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_4081272
_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         'C70 H106 Cs2 N4, 2 (C6 D6)'
_chemical_formula_sum            'C82 H106 Cs2 D12 N4'
_chemical_formula_weight         1437.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   'geom, Me from difmap'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.579(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.632(5)
_cell_length_b                   20.003(5)
_cell_length_c                   19.594(5)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.29
_cell_volume                     7658(3)
_computing_cell_refinement       'Bruker SAINT version 6.36A (Bruker, 2000)'
_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  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 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  0.094
_diffrn_reflns_av_sigmaI/netI    0.127
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39059
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2'
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.13
_refine_diff_density_min         -1.53
_refine_diff_density_rms         0.14
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.11
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         13451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.11
_refine_ls_R_factor_all          0.134
_refine_ls_R_factor_gt           0.0617
_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^)+25.70P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.094
_refine_ls_wR_factor_ref         0.113
_reflns_number_gt                7768
_reflns_number_total             13451
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400435b_si_001.cif
_cod_data_source_block           2a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4081272
_nottingham_internal_coll_name   CSAWLA
_nottingham_internal_coll_number 11860
_nottingham_internal_coll_client AW
_nottingham_internal_coll_type   hemisphere
_nottingham_internal_coll_frame_time 50
_nottingham_internal_coll_frame_width 0.3
_nottingham_internal_coll_frame_method \w
_nottingham_internal_coll_user   AW
_nottingham_internal_coll_date   17/09/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user AW/WL
_nottingham_internal_process_date 18/09/2012
_nottingham_internal_solution_user AW
_nottingham_internal_solution_date 18/09/2012
_nottingham_internal_refinement_user AW
_nottingham_internal_refinement_date 18/09/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 12/1/2013