Gateway synthesis of daphnane congeners and their protein kinase C affinities and cell-growth activities.
Wender, Paul A.; Buschmann, Nicole; Cardin, Nathan B.; Jones, Lisa R.; Kan, Cindy; Kee, Jung-Min; Kowalski, John A.; Longcore, Kate E.; Nature chemistry 3 (2011) 615–619; doi:10.1038/nchem.1074

data_1507957
_publ_section_title
;
 Gateway synthesis of daphnane congeners and their protein kinase C
 affinities and cell-growth activities.
;
_journal_issue                   8
_journal_name_full               'Nature chemistry'
_journal_page_first              615
_journal_page_last               619
_journal_paper_doi               10.1038/nchem.1074
_journal_volume                  3
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H47 Br O6 Si'
_chemical_formula_sum            'C33 H47 Br O6 Si'
_chemical_formula_weight         647.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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            8
_cell_length_a                   10.0180(3)
_cell_length_b                   10.0180(3)
_cell_length_c                   66.931(4)
_cell_measurement_reflns_used    3028
_cell_measurement_temperature    142
_cell_measurement_theta_max      19.7
_cell_measurement_theta_min      2.13
_cell_volume                     6717.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      142
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
;
;
_diffrn_measurement_method
;
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1157
_diffrn_reflns_av_sigmaI/netI    0.1386
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       74
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20310
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        'not measured'
_diffrn_standards_interval_count 'not measured'
_diffrn_standards_interval_time  'not measured'
_diffrn_standards_number         'not measured'
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.56
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker AXS XPREP, SHELXTL v6.1 (2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.725
_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   -0.011(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         4818
_refine_ls_number_restraints     118
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                2987
_reflns_number_total             4818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.1074-s4.cif
_cod_data_source_block           shelxl
_cod_database_code               1507957