A Versatile Methodology for the Regioselective C(8)-Metalation of Purine Bases.
Brackemeyer, Dirk; Hervé, Alexandre; Schulte To Brinke, Christian; Jahnke, Mareike C.; Hahn, F. Ekkehardt; Journal of the American Chemical Society 136 (2014) 7841–; doi:10.1021/ja5030904

data_4121863
_publ_section_title
;
 A Versatile Methodology for the Regioselective C(8)-Metalation of Purine
 Bases.
;
_journal_issue                   22
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7841
_journal_paper_doi               10.1021/ja5030904
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'(C42 H37 Br N5 P2 Pt), (B F4), 0.5(C H2 Cl2)'
_chemical_formula_sum            'C42.5 H38 B Br Cl F4 N5 P2 Pt'
_chemical_formula_weight         1077.99
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                89.468(2)
_cell_angle_beta                 85.019(2)
_cell_angle_gamma                85.419(2)
_cell_formula_units_Z            4
_cell_length_a                   10.4325(3)
_cell_length_b                   20.1777(7)
_cell_length_c                   20.2332(6)
_cell_measurement_reflns_used    11555
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.9435
_cell_measurement_theta_min      2.261
_cell_volume                     4229.5(2)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0836
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61623
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.879
_diffrn_reflns_theta_min         1.012
_exptl_absorpt_coefficient_mu    4.456
_exptl_absorpt_correction_T_max  0.4142
_exptl_absorpt_correction_T_min  0.1266
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       prism
_exptl_crystal_F_000             2116
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.392
_refine_diff_density_min         -1.683
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1043
_refine_ls_number_reflns         20064
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0483
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+3.6505P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14304
_reflns_number_total             20064
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5030904_si_002.cif
_cod_data_source_block           '[6]BF4'
_cod_depositor_comments
'Adding full bibliography for 4121860--4121863.cif.'
_cod_original_formula_sum        'C42.50 H38 B Br Cl F4 N5 P2 Pt'
_cod_database_code               4121863
_shelxl_version_number           2013-4
_shelx_res_checksum              77425
_shelx_hkl_checksum              88491