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_7049535
_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 K2 O8 U2)'
_chemical_formula_sum            'C72 H88 B4 K1.33 O5.33 U1.33'
_chemical_formula_weight         1451.50
_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     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                90
_cell_angle_beta                 109.680(2)
_cell_angle_gamma                90
_cell_formula_units_Z            3
_cell_length_a                   15.3907(2)
_cell_length_b                   22.7218(2)
_cell_length_c                   16.9809(2)
_cell_measurement_reflns_used    26955
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2430
_cell_measurement_theta_min      3.1960
_cell_volume                     5591.43(13)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -25.00  20.00   1.00   15.00    --  -16.53 -99.00  90.00   45
  2  \w    -87.00 -34.00   1.00   15.00    --  -16.53-179.00 150.00   53
  3  \w    -31.00  49.00   1.00   15.00    --  -16.53  57.00-150.00   80
  4  \w    -25.00  20.00   1.00   15.00    --  -16.53 -99.00 -90.00   45
  5  \w    -85.00   1.00   1.00   15.00    --  -16.53 -37.00  30.00   86
  6  \w    -31.00  49.00   1.00   15.00    --  -16.53  57.00-120.00   80
  7  \w     34.00  89.00   1.00   15.00    --   18.25 179.00  30.00   55
  8  \w    -47.00  33.00   1.00   15.00    --   18.25 -57.00-180.00   80
  9  \w      3.00  84.00   1.00   15.00    --   18.25  57.00 150.00   81
 10  \w      1.00  87.00   1.00   15.00    --   18.25  37.00  30.00   86
 11  \w    -48.00  43.00   1.00   15.00    --   18.25 -77.00  30.00   91
 12  \w      3.00  84.00   1.00   15.00    --   18.25  57.00-120.00   81
 13  \w      5.00  40.00   1.00   15.00    --   18.25-137.00 176.60   35
 14  \w    -50.00  36.00   1.00   15.00    --   18.25 -37.00  60.00   86
;
_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      0.0450628000
_diffrn_orient_matrix_UB_12      -0.0121587000
_diffrn_orient_matrix_UB_13      0.0126490000
_diffrn_orient_matrix_UB_21      -0.0134847000
_diffrn_orient_matrix_UB_22      -0.0187675000
_diffrn_orient_matrix_UB_23      -0.0354493000
_diffrn_orient_matrix_UB_31      0.0135194000
_diffrn_orient_matrix_UB_32      0.0217873000
_diffrn_orient_matrix_UB_33      -0.0234704000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            109506
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.811
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.016
_exptl_absorpt_correction_T_max  0.840
_exptl_absorpt_correction_T_min  0.743
_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            'light brown'
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             2192
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.162
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+2.0433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8129
_reflns_number_total             10220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           p18089
_cod_depositor_comments
'Adding full bibliography for 7049530--7049539.cif.'
_cod_database_code               7049535
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U2 O6 B6 C100 H100 P2'
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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.a Aromatic/amide H refined with riding coordinates:
 C234(H234), C225(H225), C333(H333), C223(H223), C335(H335), C122(H122),
 C342(H342), C124(H124), C113(H113), C232(H232), C344(H344), C115(H115)
2.b Idealised Me refined as rotating group:
 C229(H22A,H22B,H22C), C128(H12A,H12B,H12C), C238(H23A,H23B,H23C), C337(H33A,
 H33B,H33C), C227(H22D,H22E,H22F), C346(H34A,H34B,H34C), C228(H22G,H22H,H22I),
 C348(H34D,H34E,H34F), C236(H23D,H23E,H23F), C117(H11A,H11B,H11C), C126(H12D,
 H12E,H12F), C339(H33D,H33E,H33F), C338(H33G,H33H,H33I), C347(H34G,H34H,H34I),
 C119(H11D,H11E,H11F), C237(H23G,H23H,H23I), C127(H12G,H12H,H12I), C118(H11G,
 H11H,H11I)
;
_shelx_res_checksum              48741
_shelx_fab_checksum              19446
_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 1.135
_oxdiff_exptl_absorpt_empirical_full_min 0.932