Applications of boroxide ligands in supporting small molecule activation by U(iii) and U(iv) complexes.
Arnold, Polly L.; Puig-Urrea, Laura; Wells, Jordann A. L.; Yuan, Dan; Cruickshank, Faye L.; Young, Rowan D.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4894–4905; doi:10.1039/c8dt05051a

data_7049533
_publ_section_title
;
 Applications of boroxide ligands in supporting small molecule activation
 by U(iii) and U(iv) complexes.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4894
_journal_page_last               4905
_journal_paper_doi               10.1039/c8dt05051a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C54 H66 B3 O3 S2 U, C6 H6, C3'
_chemical_formula_sum            'C63 H72 B3 O3 S2 U'
_chemical_formula_weight         1211.78
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-12-21 deposited with the CCDC.    2019-02-28 downloaded from the CCDC.
;
_cell_angle_alpha                77.2060(10)
_cell_angle_beta                 87.1260(10)
_cell_angle_gamma                84.9070(10)
_cell_formula_units_Z            2
_cell_length_a                   12.3086(2)
_cell_length_b                   14.3349(2)
_cell_length_c                   21.6092(4)
_cell_measurement_reflns_used    18918
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.1830
_cell_measurement_theta_min      3.2990
_cell_volume                     3701.62(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -59.00  22.00   0.75    5.00    --  -18.04 103.00  34.26  108
  2  \w    -25.00  20.00   0.75    5.00    --  -18.04 -99.00-120.00   60
  3  \w    -85.00  -1.00   0.75    5.00    --  -18.04 -57.00 -90.00  112
  4  \w     -7.00  86.00   0.75    5.00    --   19.60  77.00 -90.00  124
  5  \w    -48.00  36.00   0.75    5.00    --   19.60 -57.00   0.00  112
  6  \w      3.00  87.00   0.75    5.00    --   19.60  57.00 -90.00  112
  7  \w    -48.00  45.00   0.75    5.00    --   19.60 -77.00 150.00  124
  8  \w    -25.00  20.00   0.75    5.00    --  -18.04 -99.00 120.00   60
  9  \w    -67.00   8.75   0.75    5.00    --  -18.04 117.00-122.00  101
 10  \w    -85.00  -1.00   0.75    5.00    --  -18.04 -57.00   0.00  112
 11  \w     34.00  91.00   0.75    5.00    --   19.60 179.00 -60.00   76
 12  \w      3.00  87.00   0.75    5.00    --   19.60  57.00-180.00  112
 13  \w    -10.00  89.75   0.75    5.00    --   19.60  19.00 150.00  133
 14  \w    -25.00  10.25   0.75    5.00    --   19.60 -99.00-150.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085544000
_diffrn_orient_matrix_UB_12      0.0005694000
_diffrn_orient_matrix_UB_13      -0.0323028000
_diffrn_orient_matrix_UB_21      0.0078122000
_diffrn_orient_matrix_UB_22      0.0497172000
_diffrn_orient_matrix_UB_23      -0.0082083000
_diffrn_orient_matrix_UB_31      0.0567119000
_diffrn_orient_matrix_UB_32      -0.0109058000
_diffrn_orient_matrix_UB_33      -0.0048205000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            78705
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.924
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.283
_exptl_absorpt_correction_T_max  0.814
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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            'translucent red'
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       plate
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.046
_refine_diff_density_max         2.258
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     638
_refine_ls_number_reflns         15098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0657P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12610
_reflns_number_total             15098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           p18033
_cod_depositor_comments
'Adding full bibliography for 7049530--7049539.cif.'
_cod_database_code               7049533
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H200 B3 O3 S2 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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C7S(0.5) C9S(0.5) C8S(0.5) C11S(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C115(H115), C232(H232), C335(H335), C333(H333), C113(H113), C344(H344),
 C124(H124), C223(H223), C3AA(H3AA), C122(H122), C225(H225), C342(H342),
 C4S(H4S), C3S(H3S), C2S(H2S), C1S(H1S)
3.b Idealised Me refined as rotating group:
 C235(H23A,H23B,H23C), C337(H33A,H33B,H33C), C346(H34A,H34B,H34C), C348(H34D,
 H34E,H34F), C227(H22A,H22B,H22C), C117(H11A,H11B,H11C), C339(H33D,H33E,H33F),
 C119(H11D,H11E,H11F), C234(H23D,H23E,H23F), C126(H12A,H12B,H12C), C229(H22D,
 H22E,H22F), C128(H12D,H12E,H12F), C118(H11G,H11H,H11I), C347(H34G,H34H,H34I),
 C338(H33G,H33H,H33I), C233(H23G,H23H,H23I), C228(H22G,H22H,H22I), C127(H12G,
 H12H,H12I)
;
_shelx_res_checksum              96678
_shelx_fab_checksum              45232
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.266
_oxdiff_exptl_absorpt_empirical_full_min 0.626