Assessment of the Stoichiometry of Multicomponent Crystals Using Only X-ray Powder Diffraction Data.
Maguire, Courtney K.; Brunskill, Andrew P. J.; Molecular pharmaceutics 12 (2015) 2061–2067; doi:10.1021/mp5008458

data_1519620
_publ_section_title
;
 Assessment of the Stoichiometry of Multicomponent Crystals Using Only
 X-ray Powder Diffraction Data.
;
_journal_issue                   6
_journal_name_full               'Molecular pharmaceutics'
_journal_page_first              2061
_journal_page_last               2067
_journal_paper_doi               10.1021/mp5008458
_journal_volume                  12
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C21 H23 N3 O5, C2 H6 O'
_chemical_formula_sum            'C23 H29 N3 O6'
_chemical_formula_weight         443.49
_chemical_name_common
;
Navarixin Ethanol Solvate
;
_chemical_name_systematic
; 
2-Hydroxy-N,N-dimethyl-3-[(2-{[(1R)-1-(5-methylfuran-2-yl)propyl]amino}
-3,4-dioxocyclobut-1-en-1-yl)amino]benzamide ethanol solvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 107.9123(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.74560(10)
_cell_length_b                   10.05200(10)
_cell_length_c                   12.3150(2)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.61
_cell_measurement_theta_min      3.77
_cell_volume                     1147.93(2)
_computing_cell_refinement       'SAINT V8.34A'
_computing_data_collection       'SAINT V8.34A'
_computing_data_reduction        'SAINT V8.34A'
_computing_molecular_graphics    'SHELXL-2014 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12646
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.487
_diffrn_reflns_theta_min         4.769
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.7528
_exptl_transmission_factor_min   0.6837
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details
; 
 Flack x determined using 1874 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.10(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         4039
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.034
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+0.1174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0944
_reflns_Friedel_coverage         0.883
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                4011
_reflns_number_total             4039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mp5008458_si_002.cif
_cod_data_source_block           mdj065_abs
_cod_depositor_comments
'Adding full bibliography for 1519620--1519621.cif.'
_cod_database_code               1519620
_shelx_estimated_absorpt_t_min   0.861
_shelx_estimated_absorpt_t_max   0.927
_shelxl_version_number           2014-3
_shelx_res_checksum              89700
_shelx_hkl_checksum              46418