Hydrogen-bond network in cyclodecaamylose hydrate at 20K; neutron diffraction study of novel structural motifs band-flip and kink in α-(1→4)-<small>D</small>-glucoside oligosaccharides
Imamura, K.; Nimz, O.; Jacob, J.; Myles, D.; Mason, S. A.; Kitamura, S.; Aree, T.; Saenger, W.; Acta Crystallographica Section B 57 (2001) 833–841; doi:10.1107/S0108768101014288

data_2103748
_publ_section_title
;
 Hydrogen-bond network in cyclodecaamylose hydrate at 20K; neutron
 diffraction study of novel structural motifs band-flip and kink in
 \a-(1\\rightarrow 4)-<small>D</small>-glucoside oligosaccharides
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              833
_journal_page_last               841
_journal_paper_doi               10.1107/S0108768101014288
_journal_volume                  57
_journal_year                    2001
_chemical_formula_moiety         '(C60 H100 O50),27.18(H2 O)'
_chemical_formula_sum            'C60 H153.42 O77.18'
_chemical_formula_weight         2108.30
_chemical_name_common            '[CA10]'
_chemical_name_systematic
;
 [Cyclodecaamylose].27.18 H2 O
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 121.07(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   29.31(5)
_cell_length_b                   9.976(10)
_cell_length_c                   19.34(2)
_cell_measurement_reflns_used    2193
_cell_measurement_temperature    20(2)
_cell_measurement_theta_max      50.85
_cell_measurement_theta_min      3.55
_cell_volume                     4844(11)
_computing_data_collection       'ILL programs Hklgen and Mad'
_computing_molecular_graphics    'MOLSCRIPT, Xtal View'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      20(2)
_diffrn_measured_fraction_theta_full .887
_diffrn_measured_fraction_theta_max .887
_diffrn_measurement_device_type  D19
_diffrn_measurement_method
'4x64 deg. position-sensitive detector (Thomas et. al., 1983)'
_diffrn_radiation_monochromator  'Cu(220) monochromateor'
_diffrn_radiation_probe          neutron
_diffrn_radiation_source         'neutron reactor at ILL'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.53200
_diffrn_reflns_av_R_equivalents  .0480
_diffrn_reflns_av_sigmaI/netI    .0499
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3929
_diffrn_reflns_theta_full        50.77
_diffrn_reflns_theta_max         50.77
_diffrn_reflns_theta_min         2.65
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  9.4-18.8sec
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.31
_exptl_absorpt_correction_T_max  .948
_exptl_absorpt_correction_T_min  .816
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             546
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          .6
_exptl_crystal_size_min          .2
_refine_diff_density_max         1.035
_refine_diff_density_min         -1.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     736
_refine_ls_number_reflns         2494
_refine_ls_number_restraints     393
_refine_ls_restrained_S_all      .987
_refine_ls_R_factor_all          .0681
_refine_ls_R_factor_gt           .0635
_refine_ls_shift/su_max          .073
_refine_ls_shift/su_mean         .003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+409.4507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .1477
_reflns_number_gt                2355
_reflns_number_total             2494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jz0013.cif
_cod_data_source_block           ca10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4843(11)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               2103748