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_4081271
_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         'C47 H77 K N2 O3'
_chemical_formula_sum            'C47 H77 K N2 O3'
_chemical_formula_weight         757.21
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.385(3)
_cell_length_b                   15.557(5)
_cell_length_c                   28.666(9)
_cell_measurement_reflns_used    8420
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.36
_cell_volume                     4631(2)
_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    'SHELXS97 (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 0.966
_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  0.092
_diffrn_reflns_av_sigmaI/netI    0.154
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            27495
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.153
_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    1.086
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.64
_refine_diff_density_min         -0.74
_refine_diff_density_rms         0.08
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(6)
_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     488
_refine_ls_number_reflns         10205
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.19
_refine_ls_R_factor_all          0.195
_refine_ls_R_factor_gt           0.0724
_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^)+(0.0001P)^2^+3.654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.104
_refine_ls_wR_factor_ref         0.131
_reflns_number_gt                5205
_reflns_number_total             10205
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400435b_si_001.cif
_cod_data_source_block           1a
_cod_original_sg_symbol_Hall     'P 2ac 2ab  '
_cod_database_code               4081271
_nottingham_internal_coll_name   KAWPLD
_nottingham_internal_coll_number 11568
_nottingham_internal_coll_client AW/STL
_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   21/06/2012
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_user AW
_nottingham_internal_process_date 22/06/2012
_nottingham_internal_solution_user AW
_nottingham_internal_solution_date 22/06/2012
_nottingham_internal_refinement_user AW
_nottingham_internal_refinement_date 22/06/2012
_nottingham_internal_validation_user AJB
_nottingham_internal_validation_date 14/1/2013