B H 0.0502 0.4691 -0.0287 0.132 Uiso 1 1 calc R . .
H15C H 0.1174 0.4444 0.0366 0.132 Uiso 1 1 calc R . .
C16 C 0.1515(11) 0.5796(10) 0.1512(8) 0.066(4) Uani 1 1 d . . .
H16A H 0.2160 0.6364 0.1276 0.099 Uiso 1 1 calc R . .
H16B H 0.1636 0.5240 0.1709 0.099 Uiso 1 1 calc R . .
H16C H 0.1287 0.6057 0.1987 0.099 Uiso 1 1 calc R . .
C17 C -0.0270(13) 0.4430(11) 0.1159(9) 0.082(5) Uani 1 1 d . . .
H17A H -0.0796 0.4149 0.0711 0.123 Uiso 1 1 calc R . .
H17B H -0.0546 0.4618 0.1648 0.123 Uiso 1 1 calc R . .
H17C H -0.0091 0.3902 0.1327 0.123 Uiso 1 1 calc R . .
O2 O 0.0000 1.0000 -0.1445(5) 0.0185(16) Uani 1 3 d S . .
C101 C 0.5722(14) 0.8231(13) 0.8488(9) 0.062(5) Uani 0.67 1 d PDU A 1
C102 C 0.6664(13) 0.7974(12) 0.8312(10) 0.039(3) Uani 0.67 1 d PDU A 1
C103 C 0.6180(14) 0.7271(14) 0.7566(10) 0.056(3) Uani 0.67 1 d PDU A 1
C104 C 0.5759(16) 0.7323(16) 0.6790(12) 0.074(4) Uani 0.67 1 d PDU A 1
C105 C 0.626(2) 0.814(2) 0.6083(17) 0.121(7) Uani 0.67 1 d PDU A 1
C106 C 0.366(3) 0.667(5) 0.577(2) 0.082(7) Uani 0.33 1 d PDU . 2
C107 C 0.460(3) 0.722(3) 0.637(3) 0.081(6) Uani 0.33 1 d PDU B 2
C108 C 0.538(3) 0.806(3) 0.6986(19) 0.077(6) Uani 0.33 1 d PDU B 2
C109 C 0.528(3) 0.848(2) 0.785(2) 0.065(6) Uani 0.33 1 d PDU B 2
C110 C 0.437(2) 0.748(2) 0.8202(19) 0.037(5) Uani 0.33 1 d PDU B 2
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'
U U -9.6767 9.6646 '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
O2 U1 O1 85.7(2) . 2_675
O2 U1 O1 85.7(2) . .
O1 U1 O1 119.44(6) 2_675 .
O2 U1 O1 85.7(2) . 3_465
O1 U1 O1 119.44(6) 2_675 3_465
O1 U1 O1 119.44(6) . 3_465
O2 U1 N1 142.08(13) . 2_675
O1 U1 N1 70.5(2) 2_675 2_675
O1 U1 N1 131.5(3) . 2_675
O1 U1 N1 81.3(2) 3_465 2_675
O2 U1 N1 142.08(13) . .
O1 U1 N1 81.3(2) 2_675 .
O1 U1 N1 70.5(2) . .
O1 U1 N1 131.5(3) 3_465 .
N1 U1 N1 64.3(2) 2_675 .
O2 U1 N1 142.08(13) . 3_465
O1 U1 N1 131.5(3) 2_675 3_465
O1 U1 N1 81.3(2) . 3_465
O1 U1 N1 70.5(2) 3_465 3_465
N1 U1 N1 64.3(2) 2_675 3_465
N1 U1 N1 64.3(2) . 3_465
C5 O1 U1 148.9(5) . .
C2 N1 C3 107.2(6) 2_675 .
C2 N1 C1 110.8(6) 2_675 .
C3 N1 C1 109.8(6) . .
C2 N1 U1 107.7(4) 2_675 .
C3 N1 U1 104.5(4) . .
C1 N1 U1 116.4(4) . .
N1 C1 C2 112.3(6) . .
N1 C1 H1A 109.1 . .
C2 C1 H1A 109.1 . .
N1 C1 H1B 109.1 . .
C2 C1 H1B 109.1 . .
H1A C1 H1B 107.9 . .
N1 C2 C1 111.2(6) 3_465 .
N1 C2 H2A 109.4 3_465 .
C1 C2 H2A 109.4 . .
N1 C2 H2B 109.4 3_465 .
C1 C2 H2B 109.4 . .
H2A C2 H2B 108.0 . .
C4 C3 N1 116.3(6) . .
C4 C3 H3A 108.2 . .
N1 C3 H3A 108.2 . .
C4 C3 H3B 108.2 . .
N1 C3 H3B 108.2 . .
H3A C3 H3B 107.4 . .
C9 C4 C5 119.6(8) . .
C9 C4 C3 121.3(7) . .
C5 C4 C3 119.2(7) . .
O1 C5 C4 117.9(7) . .
O1 C5 C6 123.9(7) . .
C4 C5 C6 118.2(7) . .
C7 C6 C5 117.9(8) . .
C7 C6 C10 120.9(7) . .
C5 C6 C10 121.2(7) . .
C6 C7 C8 124.2(8) . .
C6 C7 H7A 117.9 . .
C8 C7 H7A 117.9 . .
C9 C8 C7 115.5(8) . .
C9 C8 C14 126.1(9) . .
C7 C8 C14 118.3(9) . .
C8 C9 C4 124.4(9) . .
C8 C9 H9A 117.8 . .
C4 C9 H9A 117.8 . .
C13 C10 C12 107.0(8) . .
C13 C10 C11 107.8(7) . .
C12 C10 C11 107.6(8) . .
C13 C10 C6 113.8(7) . .
C12 C10 C6 111.0(7) . .
C11 C10 C6 109.4(7) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C15 C14 C17 103.9(12) . .
C15 C14 C16 108.1(12) . .
C17 C14 C16 110.1(11) . .
C15 C14 C8 112.5(10) . .
C17 C14 C8 111.1(11) . .
C16 C14 C8 110.9(9) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C14 C17 H17A 109.5 . .
C14 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C14 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C103 C102 C101 97.3(13) . .
C104 C103 C102 136.5(19) . .
C103 C104 C105 129(2) . .
C106 C107 C108 158(5) . .
C109 C108 C107 134(4) . .
C110 C109 C108 98(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O2 1.848(7) .
U1 O1 2.203(5) 2_675
U1 O1 2.203(5) .
U1 O1 2.203(5) 3_465
U1 N1 2.676(6) 2_675
U1 N1 2.676(6) .
U1 N1 2.676(6) 3_465
O1 C5 1.340(9) .
N1 C2 1.489(10) 2_675
N1 C3 1.501(9) .
N1 C1 1.509(10) .
C1 C2 1.510(10) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 N1 1.489(10) 3_465
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.482(11) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C9 1.368(11) .
C4 C5 1.413(10) .
C5 C6 1.425(11) .
C6 C7 1.374(12) .
C6 C10 1.546(13) .
C7 C8 1.406(13) .
C7 H7A 0.9500 .
C8 C9 1.354(12) .
C8 C14 1.522(13) .
C9 H9A 0.9500 .
C10 C13 1.525(11) .
C10 C12 1.533(13) .
C10 C11 1.545(12) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 C15 1.449(19) .
C14 C17 1.499(19) .
C14 C16 1.505(16) .
C15 H15A 0.9800 .
C15 H15B 0.9800 .
C15 H15C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C101 C102 1.644(17) .
C102 C103 1.499(16) .
C103 C104 1.396(16) .
C104 C105 1.538(18) .
C106 C107 1.54(2) .
C107 C108 1.55(2) .
C108 C109 1.54(2) .
C109 C110 1.53(2) .
