Bent and Linear Uranium(IV) Metallocenes with Terminal and Bridging Cyanide Ligands
Maynadié, Jérôme; Berthet, Jean-Claude; Thuéry, Pierre; Ephritikhine, Michel; Organometallics 26 (2007) 4585–4591; doi:10.1021/om7003173

data_4073421
_publ_section_title
;
 Bent and Linear Uranium(IV) Metallocenes with Terminal and Bridging
 Cyanide Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4585
_journal_page_last               4591
_journal_paper_doi               10.1021/om7003173
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C51 H93 N9 U'
_chemical_formula_weight         1070.37
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 118.949(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   38.6077(8)
_cell_length_b                   12.1228(4)
_cell_length_c                   38.4765(14)
_cell_measurement_reflns_used    228313
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.94
_cell_volume                     15758.2(9)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two \f and four \w 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  0.0819
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            228313
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.94
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    3.131
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.340
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            'translucent light orange'
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             6648
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.915
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1713
_refine_ls_number_reflns         29774
_refine_ls_number_restraints     71
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+42.7554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                23090
_reflns_number_total             29774
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7003173.cif
_cod_data_source_block           4.MeCN
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4073421