Synthesis and Solid-State Study of Supramolecular Host-Guest Assemblies: Bis[6-O,6-O'-(1,2:3,4-diisopropylidene-α-D- galactopyranosyl)thiophosphoryl] Dichalcogenides
Marek J. Potrzebowski; Wojciech M. Potrzebowski; Agata Jeziorna; Wlodzimierz Ciesielski; Jarosław Gajda; Grzegorz D. Bujacz; Maksymilian Chruszcz; Wladek Minor; Journal of Organic Chemistry 73 (2008) 4388–4397; doi:10.1021/jo8002997

data_4023468
_publ_section_title
;
 Synthesis and Solid-State Study of Supramolecular Host-Guest
 Assemblies: Bis[6-O,6-O'-(1,2:3,4-diisopropylidene-\a-D-
 galactopyranosyl)thiophosphoryl] Dichalcogenides
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4388
_journal_page_last               4397
_journal_paper_doi               10.1021/jo8002997
_journal_volume                  73
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H74 O24 P2 S2 Se2, 2(C3 H8 O)'
_chemical_formula_sum            'C54 H90 O26 P2 S2 Se2'
_chemical_formula_weight         1439.24
_space_group_IT_number           145
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      145
_symmetry_space_group_name_Hall  'P 32'
_symmetry_space_group_name_H-M   'P 32'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   11.883
_cell_length_b                   11.883
_cell_length_c                   43.699
_cell_measurement_reflns_used    922
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.53
_cell_measurement_theta_min      2.03
_cell_volume                     5343.8
_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      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71068
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            93310
_diffrn_reflns_theta_full        28.51
_diffrn_reflns_theta_max         28.51
_diffrn_reflns_theta_min         1.98
_exptl_absorpt_coefficient_mu    1.214
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Sheldrick, G.M.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.056(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         17025
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0483
_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^)+(0.0677P)^2^+2.4423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1275
_refine_ls_wR_factor_ref         0.1345
_reflns_number_gt                13721
_reflns_number_total             17025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8002997-File006.cif
_cod_data_source_block           struktury_dise
_cod_original_sg_symbol_Hall     P32
_cod_database_code               4023468