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_4122213
_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         'C42 H52 B3 N8 U2, C16 H32 Li1 O4, 3(C4 H8 O1)'
_chemical_formula_sum            'C70 H108 B3 Li N8 O7 U2'
_chemical_formula_weight         1676.98
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.5880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.22340(10)
_cell_length_b                   17.8038(2)
_cell_length_c                   14.22880(10)
_cell_measurement_reflns_used    70537
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      76.1130
_cell_measurement_theta_min      3.9470
_cell_volume                     3602.98(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    ORTEP
_computing_publication_material  MERCURY
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            119820
_diffrn_reflns_theta_full        76.71
_diffrn_reflns_theta_max         76.71
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    12.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            BLACK
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1660
_exptl_crystal_size_max          0.1286
_exptl_crystal_size_mid          0.1237
_exptl_crystal_size_min          0.0765
_refine_diff_density_max         2.281
_refine_diff_density_min         -1.195
_refine_diff_density_rms         0.157
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.474(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     824
_refine_ls_number_reflns         15028
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+25.2513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1003
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                14418
_reflns_number_total             15028
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja504835a_si_002.cif
_cod_data_source_block           '[Li(THF)4][(UBH4)2(u-BH4)L(Me)]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4122212--4122215.cif.
;
_cod_original_formula_moiety     'C42 H40 B3 N8 U2, C16 H32 Li1 O4, 3(C4 H8 O1)'
_cod_original_formula_sum        'C70 H96 B3 Li N8 O7 U2'
_cod_database_code               4122213