Crystal structure of diaphorin methanol monosolvate isolated from <i>Diaphorina citri</i> Kuwayama, the insect vector of citrus greening disease
Szebenyi, D. Marian; Kriksunov, Irina; Howe, Kevin J.; Ramsey, John S.; Hall, David G.; Heck, Michelle L.; Krasnoff, Stuart B.; Acta Crystallographica Section E 74 (2018) 445–449; doi:10.1107/S2056989018002992

data_2242405
_publ_section_title
;
 Crystal structure of diaphorin methanol monosolvate isolated from
 <i>Diaphorina citri</i> Kuwayama, the insect vector of citrus greening
 disease
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              445
_journal_page_last               449
_journal_paper_doi               10.1107/S2056989018002992
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          'C22 H39 N O9, C H4 O'
_chemical_formula_moiety         'C22 H39 N O9, C H4 O'
_chemical_formula_sum            'C23 H43 N O10'
_chemical_formula_weight         493.58
_chemical_name_systematic
;(<i>S</i>)-<i>N</i>-((<i>S</i>)-{(2<i>S</i>,4<i>R</i>,6<i>R</i>)-6-[(<i>S</i>)-2,3-Dihydroxypropyl]-4-hydroxy-5,5-dimethyltetrahydro-2<i>H</i>-pyran-2-yl}(hydroxy)methyl)-2-hydroxy-2-[(2<i>R</i>,5<i>R</i>,6<i>R</i>)-2-methoxy-5,6-dimethyl-4-methylenetetrahydro-2<i>H</i>-pyran-2-yl]acetamide
methanol monosolvate
;
_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-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 101.9(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.40(5)
_cell_length_b                   12.87(5)
_cell_length_c                   13.92(5)
_cell_measurement_reflns_used    7493
_cell_measurement_temperature    100(2)
_cell_volume                     1297(11)
_computing_cell_refinement
;
<i>XDS</i> (Kabsch, 2010)
;
_computing_data_collection
;
<i>ADX</i> (Szebenyi <i>et al.</i>,  1997)
;
_computing_data_reduction
;
HKL2000 (Otwinowski & Minor, 1997) and <i>XDS</i> (Kabsch, 2010)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015), PLATON (Spek, 2009) and publCIF
(Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SnB (Weeks & Miller, 1999<i>a</i>,<i>b</i>) and
COOT (Emsley <i>et al.</i>,
2010)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.8
_diffrn_measured_fraction_theta_full 0.862
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device       'single-axis goniometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9768
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7818
_diffrn_reflns_theta_full        30.981
_diffrn_reflns_theta_max         30.981
_diffrn_reflns_theta_min         2.054
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
<i>XDS</i> (Kabsch, 2010), determined correction factors
as a function of position on detector surface
and frame number
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.202
_refine_ls_extinction_coef       0.40(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
(SHELXL2016; Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         2610
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+0.1123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                2594
_reflns_number_total             2610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5424sup1.cif
_cod_data_source_block           I
_cod_database_code               2242405
_cod_database_fobs_code          2242405
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.999
_shelx_hkl_checksum              58549
_shelx_res_checksum              21067