Dinuclear uranium complexation and manipulation using robust tetraaryloxides.
Wells, Jordann A. L.; Seymour, Megan L.; Suvova, Markéta; Arnold, Polly L.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 16026–16032; doi:10.1039/c6dt02630c

data_7040507
_publ_section_title
;
 Dinuclear uranium complexation and manipulation using robust
 tetraaryloxides.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16026
_journal_page_last               16032
_journal_paper_doi               10.1039/c6dt02630c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C60 H67 I2 O4 U, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H83 I2 O6 U'
_chemical_formula_weight         1488.17
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-09 deposited with the CCDC.
2016-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.4479(17)
_cell_angle_beta                 92.5407(16)
_cell_angle_gamma                118.010(2)
_cell_formula_units_Z            2
_cell_length_a                   14.4316(3)
_cell_length_b                   15.1187(3)
_cell_length_c                   16.3119(3)
_cell_measurement_reflns_used    19342
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.1100
_cell_measurement_theta_min      3.5550
_cell_volume                     3137.41(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -25.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000  -30.0000 48

  2 omega  -22.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   19.0000   30.0000 117

  3 omega  -25.00   64.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -99.0000   90.0000 89

  4 omega  -47.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  -57.0000 -150.0000 90

  5 omega   34.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  179.0000 -120.0000 64

  6 omega  -88.00    2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -57.0000   60.0000 90

  7 omega  -25.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.2955  -99.0000   30.0000 48

  8 omega   34.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518  179.0000   60.0000 64

  9 omega    1.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   57.0000 -120.0000 90

 10 omega   17.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518 -157.0000  -29.0000 80

 11 omega   -4.00   94.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9518   38.0000 -180.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0154670000
_diffrn_orient_matrix_UB_12      0.0028351000
_diffrn_orient_matrix_UB_13      0.0422304000
_diffrn_orient_matrix_UB_21      0.0530251000
_diffrn_orient_matrix_UB_22      0.0315730000
_diffrn_orient_matrix_UB_23      -0.0090238000
_diffrn_orient_matrix_UB_31      -0.0075789000
_diffrn_orient_matrix_UB_32      0.0426841000
_diffrn_orient_matrix_UB_33      0.0056310000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            57292
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.901
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.620
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.525
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent intense green'
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             1474
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3262
_exptl_crystal_size_mid          0.173
_exptl_crystal_size_min          0.0853
_refine_diff_density_max         3.548
_refine_diff_density_min         -1.868
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         14372
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0602P)^2^+14.1643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1199
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12061
_reflns_number_total             14372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02630c2.cif
_cod_data_source_block           p15180_tri
_cod_depositor_comments
'Adding full bibliography for 7040504--7040510.cif.'
_cod_database_code               7040507
_chemical_oxdiff_formula         'C120 H120 O4 U2 I2'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O2S) = Uanis(C8S) = Uanis(C7S) = Uanis(C6S) = Uanis(C5S)
Uanis(C15S) = Uanis(C16S) = Uanis(O4S) = Uanis(C13S) = Uanis(C14S)
Uanis(C12S) = Uanis(C11S) = Uanis(C10S) = Uanis(C9S) = Uanis(O3S)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Secondary CH2 refined with riding coordinates:
 C8S(H8SA,H8SB), C7S(H7SA,H7SB), C6S(H6SA,H6SB), C5S(H5SA,H5SB), C4S(H4SA,
 H4SB), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C12S(H12G,H12H),
 C11S(H11A,H11B), C10S(H10A,H10B), C9S(H9SA,H9SB), C15S(H15A,H15B), C16S(H16A,
 H16B), C13S(H13A,H13B), C14S(H14G,H14H)
3.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C23(H23), C25(H25), C13(H13), C3(H3), C144(H144), C4(H4),
 C226(H226), C145(H145), C143(H143), C146(H146), C142(H142), C242(H242),
 C222(H222), C225(H225), C224(H224), C246(H246), C245(H245), C122(H122),
 C243(H243), C126(H126), C244(H244), C223(H223), C125(H125), C124(H124),
 C123(H123)
3.d Fitted pentagon refined as free rotating group:
 O2S(C8S,C7S,C6S,C5S), C12S(C11S,C10S,C9S,O3S), C15S(C16S,O4S,C13S,C14S)
3.e Idealised Me refined as rotating group:
 C127(H12A,H12B,H12C), C248(H24A,H24B,H24C), C228(H22A,H22B,H22C), C227(H22D,
 H22E,H22F), C128(H12D,H12E,H12F), C147(H14A,H14B,H14C), C148(H14D,H14E,H14F),
 C247(H24D,H24E,H24F)
;
_shelx_res_checksum              8100
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method THF