Cinnabaramides A-G: analogues of lactacystin and salinosporamide from a terrestrial streptomycete.
Stadler, Marc; Bitzer, Jens; Mayer-Bartschmid, Anke; Müller, Hartwig; Benet-Buchholz, Jordi; Gantner, Florian; Tichy, Hans-Volker; Reinemer, Peter; Bacon, Kevin B.; Journal of natural products 70 (2007) 246–252; doi:10.1021/np060162u

data_1505216
_publ_contact_author
;
    Dr. Benet-Buchholz, Jordi
    Institut Catal\`a d'Investigaci\'o Qu\'imica (ICIQ)
    X-ray Diffraction Unit
    Avgda. Pa\=isos Catalans 16
    E-43007 Tarragona, Spain
;
_publ_section_title
;
 Cinnabaramides A-G: analogues of lactacystin and salinosporamide from a
 terrestrial streptomycete.
;
_journal_issue                   2
_journal_name_full               'Journal of natural products'
_journal_page_first              246
_journal_page_last               252
_journal_paper_doi               10.1021/np060162u
_journal_volume                  70
_journal_year                    2007
_chemical_absolute_configuration ad
_chemical_formula_sum            'C19 H29 N O4'
_chemical_formula_weight         335.43
_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            48
_cell_length_a                   13.0624(2)
_cell_length_b                   29.0453(5)
_cell_length_c                   58.4559(11)
_cell_measurement_reflns_used    9999
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      54.04
_cell_measurement_theta_min      2.73
_cell_volume                     22178.2(7)
_computing_cell_refinement       'SAINT+ Version 6.22 Bruker AXS, 2002'
_computing_data_collection       'Bruker-Nonius, Proteum 1.37, 2002'
_computing_data_reduction        'SAINT+ Version 6.22 Bruker AXS, 2002'
_computing_molecular_graphics    'Shelxtl Version 6.10 (Sheldrick, 2000)'
_computing_publication_material  'Shelxtl Version 6.10 (Sheldrick, 2000)'
_computing_structure_refinement  'Shelxtl Version 6.10 (Sheldrick, 2000)'
_computing_structure_solution    'Shelxtl Version 6.10 (Sheldrick, 2000)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 1024
_diffrn_detector_type            'Proteum CCD area detector 6000 K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'three-circle diffractometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support
'magnetic support whith 20 micron nylon fiber cryoloop'
_diffrn_radiation_monochromator  'Multilayer Montel mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1073
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            205845
_diffrn_reflns_theta_full        54.33
_diffrn_reflns_theta_max         54.33
_diffrn_reflns_theta_min         1.51
_diffrn_source                   'rotating anode X-ray tube'
_diffrn_source_current           120
_diffrn_source_power             40
_diffrn_source_size              '3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.674
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.719869
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2.1 2003 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8736
_exptl_crystal_preparation
;
 Slow evaporation of a mixture propanol/diacetone alcohol
 (ratio 97:3) at 46 degrees celsius
;
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2674
_refine_ls_number_reflns         26995
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0781
_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^)+(0.0695P)^2^+41.5811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.1989
_reflns_number_gt                21119
_reflns_number_total             26995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            np060162usi20061107_063718.cif
_cod_data_source_block           js36010ag
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_measurement_specimen_suppport' tag replaced with
'_diffrn_measurement_specimen_support'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               1505216