Saccharothrixones A-D, Tetracenomycin-Type Polyketides from the Marine-Derived Actinomycete Saccharothrix sp. 10-10.
Gan, Maoluo; Liu, Bin; Tan, Yi; Wang, Qiang; Zhou, Hongxia; He, Hongwei; Ping, Yuhui; Yang, Zhaoyong; Wang, Yiguang; Xiao, Chunling; Journal of natural products 78 (2015) 2260–2265; doi:10.1021/acs.jnatprod.5b00577

data_1533376
_publ_section_title
;
 Saccharothrixones A-D, Tetracenomycin-Type Polyketides from the
 Marine-Derived Actinomycete Saccharothrix sp. 10-10.
;
_journal_issue                   9
_journal_name_full               'Journal of natural products'
_journal_page_first              2260
_journal_page_last               2265
_journal_paper_doi               10.1021/acs.jnatprod.5b00577
_journal_volume                  78
_journal_year                    2015
_chemical_absolute_configuration rm
_chemical_compound_source        'Saccharothrix sp. 10-10'
_chemical_formula_moiety         'C24 H22 O11,1.5(C H 4 O)'
_chemical_formula_sum            'C25.5 H28 O12.5'
_chemical_formula_weight         534.47
_chemical_name_systematic        'saccharothrixone D'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-03-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_audit_update_record
;
2015-03-16 deposited with the CCDC.
2015-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.0788(4)
_cell_length_b                   17.5135(4)
_cell_length_c                   19.2065(5)
_cell_measurement_reflns_used    8518
_cell_measurement_temperature    124(2)
_cell_measurement_theta_max      66.8970
_cell_measurement_theta_min      2.9370
_cell_volume                     5072.1(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      124(2)
_diffrn_detector_area_resol_mean 10.4713
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur,Atlas,Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0013858000
_diffrn_orient_matrix_UB_12      0.0315618000
_diffrn_orient_matrix_UB_13      0.0748795000
_diffrn_orient_matrix_UB_21      0.0899617000
_diffrn_orient_matrix_UB_22      -0.0386687000
_diffrn_orient_matrix_UB_23      0.0145192000
_diffrn_orient_matrix_UB_31      0.0484779000
_diffrn_orient_matrix_UB_32      0.0723481000
_diffrn_orient_matrix_UB_33      -0.0249336000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19166
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.068
_diffrn_reflns_theta_min         3.415
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66174
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform-methanol'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 3002 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(7)
_refine_ls_extinction_coef       0.00034(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         8336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0825P)^2^+5.9165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1713
_reflns_Friedel_coverage         0.671
_reflns_friedel_fraction_full    0.818
_reflns_friedel_fraction_max     0.828
_reflns_number_gt                7825
_reflns_number_total             8336
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            np5b00577_si_002.cif
_cod_data_source_block           mari
_cod_depositor_comments
;

2019-07-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C51 H56 O25'
_cod_original_formula_weight         1068.95
_cod_original_formula_moiety         '2(C24 H22 O11),3(C H 4 O)'
_cod_original_formula_units_Z            4
_cod_database_code               1533376
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         'C1 H1 O1 N1'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(C2"')=Sof(O1"')=Sof(H1"')=1-FVAR(1)
 Sof(O2"')=Sof(H2"')=Sof(O3"')=Sof(H3"')=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C4(H4), C4'(H4'A)
3.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C18'(H18D,H18E,H18F), C16'(H16D,H16E,H16F),
 C17'(H17D,H17E,H17F), C14'(H14D,H14E,H14F), C15'(H15D,H15E,H15F), C1"(H1"A,
 H1"B,H1"C)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C6(H6), C2'(H2'), C7'(H7'), C6'(H6')
3.d Tetrahedral OH refined with riding coordinates:
 O4(H4A), O11(H11), O9(H9), O9'(H9'), O11'(H11'), O4'(H4'), O1"(H1"),
 O2"'(H2"'), O1"'(H1"'), O3"'(H3"')
;
_shelx_res_checksum              54636
_shelx_hkl_checksum              38844
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS-1997 (Sheldrick, 2008)'