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_7049536
_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         '0.5(C90 H96 B3 O5 P2 U), 0.5(C72 H88 B5 O6 U)'
_chemical_formula_sum            'C81 H92 B4 O5.5 P U'
_chemical_formula_weight         1465.78
_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   geom
_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                72.304(2)
_cell_angle_beta                 80.146(2)
_cell_angle_gamma                70.091(2)
_cell_formula_units_Z            4
_cell_length_a                   17.2121(4)
_cell_length_b                   23.0300(4)
_cell_length_c                   23.4449(6)
_cell_measurement_reflns_used    16965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.3100
_cell_measurement_theta_min      3.0020
_cell_volume                     8300.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -94.00   4.00   0.70   15.00    --  -24.72 -77.00 120.00  140
  2  \w    -53.00  42.90   0.70   15.00    --  -24.72  77.00-120.00  137
  3  \w      1.00  85.00   0.70   15.00    --   26.28-131.00  14.37  120
  4  \w    -43.00  55.00   0.70   15.00    --   26.28 -77.00  60.00  140
  5  \w     -2.00  93.90   0.70   15.00    --   26.28  77.00-180.00  137
  6  \w     32.00  99.90   0.70   15.00    --   26.28-179.00  90.00   97
  7  \w    -45.00  95.70   0.70   15.00    --   26.28   0.00 -90.00  201
  8  \w    -99.00 -35.30   0.70   15.00    --  -24.72-179.00  60.00   91
  9  \w    -93.00  -7.60   0.70   15.00    --  -24.72 -57.00   0.00  122
 10  \w    -94.00   4.00   0.70   15.00    --  -24.72 -77.00 -90.00  140
 11  \w    -89.00  -8.50   0.70   15.00    --  -24.72 140.00 122.57  115
 12  \w    -99.00 -35.30   0.70   15.00    --  -24.72-179.00   0.00   91
 13  \w      4.00  95.70   0.70   15.00    --   26.28  37.00   0.00  131
 14  \w     -2.00  48.40   0.70   15.00    --   26.28  77.00  30.00   72
;
_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      -0.0429682000
_diffrn_orient_matrix_UB_12      0.0033995000
_diffrn_orient_matrix_UB_13      0.0044789000
_diffrn_orient_matrix_UB_21      -0.0092280000
_diffrn_orient_matrix_UB_22      0.0337302000
_diffrn_orient_matrix_UB_23      -0.0069401000
_diffrn_orient_matrix_UB_31      -0.0007381000
_diffrn_orient_matrix_UB_32      0.0022140000
_diffrn_orient_matrix_UB_33      -0.0307577000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1409
_diffrn_reflns_av_unetI/netI     0.1107
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            190436
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.838
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95135
_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            'clear colourless'
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_description       block
_exptl_crystal_F_000             2996
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.522
_refine_diff_density_min         -1.060
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1708
_refine_ls_number_reflns         33893
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0582
_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^)+(0.0454P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21884
_reflns_number_total             33893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           p18047
_cod_depositor_comments
'Adding full bibliography for 7049530--7049539.cif.'
_cod_original_cell_volume        8300.8(4)
_cod_original_formula_sum        'C81 H92 B4 O5.50 P U'
_cod_database_code               7049536
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H200 B3 O3 P2 U2'
_reflns_odcompleteness_completeness 99.85
_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.a Aromatic/amide H refined with riding coordinates:
 C452(H452), C448(H448), C450(H450), C568(H568), C93(H93), C663(H663),
 C232(H232), C446(H446), C451(H451), C449(H449), C552(H552), C558(H558),
 C458(H458), C564(H564), C442(H442), C234(H234), C124(H124), C562(H562),
 C556(H556), C775(H775), C444(H444), C454(H454), C567(H567), C113(H113),
 C115(H115), C95(H95), C443(H443), C894(H894), C773(H773), C672(H672),
 C554(H554), C333(H333), C555(H555), C885(H885), C122(H122), C883(H883),
 C782(H782), C445(H445), C553(H553), C565(H565), C566(H566), C335(H335),
 C223(H223), C457(H457), C561(H561), C455(H455), C225(H225), C674(H674),
 C559(H559), C784(H784), C665(H665), C105(H105), C456(H456), C892(H892),
 C560(H560), C103(H103), C342(H342), C344(H344)
2.b Idealised Me refined as rotating group:
 C779(H77A,H77B,H77C), C119(H11A,H11B,H11C), C667(H66A,H66B,H66C), C339(H33A,
 H33B,H33C), C117(H11D,H11E,H11F), C788(H78A,H78B,H78C), C898(H89A,H89B,H89C),
 C669(H66D,H66E,H66F), C777(H77D,H77E,H77F), C97(H97A,H97B,H97C), C237(H23A,
 H23B,H23C), C238(H23D,H23E,H23F), C98(H98A,H98B,H98C), C676(H67A,H67B,H67C),
 C896(H89D,H89E,H89F), C227(H22A,H22B,H22C), C786(H78D,H78E,H78F), C678(H67D,
 H67E,H67F), C229(H22D,H22E,H22F), C126(H12A,H12B,H12C), C128(H12D,H12E,H12F),
 C99(H99A,H99B,H99C), C887(H88A,H88B,H88C), C889(H88D,H88E,H88F), C348(H34A,
 H34B,H34C), C668(H66G,H66H,H66I), C888(H88G,H88H,H88I), C337(H33D,H33E,H33F),
 C778(H77G,H77H,H77I), C127(H12G,H12H,H12I), C346(H34D,H34E,H34F), C228(H22G,
 H22H,H22I), C677(H67G,H67H,H67I), C118(H11G,H11H,H11I), C897(H89G,H89H,H89I),
 C338(H33G,H33H,H33I), C109(H10A,H10B,H10C), C107(H10D,H10E,H10F), C108(H10G,
 H10H,H10I), C787(H78G,H78H,H78I), C347(H34G,H34H,H34I), C236(H23G,H23H,H23I)
;
_shelx_res_checksum              78181
_shelx_fab_checksum              53686
_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 1.094
_oxdiff_exptl_absorpt_empirical_full_min 0.883