Supramolecular recognition and structural elucidation of inclusion complexes of an achiral carbene precursor in beta- and permethylated beta-cyclodextrin.
Mieusset, Jean-Luc; Krois, Daniel; Pacar, Mirjana; Brecker, Lothar; Giester, Gerald; Brinker, Udo H.; Organic letters 6 (2004) 1967–1970; doi:10.1021/ol049478o

data_1507094
_publ_section_title
;
 Supramolecular recognition and structural elucidation of inclusion
 complexes of an achiral carbene precursor in beta- and permethylated
 beta-cyclodextrin.
;
_journal_issue                   12
_journal_name_full               'Organic letters'
_journal_page_first              1967
_journal_page_last               1970
_journal_paper_doi               10.1021/ol049478o
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C71 H124 N2 O36'
_chemical_formula_weight         1581.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_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                   11.188(2)
_cell_length_b                   25.291(2)
_cell_length_c                   29.152(5)
_cell_measurement_temperature    193(2)
_cell_volume                     8249(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0335
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12174
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    0.102
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3408
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(8)
_refine_ls_extinction_coef       0.0036(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   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1001
_refine_ls_number_reflns         12174
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.727
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+3.9468P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1366
_reflns_number_gt                10055
_reflns_number_total             12174
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol049478osi20040319_094127.cif
_cod_data_source_block           slm852a
_cod_database_code               1507094