#------------------------------------------------------------------------------
#$Date: 2016-03-26 01:55:57 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180115 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/13/7101310.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_7101310
loop_
_publ_author_name
J.-C.Berthet
G.Siffredi
P.Thuery
M.Ephritikhine
_publ_section_title
;
Convenient access to stable pentavalent uranyl complexes.
;
_journal_issue                   30
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b605710a
_journal_year                    2006
_chemical_formula_sum            'C35 H35 I2 K N7 O2 U'
_chemical_formula_weight         1116.63
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.794(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8453(4)
_cell_length_b                   19.1818(7)
_cell_length_c                   16.0316(5)
_cell_measurement_reflns_used    126670
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.12
_cell_volume                     3880.2(2)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and five ω scans with 2° steps'
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0324
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            126670
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.921
_exptl_absorpt_correction_T_max  0.661
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent dark orange'
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2108
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0206
_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/[σ²(Fo²)+(0.0154P)²+0.0072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0388
_refine_ls_wR_factor_ref         0.0405
_reflns_number_gt                6271
_reflns_number_total             7370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b605710a.txt
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7101310
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'
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
U U 0.880406(8) 0.756081(6) 0.040461(7) 0.01671(4) Uani 1 1 d .
K K 0.63450(5) 0.74760(4) -0.21147(4) 0.02129(14) Uani 1 1 d .
I1 I 0.470670(16) 0.853239(11) -0.109442(13) 0.02475(6) Uani 1 1 d .
I2 I 0.770214(15) 0.864509(11) -0.322674(12) 0.02298(5) Uani 1 1 d .
O1 O 0.78238(16) 0.75407(11) -0.05945(12) 0.0219(5) Uani 1 1 d .
O2 O 0.98022(16) 0.75901(11) 0.13917(12) 0.0218(5) Uani 1 1 d .
N1 N 0.78792(19) 0.86238(13) 0.09781(15) 0.0200(6) Uani 1 1 d .
N2 N 0.96417(19) 0.86656(13) -0.01241(15) 0.0197(6) Uani 1 1 d .
N3 N 1.02398(19) 0.71923(13) -0.04615(16) 0.0207(6) Uani 1 1 d .
N4 N 0.88402(19) 0.62092(14) 0.04056(15) 0.0224(6) Uani 1 1 d .
N5 N 0.73298(19) 0.71086(14) 0.11755(15) 0.0220(6) Uani 1 1 d .
N6 N 0.7712(2) 0.62622(16) -0.27500(17) 0.0306(7) Uani 1 1 d .
N7 N 0.5251(2) 0.63389(15) -0.14665(16) 0.0284(7) Uani 1 1 d .
C1 C 0.8053(2) 0.87492(17) 0.18156(19) 0.0247(7) Uani 1 1 d .
H1 H 0.8539 0.8470 0.2169 0.030 Uiso 1 1 calc R
C2 C 0.7548(2) 0.92715(18) 0.2179(2) 0.0268(8) Uani 1 1 d .
H2 H 0.7685 0.9339 0.2764 0.032 Uiso 1 1 calc R
C3 C 0.6832(2) 0.96934(18) 0.1654(2) 0.0263(7) Uani 1 1 d .
H3 H 0.6487 1.0055 0.1878 0.032 Uiso 1 1 calc R
C4 C 0.6642(2) 0.95677(18) 0.0796(2) 0.0277(8) Uani 1 1 d .
H4 H 0.6161 0.9841 0.0430 0.033 Uiso 1 1 calc R
C5 C 0.7173(2) 0.90300(18) 0.0482(2) 0.0250(7) Uani 1 1 d .
H5 H 0.7033 0.8947 -0.0099 0.030 Uiso 1 1 calc R
C6 C 0.9276(2) 0.88970(17) -0.09197(19) 0.0228(7) Uani 1 1 d .
H6 H 0.8643 0.8714 -0.1216 0.027 Uiso 1 1 calc R
C7 C 0.9790(3) 0.93893(17) -0.1313(2) 0.0278(8) Uani 1 1 d .
H7 H 0.9506 0.9538 -0.1861 0.033 Uiso 1 1 calc R
C8 C 1.0744(3) 0.96624(19) -0.0881(2) 0.0318(8) Uani 1 1 d .
H8 H 1.1113 0.9992 -0.1136 0.038 Uiso 1 1 calc R
C9 C 1.1129(3) 0.94317(18) -0.0065(2) 0.0300(8) Uani 1 1 d .
H9 H 1.1766 0.9602 0.0240 0.036 Uiso 1 1 calc R
C10 C 1.0552(2) 0.89426(17) 0.0290(2) 0.0255(7) Uani 1 1 d .
H10 H 1.0808 0.8798 0.0844 0.031 Uiso 1 1 calc R
C11 C 1.1260(2) 0.73396(17) -0.0156(2) 0.0248(7) Uani 1 1 d .
H11 H 1.1450 0.7489 0.0403 0.030 Uiso 1 1 calc R
C12 C 1.2040(3) 0.72788(18) -0.0637(2) 0.0305(8) Uani 1 1 d .
H12 H 1.2737 0.7398 -0.0409 0.037 Uiso 1 1 calc R
C13 C 1.1776(3) 0.70421(19) -0.1450(2) 0.0326(8) Uani 1 1 d .
H13 H 1.2287 0.7003 -0.1789 0.039 Uiso 1 1 calc R
C14 C 1.0727(3) 0.68590(18) -0.1767(2) 0.0318(8) Uani 1 1 d .
H14 H 1.0531 0.6676 -0.2311 0.038 Uiso 1 1 calc R
C15 C 0.9992(3) 0.69543(17) -0.12593(19) 0.0256(7) Uani 1 1 d .
H15 H 0.9288 0.6849 -0.1479 0.031 Uiso 1 1 calc R
C16 C 0.9504(2) 0.58279(18) 0.0977(2) 0.0284(8) Uani 1 1 d .
H16 H 1.0014 0.6057 0.1370 0.034 Uiso 1 1 calc R
C17 C 0.9459(3) 0.51093(18) 0.1004(2) 0.0347(9) Uani 1 1 d .
H17 H 0.9926 0.4863 0.1413 0.042 Uiso 1 1 calc R
C18 C 0.8718(3) 0.47592(18) 0.0422(2) 0.0317(8) Uani 1 1 d .
H18 H 0.8679 0.4275 0.0427 0.038 Uiso 1 1 calc R
C19 C 0.8036(3) 0.51438(18) -0.0168(2) 0.0289(8) Uani 1 1 d .
H19 H 0.7527 0.4923 -0.0570 0.035 Uiso 1 1 calc R
C20 C 0.8117(2) 0.58597(18) -0.01562(19) 0.0250(7) Uani 1 1 d .
H20 H 0.7650 0.6114 -0.0556 0.030 Uiso 1 1 calc R
C21 C 0.7565(2) 0.67602(17) 0.19140(19) 0.0252(7) Uani 1 1 d .
H21 H 0.8273 0.6668 0.2137 0.030 Uiso 1 1 calc R
C22 C 0.6812(3) 0.65344(18) 0.2356(2) 0.0280(8) Uani 1 1 d .
H22 H 0.7008 0.6299 0.2868 0.034 Uiso 1 1 calc R
C23 C 0.5756(3) 0.66630(18) 0.2025(2) 0.0277(8) Uani 1 1 d .
H23 H 0.5229 0.6514 0.2311 0.033 Uiso 1 1 calc R
C24 C 0.5495(2) 0.70179(17) 0.1263(2) 0.0264(8) Uani 1 1 d .
H24 H 0.4791 0.7112 0.1028 0.032 Uiso 1 1 calc R
C25 C 0.6300(2) 0.72296(17) 0.0857(2) 0.0246(7) Uani 1 1 d .
H25 H 0.6123 0.7465 0.0343 0.029 Uiso 1 1 calc R
C26 C 0.8170(3) 0.65594(19) -0.3341(2) 0.0313(8) Uani 1 1 d .
H26 H 0.8058 0.7033 -0.3445 0.038 Uiso 1 1 calc R
C27 C 0.8801(3) 0.6203(2) -0.3808(2) 0.0338(9) Uani 1 1 d .
H27 H 0.9101 0.6431 -0.4216 0.041 Uiso 1 1 calc R
C28 C 0.8976(3) 0.5498(2) -0.3653(2) 0.0320(8) Uani 1 1 d .
H28 H 0.9400 0.5242 -0.3953 0.038 Uiso 1 1 calc R
C29 C 0.8506(3) 0.51867(19) -0.3046(2) 0.0333(8) Uani 1 1 d .
H29 H 0.8603 0.4714 -0.2927 0.040 Uiso 1 1 calc R
C30 C 0.7892(3) 0.5586(2) -0.2618(2) 0.0327(9) Uani 1 1 d .
H30 H 0.7581 0.5368 -0.2209 0.039 Uiso 1 1 calc R
C31 C 0.5418(3) 0.56878(19) -0.1692(2) 0.0305(8) Uani 1 1 d .
H31 H 0.5881 0.5617 -0.2066 0.037 Uiso 1 1 calc R
C32 C 0.4949(3) 0.5111(2) -0.1407(2) 0.0347(9) Uani 1 1 d .
H32 H 0.5094 0.4664 -0.1582 0.042 Uiso 1 1 calc R
C33 C 0.4255(3) 0.52152(19) -0.0853(2) 0.0317(8) Uani 1 1 d .
H33 H 0.3915 0.4840 -0.0652 0.038 Uiso 1 1 calc R
C34 C 0.4078(3) 0.58877(19) -0.0603(2) 0.0296(8) Uani 1 1 d .
H34 H 0.3620 0.5976 -0.0230 0.036 Uiso 1 1 calc R
C35 C 0.4604(2) 0.64280(17) -0.09258(19) 0.0241(7) Uani 1 1 d .
H35 H 0.4494 0.6880 -0.0750 0.029 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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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 U O1 178.85(9) . .
O2 U N2 89.50(8) . .
O1 U N2 89.47(8) . .
O2 U N4 91.17(8) . .
O1 U N4 89.36(8) . .
N2 U N4 144.07(8) . .
O2 U N5 93.07(8) . .
O1 U N5 88.06(8) . .
N2 U N5 144.46(8) . .
N4 U N5 71.36(8) . .
O2 U N3 91.02(8) . .
O1 U N3 88.15(8) . .
N2 U N3 70.65(8) . .
N4 U N3 73.42(8) . .
N5 U N3 144.60(8) . .
O2 U N1 87.89(8) . .
O1 U N1 92.32(8) . .
N2 U N1 73.78(8) . .
N4 U N1 142.14(8) . .
N5 U N1 70.91(8) . .
N3 U N1 144.42(8) . .
O1 K O2 177.98(6) . 4_575
O1 K N7 90.96(7) . .
O2 K N7 87.69(7) 4_575 .
O1 K N6 89.20(7) . .
O2 K N6 92.15(7) 4_575 .
N7 K N6 84.14(8) . .
O1 K I2 95.33(5) . .
O2 K I2 86.24(5) 4_575 .
N7 K I2 169.12(6) . .
N6 K I2 87.08(6) . .
O1 K I1 86.41(5) . .
O2 K I1 91.96(5) 4_575 .
N7 K I1 83.96(6) . .
N6 K I1 167.23(6) . .
I2 K I1 105.255(19) . .
U O1 K 178.63(11) . .
U O2 K 175.62(11) . 4_676
C5 N1 C1 117.2(3) . .
C5 N1 U 123.2(2) . .
C1 N1 U 119.4(2) . .
C10 N2 C6 117.1(3) . .
C10 N2 U 122.6(2) . .
C6 N2 U 119.07(19) . .
C15 N3 C11 117.5(3) . .
C15 N3 U 122.4(2) . .
C11 N3 U 119.3(2) . .
C20 N4 C16 117.1(3) . .
C20 N4 U 119.2(2) . .
C16 N4 U 123.6(2) . .
C21 N5 C25 117.6(3) . .
C21 N5 U 121.45(19) . .
C25 N5 U 121.0(2) . .
C30 N6 C26 116.3(3) . .
C30 N6 K 138.7(2) . .
C26 N6 K 104.9(2) . .
C35 N7 C31 117.0(3) . .
C35 N7 K 123.1(2) . .
C31 N7 K 119.8(2) . .
N1 C1 C2 123.3(3) . .
C1 C2 C3 118.6(3) . .
C4 C3 C2 118.7(3) . .
C3 C4 C5 119.2(3) . .
N1 C5 C4 123.0(3) . .
N2 C6 C7 123.3(3) . .
C6 C7 C8 119.0(3) . .
C9 C8 C7 118.5(3) . .
C8 C9 C10 118.8(3) . .
N2 C10 C9 123.4(3) . .
N3 C11 C12 122.8(3) . .
C13 C12 C11 119.1(3) . .
C12 C13 C14 118.9(3) . .
C15 C14 C13 118.5(3) . .
N3 C15 C14 123.1(3) . .
N4 C16 C17 122.6(3) . .
C18 C17 C16 119.6(3) . .
C17 C18 C19 118.3(3) . .
C18 C19 C20 119.2(3) . .
N4 C20 C19 123.2(3) . .
N5 C21 C22 123.2(3) . .
C21 C22 C23 118.8(3) . .
C22 C23 C24 118.9(3) . .
C25 C24 C23 118.8(3) . .
N5 C25 C24 122.7(3) . .
N6 C26 C27 123.7(3) . .
C26 C27 C28 118.6(3) . .
C29 C28 C27 118.2(3) . .
C30 C29 C28 118.8(4) . .
N6 C30 C29 124.4(3) . .
N7 C31 C32 124.2(3) . .
C31 C32 C33 118.0(3) . .
C34 C33 C32 118.7(3) . .
C33 C34 C35 118.1(3) . .
N7 C35 C34 123.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U O2 1.8415(19) .
U O1 1.8431(19) .
U N2 2.590(3) .
U N4 2.593(3) .
U N5 2.597(3) .
U N3 2.605(3) .
U N1 2.612(3) .
K O1 2.798(2) .
K O2 2.811(2) 4_575
K N7 2.891(3) .
K N6 3.195(3) .
K I2 3.5229(7) .
K I1 3.5355(7) .
O2 K 2.811(2) 4_676
N1 C5 1.339(4) .
N1 C1 1.341(4) .
N2 C10 1.341(4) .
N2 C6 1.349(4) .
N3 C15 1.339(4) .
N3 C11 1.340(4) .
N4 C20 1.345(4) .
N4 C16 1.345(4) .
N5 C21 1.344(4) .
N5 C25 1.346(4) .
N6 C30 1.328(5) .
N6 C26 1.333(4) .
N7 C35 1.320(4) .
N7 C31 1.329(4) .
C1 C2 1.381(4) .
C2 C3 1.386(4) .
C3 C4 1.372(4) .
C4 C5 1.382(5) .
C6 C7 1.372(4) .
C7 C8 1.392(5) .
C8 C9 1.382(5) .
C9 C10 1.383(5) .
C11 C12 1.378(4) .
C12 C13 1.362(5) .
C13 C14 1.392(5) .
C14 C15 1.370(5) .
C16 C17 1.381(5) .
C17 C18 1.376(5) .
C18 C19 1.377(5) .
C19 C20 1.377(5) .
C21 C22 1.372(4) .
C22 C23 1.383(4) .
C23 C24 1.384(4) .
C24 C25 1.381(4) .
C26 C27 1.383(5) .
C27 C28 1.386(5) .
C28 C29 1.375(5) .
C29 C30 1.371(5) .
C31 C32 1.379(5) .
C32 C33 1.387(5) .
C33 C34 1.382(5) .
C34 C35 1.389(5) .
