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_7040509
_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         'C38 H67 N2 O2 Si4 U, 1.92(C3.13 H3.13)'
_chemical_formula_sum            'C44 H73 N2 O2 Si4 U'
_chemical_formula_weight         1012.43
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 94.3765(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.89502(11)
_cell_length_b                   17.73106(18)
_cell_length_c                   20.67049(18)
_cell_measurement_reflns_used    38407
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      29.4700
_cell_measurement_theta_min      3.3020
_cell_volume                     5077.81(8)
_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
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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_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  -81.00   15.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.6632  111.0000 -169.1318 96

  2 omega -111.00  -34.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.6632 -179.0000  -60.0000 77

  3 omega   -3.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069   57.0000  -30.0000 103

  4 omega  -48.00   64.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069  -77.0000  120.0000 112

  5 omega  -50.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069  -37.0000 -180.0000 118

  6 omega  -25.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.6632  -99.0000 -150.0000 50

  7 omega  -97.00    5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.6632  -57.0000 -150.0000 102

  8 omega  -25.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.6632  -99.0000   30.0000 50

  9 omega  -25.00   25.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.6632  -99.0000  -30.0000 50

 10 omega  -46.00   57.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069  -57.0000  -60.0000 103

 11 omega   -3.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069   57.0000   90.0000 103

 12 omega   34.00  113.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069  179.0000   60.0000 79

 13 omega   -3.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069   57.0000 -180.0000 103

 14 omega -102.00  -62.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.6632  -37.0000  -60.0000 40

 15 omega  -50.00   68.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       27.0069  -37.0000   60.0000 118
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0184402000
_diffrn_orient_matrix_UB_12      -0.0346933000
_diffrn_orient_matrix_UB_13      -0.0108407000
_diffrn_orient_matrix_UB_21      -0.0435222000
_diffrn_orient_matrix_UB_22      -0.0061440000
_diffrn_orient_matrix_UB_23      -0.0195176000
_diffrn_orient_matrix_UB_31      0.0196599000
_diffrn_orient_matrix_UB_32      0.0189416000
_diffrn_orient_matrix_UB_33      -0.0261948000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0200
_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       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            114610
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54141
_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.
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    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.5367
_exptl_crystal_size_mid          0.3065
_exptl_crystal_size_min          0.1279
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.060
_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     558
_refine_ls_number_reflns         11616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+2.5319P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0412
_refine_ls_wR_factor_ref         0.0431
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10176
_reflns_number_total             11616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02630c2.cif
_cod_data_source_block           p15043
_cod_depositor_comments
'Adding full bibliography for 7040504--7040510.cif.'
_cod_database_code               7040509
_chemical_oxdiff_formula         C52H62N4O4U2Si8
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C6S)=Sof(H6S)=1-FVAR(1)
 Sof(C7S)=Sof(H7S)=FVAR(1)
 Sof(C5S)=Sof(H5S)=1-FVAR(2)
 Sof(C12S)=Sof(H12S)=FVAR(2)
 Sof(C4S)=Sof(H4S)=1-FVAR(3)
 Sof(C11S)=Sof(H11S)=FVAR(3)
 Sof(C3S)=Sof(H3S)=1-FVAR(4)
 Sof(C10S)=Sof(H10S)=FVAR(4)
 Sof(C2S)=Sof(H2S)=1-FVAR(5)
 Sof(C9S)=Sof(H9S)=FVAR(5)
 Sof(C1S)=Sof(H1S)=1-FVAR(6)
 Sof(C8S)=Sof(H8S)=FVAR(6)
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C6(H6), C25(H25), C13(H13), C23(H23), C12S(H12S),
 C11S(H11S), C9S(H9S), C8S(H8S), C7S(H7S), C10S(H10S), C6S(H6S), C5S(H5S),
 C4S(H4S), C3S(H3S), C2S(H2S), C1S(H1S)
3.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C50(H50A,H50B,H50C), C60(H60A,H60B,H60C), C121(H12A,H12B,
 H12C), C122(H12D,H12E,H12F), C56(H56A,H56B,H56C), C61(H61A,H61B,H61C),
 C123(H12G,H12H,H12I), C140(H14A,H14B,H14C), C54(H54A,H54B,H54C), C221(H22A,
 H22B,H22C), C52(H52A,H52B,H52C), C223(H22D,H22E,H22F), C59(H59A,H59B,H59C),
 C58(H58A,H58B,H58C), C51(H51A,H51B,H51C), C57(H57A,H57B,H57C), C240(H24A,H24B,
 H24C), C222(H22G,H22H,H22I), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              39417
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'