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_7150545
_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 ad
_chemical_formula_moiety         'C15 H20 O5 S1'
_chemical_formula_sum            'C15 H20 O5 S'
_chemical_formula_weight         312.39
_chemical_melting_point          ?
_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             08-12-10
_audit_creation_method           CRYSTALS_ver_12.86
_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    3494
_cell_measurement_temperature    150
_cell_measurement_theta_max      55
_cell_measurement_theta_min      5
_cell_volume                     1497.4(8)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'Bruker SAINT version 6.36a (Bruker, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       Unknown
_diffrn_measurement_device_type  Serial
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68980
_diffrn_reflns_av_R_equivalents  0.028
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_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
_diffrn_reflns_number            10048
_diffrn_reflns_theta_full        26.950
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.033
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            clear_pale_colourless
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.60
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_details 'Flack (1983), 2957 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.04(8)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0051
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6755
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0763
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.000371
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 0.32P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1238
_refine_ls_wR_factor_gt          0.1102
_refine_ls_wR_factor_ref         0.1238
_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                5013
_reflns_number_total             6771
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.13
_oxford_diffrn_Wilson_scale      32.03
_oxford_refine_ls_r_factor_ref   0.0763
_oxford_refine_ls_scale          0.17938(10)
_oxford_reflns_number_all        6755
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title cam172
_cod_data_source_file            b814953d_b.txt
_cod_data_source_block           sulfone-38
_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 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        'C15 H20 O5 S1'
_cod_database_code               7150545