Double uranium oxo cations derived from uranyl by borane or silane reduction.
Cowie, Bradley E.; Nichol, Gary S.; Love, Jason B.; Arnold, Polly L.; Chemical communications (Cambridge, England) 54 (2018) 3839–3842; doi:10.1039/c8cc00341f

data_7121462
_publ_section_title
;
 Double uranium oxo cations derived from uranyl by borane or silane
 reduction.
;
_journal_issue                   31
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3839
_journal_page_last               3842
_journal_paper_doi               10.1039/c8cc00341f
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C74 H62 N10 O3 U2, 4(C4 H8 O), C6 H14'
_chemical_formula_sum            'C96 H108 N10 O7 U2'
_chemical_formula_weight         1990.0461
_chemical_name_systematic
;
 [{(py)UO(u-C6H4O2)U(py)}(LA)]
;
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-12-20 deposited with the CCDC.
2018-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(2)
_cell_angle_beta                 105.081(2)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            2
_cell_length_a                   14.0792(3)
_cell_length_b                   21.2447(5)
_cell_length_c                   14.5359(3)
_cell_measurement_reflns_used    24758
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.8540
_cell_measurement_theta_min      3.0460
_cell_volume                     4198.07(16)
_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    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 5.1574
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -32.00  63.00   1.00   15.00    --   -9.43  38.00 150.00   95
  2  \w    -20.00  30.00   1.00   15.00    --   -9.43 -99.00  60.00   50
  3  \w    -20.00  30.00   1.00   15.00    --   -9.43 -99.00 -30.00   50
  4  \w    -52.00  -5.00   1.00   15.00    --   -9.43 103.00 -75.44   47
  5  \w    -32.00  63.00   1.00   15.00    --   -9.43  38.00-180.00   95
  6  \w     16.00  85.00   1.00   15.00    --   10.92-153.00  90.37   69
  7  \w    -59.00  38.00   1.00   15.00    --   10.92 -57.00   0.00   97
  8  \w    -62.00  33.00   1.00   15.00    --   10.92 -38.00 -90.00   95
  9  \w    -44.00  38.00   1.00   15.00    --   10.92 -57.00-150.00   82
 10  \w    -62.00 -28.00   1.00   15.00    --   10.92 -38.00  30.00   34
 11  \w      7.00  38.00   1.00   15.00    --   10.92 -57.00  30.00   31
 12  \w    -50.00   6.00   1.00   15.00    --   10.92 -38.00 -30.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            86045
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    3.918
_exptl_absorpt_correction_T_max  0.6953
_exptl_absorpt_correction_T_min  0.3579
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.331
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.105
_platon_squeeze_details
;
;
_refine_diff_density_max         1.900
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         8803
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+11.3692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                7424
_reflns_number_total             8803
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8cc00341f2.cif
_cod_data_source_block           4_4THF_hexane
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121458--7121462.cif.
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7121462