Superbasicity of a Bis-guanidino Compound with a Flexible Linker: A Theoretical and Experimental Study
Martyn P. Coles; Pedro J. Aragón-Sáez; Sarah H. Oakley; Peter B. Hitchcock; Matthew G. Davidson; Zvonimir B. Maksić; Robert Vianello; Ivo Leito; Ivari Kaljurand; David C. Apperley; Journal of the American Chemical Society 131 (2009) 16858–16868; doi:10.1021/ja906618g

data_4105363
_publ_contact_author_address
;Department of Chemistry
University of Sussex
Falmer
Brighton BN1 9QJ
UK
;
_publ_contact_author_email       m.p.coles@sussex.ac.uk
_publ_contact_author_name        'Martyn P. Coles'
_publ_section_title
;
 Superbasicity of a Bis-guanidino Compound with a Flexible Linker: A
 Theoretical and Experimental Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16858
_journal_page_last               16868
_journal_paper_doi               10.1021/ja906618g
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C39 H47 B N6'
_chemical_formula_weight         610.64
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
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_cell_angle_beta                 99.7700(10)
_cell_angle_gamma                100.197(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2719(3)
_cell_length_b                   12.4868(3)
_cell_length_c                   14.3087(5)
_cell_measurement_reflns_used    15334
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      36.32
_cell_measurement_theta_min      3.59
_cell_volume                     1644.02(9)
_computing_cell_refinement       'HKL Scalepack (Otwinski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo & Scalepack (Otwinski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       ccd
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42994
_diffrn_reflns_theta_full        36.32
_diffrn_reflns_theta_max         36.32
_diffrn_reflns_theta_min         3.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Nonius Kappa CCD'
_exptl_absorpt_coefficient_mu    0.073
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         15334
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+0.2827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1269
_refine_ls_wR_factor_ref         0.1421
_reflns_number_gt                12207
_reflns_number_total             15334
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906618g_si_003.cif
_cod_data_source_block           Compound1B@110K
_cod_original_cell_volume        1644.02(8)
_cod_database_code               4105363