The Bis Metallacyclic Anion [U(N{SiMe3}2)(CH2SiMe2N{SiMe3})2]-
Olivier Bénaud; Jean-Claude Berthet; Pierre Thuéry; Michel Ephritikhine; Inorganic Chemistry 49 (2010) 8117–8130; doi:10.1021/ic1012044

data_4316461
_publ_section_title
;
 The Bis Metallacyclic Anion [U(N{SiMe3}2)(CH2SiMe2N{SiMe3})2]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8117
_journal_page_last               8130
_journal_paper_doi               10.1021/ic1012044
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C30 H72 N3 Na O7 Si6 U'
_chemical_formula_weight         1016.47
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.147(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.9607(19)
_cell_length_b                   11.0587(5)
_cell_length_c                   24.2187(11)
_cell_measurement_reflns_used    318661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.92
_cell_volume                     9639.6(8)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(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
'two \f and eight \w scans with 2\% steps (672 frames)'
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.0940
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            318661
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.92
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.565
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_correction_T_min  0.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.309
_refine_diff_density_min         -1.183
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     897
_refine_ls_number_reflns         18244
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0665P)^2^+3.7729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1442
_reflns_number_gt                10732
_reflns_number_total             18244
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1012044_si_002_08.cif
_cod_data_source_block           5c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4316461