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_7040505
_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 H55 I2 O5 U, C4 H8 O'
_chemical_formula_sum            'C42 H63 I2 O6 U'
_chemical_formula_weight         1155.75
_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                 94.6475(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1203(2)
_cell_length_b                   15.46388(16)
_cell_length_c                   22.0950(3)
_cell_measurement_reflns_used    19201
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.7120
_cell_measurement_theta_min      3.2170
_cell_volume                     4468.13(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000 -150.0000 50

  2 omega  -25.00   25.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -99.0000  -60.0000 50

  3 omega  -49.00   41.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  -57.0000  -90.0000 90

  4 omega  -25.00   61.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  -99.0000  150.0000 86

  5 omega   -2.00   88.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767   57.0000 -180.0000 90

  6 omega  -49.00   41.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  -57.0000   30.0000 90

  7 omega  -86.00    4.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.0767  -57.0000  -90.0000 90

  8 omega   34.00   96.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  179.0000  -60.0000 62

  9 omega  -25.00   61.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767  -99.0000  -30.0000 86

 10 omega   -2.00   50.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767   57.0000  -90.0000 52

 11 omega   -2.00   88.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       19.5767   57.0000   60.0000 90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0441819000
_diffrn_orient_matrix_UB_12      0.0080999000
_diffrn_orient_matrix_UB_13      -0.0156112000
_diffrn_orient_matrix_UB_21      0.0124419000
_diffrn_orient_matrix_UB_22      0.0356286000
_diffrn_orient_matrix_UB_23      0.0194306000
_diffrn_orient_matrix_UB_31      0.0288857000
_diffrn_orient_matrix_UB_32      -0.0277316000
_diffrn_orient_matrix_UB_33      0.0204027000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0367
_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       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            72103
_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         3.061
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.056
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57666
_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            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       block
_exptl_crystal_F_000             2244
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2906
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.1255
_refine_diff_density_max         2.003
_refine_diff_density_min         -1.817
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         9141
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0376P)^2^+36.4430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7365
_reflns_number_total             9141
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt02630c2.cif
_cod_data_source_block           p15141amono
_cod_depositor_comments
'Adding full bibliography for 7040504--7040510.cif.'
_cod_original_cell_volume        4468.12(10)
_cod_database_code               7040505
_chemical_oxdiff_formula         'C52 H62 O4 U2 I4'
_reflns_odcompleteness_completeness 99.81
_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
 C10S-C9S \\sim C11S-C12S
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O2S, C5S, C6S, C7S, C8S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1S, C4S, C3S, C2S, C1S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4S, C13S, C14S, C15S, C16S
 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)
4.b Secondary CH2 refined with riding coordinates:
 C9S(H9SA,H9SB), C4S(H4SA,H4SB), C12S(H12D,H12E), C8S(H8SA,H8SB), C10S(H10A,
 H10B), C5S(H5SA,H5SB), C11S(H11A,H11B), C3S(H3SA,H3SB), C1S(H1SA,H1SB),
 C6S(H6SA,H6SB), C2S(H2SA,H2SB), C7S(H7SA,H7SB), C13S(H13A,H13B), C14S(H14D,
 H14E), C15S(H15A,H15B), C16S(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C15(H15), C3(H3), C7(H7), C13(H13), C23(H23)
4.d Idealised Me refined as rotating group:
 C122(H12A,H12B,H12C), C140(H14A,H14B,H14C), C121(H12F,H12G,H12H), C221(H22A,
 H22B,H22C), C223(H22D,H22E,H22F), C123(H12I,H12J,H12K), C240(H24A,H24B,H24C),
 C222(H22G,H22H,H22I)
;
_shelx_res_checksum              459
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'