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_7049534
_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         'C36 H76 B N3 O Si6 U'
_chemical_formula_sum            'C36 H76 B N3 O Si6 U'
_chemical_formula_weight         984.37
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-12-06
_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                102.222(2)
_cell_angle_beta                 98.2700(10)
_cell_angle_gamma                90.1220(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0703(2)
_cell_length_b                   13.1641(2)
_cell_length_c                   15.6746(3)
_cell_measurement_reflns_used    20349
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0100
_cell_measurement_theta_min      3.4180
_cell_volume                     2407.48(7)
_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 0.999
_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  22.00   1.00   10.00    --  -18.68 -99.00  30.00   47
  2  \w    -93.00 -34.00   1.00   10.00    --  -18.68-179.00 -30.00   59
  3  \w    -25.00  22.00   1.00   10.00    --  -18.68 -99.00-120.00   47
  4  \w    -49.00  49.00   1.00   10.00    --   20.40 -77.00 150.00   98
  5  \w      2.00  89.00   1.00   10.00    --   20.40  57.00   0.00   87
  6  \w     34.00  95.00   1.00   10.00    --   20.40 179.00 -60.00   61
  7  \w    -18.00  93.00   1.00   10.00    --   20.40  19.00 -60.00  111
  8  \w    -87.00   0.00   1.00   10.00    --  -18.68 -57.00 150.00   87
  9  \w    -25.00  22.00   1.00   10.00    --  -18.68 -99.00 120.00   47
 10  \w    -25.00  61.00   1.00   10.00    --   20.40 -99.00-120.00   86
 11  \w    -25.00  61.00   1.00   10.00    --   20.40 -99.00   0.00   86
 12  \w      2.00  89.00   1.00   10.00    --   20.40  57.00  90.00   87
 13  \w    -48.00  39.00   1.00   10.00    --   20.40 -57.00 -60.00   87
 14  \w    -14.00  68.00   1.00   10.00    --   20.40-112.00 134.08   82
;
_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      0.0431569000
_diffrn_orient_matrix_UB_12      -0.0270313000
_diffrn_orient_matrix_UB_13      -0.0206338000
_diffrn_orient_matrix_UB_21      0.0318861000
_diffrn_orient_matrix_UB_22      0.0015946000
_diffrn_orient_matrix_UB_23      0.0419951000
_diffrn_orient_matrix_UB_31      -0.0255137000
_diffrn_orient_matrix_UB_32      -0.0480589000
_diffrn_orient_matrix_UB_33      0.0014872000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51203
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.964
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48247
_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_density_diffrn    1.358
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.792
_exptl_crystal_size_mid          0.334
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         9835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+0.9968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0533
_refine_ls_wR_factor_ref         0.0552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8900
_reflns_number_total             9835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt05051a2.cif
_cod_data_source_block           p18053_tri
_cod_depositor_comments
;
Adding full bibliography for 7049530--7049539.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C36 H76 B N3 O Si6 U)'
_cod_original_formula_sum        'C72 H152 B2 N6 O2 Si12 U2'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     1968.75
_cod_database_code               7049534
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'U1 C100 H100 B3 O3'
_reflns_odcompleteness_completeness 99.86
_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:
 C124(H124), C4AA(H4AA), C2AA(H2AA), C115(H115)
2.b Idealised Me refined as rotating group:
 C123(H12A,H12B,H12C), C351(H35A,H35B,H35C), C113(H11A,H11B,H11C), C242(H24A,
 H24B,H24C), C122(H12D,H12E,H12F), C112(H11D,H11E,H11F), C243(H24D,H24E,H24F),
 C362(H36A,H36B,H36C), C352(H35D,H35E,H35F), C128(H12G,H12H,H12I), C121(H12J,
 H12K,H12L), C232(H23A,H23B,H23C), C126(H12M,H12N,H12O), C363(H36D,H36E,H36F),
 C111(H11G,H11H,H11I), C361(H36G,H36H,H36I), C353(H35G,H35H,H35I), C117(H11J,
 H11K,H11L), C241(H24G,H24H,H24I), C119(H11M,H11N,H11O), C231(H23D,H23E,H23F),
 C233(H23G,H23H,H23I), C127(H12P,H12Q,H12R), C118(H11P,H11Q,H11R)
;
_shelx_res_checksum              66908
_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 1.603
_oxdiff_exptl_absorpt_empirical_full_min 0.711