From Bent to Linear Uranium Metallocenes: Influence of Counterion, Solvent, and Metal Ion Oxidation State
Maynadié, Jérôme; Berthet, Jean-Claude; Thuéry, Pierre; Ephritikhine, Michel; Organometallics 25 (2006) 5603–5611; doi:10.1021/om060642g

data_4074443
_publ_section_title
;
 From Bent to Linear Uranium Metallocenes: Influence of
 Counterion, Solvent, and Metal Ion Oxidation State
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5603
_journal_page_last               5611
_journal_paper_doi               10.1021/om060642g
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C70 H108 F18 Na2 O24 S6 U2'
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_symmetry_space_group_name_Hall  '-P 2ac 2ab'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.475(3)
_cell_length_b                   9.9062(7)
_cell_length_c                   30.888(4)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.98
_cell_volume                     9018.8(16)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'one \f and seven \w scans with 2\% steps'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_sigmaI/netI    0.1336
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            168083
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.841
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_correction_T_min  0.509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       needle
_exptl_crystal_F_000             4736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.372
_refine_diff_density_min         -0.853
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         8527
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0505P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                4396
_reflns_number_total             8527
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           10.2(CH~2~)~4~O
_cod_database_code               4074443