Superbases in Confined Space: Control of the Basicity and Reactivity of the Proton Transfer
Bastien Chatelet; Heinz Gornitzka; Véronique Dufaud; Erwann Jeanneau; Jean-Pierre Dutasta; Alexandre Martinez; Journal of the American Chemical Society 135 (2013) 18659–18664; doi:10.1021/ja409444s

data_4121283
_publ_section_title
;
 Superbases in Confined Space: Control of the Basicity and Reactivity of
 the Proton Transfer
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18659
_journal_page_last               18664
_journal_paper_doi               10.1021/ja409444s
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C63.5 H76.5 N7 O9 P1.5'
_chemical_formula_weight         1128.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.237(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.554(8)
_cell_length_b                   19.781(11)
_cell_length_c                   21.193(13)
_cell_measurement_temperature    180(2)
_cell_volume                     5761(6)
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            97909
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         5.12
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.127
_exptl_absorpt_correction_T_max  0.9937
_exptl_absorpt_correction_T_min  0.9751
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       plate
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         12303
_refine_ls_number_restraints     202
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+3.9174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                9130
_reflns_number_total             12303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409444s_si_003.cif
_cod_data_source_block           basealex
_cod_original_cell_volume        5760(6)
_cod_original_formula_sum        'C63.50 H76.50 N7 O9 P1.50'
_cod_database_code               4121283