Utility of the 1,3,4,6,7,8-Hexahydro-2H-pyrimido[1,2-a]pyrimidinato Ligand, (hpp)−, in Stabilizing Uranium Metallocene Mono-Alkyl and “Tuck-in” Complexes
Montalvo, Elizabeth; Ziller, Joseph W.; DiPasquale, Antonio G.; Rheingold, Arnold L.; Evans, William J.; Organometallics 29 (2010) 2104–; doi:10.1021/om100076s

data_4065689
_publ_section_title
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 Utility of the 1,3,4,6,7,8-Hexahydro-2H-pyrimido[1,2-a]pyrimidinato
 Ligand, (hpp)&#x2212;, in Stabilizing Uranium Metallocene Mono-Alkyl and
 &#x201C;Tuck-in&#x201D; Complexes
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_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2104
_journal_paper_doi               10.1021/om100076s
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C42 H55 N3 U'
_chemical_formula_weight         839.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4437(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4092(11)
_cell_length_b                   10.3444(11)
_cell_length_c                   34.255(4)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.26
_cell_volume                     3687.3(7)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0189
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            39714
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    4.434
_exptl_absorpt_correction_T_max  0.4561
_exptl_absorpt_correction_T_min  0.3596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.253
_refine_diff_density_min         -2.907
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.341
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         8123
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.341
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+30.4607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1003
_reflns_number_gt                7731
_reflns_number_total             8123
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100076s_si_001.cif
_cod_data_source_block           em33
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      P2(1)/n
_cod_database_code               4065689