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_7150352
_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         'C37 H73 N5 O5 Si3'
_chemical_formula_sum            'C37 H73 N5 O5 Si3'
_chemical_formula_weight         752.27
_chemical_name_common            2',3',5'-O-tris(triisopropylsilyl)-guanosine
_chemical_name_systematic
;
2',3',5'-O-tris(triisopropylsilyl)-guanosine
;
_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                 95.211(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8080(5)
_cell_length_b                   10.9010(4)
_cell_length_c                   21.4960(8)
_cell_measurement_reflns_used    19180
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.19
_cell_measurement_theta_min      4.13
_cell_volume                     2288.79(17)
_computing_cell_refinement       Scalepack
_computing_data_collection       'MacScience Xpress'
_computing_data_reduction        'Denzo and 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 0.863
_diffrn_measured_fraction_theta_max 0.863
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19180
_diffrn_reflns_theta_full        73.19
_diffrn_reflns_theta_max         73.19
_diffrn_reflns_theta_min         4.13
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  0.8572
_exptl_absorpt_correction_T_min  0.5670
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.092
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.323
_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   0.41(9)
_refine_ls_extinction_coef       0.012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.981
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5625
_refine_ls_number_restraints     377
_refine_ls_restrained_S_all      1.970
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.1089
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3720
_refine_ls_wR_factor_ref         0.3936
_reflns_number_gt                5202
_reflns_number_total             5625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b315769e.txt
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7150352