Structural and theoretical study of four novel norcantharidine derivatives: two new cases of conditional isomorphism
Tan, Xue-Jie; Liu, Shuai; Hei, Xiao-Ming; Yang, Feng-Cun; He, Peng-Bing; Guo, Feng; Xing, Dian-Xiang; Acta Crystallographica Section C 76 (2020) 75–86; doi:10.1107/S2053229619016164

data_2021936
_publ_section_title
;
 Structural and theoretical study of four novel norcantharidine
 derivatives: two new cases of conditional isomorphism
;
_journal_coeditor_code           YO3069
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              75
_journal_page_last               86
_journal_paper_doi               10.1107/S2053229619016164
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration syn
_chemical_formula_iupac          'C10 H13 N O4'
_chemical_formula_moiety         'C10 H13 N O4'
_chemical_formula_sum            'C10 H13 N O4'
_chemical_formula_weight         211.21
_chemical_name_common
;
norcantharidine - 2-aminoethanol
;
_chemical_name_systematic
(3a<i>R</i>,4<i>S</i>,7<i>R</i>,7a<i>S</i>)-2-(2-Hydroxyethyl)-3a,4,5,6,7,7a-hexahydro-1<i>H</i>-4,7-epoxyisoindole-1,3(2<i>H</i>)-dione
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_Hall           'P 2ac -2'
_space_group_name_H-M_alt        'P m n 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.0350(17)
_cell_length_b                   5.5937(13)
_cell_length_c                   8.9634(17)
_cell_measurement_reflns_used    380
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.45
_cell_volume                     503.14(17)
_computing_cell_refinement
;
SMART (Bruker, 2000)
;
_computing_data_collection
;
SMART (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
SHELXTL (Bruker, 2000), PLATON (Spek, 2009), WinGX2014
(Farrugia, 2012),
DIAMOND (Brandenburg & Putz, 1999) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.12
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            1569
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.658
_diffrn_reflns_theta_min         6.622
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2000)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.140
_refine_diff_density_min         -0.122
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 120 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   0.6(6)
_refine_ls_extinction_coef       0.0122(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     113
_refine_ls_number_reflns         731
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0317P)^2^+0.0793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0899
_refine_ls_wR_factor_ref         0.0990
_reflns_number_gt                594
_reflns_number_total             731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yo3069sup1.cif
_cod_data_source_block           NCA-AE
_cod_database_code               2021936
_shelx_estimated_absorpt_t_min   0.89
_shelx_estimated_absorpt_t_max   0.97
_shelx_hkl_checksum              41557
_shelx_res_checksum              5652
_cod_database_fobs_code 2021936