Experimental and computational crystal structure landscape study of nigerloxin: a fungal metabolite from Aspergillus niger
Singh, Shiv Shankar; Vasantha, K. Y.; Sattur, A. P.; Thakur, Tejender S.; CrystEngComm 18 (2016) 1740–; doi:10.1039/C5CE02572A

data_7224059
_publ_section_title
;
 Experimental and computational crystal structure landscape study of
 nigerloxin: a fungal metabolite from Aspergillus niger
;
_journal_issue                   10
_journal_name_full               CrystEngComm
_journal_page_first              1740
_journal_paper_doi               10.1039/C5CE02572A
_journal_volume                  18
_journal_year                    2016
_chemical_compound_source        'Aspergillus niger '
_chemical_formula_moiety         'C10 H7 N O5, 0.5(C4 H8 O2), H2 O'
_chemical_formula_sum            'C12 H13 N O7'
_chemical_formula_weight         283.23
_chemical_name_common            'Nigerloxin dioxane water solvate'
_chemical_name_systematic        'Nigerloxin dioxane water solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-01-27 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.17(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.77(3)
_cell_length_b                   8.771(8)
_cell_length_c                   10.2110(10)
_cell_measurement_reflns_used    1657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     2448(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b24 (Rigaku, 2012)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
scan:
    Number of images: 200
               Slice: -30.0000 - 70.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 60.0000
                 Phi: 0.0000
                 XTD: 45.0467
              2theta: -19.6352
scan:
    Number of images: 200
               Slice: -30.0000 - 70.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: 60.0000
                 Phi: 90.0000
                 XTD: 45.0467
              2theta: -19.6352
scan:
    Number of images: 200
               Slice: -110.0000 - -10.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -60.0000
                 Phi: 180.0000
                 XTD: 45.0467
              2theta: -19.6352
scan:
    Number of images: 200
               Slice: -110.0000 - -10.0000
         Image width: 0.5000
            Exp time: 16.0000
       Rotation axis: Omega
               Omega: 0.0000
               Kappa: -60.0000
                 Phi: 270.0000
                 XTD: 45.0467
              2theta: -19.6352

;
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (4x4 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Loop
_diffrn_orient_matrix_type       XPlain
_diffrn_orient_matrix_UB_11      -0.093391
_diffrn_orient_matrix_UB_12      0.036194
_diffrn_orient_matrix_UB_13      -0.024317
_diffrn_orient_matrix_UB_21      0.045289
_diffrn_orient_matrix_UB_22      0.058635
_diffrn_orient_matrix_UB_23      -0.086662
_diffrn_orient_matrix_UB_31      0.098667
_diffrn_orient_matrix_UB_32      -0.067394
_diffrn_orient_matrix_UB_33      0.005964
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0621
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8972
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.309
_diffrn_reflns_theta_min         3.063
_diffrn_reflns_transf_matrix_11  -0.093391
_diffrn_reflns_transf_matrix_12  0.036194
_diffrn_reflns_transf_matrix_13  -0.024317
_diffrn_reflns_transf_matrix_21  0.045289
_diffrn_reflns_transf_matrix_22  0.058635
_diffrn_reflns_transf_matrix_23  -0.086662
_diffrn_reflns_transf_matrix_31  0.098667
_diffrn_reflns_transf_matrix_32  -0.067394
_diffrn_reflns_transf_matrix_33  0.005964
_diffrn_source                   MicroMax003_Mo
_diffrn_source_current           0.6
_diffrn_source_power             0.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.128
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.301
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       Block
_exptl_crystal_F_000             1184
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethanol'
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0636
_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^)+(0.1168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1703
_refine_ls_wR_factor_ref         0.2050
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1674
_reflns_number_total             2200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02572a2.cif
_cod_data_source_block           TSAS001b_100K
_cod_depositor_comments
'Adding full bibliography for 7224059--7224060.cif.'
_cod_database_code               7224059
_shelx_estimated_absorpt_t_min   0.944
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-3
_shelx_res_checksum              43995