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_7049531
_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         'B6 C181 O9 U2'
_chemical_formula_sum            'C181 B6 O9 U2'
_chemical_formula_weight         2858.73
_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'
_audit_creation_date             2018-12-13
_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                89.191(3)
_cell_angle_beta                 89.908(2)
_cell_angle_gamma                66.724(3)
_cell_formula_units_Z            2
_cell_length_a                   15.9113(5)
_cell_length_b                   16.1748(7)
_cell_length_c                   36.3982(10)
_cell_measurement_reflns_used    17885
_cell_measurement_temperature    170
_cell_measurement_theta_max      24.0850
_cell_measurement_theta_min      3.2000
_cell_volume                     8604.2(6)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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    -47.00  51.00   1.00   17.50    --  -18.68  77.00-150.00   98
  2  \w    -93.00 -34.00   1.00   17.50    --  -18.68-179.00 -90.00   59
  3  \w    -93.00 -34.00   1.00   17.50    --  -18.68-179.00   0.00   59
  4  \w    -25.00  22.00   1.00   17.50    --  -18.68 -99.00 120.00   47
  5  \w    -25.00  22.00   1.00   17.50    --  -18.68 -99.00  30.00   47
  6  \w      2.00  89.00   1.00   17.50    --   20.25  57.00 -30.00   87
  7  \w    -50.00  43.00   1.00   17.50    --   20.25 -37.00 150.00   93
  8  \w    -52.00  58.00   1.00   17.50    --   20.25 -19.00-150.00  110
  9  \w    -25.00  22.00   1.00   17.50    --  -18.68 -99.00-150.00   47
 10  \w    -82.00  -5.00   1.00   17.50    --  -18.68 138.00  75.74   77
 11  \w    -88.00  10.00   1.00   17.50    --  -18.68 -77.00  60.00   98
 12  \w    -25.00  61.00   1.00   17.50    --   20.25 -99.00   0.00   86
 13  \w    -48.00  39.00   1.00   17.50    --   20.25 -57.00  60.00   87
 14  \w      2.00  89.00   1.00   17.50    --   20.25  57.00-150.00   87
;
_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      0.0125420000
_diffrn_orient_matrix_UB_12      -0.0012175000
_diffrn_orient_matrix_UB_13      -0.0187619000
_diffrn_orient_matrix_UB_21      -0.0074936000
_diffrn_orient_matrix_UB_22      -0.0400612000
_diffrn_orient_matrix_UB_23      -0.0022079000
_diffrn_orient_matrix_UB_31      -0.0462764000
_diffrn_orient_matrix_UB_32      0.0259419000
_diffrn_orient_matrix_UB_33      -0.0048135000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1255
_diffrn_reflns_av_unetI/netI     0.1035
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            151109
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        24.295
_diffrn_reflns_theta_max         24.295
_diffrn_reflns_theta_min         2.870
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.930
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light grey'
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.212
_refine_diff_density_max         6.516
_refine_diff_density_min         -6.769
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         27315
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1890
_refine_ls_R_factor_gt           0.1161
_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^)+(0.1250P)^2^+241.4568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2673
_refine_ls_wR_factor_ref         0.3190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14908
_reflns_number_total             27315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           p17058_tri087
_cod_depositor_comments
'Adding full bibliography for 7049530--7049539.cif.'
_cod_original_cell_volume        8604.2(5)
_cod_database_code               7049531
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C70 H70 O5 U1 B3'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_olex2_refinement_description
;
1. Restrained distances
 O6-C1 \\sim O5-C1 \\sim O4-C1
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: O5(0.5) O4(0.5) O6(0.5) C1(0.5) O4A(0.5) O5A(0.5) O6A(0.5) C1A(0.5)
;
_shelx_res_checksum              45597
_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 1.482
_oxdiff_exptl_absorpt_empirical_full_min 0.697