Conformational Control in Activation of an Enediyne
M. F. Semmelhack; Lingyun Wu; Robert A. Pascal; Douglas M. Ho; Journal of the American Chemical Society 125 (2003) 10496–10497; doi:10.1021/ja036763e

data_4114122
_publ_contact_author_address
; Princeton University
  Department of Chemistry
  Princeton, NJ   08544-1009
  USA
;
_publ_contact_author_email       ho@princeton.edu
_publ_contact_author_fax         (609)2586746
_publ_contact_author_name        'Dr. Douglas M. Ho'
_publ_contact_author_phone       (609)2583160
_publ_section_title
;
 Conformational Control in Activation of an Enediyne
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10496
_journal_page_last               10497
_journal_paper_doi               10.1021/ja036763e
_journal_volume                  125
_journal_year                    2003
_chemical_compound_source        'chemical synthesis'
_chemical_formula_iupac          'C28 H24 O6 . C H2 Cl2'
_chemical_formula_moiety         'C28 H24 O6, C H2 Cl2'
_chemical_formula_structural     'C28 H24 O6, C H2 Cl2'
_chemical_formula_sum            'C29 H26 Cl2 O6'
_chemical_formula_weight         541.40
_chemical_name_systematic
; 
 2,15-Dihydroxy-11,24-dioxapentacyclo[7.4.1.1^10,13^,7.4.1.1^23,26^]-
 triaconta-5,18-diene-3,7,16,20-tetrayne-12,25-dione Dichloromethane Solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                97.534(2)
_cell_angle_beta                 96.639(3)
_cell_angle_gamma                100.131(3)
_cell_formula_units_Z            2
_cell_length_a                   7.0970(4)
_cell_length_b                   12.8795(8)
_cell_length_c                   14.9886(9)
_cell_measurement_reflns_used    8303
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.38
_cell_volume                     1323.47(14)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'DENZO-SMN, PLATON'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       '\w scans; 800 0.5\% rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0743
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8303
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       Prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.200
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.054
_refine_ls_goodness_of_fit_obs   1.228
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_restrained_S_obs      1.228
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_obs          0.0587
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0878P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1674
_refine_ls_wR_factor_obs         0.1528
_reflns_number_observed          2889
_reflns_number_total             4540
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            ja036763esi20030619_121828_3.cif
_cod_data_source_block           mfs016f
_cod_database_code               4114122