Structure and reactions of a metallacyclic complex containing a remarkably long uranium‒carbon bond
Boaretto, Rita; Roussel, Paul; Kingsley, Andrew J.; Munslow, Ian J.; Sanders, Christopher J.; Alcock, Nathaniel W.; Scott, Peter; Chemical Communications  (1999) 1701–; doi:10.1039/a903783g

data_7110587
_publ_section_title
;
 Structure and reactions of a metallacyclic complex containing a
 remarkably long uranium--carbon bond
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1701
_journal_paper_doi               10.1039/a903783g
_journal_year                    1999
_chemical_formula_sum            'C24 H56 N4 Si3 U'
_chemical_formula_weight         723.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                119.3350(10)
_cell_angle_beta                 109.0980(10)
_cell_angle_gamma                92.8980(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7602(5)
_cell_length_b                   13.3286(5)
_cell_length_c                   13.3902(5)
_cell_measurement_reflns_used    9181
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      1.81
_cell_volume                     1813.56(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.878
_diffrn_measured_fraction_theta_max 0.878
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0755
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11113
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    4.590
_exptl_absorpt_correction_T_max  0.4604
_exptl_absorpt_correction_T_min  0.2074
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.834
_refine_diff_density_min         -4.478
_refine_diff_density_rms         0.220
_refine_ls_extinction_coef       0.0027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         8070
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1206
_reflns_number_gt                6567
_reflns_number_total             8070
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903783gsup1.cif
_cod_data_source_block           uch
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110587