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_4121282
_publ_section_title
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 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            'C75 H76 Cl19.25 N4 O11.75 P'
_chemical_formula_weight         1934.78
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.074(4)
_cell_angle_beta                 89.875(4)
_cell_angle_gamma                86.771(4)
_cell_formula_units_Z            4
_cell_length_a                   15.3011(17)
_cell_length_b                   19.814(2)
_cell_length_c                   30.622(3)
_cell_measurement_temperature    180(2)
_cell_volume                     8866.6(16)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.1924
_diffrn_reflns_av_sigmaI/netI    0.1297
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            244575
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         5.10
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  0.8778
_exptl_absorpt_correction_T_min  0.7308
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             3961
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2364
_refine_ls_number_reflns         25018
_refine_ls_number_restraints     2694
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.2236
_refine_ls_R_factor_gt           0.1446
_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^)+(0.0628P)^2^+124.9666P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3008
_refine_ls_wR_factor_ref         0.3392
_reflns_number_gt                14352
_reflns_number_total             25018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409444s_si_002.cif
_cod_data_source_block           alex158m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_cell_volume        8866.5(17)
_cod_database_code               4121282