Use of an adjustable soft segment as an effective molecular design for crystal engineering of hydrogen-bonded tape motifs.
Takasawa, Ryoichi; Yoshikawa, Isao; Araki, Koji; Organic & biomolecular chemistry 2 (2004) 1125–1132; doi:10.1039/b315769e

data_7150356
_publ_section_title
;
 Use of an adjustable soft segment as an effective molecular design for
 crystal engineering of hydrogen-bonded tape motifs.
;
_journal_issue                   8
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1125
_journal_page_last               1132
_journal_paper_doi               10.1039/b315769e
_journal_volume                  2
_journal_year                    2004
_chemical_formula_moiety         'C22 H41 N5 O4 Si2'
_chemical_formula_sum            'C22 H41 N5 O4 Si2'
_chemical_formula_weight         495.78
_chemical_name_common            2',3'-O-bis(tert-butyldimethylsilyl)-adenosine
_chemical_name_systematic
;
2',3'-O-bis(tert-butyldimethylsilyl)-adenosine
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 104.988(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.428(4)
_cell_length_b                   7.794(6)
_cell_length_c                   23.465(5)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.8
_cell_measurement_theta_min      11.1
_cell_volume                     2902(2)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_molecular_graphics    teXsan
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.06230
_diffrn_orient_matrix_UB_12      0.01535
_diffrn_orient_matrix_UB_13      0.01499
_diffrn_orient_matrix_UB_21      -0.00691
_diffrn_orient_matrix_UB_22      0.02530
_diffrn_orient_matrix_UB_23      0.04027
_diffrn_orient_matrix_UB_31      0.00626
_diffrn_orient_matrix_UB_32      -0.12484
_diffrn_orient_matrix_UB_33      0.01000
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            7376
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0.01
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.155
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1072.00
_exptl_crystal_size_max          0.520
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.160
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.13(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     616
_refine_ls_number_reflns         7133
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                3767
_reflns_number_total             7133
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b315769e.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7150356