#------------------------------------------------------------------------------
#$Date: 2015-12-06 08:31:10 +0200 (Sun, 06 Dec 2015) $
#$Revision: 170792 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/44/4344438.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_4344438
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 Mn N6 O16 U2'
_chemical_formula_weight         1820.45
_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                   13.4661(3)
_cell_length_b                   13.4661(3)
_cell_length_c                   22.3796(8)
_cell_measurement_reflns_used    90133
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      3.24
_cell_volume                     3514.52(17)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method
'two φ and three ω scans with 2° steps (340 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  0.0368
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            90133
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.674
_diffrn_reflns_theta_min         3.242
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.845
_exptl_absorpt_correction_T_max  0.616
_exptl_absorpt_correction_T_min  0.498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1790
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.661
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2240
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0470P)²+16.2993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1893
_reflns_number_total             2240
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b02348_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4344436--4344441.cif.'
_cod_original_cell_volume        3514.5(2)
_cod_database_code               4344438
_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 0.03752(2) 0.03510(15) Uani 1 3 d S T P
Mn1 Mn 0.3333 0.6667 0.2500 0.0361(5) Uani 1 6 d S T P
O1 O 0.6667 0.3333 0.1171(3) 0.0466(18) Uani 1 3 d S T P
O2 O 0.6667 0.3333 -0.0422(3) 0.0421(17) Uani 1 3 d S T P
O3 O 0.4541(4) 0.2089(3) 0.0398(2) 0.0476(10) Uani 1 1 d D U .
O4 O 0.5535(3) 0.1256(4) 0.04031(19) 0.0473(10) Uani 1 1 d D U .
N1 N 0.3599(4) 0.5405(4) 0.1972(2) 0.0406(11) Uani 1 1 d . . .
C1 C 0.4588(3) 0.1199(4) 0.0437(3) 0.0439(12) Uani 1 1 d D U .
C2A C 0.3516(7) 0.0017(6) 0.0444(7) 0.048(3) Uani 0.5 1 d D U P
H2A H 0.3617 -0.0553 0.0648 0.057 Uiso 0.5 1 d R U P
H2B H 0.3361 -0.0196 0.0031 0.057 Uiso 0.5 1 d R U P
C3A C 0.2499(7) 0.0090(14) 0.0674(5) 0.071(3) Uani 0.5 1 d D U P
H3A H 0.1799 -0.0396 0.0465 0.085 Uiso 0.5 1 d R U P
H3B H 0.2644 0.0862 0.0658 0.085 Uiso 0.5 1 d R U P
C4A C 0.2724(10) 0.0428(17) 0.1332(5) 0.101(4) Uani 0.5 1 d D U P
H4A H 0.3265 0.1217 0.1412 0.121 Uiso 0.5 1 d R U P
H4B H 0.3032 -0.0030 0.1480 0.121 Uiso 0.5 1 d R U P
C5A C 0.1589(10) -0.0129(15) 0.1654(5) 0.112(4) Uani 0.5 1 d D U P
H5A H 0.1024 -0.0888 0.1535 0.134 Uiso 0.5 1 d R U P
H5B H 0.1326 0.0386 0.1539 0.134 Uiso 0.5 1 d R U P
C6A C 0.1793(15) -0.0027(7) 0.2321(4) 0.093(3) Uani 0.5 1 d D U P
H6A H 0.2232 -0.0404 0.2369 0.112 Uiso 0.5 1 d R U P
H6B H 0.1066 -0.0479 0.2512 0.112 Uiso 0.5 1 d R U P
C2B C 0.3533(8) 0.3469(11) 0.4406(5) 0.050(3) Uani 0.5 1 d D U P
H2C H 0.3239 0.3592 0.4772 0.060 Uiso 0.5 1 d R U P
H2D H 0.3721 0.4102 0.4144 0.060 Uiso 0.5 1 d R U P
C3B C 0.2641(8) 0.2416(12) 0.4081(4) 0.064(3) Uani 0.5 1 d D U P
H3C H 0.1889 0.2313 0.4129 0.077 Uiso 0.5 1 d R U P
H3D H 0.2657 0.1779 0.4261 0.077 Uiso 0.5 1 d R U P
C4B C 0.2930(14) 0.2452(11) 0.3421(4) 0.074(3) Uani 0.5 1 d D U P
H4C H 0.3742 0.2794 0.3372 0.089 Uiso 0.5 1 d R U P
H4D H 0.2682 0.2913 0.3214 0.089 Uiso 0.5 1 d R U P
C5B C 0.2160(13) 0.1273(10) 0.3156(3) 0.075(3) Uani 0.5 1 d D U P
H5C H 0.1346 0.0942 0.3189 0.089 Uiso 0.5 1 d R U P
H5D H 0.2384 0.0803 0.3373 0.089 Uiso 0.5 1 d R U P
C6B C 0.2462(10) 0.1231(5) 0.2500 0.080(2) Uani 1 2 d DS TU P
H6C H 0.2268 0.1704 0.2330 0.097 Uiso 0.5 1 d R U P
H6D H 0.3273 0.1512 0.2511 0.097 Uiso 0.5 1 d R U P
C7 C 0.3092(6) 0.4904(6) 0.1458(3) 0.0507(16) Uani 1 1 d . . .
H7 H 0.2567 0.5094 0.1283 0.061 Uiso 1 1 calc R U .
C8 C 0.3306(7) 0.4112(6) 0.1171(3) 0.0601(19) Uani 1 1 d . . .
H8 H 0.2933 0.3777 0.0804 0.072 Uiso 1 1 calc R U .
C9 C 0.4044(7) 0.3823(6) 0.1413(3) 0.0595(19) Uani 1 1 d . . .
H9 H 0.4189 0.3281 0.1218 0.071 Uiso 1 1 calc R U .
C10 C 0.4596(6) 0.4325(6) 0.1953(3) 0.0515(17) Uani 1 1 d . . .
C11 C 0.4345(5) 0.5118(5) 0.2223(3) 0.0427(14) Uani 1 1 d . . .
C12 C 0.5395(7) 0.4077(6) 0.2236(4) 0.065(2) Uani 1 1 d . . .
H12 H 0.5566 0.3540 0.2058 0.078 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'
Mn Mn 0.3368 0.7283 '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 88.52(10) . .
O2 U1 O4 91.48(10) . .
O1 U1 O4 88.52(10) . 2_655
O2 U1 O4 91.48(10) . 2_655
O4 U1 O4 119.933(9) . 2_655
O1 U1 O4 88.52(10) . 3_665
O2 U1 O4 91.48(10) . 3_665
O4 U1 O4 119.934(9) . 3_665
O4 U1 O4 119.935(9) 2_655 3_665
O1 U1 O3 88.84(10) . 2_655
O2 U1 O3 91.16(10) . 2_655
O4 U1 O3 68.56(11) . 2_655
O4 U1 O3 51.41(11) 2_655 2_655
O4 U1 O3 171.03(12) 3_665 2_655
O1 U1 O3 88.84(10) . 3_665
O2 U1 O3 91.16(10) . 3_665
O4 U1 O3 171.03(12) . 3_665
O4 U1 O3 68.56(11) 2_655 3_665
O4 U1 O3 51.41(11) 3_665 3_665
O3 U1 O3 119.958(8) 2_655 3_665
O1 U1 O3 88.84(10) . .
O2 U1 O3 91.16(10) . .
O4 U1 O3 51.41(11) . .
O4 U1 O3 171.03(12) 2_655 .
O4 U1 O3 68.56(11) 3_665 .
O3 U1 O3 119.959(7) 2_655 .
O3 U1 O3 119.960(7) 3_665 .
N1 Mn1 N1 97.9(3) 5_565 3_565
N1 Mn1 N1 94.76(17) 5_565 6
N1 Mn1 N1 74.6(3) 3_565 6
N1 Mn1 N1 74.6(3) 5_565 2_665
N1 Mn1 N1 94.76(17) 3_565 2_665
N1 Mn1 N1 164.1(3) 6 2_665
N1 Mn1 N1 164.1(3) 5_565 .
N1 Mn1 N1 94.76(17) 3_565 .
N1 Mn1 N1 97.9(3) 6 .
N1 Mn1 N1 94.76(17) 2_665 .
N1 Mn1 N1 94.76(17) 5_565 4_665
N1 Mn1 N1 164.1(3) 3_565 4_665
N1 Mn1 N1 94.76(17) 6 4_665
N1 Mn1 N1 97.9(3) 2_665 4_665
N1 Mn1 N1 74.6(3) . 4_665
C1 O3 U1 93.1(3) . .
C1 O4 U1 96.1(3) . .
C7 N1 C11 118.3(6) . .
C7 N1 Mn1 127.0(5) . .
C11 N1 Mn1 114.6(4) . .
O3 C1 O4 119.1(4) . .
O3 C1 C2B 121.1(6) . 5
O4 C1 C2B 119.4(6) . 5
O3 C1 C2A 122.2(5) . .
O4 C1 C2A 118.2(5) . .
C3A C2A C1 110.5(6) . .
C3A C2A H2A 112.7 . .
C1 C2A H2A 113.7 . .
C3B C2A H2A 102.7 5 .
C3A C2A H2B 106.1 . .
C1 C2A H2B 104.6 . .
H2A C2A H2B 108.5 . .
C2A C3A C4A 107.2(7) . .
C2A C3A H3A 113.8 . .
C4A C3A H3A 131.0 . .
C2A C3A H3B 111.0 . .
C4A C3A H3B 79.1 . .
H3A C3A H3B 108.7 . .
C5A C4A C3A 108.2(7) . .
C5A C4A H4A 118.8 . .
C3A C4A H4A 116.0 . .
C5A C4A H4B 99.9 . .
C3A C4A H4B 103.2 . .
H4A C4A H4B 108.4 . .
C4A C5A C6A 109.5(7) . .
C4A C5A H5A 117.7 . .
C6A C5A H5A 112.5 . .
C4A C5A H5B 99.3 . .
C6A C5A H5B 108.5 . .
H5A C5A H5B 108.3 . .
C5A C6A C6B 109.9(7) . .
C5A C6A H6A 101.4 . .
C6B C6A H6A 112.4 . .
C5A C6A H6B 107.6 . .
C6B C6A H6B 115.9 . .
H6A C6A H6B 108.6 . .
C3B C2B H2C 111.7 . .
C3B C2B H2D 105.7 . .
H2C C2B H2D 108.5 . .
C2B C3B C4B 111.6(6) . .
C2B C3B H3C 111.6 . .
C4B C3B H3C 110.4 . .
C2B C3B H3D 105.9 . .
C4B C3B H3D 108.5 . .
H3C C3B H3D 108.6 . .
C5B C4B C3B 108.4(6) . .
C5B C4B H4C 118.6 . .
C3B C4B H4C 109.7 . .
C5B C4B H4D 102.2 . .
C3B C4B H4D 108.8 . .
C4B C5B C6B 111.0(6) . .
C4B C5B H5C 118.8 . .
C6B C5B H5C 108.7 . .
C4B C5B H5D 102.5 . .
C6B C5B H5D 106.5 . .
H5C C5B H5D 108.6 . .
C6A C6B C5B 105.9(5) . .
C6A C6B H6C 117.6 . .
C5B C6B H6C 101.8 . .
C6A C6B H6D 111.6 . .
C5B C6B H6D 103.4 . .
H6C C6B H6D 114.4 . .
N1 C7 C8 122.4(7) . .
N1 C7 H7 118.8 . .
C8 C7 H7 118.8 . .
C9 C8 C7 120.0(7) . .
C9 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C8 C9 C10 119.7(6) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C9 C10 C11 117.7(6) . .
C9 C10 C12 123.4(6) . .
C11 C10 C12 118.9(7) . .
N1 C11 C10 121.9(6) . .
N1 C11 C11 118.0(3) . 4_665
C10 C11 C11 120.1(4) . 4_665
C12 C12 C10 121.0(4) 4_665 .
C12 C12 H12 119.5 4_665 .
C10 C12 H12 119.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O1 1.781(7) .
U1 O2 1.784(7) .
U1 O4 2.427(4) .
U1 O4 2.427(4) 2_655
U1 O4 2.427(4) 3_665
U1 O3 2.492(4) 2_655
U1 O3 2.492(4) 3_665
U1 O3 2.492(4) .
Mn1 N1 2.241(5) 5_565
Mn1 N1 2.241(5) 3_565
Mn1 N1 2.241(5) 6
Mn1 N1 2.241(5) 2_665
Mn1 N1 2.241(5) .
Mn1 N1 2.241(5) 4_665
O3 C1 1.235(3) .
O4 C1 1.241(3) .
N1 C7 1.335(8) .
N1 C11 1.364(8) .
C1 C2B 1.519(5) 5
C1 C2A 1.524(4) .
C2A C3A 1.513(5) .
C2A H2A 0.9579 .
C2A H2B 0.9591 .
C3A C4A 1.526(5) .
C3A H3A 0.9580 .
C3A H3B 0.9575 .
C4A C5A 1.508(5) .
C4A H4A 0.9576 .
C4A H4B 0.9576 .
C5A C6A 1.510(5) .
C5A H5A 0.9578 .
C5A H5B 0.9575 .
C6A C6B 1.523(5) .
C6A H6A 0.9576 .
C6A H6B 0.9578 .
C2B C3B 1.511(5) .
C2B H2C 0.9587 .
C2B H2D 0.9582 .
C3B C4B 1.521(5) .
C3B H3C 0.9578 .
C3B H3D 0.9575 .
C4B C5B 1.517(5) .
C4B H4C 0.9576 .
C4B H4D 0.9579 .
C5B C6B 1.532(5) .
C5B H5C 0.9575 .
C5B H5D 0.9578 .
C6B H6C 0.8865 .
C6B H6D 0.9609 .
C7 C8 1.393(10) .
C7 H7 0.9500 .
C8 C9 1.348(11) .
C8 H8 0.9500 .
C9 C10 1.404(11) .
C9 H9 0.9500 .
C10 C11 1.407(9) .
C10 C12 1.424(10) .
C11 C11 1.436(13) 4_665
C12 C12 1.379(17) 4_665
C12 H12 0.9500 .
