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_4081276
_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         'C35 H59 I N3 Si2 U'
_chemical_formula_sum            'C35 H59 I N3 Si2 U'
_chemical_formula_weight         942.96
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     heavy
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_audit_creation_method           SHELXL-2012
_cell_angle_alpha                87.864(3)
_cell_angle_beta                 76.519(3)
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_cell_formula_units_Z            2
_cell_length_a                   11.3021(4)
_cell_length_b                   11.9853(4)
_cell_length_c                   16.7492(5)
_cell_measurement_reflns_used    15077
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.24
_cell_measurement_theta_min      4.04
_cell_volume                     2015.15(13)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
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'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'
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_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.977
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25505
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.410
_diffrn_reflns_theta_min         4.038
_exptl_absorpt_coefficient_mu    18.097
_exptl_absorpt_correction_T_max  0.466
_exptl_absorpt_correction_T_min  0.225
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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            'dark blue'
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       block
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.178
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.081
_refine_diff_density_max         5.38
_refine_diff_density_min         -2.17
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         8020
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.047P)^2^+9.275P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0914
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7747
_reflns_number_total             8020
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400435b_si_001.cif
_cod_data_source_block           6
_cod_original_cell_volume        2015.15(12)
_cod_database_code               4081276
_nottingham_internal_coll_name   UAWALR
_nottingham_internal_coll_number 11944
_nottingham_internal_coll_client AW
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_time '10 and 40'
_nottingham_internal_coll_frame_width 1
_nottingham_internal_coll_frame_method '\w scans'
_nottingham_internal_coll_user   WL/AW
_nottingham_internal_coll_date   22/10/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user AW
_nottingham_internal_process_date 23/10/2012
_nottingham_internal_solution_user AW
_nottingham_internal_solution_date 23/10/2012
_nottingham_internal_refinement_user AW
_nottingham_internal_refinement_date 23/10/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 15/1/2013
_shelx_estimated_absorpt_t_min   0.141
_shelx_estimated_absorpt_t_max   0.323
_diffrn_reflns_sigmai/neti       0.029