Antimycobacterial Rufomycin Analogues from <i>Streptomyces atratus</i> Strain MJM3502.
Zhou, Bin; Shetye, Gauri; Yu, Yang; Santarsiero, Bernard D.; Klein, Larry L.; Abad-Zapatero, Cele; Wolf, Nina M.; Cheng, Jinhua; Jin, Yingyu; Lee, Hanki; Suh, Joo-Won; Lee, Hyun; Bisson, Jonathan; McAlpine, James B.; Chen, Shao-Nong; Cho, Sang-Hyun; Franzblau, Scott G.; Pauli, Guido F.; Journal of natural products  (2020) –; doi:10.1021/acs.jnatprod.9b01095

data_1557271
_publ_section_title
;
 Antimycobacterial Rufomycin Analogues from <i>Streptomyces atratus</i>
 Strain MJM3502.
;
_journal_name_full               'Journal of natural products'
_journal_paper_doi               10.1021/acs.jnatprod.9b01095
_journal_year                    2020
_chemical_formula_moiety         '2(C54 H77 N9 O9), 3(O)'
_chemical_formula_sum            'C108 H154 N18 O27'
_chemical_formula_weight         2136.49
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 109.574(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9590(10)
_cell_length_b                   25.347(2)
_cell_length_c                   18.606(2)
_cell_measurement_reflns_used    45971
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.169
_cell_measurement_theta_min      1.369
_cell_volume                     6202.7(9)
_computing_cell_refinement       'XDS (Kabsch)'
_computing_data_collection       LS-CAT
_computing_data_reduction        'XDS (Kabsch)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'Eiger 9M'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68877
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.914
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45971
_diffrn_reflns_point_group_measured_fraction_full 0.934
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_theta_full        24.410
_diffrn_reflns_theta_max         27.169
_diffrn_reflns_theta_min         1.369
_diffrn_source                   'APS 21-ID-D'
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       block
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.727
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Flack x determined using 9092 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
 Bijvoet analysis using PLATON.
;
_refine_ls_abs_structure_Flack   0.3(3)
_refine_ls_extinction_coef       0.111(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.634
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1425
_refine_ls_number_reflns         26475
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.642
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.1163
_refine_ls_shift/su_max          1.785
_refine_ls_shift/su_mean         0.011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3449
_refine_ls_wR_factor_ref         0.3632
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    0.897
_reflns_Friedel_fraction_max     0.833
_reflns_number_gt                22795
_reflns_number_total             26475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np9b01095_si_001.cif
_cod_data_source_block           h41d-20190702
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1557271
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              45477
_shelx_hkl_checksum              26655