Structure and Biosynthesis of the Marine Streptomycete Ansamycin Ansalactam A and Its Distinctive Branched Chain Polyketide Extender Unit
Micheal C. Wilson; Sang-Jip Nam; Tobias A. M. Gulder; Christopher A. Kauffman; Paul R. Jensen; William Fenical; Bradley S. Moore; Journal of the American Chemical Society 133 (2011) 1971–1977; doi:10.1021/ja109226s

data_4105624
_publ_section_title
;
 Structure and Biosynthesis of the Marine Streptomycete Ansamycin
 Ansalactam A and Its Distinctive Branched Chain Polyketide Extender Unit
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1971
_journal_page_last               1977
_journal_paper_doi               10.1021/ja109226s
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'C34.38 H41.75 Cl2.75 N O6'
_chemical_formula_weight         662.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.564(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7897(12)
_cell_length_b                   14.5693(14)
_cell_length_c                   19.106(2)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.56
_cell_measurement_theta_min      3.82
_cell_volume                     3266.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34969
_diffrn_reflns_theta_full        65.00
_diffrn_reflns_theta_max         65.89
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    2.728
_exptl_absorpt_correction_T_max  0.8757
_exptl_absorpt_correction_T_min  0.5981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       Block
_exptl_crystal_F_000             1399
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.944
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     830
_refine_ls_number_reflns         10167
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0915P)^2^+2.0814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                9769
_reflns_number_total             10167
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja109226s_si_002.cif
_cod_data_source_block           sio28
_cod_original_cell_volume        3266.4(6)
_cod_database_code               4105624