Insertion Reactivity of CO2, PhNCO, Me3CC≡N, and Me3CN≡C with the Uranium−Alkynyl Bonds in (C5Me5)2U(C≡CPh)2
Evans, William J.; Walensky, Justin R.; Ziller, Joseph W.; Organometallics 29 (2010) 945–; doi:10.1021/om901006t

data_4067536
_publ_section_title
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 Insertion Reactivity of CO2, PhNCO, Me3CC\\tb N, and Me3CN\\tb C with the
 Uranium&#x2212;Alkynyl Bonds in (C5Me5)2U(C\\tb CPh)2
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_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              945
_journal_paper_doi               10.1021/om901006t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C48 H63 N2 O0.5 U'
_chemical_formula_weight         914.03
_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           SHELXTL
_cell_angle_alpha                76.1631(13)
_cell_angle_beta                 87.8792(14)
_cell_angle_gamma                73.2747(13)
_cell_formula_units_Z            2
_cell_length_a                   10.2805(11)
_cell_length_b                   14.6471(15)
_cell_length_c                   15.5586(16)
_cell_measurement_reflns_used    9128
_cell_measurement_temperature    148(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.24
_cell_volume                     2177.3(4)
_computing_cell_refinement       'Bruker SMART APEX2/SAINT'
_computing_data_collection       'Bruker SMART APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      148(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'phi and omega'
_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  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23208
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    3.761
_exptl_absorpt_correction_T_max  0.7529
_exptl_absorpt_correction_T_min  0.4413
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             922
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.316
_refine_diff_density_min         -1.045
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         8832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0419
_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^)+(0.0755P)^2^+2.2342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                7924
_reflns_number_total             8832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om901006t_si_002.cif
_cod_data_source_block           (C5Me5)2U[N=CCMe3(CCPh)]2
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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-1
_cod_original_formula_sum        'C48 H63 N2 O0.50 U'
_cod_database_code               4067536