2-(2',3',4',6'-Tetra-<i>O</i>-acetyl-β-<small>D</small>-glucopyranosylthio)-4-pyridin-4-yl-6,7,8,9-tetrahydro-5<i>H</i>-cyclohepta[<i>b</i>]pyridine-3-carbonitrile
Elgemeie, Galal H.; Hussein, Mona M.; Jones, Peter G.; Acta Crystallographica Section E 58 (2002) o1244–o1246; doi:10.1107/S160053680201872X

data_2201312
_publ_section_title
2-(2',3',4',6'-Tetra-<i>O</i>-acetyl-\b-<small>D</small>-glucopyranosylthio)-4-pyridin-4-yl-6,7,8,9-tetrahydro-5<i>H</i>-cyclohepta[<i>b</i>]pyridine-3-carbonitrile
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1244
_journal_page_last               o1246
_journal_paper_doi               10.1107/S160053680201872X
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C30 H33 N3 O9 S'
_chemical_formula_weight         611.65
_chemical_name_systematic
;
 2-(2',3',4',6'-Tetra-O-acetyl-\b-D-glucopyranosylthio)-4-pyridin-4-yl-
 6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridine-3-carbonitrile
;
_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                   8.0237(14)
_cell_length_b                   10.2293(14)
_cell_length_c                   38.636(6)
_cell_measurement_reflns_used    61
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      4.5
_cell_volume                     3171.1(9)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       \w-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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7824
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.158
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.276
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         7289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0643P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1046
_refine_ls_wR_factor_ref         0.1110
_reflns_number_gt                5529
_reflns_number_total             7289
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6201.cif
_cod_data_source_block           4
_cod_database_code               2201312
_cod_database_fobs_code          2201312