Organolutetium-Mediated Dearomatization and Functionalization of Pyrimidine Rings
Johnson, Kevin R. D.; Hayes, Paul G.; Organometallics 32 (2013) 4046–; doi:10.1021/om400413e

data_4081077
_publ_section_title
;
 Organolutetium-Mediated Dearomatization and Functionalization of
 Pyrimidine Rings
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4046
_journal_paper_doi               10.1021/om400413e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C112 H124 Lu2 N14 O P4 Si4'
_chemical_formula_weight         2268.43
_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           SHELXL-97
_cell_angle_alpha                95.886(2)
_cell_angle_beta                 103.004(2)
_cell_angle_gamma                95.355(2)
_cell_formula_units_Z            2
_cell_length_a                   16.935(2)
_cell_length_b                   18.699(2)
_cell_length_c                   20.754(3)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.29
_cell_measurement_theta_min      2.24
_cell_volume                     6323.7(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker 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      173(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0506
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            89676
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_T_max  0.7932
_exptl_absorpt_correction_T_min  0.5834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
The structure contained a severely disordered solvent molecule
in the asymmetric unit, for which no suitable model could be found. 
The electron density associated with the disordered regions was removed
using the SQUEEZE subroutine of PLATON, leaving a void of ca. 1133 A^3.
;
_refine_diff_density_max         3.124
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         27765
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.115
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1812
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                16247
_reflns_number_total             27765
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400413e_si_002.cif
_cod_data_source_block           Compound3
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081077