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_7150357
_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 O3 Si2'
_chemical_formula_sum            'C22 H41 N5 O3 Si2'
_chemical_formula_weight         479.78
_chemical_name_common
3',5'-O-bis(tert-butyldimethylsiyl)-2'-deoxy-adenosine
_chemical_name_systematic
;
3',5'-O-bis(tert-butyldimethylsiyl)-2'-deoxy-adenosine
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.50000(10)
_cell_length_b                   8.32900(10)
_cell_length_c                   43.3190(4)
_cell_measurement_reflns_used    24965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.32
_cell_measurement_theta_min      4.08
_cell_volume                     2706.03(5)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        'Denzo and HKL Scalepack'
_computing_molecular_graphics    maXus
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.832
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device_type  'MacScience DIPLabo'
_diffrn_measurement_method       IP
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_av_sigmaI/netI    0.0157
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            24965
_diffrn_reflns_theta_full        73.32
_diffrn_reflns_theta_max         73.32
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    1.480
_exptl_absorpt_correction_T_max  0.8609
_exptl_absorpt_correction_T_min  0.6823
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.17(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0707P)^2^+2.0518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                4138
_reflns_number_total             4159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b315769e.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      p212121
_cod_database_code               7150357