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_4023465
_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_sum            'C62 H92 O24 P2 S2.79 Se1.22'
_chemical_formula_weight         1468.52
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      5
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.ac.uk/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-07-22
_audit_creation_method
'HKL2000-CIF automatic completion and interactive editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 93.891(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   29.875(1)
_cell_length_b                   10.400(1)
_cell_length_c                   11.628(1)
_cell_measurement_reflns_used    16783
_cell_measurement_temperature    103(1)
_cell_measurement_theta_max      36.37
_cell_measurement_theta_min      2.69
_cell_volume                     3604.5(5)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'HKL2000 (Otwinowski & Minor, 1997)'
_computing_publication_material  'HKL2000 (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'HKL2000 (Otwinowski & Minor, 1997)'
_diffrn_ambient_temperature      103(1)
_diffrn_detector_area_resol_mean 10.00
_diffrn_detector_type            RAXIS3S
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'RIGAKU R-AXIS RAPID'
_diffrn_measurement_method
;
 '\w scan with \c offset
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_polarisn_ratio -0.03
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71074
_diffrn_radiation_wavelength_id  1
_diffrn_radiation_wavelength_wt  1.0
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16783
_diffrn_reflns_theta_full        36.37
_diffrn_reflns_theta_max         36.37
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Otwinowski et al., 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_id                crystal1
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.16
_exptl_crystals_number           1
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         16783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.3687P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                12827
_reflns_number_total             16783
_reflns_observed_criterion       >-3sigma(I)
_reflns_scale_group_code         SG1
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo8002997-File003.cif
_cod_data_source_block           sm_w1
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               4023465