A short asymmetric route to the bromophycolide A and D skeleton.
Lin, Hongkun; Pochapsky, Susan S.; Krauss, Isaac J.; Organic letters 13 (2011) 1222–1225; doi:10.1021/ol200099n

data_1502027
_publ_section_title
;
 A short asymmetric route to the bromophycolide A and D skeleton.
;
_journal_issue                   5
_journal_name_full               'Organic letters'
_journal_page_first              1222
_journal_page_last               1225
_journal_paper_doi               10.1021/ol200099n
_journal_volume                  13
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C29 H41 Br1 O4'
_chemical_formula_sum            'C29 H41 Br O4'
_chemical_formula_weight         533.55
_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
_audit_creation_date             09-09-22
_audit_creation_method           CRYSTALS_ver_12.87
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4428(6)
_cell_length_b                   10.0656(7)
_cell_length_c                   32.412(2)
_cell_measurement_reflns_used    8273
_cell_measurement_temperature    120
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2754.4(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
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_diffrn_reflns_limit_h_min       -10
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -41
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_diffrn_reflns_theta_max         27.028
_diffrn_reflns_theta_min         1.256
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.523
_exptl_absorpt_correction_T_max  0.83
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_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'acicular fragment'
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_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.126
_refine_diff_density_max         0.52
_refine_diff_density_min         -0.63
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.000(6)
_refine_ls_extinction_method     None
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_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         6023
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.0135880
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.03P)^2^ + 0.89P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0673
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0673
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              41
_reflns_limit_l_min              0
_reflns_number_gt                5179
_reflns_number_total             6023
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.10
_oxford_diffrn_Wilson_scale      3.78
_oxford_refine_ls_r_factor_ref   0.0427
_oxford_refine_ls_scale          0.18838(8)
_oxford_reflns_number_all        6023
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'LHK1_101_1_0m in P2(1)2(1)2(1)'
_cod_data_source_file            ol200099n_si_001.cif
_cod_data_source_block           global
_cod_depositor_comments
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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      'P 21 21 21 '
_cod_original_formula_sum        'C29 H41 Br1 O4'
_cod_database_code               1502027