Encaging the Verkade's Superbases: Thermodynamic and Kinetic Consequences
Pascal Dimitrov Raytchev; Alexandre Martinez; Heinz Gornitzka; Jean-Pierre Dutasta; Journal of the American Chemical Society 133 (2011) 2157–2159; doi:10.1021/ja1110333

data_4105667
_publ_section_title
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 Encaging the Verkade's Superbases: Thermodynamic and Kinetic Consequences
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2157
_journal_page_last               2159
_journal_paper_doi               10.1021/ja1110333
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C61.5 H78 Cl10 N4 O11.5 P'
_chemical_formula_weight         1442.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 123.69(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.8(3)
_cell_length_b                   26.2(3)
_cell_length_c                   21.3(2)
_cell_measurement_reflns_used    2050
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.34
_cell_measurement_theta_min      2.87
_cell_volume                     12908(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.4040
_diffrn_reflns_av_sigmaI/netI    0.3143
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            48340
_diffrn_reflns_theta_full        21.73
_diffrn_reflns_theta_max         21.73
_diffrn_reflns_theta_min         5.18
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.8188
_exptl_absorpt_correction_T_min  0.7808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       block
_exptl_crystal_F_000             6016
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0046(6)
_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   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     895
_refine_ls_number_reflns         7075
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.3150
_refine_ls_R_factor_gt           0.1305
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3094
_refine_ls_wR_factor_ref         0.4145
_reflns_number_gt                2250
_reflns_number_total             7075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1110333_si_002.cif
_cod_data_source_block           alex3cc
_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        12907(258)
_cod_original_formula_sum        'C61.50 H78 Cl10 N4 O11.50 P'
_cod_database_code               4105667