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_4065692
_publ_section_title
;
 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            'C27 H41 N3 U'
_chemical_formula_weight         645.66
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                82.0205(10)
_cell_angle_beta                 84.9103(10)
_cell_angle_gamma                67.1607(10)
_cell_formula_units_Z            2
_cell_length_a                   8.6188(8)
_cell_length_b                   9.2322(9)
_cell_length_c                   17.4294(16)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      28.60
_cell_measurement_theta_min      2.41
_cell_volume                     1264.8(2)
_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      103(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14730
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    6.435
_exptl_absorpt_correction_T_max  0.2754
_exptl_absorpt_correction_T_min  0.1730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.895
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5818
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+3.2918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0550
_reflns_number_gt                5692
_reflns_number_total             5818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100076s_si_001.cif
_cod_data_source_block           em28
_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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap & geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4065692