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_7049537
_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         'C94 H147.98 B3 O4 U'
_chemical_formula_sum            'C94 H147.98 B3 O4 U'
_chemical_formula_weight         1612.56
_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     direct
_audit_creation_date             2018-12-11
_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                 97.880(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5344(7)
_cell_length_b                   27.8539(8)
_cell_length_c                   20.2709(7)
_cell_measurement_reflns_used    4724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18.7660
_cell_measurement_theta_min      3.3100
_cell_volume                     9247.6(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (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    -37.00  50.00   1.00   45.00    --  -18.53  57.00-120.00   87
  2  \w    -90.00  53.00   1.00   45.00    --  -18.53   0.00  30.00  143
  3  \w    -25.00  22.00   1.00   45.00    --  -18.53 -99.00 -90.00   47
  4  \w    -25.00  22.00   1.00   45.00    --  -18.53 -99.00 120.00   47
  5  \w    -88.00  10.00   1.00   45.00    --  -18.53 -77.00  30.00   98
  6  \w    -25.00  22.00   1.00   45.00    --  -18.53 -99.00  90.00   47
  7  \w    -18.00  92.00   1.00   45.00    --   20.09  19.00 -30.00  110
  8  \w    -93.00 -32.00   1.00   45.00    --  -18.53 179.00  30.00   61
  9  \w    -47.00  51.00   1.00   45.00    --  -18.53  77.00 150.00   98
 10  \w    -25.00   0.00   1.00   45.00    --  -18.53 -99.00 150.00   25
 11  \w    -25.00  61.00   1.00   45.00    --   20.09 -99.00  30.00   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      -0.0390978000
_diffrn_orient_matrix_UB_12      0.0061814000
_diffrn_orient_matrix_UB_13      0.0080679000
_diffrn_orient_matrix_UB_21      -0.0173632000
_diffrn_orient_matrix_UB_22      -0.0044786000
_diffrn_orient_matrix_UB_23      -0.0334045000
_diffrn_orient_matrix_UB_31      -0.0067147000
_diffrn_orient_matrix_UB_32      -0.0242956000
_diffrn_orient_matrix_UB_33      0.0081811000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2674
_diffrn_reflns_av_unetI/netI     0.1604
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            131250
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.108
_diffrn_reflns_theta_max         24.108
_diffrn_reflns_theta_min         2.886
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.800
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.976
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.158
_exptl_crystal_description       block
_exptl_crystal_F_000             3404
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.759
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         14671
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1509
_refine_ls_R_factor_gt           0.0801
_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^)+(0.0180P)^2^+13.3799P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8850
_reflns_number_total             14671
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           p16133_087mono
_cod_depositor_comments
'Adding full bibliography for 7049530--7049539.cif.'
_cod_database_code               7049537
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H100 B3 O3 U'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C601 \\sim C600: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C640) = Uanis(C540)
3. Rigid body (RIGU) restrains
 C601, C600
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H60f(0.33) H60g(0.33) H60h(0.66) H60i(0.66) C603(0.33) H60j(0.33)
 H60k(0.33) H60l(0.33) C604(0.67) H60m(0.67) H60n(0.67) H60o(0.67)
5.a Ternary CH refined with riding coordinates:
 C620(H620), C420(H420), C520(H520), C320(H320), C560(H560), C220(H220),
 C360(H360), C460(H460), C660(H660), C140(H140), C260(H260), C340(H340),
 C120(H120), C160(H160), C540(H540), C240(H240), C440(H440), C640(H640)
5.b Secondary CH2 refined with riding coordinates:
 C600(H60a,H60b), C602(H60f,H60g), C602(H60h,H60i)
5.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C23(H23), C45(H45), C43(H43), C35(H35), C63(H63), C55(H55),
 C33(H33), C25(H25), C13(H13), C53(H53), C65(H65)
5.d Idealised Me refined as rotating group:
 C621(H62a,H62b,H62c), C321(H32a,H32b,H32c), C422(H42a,H42b,H42c), C322(H32d,
 H32e,H32f), C221(H22a,H22b,H22c), C362(H36a,H36b,H36c), C141(H14a,H14b,H14c),
 C561(H56a,H56b,H56c), C622(H62d,H62e,H62f), C661(H66a,H66b,H66c), C461(H46a,
 H46b,H46c), C421(H42d,H42e,H42f), C562(H56d,H56e,H56f), C162(H16a,H16b,H16c),
 C541(H54a,H54b,H54c), C161(H16d,H16e,H16f), C262(H26a,H26b,H26c), C361(H36d,
 H36e,H36f), C342(H34a,H34b,H34c), C601(H60c,H60d,H60e), C242(H24a,H24b,H24c),
 C142(H14d,H14e,H14f), C261(H26d,H26e,H26f), C341(H34d,H34e,H34f), C121(H12a,
 H12b,H12c), C441(H44a,H44b,H44c), C521(H52a,H52b,H52c), C462(H46d,H46e,H46f),
 C522(H52d,H52e,H52f), C122(H12d,H12e,H12f), C222(H22d,H22e,H22f), C241(H24d,
 H24e,H24f), C662(H66d,H66e,H66f), C641(H64a,H64b,H64c), C442(H44d,H44e,H44f),
 C542(H54d,H54e,H54f), C642(H64d,H64e,H64f), C603(H60j,H60k,H60l), C604(H60m,
 H60n,H60o)
;
_shelx_res_checksum              2945
_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 1.103
_oxdiff_exptl_absorpt_empirical_full_min 0.903