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_7040506
_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         'C32 H43 I2 O5 U, 5.5(C6 H6)'
_chemical_formula_sum            'C65 H76 I2 O5 U'
_chemical_formula_weight         1429.08
_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
_audit_creation_date             2016-05-09
_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                69.881(2)
_cell_angle_beta                 89.136(2)
_cell_angle_gamma                76.2616(19)
_cell_formula_units_Z            2
_cell_length_a                   13.8429(3)
_cell_length_b                   15.6696(4)
_cell_length_c                   15.8357(5)
_cell_measurement_reflns_used    8889
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      23.7090
_cell_measurement_theta_min      3.4090
_cell_volume                     3124.72(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (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  -41.00   52.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.6840   38.0000    0.0000 93

  2 omega  -25.00   22.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.6840  -99.0000  120.0000 47

  3 omega  -25.00   22.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.6840  -99.0000    0.0000 47

  4 omega   34.00   94.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  179.0000  150.0000 60

  5 omega  -17.00   29.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   95.0000 -112.0000 46

  6 omega  -49.00   49.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -77.0000 -120.0000 98

  7 omega  -48.00   39.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -57.0000   90.0000 87

  8 omega  -52.00   58.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -19.0000  150.0000 110

  9 omega  -87.00    0.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.6840  -57.0000  -60.0000 87

 10 omega    2.00   89.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   57.0000  120.0000 87

 11 omega  -25.00    0.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -99.0000   30.0000 25

 12 omega    2.00   89.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   57.0000 -120.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0047104000
_diffrn_orient_matrix_UB_12      -0.0029623000
_diffrn_orient_matrix_UB_13      -0.0436333000
_diffrn_orient_matrix_UB_21      -0.0522676000
_diffrn_orient_matrix_UB_22      0.0180111000
_diffrn_orient_matrix_UB_23      -0.0096133000
_diffrn_orient_matrix_UB_31      0.0065733000
_diffrn_orient_matrix_UB_32      0.0462856000
_diffrn_orient_matrix_UB_33      -0.0170700000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            58171
_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         27.485
_diffrn_reflns_theta_min         2.946
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.630
_exptl_absorpt_correction_T_max  0.997
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.5117
_exptl_crystal_size_mid          0.3182
_exptl_crystal_size_min          0.1289
_refine_diff_density_max         1.708
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.149
_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     528
_refine_ls_number_reflns         14313
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0669
_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/[\s^2^(Fo^2^)+(0.0561P)^2^+11.5426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10213
_reflns_number_total             14313
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02630c2.cif
_cod_data_source_block           p16021d
_cod_depositor_comments
'Adding full bibliography for 7040504--7040510.cif.'
_cod_original_cell_volume        3124.73(14)
_cod_database_code               7040506
_chemical_oxdiff_formula         'C70 H70 O4 U2 I4'
_reflns_odcompleteness_completeness 99.86
_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. Restrained distances
 C36S-C35S \\sim C37S-C38S
 with sigma of 0.02
 C35S-C34S \\sim C39S-C38S
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C24S) = Uanis(C17S)
Uanis(C23S) = Uanis(C16S)
Uanis(C15S) = Uanis(C22S)
Uanis(C14S) = Uanis(C21S)
Uanis(C20S) = Uanis(C13S)
Uanis(C18S) = Uanis(C19S)
Uanis(C18S) = Uanis(C27S)
Uanis(C28S) = Uanis(C17S)
Uanis(C16S) = Uanis(C29S)
Uanis(C15S) = Uanis(C30S)
Uanis(C14S) = Uanis(C25S)
Uanis(C13S) = Uanis(C26S)
Uanis(C26S) = Uanis(C35S)
Uanis(C36S) = Uanis(C27S)
Uanis(C31S) = Uanis(C28S)
Uanis(C29S) = Uanis(C32S)
Uanis(C30S) = Uanis(C33S)
Uanis(C25S) = Uanis(C34S)
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C6S(H6SA,H6SB), C5S(H5SA,H5SB), C4S(H4SA,H4SB), C1S(H1SA,H1SB), C3S(H3SA,
 H3SB), C2S(H2SA,H2SB)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C23(H23), C13(H13), C25(H25), C3(H3), C4(H4), C20S(H20S), C9S(H9S),
 C11S(H11S), C10S(H10S), C21S(H21S), C19S(H19S), C12S(H12S), C8S(H8S),
 C22S(H22S), C7S(H7S), C23S(H23S), C30S(H30S), C25S(H25S), C26S(H26S),
 C27S(H27S), C28S(H28S), C29S(H29S), C24S(H24S), C32S(H32S), C33S(H33S),
 C34S(H34S), C35S(H35S), C36S(H36S), C31S(H31S), C14S(H14S), C13S(H13S),
 C18S(H18S), C17S(H17S), C16S(H16S), C15S(H15S), C38S(H38S), C39S(H39S),
 C37S(H37S)
4.d Fitted hexagon refined as free rotating group:
 C30S(C25S,C26S,C27S,C28S,C29S), C32S(C33S,C34S,C35S,C36S,C31S), C14S(C13S,
 C18S,C17S,C16S,C15S)
4.e Idealised Me refined as rotating group:
 C121(H12A,H12B,H12C), C222(H22A,H22B,H22C), C122(H12D,H12E,H12F), C221(H22D,
 H22E,H22F), C140(H14A,H14B,H14C), C223(H22G,H22H,H22I), C123(H12G,H12H,H12I),
 C240(H24A,H24B,H24C)
;
_shelx_res_checksum              70150
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'