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_7040504
_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         'C68 H94 I4 O8 U2, 3(C4 H8 O)'
_chemical_formula_sum            'C80 H118 I4 O11 U2'
_chemical_formula_weight         2239.40
_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                68.627(4)
_cell_angle_beta                 71.761(3)
_cell_angle_gamma                62.142(4)
_cell_formula_units_Z            2
_cell_length_a                   15.8678(6)
_cell_length_b                   16.2835(7)
_cell_length_c                   21.4232(7)
_cell_measurement_reflns_used    7620
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      20.3080
_cell_measurement_theta_min      3.1960
_cell_volume                     4488.4(3)
_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)'
_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 0.998
_diffrn_measurement_details
;
  1 omega  -25.00   22.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  -30.0000 47

  2 omega  -25.00   22.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  -90.0000 47

  3 omega  -93.00  -34.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277 -179.0000  -30.0000 59

  4 omega  -93.00  -34.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277 -179.0000   30.0000 59

  5 omega    2.00   89.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   57.0000 -180.0000 87

  6 omega   -2.00   91.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   38.0000  -30.0000 93

  7 omega   34.00   94.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  179.0000 -150.0000 60

  8 omega  -25.00   61.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -99.0000   60.0000 86

  9 omega  -49.00   49.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -77.0000  -30.0000 98

 10 omega  -48.00   39.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -57.0000 -180.0000 87

 11 omega  -87.00    0.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -57.0000 -180.0000 87

 12 omega   34.00   94.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  179.0000  -30.0000 60

 13 omega  -49.00   49.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -77.0000 -180.0000 98

 14 omega    2.00   89.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   57.0000   90.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0498420000
_diffrn_orient_matrix_UB_12      0.0250660000
_diffrn_orient_matrix_UB_13      0.0116054000
_diffrn_orient_matrix_UB_21      0.0118993000
_diffrn_orient_matrix_UB_22      0.0264111000
_diffrn_orient_matrix_UB_23      0.0134134000
_diffrn_orient_matrix_UB_31      -0.0031056000
_diffrn_orient_matrix_UB_32      0.0357404000
_diffrn_orient_matrix_UB_33      -0.0314425000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1353
_diffrn_reflns_av_unetI/netI     0.1224
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            77490
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         2.883
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.029
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84961
_exptl_absorpt_correction_type   multi-scan
_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)
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    1.657
_exptl_crystal_description       plate
_exptl_crystal_F_000             2164
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2868
_exptl_crystal_size_mid          0.1113
_exptl_crystal_size_min          0.0164
_refine_diff_density_max         2.510
_refine_diff_density_min         -1.306
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         14234
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1466
_refine_ls_R_factor_gt           0.0876
_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/[\s^2^(Fo^2^)+(0.0799P)^2^+62.4357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1843
_refine_ls_wR_factor_ref         0.2113
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8754
_reflns_number_total             14234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02630c2.cif
_cod_data_source_block           p16001-tri_sq
_cod_depositor_comments
'Adding full bibliography for 7040504--7040510.cif.'
_cod_database_code               7040504
_chemical_oxdiff_formula         'C70 H70 O4 U2 I4'
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_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(O6) = Uanis(O0AA)
Uanis(C1BA) = Uanis(C1CA)
Uanis(C2BA) = Uanis(C3AA)
Uanis(C9AA) = Uanis(C0AA)
Uanis(C6BA) = Uanis(C3BA)
3. Rigid body (RIGU) restrains
 O6S, C21S, C22S, C23S, C24S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O6, C2BA, C3BA, C9AA, C1BA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O0AA, C3AA, C6BA, C0AA, C1CA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4S, C16S, C15S, C14S, C13S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O3S, C9S, C10S, C11S, C12S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1S, C1S, C2S, C3S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2S, C8S, C7S, C6S, C5S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), C1S(H1SA,H1SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB), C9S(H9SA,
 H9SB), C7S(H7SA,H7SB), C5S(H5SA,H5SB), C15S(H15A,H15B), C13S(H13A,H13B),
 C6S(H6SA,H6SB), C10S(H10A,H10B), C8S(H8SA,H8SB), C16S(H16A,H16B), C14S(H14A,
 H14B), C12S(H12A,H12B), C11S(H11A,H11B), C21S(H21A,H21B), C22S(H22A,H22B),
 C23S(H23A,H23B), C24S(H24A,H24B), C1BA(H1BA,H1BB), C9AA(H9AA,H9AB), C3BA(H3BA,
 H3BB), C2BA(H2BA,H2BB), C3AA(H3AA,H3AB), C6BA(H6BA,H6BB), C0AA(H0AA,H0AB),
 C1CA(H1CA,H1CB)
4.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C3(H3), C33(H33), C13(H13), C5(H5), C45(H45), C7(H7), C6(H6),
 C25(H25), C35(H35), C23(H23), C43(H43)
4.d Fitted pentagon refined as free rotating group:
 C4S(O1S,C1S,C2S,C3S), O6S(C21S,C22S,C23S,C24S), O6(C1BA,C9AA,C3BA,C2BA),
 O0AA(C3AA,C6BA,C0AA,C1CA)
4.e Idealised Me refined as rotating group:
 C6AA(H6AA,H6AB,H6AC), C321(H32A,H32B,H32C), C323(H32D,H32E,H32F), C17(H17A,
 H17B,H17C), C7AA(H7AA,H7AB,H7AC), C322(H32G,H32H,H32I), C422(H42A,H42B,H42C),
 C421(H42D,H42E,H42F), C4AA(H4AA,H4AB,H4AC), C440(H44A,H44B,H44C), C423(H42G,
 H42H,H42I), C9(H9A,H9B,H9C), C18(H18A,H18B,H18C), C8BA(H8BA,H8BB,H8BC),
 C340(H34A,H34B,H34C), C9BA(H9BA,H9BB,H9BC)
;
_shelx_res_checksum              24256
_shelx_fab_checksum              89886
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method THF