Synthesis and X-ray crystal structure of [Na(18-crown-6)][U(Cp*)2(SBut)(S)], the first f-element compound containing a metal‒sulfur double bond
Ventelon, Lionel; Lescop, Christophe; Arliguie, Thérèse; Ephritikhine, Michel; Leverd, Pascal C.; Lance, Monique; Nierlich, Martine; Chemical Communications  (1999) 659–; doi:10.1039/a900466a

data_7110453
_publ_section_title
;
 Synthesis and X-ray crystal structure of
 [Na(18-crown-6)][U(Cp*)2(SBut)(S)], the first f-element compound
 containing a metal--sulfur double bond
;
_journal_issue                   7
_journal_name_full               'Chemical Communications'
_journal_page_first              659
_journal_paper_doi               10.1039/a900466a
_journal_year                    1999
_chemical_formula_sum            'C36 H63 Na O6 S2 U'
_chemical_formula_weight         917.00
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.31(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.174(4)
_cell_length_b                   18.548(4)
_cell_length_c                   23.132(5)
_cell_measurement_reflns_used    'about 1000'
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.79
_cell_volume                     8006(3)
_computing_cell_refinement       'DENZO(Otwinowski& Minor,1997'
_computing_data_collection       'DENZO(Otwinowski& Minor,1997'
_computing_data_reduction        'DENZO(Otwinowski& Minor,1997'
_computing_molecular_graphics    'SHELXTL (Bruker,1997)'
_computing_publication_material  'SHELXTL (Bruker,1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1990)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measurement_device       'Nonius Kappa CCD diffractometer'
_diffrn_measurement_method       '\f rotation scans with 2\%steps'
_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  0.075
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31073
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         5.10
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    4.210
_exptl_absorpt_correction_type   no
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.782
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.970
_refine_ls_goodness_of_fit_obs   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     808
_refine_ls_number_reflns         8142
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.043
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_obs          0.0334
_refine_ls_shift/esd_max         -0.011
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0748
_refine_ls_wR_factor_obs         0.0641
_reflns_number_observed          5896
_reflns_number_total             8203
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            900466asup1.cif
_cod_data_source_block           struc
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0287P)^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^)+(0.0287P)^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 
;
_cod_original_cell_volume        8005.5(28)
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               7110453