Crystal structure of 7-phenyl-7-(2,4,5-trimethyl-3,6-dioxocyclohexa-1,4-dien-1-yl)heptanoate 1,3-dihydroxy-2-(hydroxymethyl)propan-2-aminium monohydrate: a new solid form of seratrodast
Lou, Benyong; Acta Crystallographica Section E 70 (2014) 228–230; doi:10.1107/S1600536814020625

data_2240018
_publ_section_title
;
 Crystal structure of
 7-phenyl-7-(2,4,5-trimethyl-3,6-dioxocyclohexa-1,4-dien-1-yl)heptanoate
 1,3-dihydroxy-2-(hydroxymethyl)propan-2-aminium monohydrate: a new solid
 form of seratrodast
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              228
_journal_page_last               230
_journal_paper_doi               10.1107/S1600536814020625
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C4 H12 N O3 +, C22 H25 O4 -, H2 O'
_chemical_formula_moiety         'C4 H12 N O3 +, C22 H25 O4 -, H2 O'
_chemical_formula_sum            'C26 H39 N O8'
_chemical_formula_weight         493.58
_chemical_name_systematic
;
7-Phenyl-7-(2,4,5-trimethyl-3,6-dioxocyclohexa-1,4-dien-1-yl)heptanoate
1,3-dihydroxy-2-(hydroxymethyl)propan-2-aminium monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 94.223(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.506(9)
_cell_length_b                   9.665(4)
_cell_length_c                   11.344(5)
_cell_measurement_reflns_used    6295
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5243
_cell_measurement_theta_min      2.1073
_cell_volume                     2570.2(18)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2000)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2000)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2000)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and
publcif (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20028
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrystalClear; Rigaku, 2000)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.553
_refine_diff_density_min         -0.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         5762
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1284
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1567P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2085
_refine_ls_wR_factor_ref         0.2880
_reflns_number_gt                3564
_reflns_number_total             5762
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            su2780sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2570.0(17)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2240018
_cod_database_fobs_code          2240018