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_7040508
_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         'C76 H134 N4 O4 Si8 U2, C3 H7'
_chemical_formula_sum            'C79 H141 N4 O4 Si8 U2'
_chemical_formula_weight         1911.73
_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                65.3765(19)
_cell_angle_beta                 88.1786(17)
_cell_angle_gamma                88.3450(17)
_cell_formula_units_Z            2
_cell_length_a                   12.9013(3)
_cell_length_b                   18.8759(4)
_cell_length_c                   21.4638(4)
_cell_measurement_reflns_used    11460
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      22.0760
_cell_measurement_theta_min      3.1220
_cell_volume                     4748.53(19)
_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 0.998
_diffrn_measurement_details
;
  1 omega  -87.00    0.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -57.0000  120.0000 87

  2 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  -90.0000 47

  3 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000   90.0000 47

  4 omega   -2.00   91.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   38.0000  -60.0000 93

  5 omega  -52.00   58.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -19.0000  150.0000 110

  6 omega    2.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   57.0000  -30.0000 87

  7 omega   -8.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465   77.0000   60.0000 97

  8 omega  -25.00   22.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277  -99.0000  150.0000 47

  9 omega  -93.00  -34.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5277 -179.0000 -120.0000 59

 10 omega  -25.00   61.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -99.0000  -90.0000 86

 11 omega  -48.00   39.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -57.0000    0.0000 87

 12 omega    3.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465 -135.0000  165.8975 78

 13 omega   34.00   94.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  179.0000 -180.0000 60

 14 omega  -25.00   55.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       20.2465  -99.0000  -60.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0245853000
_diffrn_orient_matrix_UB_12      -0.0138781000
_diffrn_orient_matrix_UB_13      0.0328525000
_diffrn_orient_matrix_UB_21      0.0471811000
_diffrn_orient_matrix_UB_22      0.0034533000
_diffrn_orient_matrix_UB_23      0.0145160000
_diffrn_orient_matrix_UB_31      -0.0140057000
_diffrn_orient_matrix_UB_32      0.0387897000
_diffrn_orient_matrix_UB_33      -0.0056643000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            85138
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.550
_exptl_absorpt_correction_T_max  0.971
_exptl_absorpt_correction_T_min  0.758
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       plate
_exptl_crystal_F_000             1942
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3216
_exptl_crystal_size_mid          0.0754
_exptl_crystal_size_min          0.0229
_refine_diff_density_max         1.073
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         16783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0947
_refine_ls_R_factor_gt           0.0540
_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^)+(0.0184P)^2^+12.2734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0964
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11693
_reflns_number_total             16783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02630c2.cif
_cod_data_source_block           p16033_tri077
_cod_depositor_comments
'Adding full bibliography for 7040504--7040510.cif.'
_cod_original_cell_volume        4748.51(18)
_cod_database_code               7040508
_chemical_oxdiff_formula         'C100 H100 O4 U2 N4 Si8'
_reflns_odcompleteness_completeness 99.87
_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
 C2S-C3S \\sim C2S-C1S
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C3S(H3SA,H3SB), C2S(H2SA,H2SB)
3.c Aromatic/amide H refined with riding coordinates:
 C45(H45), C25(H25), C35(H35), C3(H3), C5(H5), C7(H7), C15(H15), C6(H6),
 C43(H43), C13(H13), C23(H23), C33(H33)
3.d Idealised Me refined as rotating group:
 C51(H51A,H51B,H51C), C123(H12A,H12B,H12C), C122(H12D,H12E,H12F), C69(H69A,
 H69B,H69C), C322(H32A,H32B,H32C), C57(H57A,H57B,H57C), C55(H55A,H55B,H55C),
 C440(H44A,H44B,H44C), C68(H68A,H68B,H68C), C121(H12G,H12H,H12I), C140(H14A,
 H14B,H14C), C56(H56A,H56B,H56C), C340(H34A,H34B,H34C), C323(H32D,H32E,H32F),
 C73(H73A,H73B,H73C), C64(H64A,H64B,H64C), C240(H24A,H24B,H24C), C65(H65A,H65B,
 H65C), C222(H22A,H22B,H22C), C321(H32G,H32H,H32I), C422(H42A,H42B,H42C),
 C223(H22D,H22E,H22F), C61(H61A,H61B,H61C), C58(H58A,H58B,H58C), C70(H70A,H70B,
 H70C), C423(H42D,H42E,H42F), C72(H72A,H72B,H72C), C54(H54A,H54B,H54C),
 C221(H22G,H22H,H22I), C421(H42G,H42H,H42I), C53(H53A,H53B,H53C), C60(H60A,H60B,
 H60C), C66(H66A,H66B,H66C), C50(H50A,H50B,H50C), C59(H59A,H59B,H59C), C52(H52A,
 H52B,H52C), C67(H67A,H67B,H67C), C62(H62A,H62B,H62C), C71(H71A,H71B,H71C),
 C63(H63A,H63B,H63C), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              91713
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'