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_4121284
_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_moiety         'C30 H40 N4 O3 P, Cl, H2 O'
_chemical_formula_sum            'C30 H42 Cl N4 O4 P'
_chemical_formula_weight         589.11
_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   difmap
_atom_sites_solution_primary     direct
_cell_angle_alpha                83.500(5)
_cell_angle_beta                 78.831(5)
_cell_angle_gamma                83.766(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7981(7)
_cell_length_b                   10.3144(7)
_cell_length_c                   15.3068(8)
_cell_measurement_reflns_used    7986
_cell_measurement_temperature    150
_cell_measurement_theta_max      66.8850
_cell_measurement_theta_min      4.6020
_cell_volume                     1501.90(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.4678
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) x-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16849
_diffrn_reflns_theta_full        67.231
_diffrn_reflns_theta_max         67.231
_diffrn_reflns_theta_min         2.956
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.965
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       plate
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.059
_refine_diff_density_max         0.26
_refine_diff_density_min         -0.21
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9512
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5284
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.0003586
_refine_ls_shift/su_mean         0.0000652
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.101E+04 0.157E+04 793. 204. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0767
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0767
_reflns_limit_h_max              11
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4747
_reflns_number_total             5288
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            ja409444s_si_004.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C30 H42 Cl1 N4 O4 P1'
_cod_database_code               4121284