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_7040510
_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         'C64 H87 N2 O2 Si4 U, C4 H8 O, C3 H3'
_chemical_formula_sum            'C71 H98 N2 O3 Si4 U'
_chemical_formula_weight         1377.90
_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                105.6517(16)
_cell_angle_beta                 103.7133(17)
_cell_angle_gamma                95.6555(16)
_cell_formula_units_Z            2
_cell_length_a                   13.1696(3)
_cell_length_b                   13.7113(3)
_cell_length_c                   20.4909(4)
_cell_measurement_reflns_used    18700
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.8340
_cell_measurement_theta_min      3.2210
_cell_volume                     3408.70(14)
_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
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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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -25.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000  150.0000 50

  2 omega  -25.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000  -90.0000 50

  3 omega  -25.00   62.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330  -99.0000  120.0000 87

  4 omega  -49.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330  -57.0000 -120.0000 90

  5 omega  -49.00   41.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330  -57.0000    0.0000 90

  6 omega   -2.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330   57.0000  150.0000 91

  7 omega  -86.00    4.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -57.0000 -120.0000 90

  8 omega   34.00   96.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330  179.0000  -90.0000 62

  9 omega   -2.00   78.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330 -127.0000  -41.0000 80

 10 omega   -2.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330   57.0000 -120.0000 91

 11 omega   -2.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330   57.0000   30.0000 91

 12 omega  -37.00   52.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767   57.0000  150.0000 89

 13 omega  -25.00   25.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000   30.0000 50

 14 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       19.7330  -99.0000 -180.0000 47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0173830000
_diffrn_orient_matrix_UB_12      0.0122058000
_diffrn_orient_matrix_UB_13      0.0372283000
_diffrn_orient_matrix_UB_21      -0.0147319000
_diffrn_orient_matrix_UB_22      -0.0524420000
_diffrn_orient_matrix_UB_23      -0.0027761000
_diffrn_orient_matrix_UB_31      0.0514776000
_diffrn_orient_matrix_UB_32      -0.0087661000
_diffrn_orient_matrix_UB_33      -0.0021149000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            70327
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.227
_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    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             1420
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.5693
_exptl_crystal_size_mid          0.1736
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.659
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         13932
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+2.5200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12437
_reflns_number_total             13932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02630c2.cif
_cod_data_source_block           p15149c
_cod_depositor_comments
'Adding full bibliography for 7040504--7040510.cif.'
_cod_original_cell_volume        3408.69(12)
_cod_database_code               7040510
_chemical_oxdiff_formula         'C100 H120 O4 N4 Si8 U2'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C2S-C1S \\sim C2S-C3S
 with sigma of 0.02
 C3S_$1-C1S \\sim C2S-C1S \\sim C2S-C3S \\sim C3S-C1S_$1 \\sim C2S_$1-C1S_$1
\\sim C2S_$1-C3S_$1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C7S) = Uanis(C6S) = Uanis(C5S) = Uanis(C4S) = Uanis(O1S) = Uanis(O2S)
Uanis(C1S) = Uanis(C2S) = Uanis(C3S)
4. Others
 Sof(O2S)=1-FVAR(1)
 Sof(O1S)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C4S(H4SA,H4SB), C7S(H7SA,H7SB), C6S(H6SA,H6SB), C5S(H5SA,H5SB)
5.c Aromatic/amide H refined with riding coordinates:
 C23(H23), C25(H25), C3(H3), C15(H15), C7(H7), C126(H126), C13(H13),
 C142(H142), C222(H222), C122(H122), C246(H246), C124(H124), C242(H242),
 C123(H123), C125(H125), C223(H223), C244(H244), C245(H245), C226(H226),
 C243(H243), C224(H224), C143(H143), C225(H225), C146(H146), C144(H144),
 C145(H145), C1S(H1S), C3S(H3S), C2S(H2S)
5.d Idealised Me refined as rotating group:
 C57(H57A,H57B,H57C), C54(H54A,H54B,H54C), C128(H12A,H12B,H12C), C51(H51A,H51B,
 H51C), C228(H22A,H22B,H22C), C60(H60A,H60B,H60C), C55(H55A,H55B,H55C),
 C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C247(H24A,H24B,H24C), C58(H58A,H58B,
 H58C), C227(H22D,H22E,H22F), C59(H59A,H59B,H59C), C248(H24D,H24E,H24F),
 C61(H61A,H61B,H61C), C127(H12D,H12E,H12F), C52(H52A,H52B,H52C), C148(H14A,H14B,
 H14C), C62(H62A,H62B,H62C), C147(H14D,H14E,H14F)
;
_shelx_res_checksum              60125
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_solvent_exptl_crystal_recrystallization_method THF