#------------------------------------------------------------------------------
#$Date: 2015-12-06 08:31:10 +0200 (Sun, 06 Dec 2015) $
#$Revision: 170792 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/44/4344439.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_4344439
loop_
_publ_author_name
'Thuéry, Pierre'
'Harrowfield, Jack'
_publ_section_title
;
 A New Form of Triple-Stranded Helicate Found in Uranyl Complexes of
 Aliphatic α,ω-Dicarboxylates.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10539
_journal_page_last               10541
_journal_paper_doi               10.1021/acs.inorgchem.5b02348
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C72 H84 Co N6 O16 U2'
_chemical_formula_weight         1824.44
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.4057(3)
_cell_length_b                   13.4057(3)
_cell_length_c                   22.2777(9)
_cell_measurement_reflns_used    81658
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.26
_cell_volume                     3467.21(18)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and three ω scans with 2° steps (318 frames)'
_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  0.0289
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            81658
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         3.257
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.968
_exptl_absorpt_correction_T_max  0.672
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1794
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.878
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2211
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0515P)²+19.5945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1866
_reflns_number_total             2211
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02348_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4344436--4344441.cif.'
_cod_original_cell_volume        3467.2(2)
_cod_database_code               4344439
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'x, x-y, -z+1/2'
'-x+y, y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'-x, -x+y, z-1/2'
'x-y, -y, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
U1 U 0.6667 0.3333 0.03853(2) 0.03165(16) Uani 1 3 d S T P
Co1 Co 0.3333 0.6667 0.2500 0.0321(4) Uani 1 6 d S T P
O1 O 0.6667 0.3333 0.1182(4) 0.0434(19) Uani 1 3 d S T P
O2 O 0.6667 0.3333 -0.0416(3) 0.0391(18) Uani 1 3 d S T P
O3 O 0.4531(4) 0.2097(4) 0.0398(2) 0.0429(11) Uani 1 1 d D U .
O4 O 0.5519(3) 0.1245(4) 0.0415(2) 0.0431(11) Uani 1 1 d D U .
N1 N 0.3524(5) 0.5431(5) 0.1987(2) 0.0362(12) Uani 1 1 d . . .
C1 C 0.4572(4) 0.1200(4) 0.0440(3) 0.0398(13) Uani 1 1 d D U .
C2A C 0.3482(7) 0.0021(6) 0.0436(7) 0.042(3) Uani 0.5 1 d D U P
H2A H 0.3583 -0.0549 0.0640 0.050 Uiso 0.5 1 d R U P
H2B H 0.3326 -0.0192 0.0023 0.050 Uiso 0.5 1 d R U P
C3A C 0.2460(7) 0.0119(14) 0.0646(5) 0.063(3) Uani 0.5 1 d D U P
H3A H 0.1761 -0.0367 0.0437 0.075 Uiso 0.5 1 d R U P
H3B H 0.2606 0.0891 0.0630 0.075 Uiso 0.5 1 d R U P
C4A C 0.2681(11) 0.0501(16) 0.1301(5) 0.092(4) Uani 0.5 1 d D U P
H4A H 0.3221 0.1290 0.1380 0.110 Uiso 0.5 1 d R U P
H4B H 0.2988 0.0043 0.1449 0.110 Uiso 0.5 1 d R U P
C5A C 0.1569(11) -0.0137(15) 0.1645(4) 0.101(4) Uani 0.5 1 d D U P
H5A H 0.1004 -0.0896 0.1526 0.122 Uiso 0.5 1 d R U P
H5B H 0.1306 0.0377 0.1529 0.122 Uiso 0.5 1 d R U P
C6A C 0.1806(15) -0.0035(7) 0.2311(4) 0.078(3) Uani 0.5 1 d D U P
H6A H 0.2245 -0.0411 0.2359 0.093 Uiso 0.5 1 d R U P
H6B H 0.1079 -0.0486 0.2502 0.093 Uiso 0.5 1 d R U P
C2B C 0.3507(8) 0.3450(11) 0.4409(5) 0.046(3) Uani 0.5 1 d D U P
H2C H 0.3213 0.3573 0.4775 0.055 Uiso 0.5 1 d R U P
H2D H 0.3695 0.4082 0.4147 0.055 Uiso 0.5 1 d R U P
C3B C 0.2612(8) 0.2385(12) 0.4087(4) 0.054(3) Uani 0.5 1 d D U P
H3C H 0.1859 0.2282 0.4135 0.065 Uiso 0.5 1 d R U P
H3D H 0.2627 0.1748 0.4267 0.065 Uiso 0.5 1 d R U P
C4B C 0.2854(15) 0.2450(10) 0.3417(4) 0.063(3) Uani 0.5 1 d D U P
H4C H 0.3667 0.2792 0.3368 0.076 Uiso 0.5 1 d R U P
H4D H 0.2607 0.2911 0.3210 0.076 Uiso 0.5 1 d R U P
C5B C 0.2127(13) 0.1252(10) 0.3156(3) 0.060(3) Uani 0.5 1 d D U P
H5C H 0.1313 0.0920 0.3189 0.072 Uiso 0.5 1 d R U P
H5D H 0.2351 0.0782 0.3372 0.072 Uiso 0.5 1 d R U P
C6B C 0.2447(10) 0.1223(5) 0.2500 0.062(2) Uani 1 2 d DS TU P
H6C H 0.2253 0.1704 0.2330 0.074 Uiso 0.5 1 d R U P
H6D H 0.3258 0.1512 0.2511 0.074 Uiso 0.5 1 d R U P
C7 C 0.3010(7) 0.4926(6) 0.1471(3) 0.0446(17) Uani 1 1 d . . .
H7 H 0.2470 0.5108 0.1303 0.053 Uiso 1 1 calc R U .
C8 C 0.3231(7) 0.4146(7) 0.1169(3) 0.0511(19) Uani 1 1 d . . .
H8 H 0.2852 0.3813 0.0801 0.061 Uiso 1 1 calc R U .
C9 C 0.3993(7) 0.3866(6) 0.1407(3) 0.0504(19) Uani 1 1 d . . .
H9 H 0.4151 0.3336 0.1205 0.060 Uiso 1 1 calc R U .
C10 C 0.4547(6) 0.4364(6) 0.1953(3) 0.0442(17) Uani 1 1 d . . .
C11 C 0.4291(6) 0.5154(6) 0.2227(3) 0.0358(14) Uani 1 1 d . . .
C12 C 0.5362(7) 0.4115(7) 0.2232(4) 0.055(2) Uani 1 1 d . . .
H12 H 0.5544 0.3586 0.2048 0.066 Uiso 1 1 calc R U .
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'
Co Co 0.3494 0.9721 '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
O1 U1 O2 180.0 . .
O1 U1 O4 88.46(11) . 2_655
O2 U1 O4 91.54(11) . 2_655
O1 U1 O4 88.46(11) . .
O2 U1 O4 91.54(11) . .
O4 U1 O4 119.928(11) 2_655 .
O1 U1 O4 88.46(11) . 3_665
O2 U1 O4 91.54(11) . 3_665
O4 U1 O4 119.928(11) 2_655 3_665
O4 U1 O4 119.929(11) . 3_665
O1 U1 O3 89.36(11) . 2_655
O2 U1 O3 90.64(11) . 2_655
O4 U1 O3 51.51(12) 2_655 2_655
O4 U1 O3 68.48(12) . 2_655
O4 U1 O3 171.23(12) 3_665 2_655
O1 U1 O3 89.36(11) . .
O2 U1 O3 90.64(11) . .
O4 U1 O3 171.23(12) 2_655 .
O4 U1 O3 51.51(12) . .
O4 U1 O3 68.48(12) 3_665 .
O3 U1 O3 119.988(4) 2_655 .
O1 U1 O3 89.36(11) . 3_665
O2 U1 O3 90.64(11) . 3_665
O4 U1 O3 68.48(12) 2_655 3_665
O4 U1 O3 171.23(12) . 3_665
O4 U1 O3 51.51(12) 3_665 3_665
O3 U1 O3 119.988(5) 2_655 3_665
O3 U1 O3 119.987(5) . 3_665
N1 Co1 N1 95.3(3) 5_565 3_565
N1 Co1 N1 93.9(2) 5_565 6
N1 Co1 N1 78.0(3) 3_565 6
N1 Co1 N1 78.0(3) 5_565 2_665
N1 Co1 N1 93.9(2) 3_565 2_665
N1 Co1 N1 168.1(3) 6 2_665
N1 Co1 N1 93.9(2) 5_565 4_665
N1 Co1 N1 168.1(3) 3_565 4_665
N1 Co1 N1 93.9(2) 6 4_665
N1 Co1 N1 95.3(3) 2_665 4_665
N1 Co1 N1 168.1(3) 5_565 .
N1 Co1 N1 93.9(2) 3_565 .
N1 Co1 N1 95.3(3) 6 .
N1 Co1 N1 93.9(2) 2_665 .
N1 Co1 N1 78.0(3) 4_665 .
C1 O3 U1 93.0(3) . .
C1 O4 U1 95.8(3) . .
C7 N1 C11 117.8(6) . .
C7 N1 Co1 128.6(5) . .
C11 N1 Co1 113.6(4) . .
O3 C1 O4 119.4(5) . .
O3 C1 C2A 121.5(5) . .
O4 C1 C2A 118.5(5) . .
O3 C1 U1 61.2(3) . .
O4 C1 U1 58.4(3) . .
C2A C1 U1 175.9(5) . .
C3A C2A C1 110.4(6) . .
C3A C2A H2A 114.7 . .
C1 C2A H2A 112.4 . .
C3A C2A H2B 104.6 . .
C1 C2A H2B 105.6 . .
H2A C2A H2B 108.5 . .
C2A C3A C4A 107.1(7) . .
C2A C3A H3A 114.4 . .
C4A C3A H3A 131.0 . .
C2A C3A H3B 112.3 . .
C4A C3A H3B 76.8 . .
H3A C3A H3B 108.7 . .
C5A C4A C3A 109.0(7) . .
C5A C4A H4A 121.5 . .
C3A C4A H4A 117.6 . .
C5A C4A H4B 94.7 . .
C3A C4A H4B 100.9 . .
H4A C4A H4B 108.4 . .
C4A C5A C6A 110.2(7) . .
C4A C5A H5A 119.8 . .
C6A C5A H5A 112.9 . .
C4A C5A H5B 94.1 . .
C6A C5A H5B 109.7 . .
H5A C5A H5B 108.3 . .
C5A C6A C6B 110.5(7) . .
C5A C6A H6A 102.8 . .
C6B C6A H6A 113.6 . .
C5A C6A H6B 106.3 . .
C6B C6A H6B 114.3 . .
H6A C6A H6B 108.6 . .
C3B C2B H2C 111.5 . .
C3B C2B H2D 106.3 . .
H2C C2B H2D 108.5 . .
C2B C3B C4B 111.5(7) . .
C2B C3B H3C 111.5 . .
C4B C3B H3C 107.5 . .
C2B C3B H3D 106.4 . .
C4B C3B H3D 111.4 . .
H3C C3B H3D 108.6 . .
C5B C4B C3B 108.1(6) . .
C5B C4B H4C 116.2 . .
C3B C4B H4C 107.4 . .
C5B C4B H4D 104.7 . .
C3B C4B H4D 112.1 . .
C4B C5B C6B 110.7(6) . .
C4B C5B H5C 116.4 . .
C6B C5B H5C 109.4 . .
C4B C5B H5D 104.9 . .
C6B C5B H5D 106.4 . .
H5C C5B H5D 108.6 . .
C6A C6B C5B 106.4(5) . .
C5B C6B H6C 101.6 . .
C6A C6B H6D 110.7 . .
C5B C6B H6D 104.0 . .
H6C C6B H6D 113.8 . .
N1 C7 C8 123.1(7) . .
N1 C7 H7 118.4 . .
C8 C7 H7 118.4 . .
C9 C8 C7 119.3(7) . .
C9 C8 H8 120.4 . .
C7 C8 H8 120.4 . .
C8 C9 C10 119.8(7) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C11 C10 C9 117.6(7) . .
C11 C10 C12 119.2(7) . .
C9 C10 C12 123.2(7) . .
N1 C11 C10 122.3(6) . .
N1 C11 C11 117.4(4) . 4_665
C10 C11 C11 120.3(4) . 4_665
C12 C12 C10 120.6(4) 4_665 .
C12 C12 H12 119.7 4_665 .
C10 C12 H12 119.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.775(8) .
U1 O2 1.785(7) .
U1 O4 2.429(5) 2_655
U1 O4 2.429(5) .
U1 O4 2.429(5) 3_665
U1 O3 2.490(5) 2_655
U1 O3 2.490(5) .
U1 O3 2.490(5) 3_665
Co1 N1 2.130(5) 5_565
Co1 N1 2.130(5) 3_565
Co1 N1 2.130(6) 6
Co1 N1 2.130(6) 2_665
Co1 N1 2.130(5) 4_665
Co1 N1 2.130(5) .
O3 C1 1.235(3) .
O4 C1 1.241(3) .
N1 C7 1.336(9) .
N1 C11 1.366(9) .
C1 C2B 1.520(5) 5
C1 C2A 1.525(4) .
C2A C3A 1.514(5) .
C2A H2A 0.9536 .
C2A H2B 0.9548 .
C3A C4A 1.524(5) .
C3A H3A 0.9537 .
C3A H3B 0.9533 .
C4A C5A 1.505(5) .
C4A H4A 0.9533 .
C4A H4B 0.9533 .
C5A C6A 1.509(5) .
C5A H5A 0.9535 .
C5A H5B 0.9532 .
C6A C6B 1.521(5) .
C6A H6A 0.9534 .
C6A H6B 0.9534 .
C2B C3B 1.511(5) .
C2B H2C 0.9544 .
C2B H2D 0.9539 .
C3B C4B 1.520(5) .
C3B H3C 0.9535 .
C3B H3D 0.9532 .
C4B C5B 1.518(5) .
C4B H4C 0.9533 .
C4B H4D 0.9536 .
C5B C6B 1.528(5) .
C5B H5C 0.9533 .
C5B H5D 0.9536 .
C6B H6C 0.8914 .
C6B H6D 0.9549 .
C7 C8 1.394(10) .
C7 H7 0.9500 .
C8 C9 1.360(12) .
C8 H8 0.9500 .
C9 C10 1.407(11) .
C9 H9 0.9500 .
C10 C11 1.406(9) .
C10 C12 1.434(11) .
C11 C11 1.424(13) 4_665
C12 C12 1.383(18) 4_665
C12 H12 0.9500 .
