Reactivity of U3+Metallocene Allyl Complexes Leads to a Nanometer-Sized Uranium Carbonate, [(C5Me5)2U]6(μ-κ1:κ2-CO3)6
Webster, Christopher L.; Ziller, Joseph W.; Evans, William J.; Organometallics 32 (2013) 4820–; doi:10.1021/om400526h

data_4081304
_publ_section_title
;
 Reactivity of U3+Metallocene Allyl Complexes Leads to a Nanometer-Sized
 Uranium Carbonate, [(C5Me5)2U]6(\m-\k1:\k2-CO3)6
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4820
_journal_paper_doi               10.1021/om400526h
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C132 H186 O18 U6'
_chemical_formula_weight         3488.98
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   31.339(2)
_cell_length_b                   31.339(2)
_cell_length_c                   10.9920(8)
_cell_measurement_reflns_used    9150
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.25
_cell_volume                     9349.3(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0145
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30788
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.249
_diffrn_reflns_theta_min         1.999
_exptl_absorpt_coefficient_mu    7.830
_exptl_absorpt_correction_T_max  0.2791
_exptl_absorpt_correction_T_min  0.1612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.859
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5022
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.136
_refine_diff_density_max         4.202
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+52.3120P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0765
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3355
_reflns_number_total             3759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400526h_si_002.cif
_cod_data_source_block           clw40
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        9349.4(15)
_cod_database_code               4081304
_shelx_estimated_absorpt_t_min   0.158
_shelx_estimated_absorpt_t_max   0.416
_shelxl_version_number           2012-9
_shelx_res_checksum              37662
_shelx_hkl_checksum              62869