Structural Elucidation of the Neuraminidase Inhibitor Zanamivir (Relenza): Creeping and Diffusion for Polymorph Separation
Nath, Naba K.; Yasuda, Nobuhiro; Rabeh, Wael M.; Sahoo, Subash Chandra; Naumov, Panče; Crystal Growth & Design 14 (2014) 770–; doi:10.1021/cg4016383

data_4509889
_publ_section_title
;
 Structural Elucidation of the Neuraminidase Inhibitor Zanamivir
 (Relenza): Creeping and Diffusion for Polymorph Separation
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              770
_journal_paper_doi               10.1021/cg4016383
_journal_volume                  14
_journal_year                    2014
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C12 H20 N4 O7, 1.9(H2 O)'
_chemical_formula_sum            'C12 H23.8 N4 O8.9'
_chemical_formula_weight         366.54
_chemical_melting_point          ?
_chemical_name_systematic
; 
 ? 
;
_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                 98.548(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5932(19)
_cell_length_b                   4.7331(8)
_cell_length_c                   17.179(3)
_cell_measurement_reflns_used    6729
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      21.91
_cell_measurement_theta_min      1.04
_cell_volume                     851.8(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Large cylindrical image-plate camera'
_diffrn_measurement_method       'Oscillation Photograph'
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_source         'synchrotron radiation SPring-8 BL02B1'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.61948
_diffrn_reflns_av_R_equivalents  0.0799
_diffrn_reflns_av_sigmaI/netI    0.0756
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6729
_diffrn_reflns_theta_full        21.91
_diffrn_reflns_theta_max         21.91
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  1.6078
_exptl_absorpt_correction_T_min  0.7847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (T.Higashi, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.007
_refine_diff_density_max         0.324
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         2987
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0767P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                2142
_reflns_number_total             2987
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg4016383_si_002.cif
_cod_data_source_block           shelxl
_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 2281 2013-09-26 08:29:07Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_formula_sum        'C12 H23.80 N4 O8.90'
_cod_database_code               4509889