Synthesis of 19-substituted geldanamycins with altered conformations and their binding to heat shock protein Hsp90
Russell R. A. Kitson; Chuan-Hsin Chang; Rui Xiong; Huw E. L. Williams; Adrienne L. Davis; William Lewis; Donna L. Dehn; David Siegel; S. Mark Roe; Chrisostomos Prodromou; David Ross; Christopher J. Moody; Nature Chemistry 5 (2013) 307–314; doi:10.1038/nchem.1596

data_1551419
_publ_section_title
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 Synthesis of 19-substituted geldanamycins with altered conformations and
 their binding to heat shock protein Hsp90
;
_journal_name_full               'Nature Chemistry'
_journal_page_first              307
_journal_page_last               314
_journal_paper_doi               10.1038/nchem.1596
_journal_volume                  5
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C33 H42 N2 O10, C4 H8 O'
_chemical_formula_sum            'C37 H50 N2 O11'
_chemical_formula_weight         698.79
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 93.853(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.5002(7)
_cell_length_b                   10.3073(10)
_cell_length_c                   16.5868(17)
_cell_measurement_reflns_used    5445
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      75.61
_cell_measurement_theta_min      4.22
_cell_volume                     1791.1(3)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    ' ? '
_computing_publication_material  'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_sigmaI/netI    0.0999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18836
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         75.80
_diffrn_reflns_theta_min         4.22
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  1.23
_exptl_absorpt_correction_T_min  0.852
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) 
(compiled Jan  5 2010,16:28:46) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       plate
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.3928
_exptl_crystal_size_mid          0.1871
_exptl_crystal_size_min          0.0139
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 2381 Friedel pairs'
_refine_ls_abs_structure_Flack   0.2(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     459
_refine_ls_number_reflns         6786
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0844
_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^)+(0.0760P)^2^+4.4733P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1962
_refine_ls_wR_factor_ref         0.2266
_reflns_number_gt                4603
_reflns_number_total             6786
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            nchem.1596-s2.cif
_cod_data_source_block           RKCJMA
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1551419