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#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/44/1514400.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_1514400
loop_
_publ_author_name
'Yin, Haolin'
'Lewis, Andrew J.'
'Williams, Ursula J.'
'Carroll, Patrick J.'
'Schelter, Eric J.'
_publ_section_title
;
 Fluorinated diarylamide complexes of uranium(iii, iv) incorporating
 ancillary fluorine-to-uranium dative interactions
;
_journal_issue                   2
_journal_name_full               'Chemical Science'
_journal_page_first              798
_journal_paper_doi               10.1039/c2sc21458j
_journal_volume                  4
_journal_year                    2013
_chemical_formula_sum            'C48 F40 N4 U'
_chemical_formula_weight         1630.55
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.846(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.5319(8)
_cell_length_b                   12.9011(5)
_cell_length_c                   16.0719(6)
_cell_measurement_temperature    143(1)
_cell_volume                     4669.8(3)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            47650
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    3.682
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    2.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         5367
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0204
_refine_ls_R_factor_gt           0.0179
_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)+(0.0284P)²+4.1986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0456
_reflns_number_gt                5068
_reflns_number_total             5367
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc21458j.txt
_cod_data_source_block           UP4247(1-PhF2)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               1514400
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
U1 U 0.5000 0.620115(7) 0.7500 0.01960(4) Uani 1 2 d S
N1 N 0.5000 0.43508(18) 0.7500 0.0211(5) Uani 1 2 d S
N2 N 0.5000 0.80383(18) 0.7500 0.0200(4) Uani 1 2 d S
N3 N 0.59573(8) 0.63785(14) 0.83412(11) 0.0250(3) Uani 1 1 d .
C1 C 0.45268(9) 0.38087(14) 0.76612(13) 0.0212(4) Uani 1 1 d .
C2 C 0.42072(9) 0.43069(15) 0.81506(12) 0.0220(4) Uani 1 1 d .
C3 C 0.37041(9) 0.39175(16) 0.83085(13) 0.0249(4) Uani 1 1 d .
C4 C 0.34953(9) 0.29659(18) 0.79684(14) 0.0280(4) Uani 1 1 d .
C5 C 0.37873(9) 0.24425(17) 0.74679(14) 0.0280(4) Uani 1 1 d .
C6 C 0.42873(9) 0.28615(16) 0.73075(14) 0.0251(4) Uani 1 1 d .
C7 C 0.48301(9) 0.85647(15) 0.67071(13) 0.0215(4) Uani 1 1 d .
C8 C 0.48947(9) 0.80457(15) 0.59807(13) 0.0232(4) Uani 1 1 d .
C9 C 0.46976(10) 0.84055(18) 0.51416(13) 0.0290(4) Uani 1 1 d .
C10 C 0.44109(10) 0.93496(19) 0.49952(14) 0.0315(5) Uani 1 1 d .
C11 C 0.43269(10) 0.98981(17) 0.56873(14) 0.0289(4) Uani 1 1 d .
C12 C 0.45279(9) 0.95092(16) 0.65270(13) 0.0243(4) Uani 1 1 d .
C13 C 0.62271(9) 0.54648(17) 0.87817(13) 0.0248(4) Uani 1 1 d .
C14 C 0.67340(9) 0.50279(18) 0.86378(13) 0.0265(4) Uani 1 1 d .
C15 C 0.69752(10) 0.4120(2) 0.90274(16) 0.0333(5) Uani 1 1 d .
C16 C 0.67071(11) 0.35940(19) 0.95642(16) 0.0349(5) Uani 1 1 d .
C17 C 0.62097(10) 0.40054(19) 0.97217(14) 0.0307(5) Uani 1 1 d .
C18 C 0.59829(9) 0.49291(17) 0.93435(13) 0.0263(4) Uani 1 1 d .
C19 C 0.63345(9) 0.72612(17) 0.85150(14) 0.0257(4) Uani 1 1 d .
C20 C 0.65808(9) 0.76298(18) 0.93559(14) 0.0288(4) Uani 1 1 d .
C21 C 0.69194(10) 0.8515(2) 0.95360(16) 0.0334(5) Uani 1 1 d .
C22 C 0.70197(10) 0.90828(19) 0.88677(18) 0.0354(5) Uani 1 1 d .
C23 C 0.67937(11) 0.87357(18) 0.80253(17) 0.0353(5) Uani 1 1 d .
C24 C 0.64624(9) 0.78355(19) 0.78590(14) 0.0308(5) Uani 1 1 d .
F1 F 0.43930(5) 0.52832(9) 0.84458(8) 0.0270(2) Uani 1 1 d .
F2 F 0.34172(6) 0.44698(11) 0.87623(8) 0.0323(3) Uani 1 1 d .
F3 F 0.30014(6) 0.25701(11) 0.80963(9) 0.0381(3) Uani 1 1 d .
F4 F 0.35662(6) 0.15456(11) 0.70992(10) 0.0403(3) Uani 1 1 d .
F5 F 0.45302(6) 0.23559(10) 0.67661(9) 0.0314(3) Uani 1 1 d .
F6 F 0.51454(5) 0.70775(9) 0.61203(8) 0.0259(2) Uani 1 1 d .
F7 F 0.47716(7) 0.78456(12) 0.44838(8) 0.0385(3) Uani 1 1 d .
F8 F 0.42064(7) 0.97237(12) 0.41860(9) 0.0450(4) Uani 1 1 d .
F9 F 0.40294(7) 1.07916(11) 0.55428(9) 0.0418(3) Uani 1 1 d .
F10 F 0.44030(6) 1.00342(10) 0.71698(8) 0.0304(3) Uani 1 1 d .
F11 F 0.69834(6) 0.54958(11) 0.80868(8) 0.0332(3) Uani 1 1 d .
F12 F 0.74529(7) 0.37172(12) 0.88559(12) 0.0503(4) Uani 1 1 d .
F13 F 0.69190(7) 0.26892(14) 0.99167(12) 0.0570(5) Uani 1 1 d .
F14 F 0.59513(7) 0.35068(12) 1.02453(10) 0.0418(3) Uani 1 1 d .
F15 F 0.55019(6) 0.53198(11) 0.95242(9) 0.0371(3) Uani 1 1 d .
F16 F 0.64657(6) 0.71202(11) 1.00222(8) 0.0376(3) Uani 1 1 d .
F17 F 0.71302(8) 0.88496(12) 1.03589(10) 0.0477(4) Uani 1 1 d .
F18 F 0.73330(7) 0.99633(12) 0.90366(11) 0.0486(4) Uani 1 1 d .
F19 F 0.68942(8) 0.92706(14) 0.73728(11) 0.0519(4) Uani 1 1 d .
F20 F 0.62534(7) 0.75121(12) 0.70351(9) 0.0417(3) Uani 1 1 d .
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'
F F 0.0171 0.0103 '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'
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
N3 U1 N3 168.47(9) . 2_656
N3 U1 N2 84.24(5) . .
N3 U1 N2 84.24(5) 2_656 .
N3 U1 N1 95.76(5) . .
N3 U1 N1 95.76(5) 2_656 .
N2 U1 N1 180.000(1) . .
N3 U1 F6 96.35(5) . .
N3 U1 F6 78.58(5) 2_656 .
N2 U1 F6 64.21(3) . .
N1 U1 F6 115.79(2) . .
N3 U1 F6 78.58(5) . 2_656
N3 U1 F6 96.35(5) 2_656 2_656
N2 U1 F6 64.21(3) . 2_656
N1 U1 F6 115.79(3) . 2_656
F6 U1 F6 128.42(5) . 2_656
N3 U1 F1 77.32(5) . 2_656
N3 U1 F1 108.02(5) 2_656 2_656
N2 U1 F1 116.57(3) . 2_656
N1 U1 F1 63.43(3) . 2_656
F6 U1 F1 58.56(4) . 2_656
F6 U1 F1 155.61(4) 2_656 2_656
N3 U1 F1 108.02(5) . .
N3 U1 F1 77.32(5) 2_656 .
N2 U1 F1 116.57(3) . .
N1 U1 F1 63.43(3) . .
F6 U1 F1 155.61(4) . .
F6 U1 F1 58.56(4) 2_656 .
F1 U1 F1 126.87(5) 2_656 .
C1 N1 C1 120.1(2) 2_656 .
C1 N1 U1 119.94(12) 2_656 .
C1 N1 U1 119.94(11) . .
C7 N2 C7 121.8(2) . 2_656
C7 N2 U1 119.10(12) . .
C7 N2 U1 119.10(12) 2_656 .
C19 N3 C13 113.71(17) . .
C19 N3 U1 130.62(13) . .
C13 N3 U1 115.66(13) . .
C2 C1 C6 114.43(18) . .
C2 C1 N1 117.53(18) . .
C6 C1 N1 127.61(18) . .
F1 C2 C3 118.45(17) . .
F1 C2 C1 116.67(17) . .
C3 C2 C1 124.75(19) . .
F2 C3 C4 120.97(19) . .
F2 C3 C2 120.31(19) . .
C4 C3 C2 118.69(19) . .
F3 C4 C3 120.36(19) . .
F3 C4 C5 120.3(2) . .
C3 C4 C5 119.25(19) . .
F4 C5 C4 119.21(19) . .
F4 C5 C6 119.90(19) . .
C4 C5 C6 120.8(2) . .
F5 C6 C5 118.41(18) . .
F5 C6 C1 119.51(18) . .
C5 C6 C1 122.02(19) . .
C8 C7 N2 117.36(18) . .
C8 C7 C12 114.72(18) . .
N2 C7 C12 127.36(18) . .
F6 C8 C9 118.36(18) . .
F6 C8 C7 116.57(17) . .
C9 C8 C7 125.0(2) . .
F7 C9 C8 120.7(2) . .
F7 C9 C10 120.88(19) . .
C8 C9 C10 118.38(19) . .
F8 C10 C9 120.3(2) . .
F8 C10 C11 120.2(2) . .
C9 C10 C11 119.51(19) . .
F9 C11 C10 119.56(19) . .
F9 C11 C12 119.7(2) . .
C10 C11 C12 120.7(2) . .
F10 C12 C11 118.60(18) . .
F10 C12 C7 119.60(18) . .
C11 C12 C7 121.73(19) . .
C18 C13 C14 116.2(2) . .
C18 C13 N3 121.76(18) . .
C14 C13 N3 121.98(19) . .
F11 C14 C15 118.95(19) . .
F11 C14 C13 119.08(19) . .
C15 C14 C13 121.9(2) . .
F12 C15 C14 119.9(2) . .
F12 C15 C16 120.0(2) . .
C14 C15 C16 120.0(2) . .
F13 C16 C17 119.7(2) . .
F13 C16 C15 120.9(2) . .
C17 C16 C15 119.5(2) . .
F14 C17 C18 120.4(2) . .
F14 C17 C16 119.8(2) . .
C18 C17 C16 119.7(2) . .
F15 C18 C17 118.21(19) . .
F15 C18 C13 119.14(19) . .
C17 C18 C13 122.6(2) . .
C20 C19 C24 115.7(2) . .
C20 C19 N3 121.71(19) . .
C24 C19 N3 122.54(19) . .
F16 C20 C21 118.4(2) . .
F16 C20 C19 118.79(19) . .
C21 C20 C19 122.8(2) . .
F17 C21 C20 120.1(2) . .
F17 C21 C22 120.0(2) . .
C20 C21 C22 119.9(2) . .
F18 C22 C21 120.2(2) . .
F18 C22 C23 120.5(2) . .
C21 C22 C23 119.3(2) . .
F19 C23 C22 119.9(2) . .
F19 C23 C24 120.1(2) . .
C22 C23 C24 119.9(2) . .
F20 C24 C23 118.6(2) . .
F20 C24 C19 119.0(2) . .
C23 C24 C19 122.4(2) . .
C2 F1 U1 112.51(10) . .
C8 F6 U1 112.26(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 N3 2.2781(17) .
U1 N3 2.2781(17) 2_656
U1 N2 2.370(2) .
U1 N1 2.387(2) .
U1 F6 2.5985(11) .
U1 F6 2.5985(11) 2_656
U1 F1 2.6480(11) 2_656
U1 F1 2.6480(11) .
N1 C1 1.401(2) 2_656
N1 C1 1.401(2) .
N2 C7 1.396(2) .
N2 C7 1.396(2) 2_656
N3 C19 1.421(3) .
N3 C13 1.426(3) .
C1 C2 1.393(3) .
C1 C6 1.396(3) .
C2 F1 1.372(2) .
C2 C3 1.376(3) .
C3 F2 1.335(2) .
C3 C4 1.375(3) .
C4 F3 1.339(2) .
C4 C5 1.377(3) .
C5 F4 1.335(2) .
C5 C6 1.385(3) .
C6 F5 1.341(2) .
C7 C8 1.392(3) .
C7 C12 1.398(3) .
C8 F6 1.372(2) .
C8 C9 1.374(3) .
C9 F7 1.333(2) .
C9 C10 1.379(3) .
C10 F8 1.339(2) .
C10 C11 1.380(3) .
C11 F9 1.334(3) .
C11 C12 1.388(3) .
C12 F10 1.337(2) .
C13 C18 1.387(3) .
C13 C14 1.398(3) .
C14 F11 1.340(2) .
C14 C15 1.372(3) .
C15 F12 1.337(3) .
C15 C16 1.385(3) .
C16 F13 1.330(3) .
C16 C17 1.374(3) .
C17 F14 1.337(3) .
C17 C18 1.373(3) .
C18 F15 1.345(2) .
C19 C20 1.391(3) .
C19 C24 1.391(3) .
C20 F16 1.349(3) .
C20 C21 1.374(3) .
C21 F17 1.342(3) .
C21 C22 1.376(4) .
C22 F18 1.339(3) .
C22 C23 1.378(4) .
C23 F19 1.333(3) .
C23 C24 1.381(3) .
C24 F20 1.339(3) .
