New Chemistry from an Old Reagent: Mono- and Dinuclear Macrocyclic Uranium(III) Complexes from [U(BH4)3(THF)2].
Arnold, Polly L.; Stevens, Charlotte J.; Farnaby, Joy H.; Gardiner, Michael G.; Nichol, Gary S.; Love, Jason B.; Journal of the American Chemical Society 136 (2014) 10218–10221; doi:10.1021/ja504835a

data_4122212
_publ_section_title
;
 New Chemistry from an Old Reagent: Mono- and Dinuclear Macrocyclic
 Uranium(III) Complexes from [U(BH4)3(THF)2].
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10218
_journal_page_last               10221
_journal_paper_doi               10.1021/ja504835a
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C32 H40 B N2 U'
_chemical_formula_sum            'C32 H40 B N2 U'
_chemical_formula_weight         697.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                79.413(5)
_cell_angle_beta                 72.025(5)
_cell_angle_gamma                75.355(5)
_cell_formula_units_Z            2
_cell_length_a                   10.186(5)
_cell_length_b                   11.735(5)
_cell_length_c                   13.030(5)
_cell_measurement_reflns_used    20678
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      30.0490
_cell_measurement_theta_min      3.3020
_cell_volume                     1423.9(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    ortep
_computing_publication_material  mercury
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0235
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            38645
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    5.722
_exptl_absorpt_correction_T_max  0.227
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
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)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.9602
_exptl_crystal_size_mid          0.5317
_exptl_crystal_size_min          0.2900
_refine_diff_density_max         4.699
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6529
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+2.5479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                6173
_reflns_number_total             6529
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja504835a_si_002.cif
_cod_data_source_block           '[U(BH4)(L)]'
_cod_depositor_comments
'Adding full bibliography for 4122212--4122215.cif.'
_cod_original_formula_moiety     'C32 H36 B N2 U'
_cod_original_formula_sum        'C32 H36 B N2 U'
_cod_database_code               4122212