Complexes of Triamidoamines with the Early Actinides. Synthetic Routes to Monomeric Compounds of Tetravalent Uranium and Thorium Containing Halide and Amide Ligands
Paul Roussel; Nathaniel W. Alcock; Rita Boaretto; Andrew J. Kingsley; Ian J. Munslow; Christopher J. Sanders; Peter Scott; Inorganic Chemistry 38 (1999) 3651–3656; doi:10.1021/ic990563f

data_4322194
_publ_section_title
;
 Complexes of Triamidoamines with the Early Actinides. Synthetic Routes to
 Monomeric Compounds of Tetravalent Uranium and Thorium Containing Halide
 and Amide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3651
_journal_page_last               3656
_journal_paper_doi               10.1021/ic990563f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C28 H67 N5 Si3 U'
_chemical_formula_weight         796.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.2170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0133(15)
_cell_length_b                   23.364(3)
_cell_length_c                   16.599(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     3843.5(10)
_computing_structure_refinement  'SHELXL-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.1026
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22995
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    4.339
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       Block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.710
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.909
_refine_ls_goodness_of_fit_obs   1.019
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         8926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_restrained_S_obs      1.019
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_obs          0.0435
_refine_ls_shift/esd_max         0.078
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0918
_refine_ls_wR_factor_obs         0.0797
_reflns_number_observed          5463
_reflns_number_total             8926
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990563f_4.cif
_cod_data_source_block           snm
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322194