Heterodinuclear Uranium/Molybdenum Dinitrogen Complexes
Aaron L. Odom; Polly L. Arnold; Christopher C. Cummins; Journal of the American Chemical Society 120 (1998) 5836–5837; doi:10.1021/ja980095t

data_4116724
_publ_contact_author
;
    Christopher C. Cummins
    Massachusetts Institute of Technology
    Department of Chemistry
    77 Massachusetts Ave.
    Cambridge, MA 02139-4307
    USA
;
_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_fax         '(1) 617 253 7030'
_publ_contact_author_phone       '(1) 617 253 5332'
_publ_section_title
;
 Heterodinuclear Uranium/Molybdenum Dinitrogen Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5836
_journal_page_last               5837
_journal_paper_doi               10.1021/ja980095t
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C66 H96 Mo N8 U'
_chemical_formula_weight         1335.48
_chemical_name_systematic
;
tris(N-tert-butyl-3,5-dimethylanilido)uranium-m-dinitrogen-
tris(N-tert-butyl-anilido)molybdenum
;
_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
_cell_angle_alpha                71.6570(10)
_cell_angle_beta                 89.0980(10)
_cell_angle_gamma                76.25
_cell_formula_units_Z            2
_cell_length_a                   10.9037(2)
_cell_length_b                   15.6529(2)
_cell_length_c                   20.3828(4)
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      23.29
_cell_measurement_theta_min      1.47
_cell_volume                     3200.85(10)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0511
_diffrn_reflns_av_sigmaI/netI    0.0631
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            12985
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    2.767
_exptl_absorpt_correction_type   'semi-empirical from pseudo-psi-scans'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       plate
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.767
_refine_diff_density_min         -1.242
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       0.00042(12)
_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_all   1.235
_refine_ls_goodness_of_fit_obs   1.194
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         8895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_restrained_S_obs      1.194
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_obs          0.0610
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+45.9562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1401
_refine_ls_wR_factor_obs         0.1255
_reflns_number_observed          7727
_reflns_number_total             8896
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja980095t_2.cif
_cod_data_source_block           f
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+45.9562P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+45.9562P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3200.82(10)
_cod_original_sg_symbol_H-M      'P 1'
_cod_database_code               4116724