Chemical and Metagenomic Studies of the Lethal Black Band Disease of Corals Reveal Two Broadly Distributed, Redox-Sensitive Mixed Polyketide/Peptide Macrocycles.
Gunasekera, Sarath P.; Meyer, Julie L.; Ding, Yousong; Abboud, Khalil A.; Luo, Danmeng; Campbell, Justin E.; Angerhofer, Alexander; Goodsell, Justin L.; Raymundo, Laurie J.; Liu, Junyang; Ye, Tao; Luesch, Hendrik; Teplitski, Max; Paul, Valerie J.; Journal of natural products 82 (2019) 111–121; doi:10.1021/acs.jnatprod.8b00804

data_1552606
_publ_section_title
;
 Chemical and Metagenomic Studies of the Lethal Black Band Disease of
 Corals Reveal Two Broadly Distributed, Redox-Sensitive Mixed
 Polyketide/Peptide Macrocycles.
;
_journal_issue                   1
_journal_name_full               'Journal of natural products'
_journal_page_first              111
_journal_page_last               121
_journal_paper_doi               10.1021/acs.jnatprod.8b00804
_journal_volume                  82
_journal_year                    2019
_chemical_formula_moiety         'C31 H54 N O11, (H2 O)'
_chemical_formula_sum            'C31 H56 N O12'
_chemical_formula_weight         634.76
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-02-12 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 95.4828(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1769(3)
_cell_length_b                   9.0209(2)
_cell_length_c                   15.9736(4)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1746.62(7)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0128
_diffrn_reflns_av_unetI/netI     0.0121
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22885
_diffrn_reflns_point_group_measured_fraction_full 0.947
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.000
_diffrn_reflns_theta_min         2.779
_diffrn_source                   'I\mS microsource'
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.9757
_exptl_absorpt_correction_T_min  0.8921
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_description       needles
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
; 
 Classical Flack method preferred over Parsons because s.u. lower. 
;
_refine_ls_abs_structure_Flack   0.02(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0524P)^2^+0.5280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.828
_reflns_Friedel_fraction_full    0.925
_reflns_Friedel_fraction_max     0.920
_reflns_number_gt                5945
_reflns_number_total             6020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np8b00804_si_002.cif
_cod_data_source_block           paulv
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1552606
_shelx_estimated_absorpt_t_min   0.794
_shelx_estimated_absorpt_t_max   0.969
_shelxl_version_number           2013-3
_shelx_res_checksum              93531
_shelx_hkl_checksum              32547