A dinuclear uranium(IV) complex of the chelating ligand 1,2,3,4-tetramethyl-5-(2-pyridyl)cyclopentadiene
Le Borgne, Thierry; Thuéry, Pierre; Ephritikhine, Michel; Acta Crystallographica Section C 58 (2002) m8–m9; doi:10.1107/S0108270101016961

data_2012409
_publ_section_title
;
 A dinuclear uranium(IV) complex of the chelating ligand
 1,2,3,4-tetramethyl-5-(2-pyridyl)cyclopentadiene
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m8
_journal_page_last               m9
_journal_paper_doi               10.1107/S0108270101016961
_journal_volume                  58
_journal_year                    2002
_chemical_formula_moiety         'C36 H52 Cl2 N2 O4 U2'
_chemical_formula_sum            'C36 H52 Cl2 N2 O4 U2'
_chemical_formula_weight         1123.76
_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                 106.420(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6695(8)
_cell_length_b                   18.2129(12)
_cell_length_c                   19.1940(13)
_cell_measurement_reflns_used    20390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      3.15
_cell_volume                     3913.0(5)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'kappaCCD software (Nonius, 1997)'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL (Bruker, 1997)'
_computing_publication_material  'SHELXTL and PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full .953
_diffrn_measured_fraction_theta_max .953
_diffrn_measurement_device_type  'Nonius kappaCCD'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .093
_diffrn_reflns_av_sigmaI/netI    .103
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20386
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         3.15
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    8.441
_exptl_absorpt_correction_T_max  .430
_exptl_absorpt_correction_T_min  .108
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'PLATON DELABS (Spek, 2000)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.908
_exptl_crystal_density_meas      ?
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .10
_refine_diff_density_max         .81
_refine_diff_density_min         -1.13
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .917
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         7087
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      .908
_refine_ls_R_factor_all          .290
_refine_ls_R_factor_gt           .0866
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0166P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          .117
_refine_ls_wR_factor_ref         .184
_reflns_number_gt                2097
_reflns_number_total             7087
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bm1473.cif
_cod_data_source_block           (I)
_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_sg_symbol_H-M      'P 21/c'
_cod_database_code               2012409