Design, synthesis and biological evaluation of bridged epothilone D analogues
Chen, Qiao-Hong; Ganesh, Thota; Brodie, Peggy; Slebodnick, Carla; Jiang, Yi; Banerjee, Abhijit; Bane, Susan; Snyder, James P.; Kingston, David G. I.; Organic & Biomolecular Chemistry 6 (2008) 4542–4552; doi:10.1039/b814823f

data_7151035
_publ_section_title
;
 Design, synthesis and biological evaluation of bridged epothilone D
 analogues
;
_journal_issue                   24
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              4542
_journal_page_last               4552
_journal_paper_doi               10.1039/b814823f
_journal_volume                  6
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C36 H47 N O8 S'
_chemical_formula_sum            'C36 H47 N O8 S'
_chemical_formula_weight         653.81
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.0080(11)
_cell_length_b                   17.848(2)
_cell_length_c                   30.989(4)
_cell_measurement_reflns_used    1295
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      51.5277
_cell_measurement_theta_min      3.7929
_cell_volume                     3323.0(8)
_computing_cell_refinement       'CrysAlisPro (Oxford Diffraction)'
_computing_data_collection       'CrysAlisPro (Oxford Diffraction)'
_computing_data_reduction        'CrysAlisPro (Oxford Diffraction)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_publication_material
'SHELXTL (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_computing_structure_solution
'SHELXS-97 (Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            'Oxford Diffraction Sapphire 3 CCD'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1684
_diffrn_reflns_av_sigmaI/netI    0.2356
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10746
_diffrn_reflns_theta_full        50.35
_diffrn_reflns_theta_max         52.68
_diffrn_reflns_theta_min         3.78
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_source_current           45
_diffrn_source_voltage           45
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.305
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.668
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.9 (release 17-07-2007 CrysAlis171 .NET)
(compiled Aug 17 2007,17:36:27)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         3558
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.1304
_refine_ls_R_factor_gt           0.0602
_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^)+(0.0633P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1492
_reflns_number_gt                1655
_reflns_number_total             3558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814823f.txt
_cod_data_source_block           cs1165
_cod_database_code               7151035