Regioselective C8-metalation of N-phosphine tethered adenine derivatives via C8-H activation.
Brackemeyer, D.; Schulte To Brinke, C.; Roelfes, F.; Hahn, F. E.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 4510–4513; doi:10.1039/c7dt00682a

data_7042336
_publ_section_title
;
 Regioselective C8-metalation of N-phosphine tethered adenine derivatives
 via C8-H activation.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4510
_journal_page_last               4513
_journal_paper_doi               10.1039/c7dt00682a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         '(C31 H36 N6 P Ru), Cl, 0.5(C2 H3 N)'
_chemical_formula_sum            'C32 H37.5 Cl N6.5 P Ru'
_chemical_formula_weight         680.67
_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-2014/7
_audit_update_record
;
2017-03-04 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                100.1770(10)
_cell_angle_beta                 91.9820(10)
_cell_angle_gamma                93.9450(10)
_cell_formula_units_Z            4
_cell_length_a                   10.4157(2)
_cell_length_b                   10.7643(3)
_cell_length_c                   29.2352(7)
_cell_measurement_reflns_used    14769
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      28.999
_cell_measurement_theta_min      2.601
_cell_volume                     3214.92(13)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_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  0.0390
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            53550
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.296
_diffrn_reflns_theta_min         2.475
_exptl_absorpt_coefficient_mu    0.653
_exptl_absorpt_correction_T_max  0.8612
_exptl_absorpt_correction_T_min  0.7847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       prism
_exptl_crystal_F_000             1404
_exptl_crystal_size_max          0.316
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.082
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1121
_refine_ls_number_reflns         17380
_refine_ls_number_restraints     739
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0334
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0310P)^2^+1.6515P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14135
_reflns_number_total             17380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00682a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7042336--7042339.cif.'
_cod_original_formula_sum        'C32 H37.50 Cl N6.50 P Ru'
_cod_database_code               7042336
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              2007