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_7049538
_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         'C120 H184 B4 O4 U, C7 H8'
_chemical_formula_sum            'C127 H192 B4 O4 U'
_chemical_formula_weight         2064.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-21
_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                 108.923(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.0131(4)
_cell_length_b                   19.4020(3)
_cell_length_c                   30.6714(6)
_cell_measurement_reflns_used    28581
_cell_measurement_temperature    170
_cell_measurement_theta_max      23.2550
_cell_measurement_theta_min      3.0280
_cell_volume                     12391.7(4)
_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    -87.00   0.00   1.00   30.00    --  -18.53 -57.00   0.00   87
  2  \w    -25.00  22.00   1.00   30.00    --  -18.53 -99.00-150.00   47
  3  \w    -25.00  61.00   1.00   30.00    --   20.25 -99.00 -30.00   86
  4  \w    -48.00  39.00   1.00   30.00    --   20.25 -57.00 -60.00   87
  5  \w      2.00  89.00   1.00   30.00    --   20.25  57.00-180.00   87
  6  \w      2.00  89.00   1.00   30.00    --   20.25  57.00 -90.00   87
  7  \w    -50.00  43.00   1.00   30.00    --   20.25 -38.00  30.00   93
  8  \w    -37.00  50.00   1.00   30.00    --  -18.53  57.00 150.00   87
  9  \w    -25.00  22.00   1.00   30.00    --  -18.53 -99.00 -90.00   47
 10  \w    -93.00 -32.00   1.00   30.00    --  -18.53 179.00 120.00   61
 11  \w    -25.00  61.00   1.00   30.00    --   20.25 -99.00  30.00   86
 12  \w      2.00  89.00   1.00   30.00    --   20.25  57.00  90.00   87
 13  \w     34.00  94.00   1.00   30.00    --   20.25 179.00 -90.00   60
 14  \w    -12.00  47.00   1.00   30.00    --   20.25-114.00 174.00   59
;
_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      0.0029396000
_diffrn_orient_matrix_UB_12      0.0232024000
_diffrn_orient_matrix_UB_13      0.0184447000
_diffrn_orient_matrix_UB_21      0.0046040000
_diffrn_orient_matrix_UB_22      -0.0281896000
_diffrn_orient_matrix_UB_23      0.0154557000
_diffrn_orient_matrix_UB_31      0.0336244000
_diffrn_orient_matrix_UB_32      0.0018457000
_diffrn_orient_matrix_UB_33      0.0043023000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            218483
_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         2.800
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.357
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.955
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_description       block
_exptl_crystal_F_000             4392
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.484
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1262
_refine_ls_number_reflns         19685
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0498P)^2^+19.3178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1016
_refine_ls_wR_factor_ref         0.1164
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12561
_reflns_number_total             19685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           p16121_087mono
_cod_depositor_comments
'Adding full bibliography for 7049530--7049539.cif.'
_cod_database_code               7049538
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H100 B3 O3 U'
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.784
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.06
_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. Uiso/Uaniso restraints and constraints
C740 \\sim C741 \\sim C742: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1S \\sim C2S \\sim C3S \\sim C4S \\sim C5S \\sim C6S: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C740, C741, C742
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1S, C2S, C3S, C4S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
 C560(H560), C360(H360), C440(H440), C620(H620), C760(H760), C140(H140),
 C160(H160), C460(H460), C420(H420), C720(H720), C840(H840), C220(H220),
 C640(H640), C860(H860), C120(H120), C260(H260), C660(H660), C820(H820),
 C740(H740), C540(H540), C320(H320), C240(H240), C520(H520), C340(H340)
4.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C23(H23), C33(H33), C45(H45), C73(H73), C63(H63), C25(H25),
 C83(H83), C65(H65), C85(H85), C55(H55), C35(H35), C15(H15), C75(H75), C13(H13),
  C53(H53), C6S(H6S), C2S(H2S), C3S(H3S), C4S(H4S), C5S(H5S)
4.c Fitted hexagon refined as free rotating group:
 C6S(C1S,C2S,C3S,C4S,C5S)
4.d Idealised Me refined as rotating group:
 C421(H42A,H42B,H42C), C621(H62A,H62B,H62C), C762(H76A,H76B,H76C), C521(H52A,
 H52B,H52C), C122(H12A,H12B,H12C), C262(H26A,H26B,H26C), C341(H34A,H34B,H34C),
 C822(H82A,H82B,H82C), C142(H14A,H14B,H14C), C221(H22A,H22B,H22C), C361(H36A,
 H36B,H36C), C661(H66A,H66B,H66C), C721(H72A,H72B,H72C), C222(H22D,H22E,H22F),
 C541(H54A,H54B,H54C), C322(H32A,H32B,H32C), C761(H76D,H76E,H76F), C261(H26D,
 H26E,H26F), C162(H16A,H16B,H16C), C422(H42D,H42E,H42F), C862(H86A,H86B,H86C),
 C622(H62D,H62E,H62F), C861(H86D,H86E,H86F), C522(H52D,H52E,H52F), C442(H44A,
 H44B,H44C), C462(H46A,H46B,H46C), C362(H36D,H36E,H36F), C842(H84A,H84B,H84C),
 C342(H34D,H34E,H34F), C562(H56A,H56B,H56C), C542(H54D,H54E,H54F), C662(H66D,
 H66E,H66F), C242(H24A,H24B,H24C), C461(H46D,H46E,H46F), C321(H32D,H32E,H32F),
 C641(H64A,H64B,H64C), C441(H44D,H44E,H44F), C722(H72D,H72E,H72F), C121(H12D,
 H12E,H12F), C642(H64D,H64E,H64F), C561(H56D,H56E,H56F), C141(H14D,H14E,H14F),
 C241(H24D,H24E,H24F), C821(H82D,H82E,H82F), C742(H74A,H74B,H74C), C841(H84D,
 H84E,H84F), C161(H16D,H16E,H16F), C741(H74D,H74E,H74F), C7S(H7SA,H7SB,H7SC)
;
_shelx_res_checksum              22876
_shelx_fab_checksum              56033
_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 1.155
_oxdiff_exptl_absorpt_empirical_full_min 0.864