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_7049530
_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         '0.67(C108 H132 B6 O6 U2), 1.33(C6 H14)'
_chemical_formula_sum            'C80 H106.67 B4 O4 U1.33'
_chemical_formula_weight         1492.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-20
_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                90
_cell_angle_beta                 96.5210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            3
_cell_length_a                   13.8450(2)
_cell_length_b                   14.9545(2)
_cell_length_c                   31.6940(4)
_cell_measurement_reflns_used    39951
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      26.8230
_cell_measurement_theta_min      3.2570
_cell_volume                     6519.63(15)
_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_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.929
_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    -52.00 -26.50   0.75    5.00    --   -9.43 104.00  62.36   34
  2  \w    -20.00  27.25   0.75    5.00    --   -9.43 -99.00 150.00   63
  3  \w    -67.00   0.50   0.75    5.00    --   -9.43 -77.00 -90.00   90
  4  \w    -20.00   5.50   0.75    5.00    --   -9.43 -99.00   0.00   34
  5  \w    -79.00 -20.50   0.75    5.00    --   -9.43 -57.00  60.00   78
  6  \w    -84.00 -40.50   0.75    5.00    --   -9.43 155.00   7.53   58
  7  \w    -19.00  28.25   0.75    5.00    --   -9.43 -99.00 -90.00   63
  8  \w      2.00  48.50   0.75    5.00    --   -9.43  57.00-150.00   62
  9  \w     18.00  45.00   0.75    5.00    --   10.84-128.00  22.96   36
 10  \w    -58.00 -31.00   0.75    5.00    --   10.84 -57.00 150.00   36
 11  \w     52.00  79.00   0.75    5.00    --   10.84  57.00  60.00   36
 12  \w     20.00  78.50   0.75    5.00    --   10.84  57.00 -90.00   78
 13  \w     12.00  39.00   0.75    5.00    --   10.84  57.00  30.00   36
 14  \w     22.00  84.25   0.75    5.00    --   10.84  77.00 -30.00   83
 15  \w     23.00  50.00   0.75    5.00    --   10.84 -99.00  90.00   36
 16  \w    -37.00 -10.00   0.75    5.00    --   10.84 -57.00   0.00   36
 17  \w     59.00  84.50   0.75    5.00    --   10.84  77.00   0.00   34
 18  \w    -52.25  37.00   0.75    5.00    --   10.84 -57.00-180.00  119
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0064000000
_diffrn_orient_matrix_UB_12      -0.0460979000
_diffrn_orient_matrix_UB_13      -0.0041706000
_diffrn_orient_matrix_UB_21      0.0350691000
_diffrn_orient_matrix_UB_22      0.0109186000
_diffrn_orient_matrix_UB_23      -0.0138397000
_diffrn_orient_matrix_UB_31      0.0372522000
_diffrn_orient_matrix_UB_32      -0.0023592000
_diffrn_orient_matrix_UB_33      0.0172765000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            139328
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.743
_diffrn_reflns_theta_min         2.800
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.168
_refine_diff_density_max         0.995
_refine_diff_density_min         -1.419
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         17270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0253P)^2^+6.2846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0752
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13836
_reflns_number_total             17270
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           po17030_refinalized
_cod_depositor_comments
'Adding full bibliography for 7049530--7049539.cif.'
_cod_database_code               7049530
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C108 H132 B6 O6 U2'
_chemical_oxdiff_usercomment     '@ 120 K LP_01_12'
_reflns_odcompleteness_completeness 99.80
_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.a Secondary CH2 refined with riding coordinates:
 C01Q(H01A,H01B), C32(H32A,H32B), C01V(H01F,H01G), C027(H02A,H02B)
2.b Aromatic/amide H refined with riding coordinates:
 C333(H333), C335(H335), C225(H225), C124(H124), C113(H113), C223(H223),
 C115(H115), C232(H232), C234(H234), C122(H122), C342(H342), C344(H344)
2.c Idealised Me refined as rotating group:
 C348(H34A,H34B,H34C), C339(H33A,H33B,H33C), C128(H12A,H12B,H12C), C119(H11A,
 H11B,H11C), C229(H22A,H22B,H22C), C117(H11D,H11E,H11F), C236(H23A,H23B,H23C),
 C238(H23D,H23E,H23F), C337(H33D,H33E,H33F), C338(H33G,H33H,H33I), C228(H22D,
 H22E,H22F), C126(H12D,H12E,H12F), C227(H22G,H22H,H22I), C127(H12G,H12H,H12I),
 C346(H34D,H34E,H34F), C118(H11G,H11H,H11I), C237(H23G,H23H,H23I), C347(H34G,
 H34H,H34I), C01R(H01C,H01D,H01E), C01W(H01H,H01I,H01J)
;
_shelx_res_checksum              42263
_shelx_fab_checksum              63995
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.830