Regioselective opening of proximally sulfato-capped cyclodextrins
Matthieu Jouffroy; Rafael Gramage-Doria; Dominique Armspach; Dominique Matt; Loic Toupet; Chem.Commun. 48 (2012) 6028–; doi:10.1039/c2cc31302b

data_7107822
_publ_section_title
;
 Regioselective opening of proximally sulfato-capped cyclodextrins
;
_journal_name_full               Chem.Commun.
_journal_page_first              6028
_journal_paper_doi               10.1039/c2cc31302b
_journal_volume                  48
_journal_year                    2012
_chemical_absolute_configuration rm
_chemical_formula_sum            'C84.5 H136 B2 Cl6 O28 P2'
_chemical_formula_weight         1896.19
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0969(4)
_cell_length_b                   22.4367(5)
_cell_length_c                   27.7516(7)
_cell_measurement_reflns_used    14444
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      2.62
_cell_volume                     10022.8(4)
_computing_cell_refinement
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26'
_computing_data_collection
'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26'
_computing_data_reduction
'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26'
_computing_molecular_graphics    'PLATON_(Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97_(Altomare & al., 1998)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 19.64
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD Saphire 3 Xcalibur'
_diffrn_measurement_method       'omega scan'
_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  0.0994
_diffrn_reflns_av_sigmaI/netI    0.2294
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            79214
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.274
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4036
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         21429
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.2114
_refine_ls_R_factor_gt           0.0935
_refine_ls_shift/su_max          0.236
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1316P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2645
_reflns_number_gt                8413
_reflns_number_total             21429
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc31302b.txt
_cod_data_source_block           mj48
_cod_original_sg_symbol_H-M      P212121
_cod_original_formula_sum        'C84.50 H136 B2 Cl6 O28 P2'
_cod_database_code               7107822