van der Waals versus Hydrogen-Bonding Forces in a Crystalline Analog of Cellotetraose: Cyclohexyl 4'-O-Cyclohexyl β-d-Cellobioside Cyclohexane Solvate
Yuko Yoneda; Kurt Mereiter; Christian Jaeger; Lothar Brecker; Paul Kosma; Thomas Rosenau; Alfred French; Journal of the American Chemical Society 130 (2008) 16678–16690; doi:10.1021/ja805147t

data_4108810
_publ_contact_author
;
Alfred French
Southern Regional Research Center,
U.S. Department of Agriculture, 
1100 Robert E. Lee Blvd., 
New Orleans, 
LA 70124, USA
;
_publ_contact_author_email       afrench@srrc.ars.usda.gov
_publ_contact_author_fax         '+1 504 286-4217'
_publ_contact_author_phone       '+1 504 286-4410'
_publ_section_title
;
 van der Waals versus Hydrogen-Bonding Forces in a Crystalline Analog of
 Cellotetraose: Cyclohexyl 4'-O-Cyclohexyl \b-d-Cellobioside Cyclohexane
 Solvate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16678
_journal_page_last               16690
_journal_paper_doi               10.1021/ja805147t
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration rm
_chemical_formula_moiety         '3(C24 H42 O11), 2(C6 H12)'
_chemical_formula_sum            'C84 H150 O33'
_chemical_formula_weight         1688.04
_chemical_name_common
;
1209 YY-056 1209a2.CIF, X-ray H positions, unconventional
unit cell (not reduced) 
;
_chemical_name_systematic
; 
Cyclohexyl 4'-O-cyclohexyl-beta-D-glucopyranosyl- 
(1->-4)-beta-D-glucopyranoside, solvate with cyclohexane in 
3:2 ratio 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.0430(10)
_cell_angle_beta                 52.8280(10)
_cell_angle_gamma                89.3140(10)
_cell_formula_units_Z            1
_cell_length_a                   10.7024(7)
_cell_length_b                   10.9502(7)
_cell_length_c                   23.4669(15)
_cell_measurement_reflns_used    6952
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.40
_cell_volume                     2143.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT, SADABS, XPREP'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            38659
_diffrn_reflns_theta_full        30.07
_diffrn_reflns_theta_max         30.07
_diffrn_reflns_theta_min         2.40
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.308
_exptl_crystal_description       plate
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.772
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.1(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1112
_refine_ls_number_reflns         12443
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0822P)^2^+0.2920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1161
_reflns_number_gt                11584
_reflns_number_total             12443
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja805147t_si_002_2.cif
_cod_data_source_block           1209a2
_cod_depositor_comments
;
 Replacing the _cod_related_optimal_structure data name with the shorter
 version (_cod_related_optimal_struct) that is formally defined in the
 'cif_cod' dictionary.

 Antanas Vaitkus,
 2018-11-16

 Removed the _cod_suboptimal_structure data item in preparation for
 its deprecation. The fact that the structure is a suboptimal one
 should be derived from the presence of the _cod_related_optimal_struct
 data item.

 Antanas Vaitkus,
 2019-05-21
;
_cod_related_optimal_struct      4108791
_cod_database_code               4108810