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_4081278
_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         'C64 H88 I2 N4 U2, 2(C7 H8)'
_chemical_formula_sum            'C78 H104 I2 N4 U2'
_chemical_formula_weight         1827.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 124.089(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.2666(16)
_cell_length_b                   12.9502(5)
_cell_length_c                   21.3847(11)
_cell_measurement_reflns_used    11685
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.4203
_cell_measurement_theta_min      3.7898
_cell_volume                     7400.3(9)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'enCIFer (Allen et al., 2004); PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.027
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20226
_diffrn_reflns_theta_full        67.49
_diffrn_reflns_theta_max         67.49
_diffrn_reflns_theta_min         5.49
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    19.090
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'DARK BLUE'
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       LATH
_exptl_crystal_F_000             3560
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         6.81
_refine_diff_density_min         -1.41
_refine_diff_density_rms         0.68
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.18
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         6654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.18
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0827
_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^)+(0.141P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.181
_refine_ls_wR_factor_ref         0.184
_reflns_number_gt                6227
_reflns_number_total             6654
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400435b_si_001.cif
_cod_data_source_block           8
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4081278
_nottingham_internal_coll_name   UAWALK
_nottingham_internal_coll_number 11767
_nottingham_internal_coll_client AW/STL
_nottingham_internal_coll_type   CUSTOM
_nottingham_internal_coll_frame_time '21 AND 84'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   AW
_nottingham_internal_coll_date   16/08/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user AW/WL
_nottingham_internal_process_date 17/08/2012
_nottingham_internal_solution_user AW
_nottingham_internal_solution_date 17/08/2012
_nottingham_internal_refinement_user AW
_nottingham_internal_refinement_date 17/08/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 15/1/2013