β-Diketiminate Derivatives of Alkali Metals and Uranium
Wooles, Ashley J.; Lewis, William; Blake, Alexander J.; Liddle, Stephen T.; Organometallics 32 (2013) 5058–; doi:10.1021/om400435b

data_4081275
_publ_section_title
;
 \b-Diketiminate Derivatives of Alkali Metals and Uranium
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              5058
_journal_paper_doi               10.1021/om400435b
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C39 H56 I N2 U'
_chemical_formula_sum            'C39 H56 I N2 U'
_chemical_formula_weight         917.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6738(13)
_cell_length_b                   18.0264(12)
_cell_length_c                   21.1293(14)
_cell_measurement_reflns_used    21574
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.36
_cell_volume                     7493.5(9)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_Laue_measured_fraction_full 0.999
_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       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            64631
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.523
_diffrn_reflns_theta_min         1.928
_exptl_absorpt_coefficient_mu    5.183
_exptl_absorpt_correction_T_max  0.123
_exptl_absorpt_correction_T_min  0.089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            'DARK BLUE'
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3592
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.29
_refine_diff_density_max         2.61
_refine_diff_density_min         -0.45
_refine_diff_density_rms         0.12
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.07
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     403
_refine_ls_number_reflns         8611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.07
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+4.0879P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0625
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7538
_reflns_number_total             8611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400435b_si_001.cif
_cod_data_source_block           5
_cod_database_code               4081275
_nottingham_internal_coll_name   UAWALT
_nottingham_internal_coll_number 11969
_nottingham_internal_coll_type   sphere
_nottingham_internal_coll_frame_time 25
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   AW
_nottingham_internal_coll_date   31/10/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user AW
_nottingham_internal_process_date 01/11/2012
_nottingham_internal_solution_user AW
_nottingham_internal_solution_date 01/11/2012
_nottingham_internal_refinement_user AW
_nottingham_internal_refinement_date 01/11/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 15/1/2013
_shelx_estimated_absorpt_t_min   0.231
_shelx_estimated_absorpt_t_max   0.315
_diffrn_reflns_sigmai/neti       0.020