Synthesis of the originally proposed structures of elatenyne and an enyne from Laurencia majuscula
Sheldrake, Helen M.; Jamieson, Craig; Pascu, Sofia I.; Burton, Jonathan W.; Organic & Biomolecular Chemistry 7 (2009) 238–252; doi:10.1039/b814953d

data_7150544
_publ_section_title
;
 Synthesis of the originally proposed structures of elatenyne and an
 enyne from Laurencia majuscula
;
_journal_issue                   2
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              238
_journal_page_last               252
_journal_paper_doi               10.1039/b814953d
_journal_volume                  7
_journal_year                    2009
_chemical_absolute_configuration syn
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C15 H20 O5 S1 '
_chemical_formula_sum            'C15 H20 O5 S'
_chemical_formula_weight         312.38
_space_group_IT_number           4
_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
_audit_creation_date             03-20-11
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 105.644(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.5615(17)
_cell_length_b                   27.699(8)
_cell_length_c                   10.094(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    293
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1497.4(8)
_computing_cell_refinement
;
Bruker SAINT version 6.36a (Bruker, 2002)
;
_computing_data_collection
;
SMART (Siemens, 1993)
;
_computing_data_reduction
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Bruker SAINT version 6.36a (Bruker, 2002)
;
_computing_molecular_graphics
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CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SHELXS 86 (Sheldrick, 1986)
;
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type
;
Bruker AXS SMART 1K CCD diffractometer
;
_diffrn_measurement_method       'thin slice \w-scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_av_R_equivalents  0.02
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -13
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_diffrn_reflns_theta_full        27.841
_diffrn_reflns_theta_max         28.409
_diffrn_reflns_theta_min         2.095
_diffrn_standards_decay_%        0.00
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_exptl_absorpt_correction_T_max  1.00
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS
;
_exptl_crystal_colour            ' white '
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_exptl_crystal_description       ' prism '
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_exptl_crystal_size_mid          0.02
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_refine_ls_abs_structure_details 'Flack, 3243 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.008(80)
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4429
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002658
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2]^2
A~i~ are:
0.338 0.262 0.184
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0728
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0493
_reflns_limit_h_max              7
_reflns_limit_h_min              -7
_reflns_limit_k_max              36
_reflns_limit_k_min              -36
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                4429
_reflns_number_total             6771
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b814953d_a.txt
_cod_data_source_block           cam174S_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C15 H20 O5 S1 '
_cod_database_code               7150544