Photoactivated Tungsten Hexacarbonyl-Catalyzed Conversion of Alkynols to Glycals
Peter Wipf; Thomas H. Graham; Journal of Organic Chemistry 68 (2003) 8798–8807; doi:10.1021/jo034813s

data_4022529
_publ_section_title
;
 Photoactivated Tungsten Hexacarbonyl-Catalyzed Conversion
 of Alkynols to Glycals
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              8798
_journal_page_last               8807
_journal_paper_doi               10.1021/jo034813s
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C19 H22 N2 O5'
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.7250(10)
_cell_angle_gamma                90.00
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_cell_length_b                   12.0213(6)
_cell_length_c                   20.2975(10)
_cell_measurement_reflns_used    8652
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.41
_cell_measurement_theta_min      2.63
_cell_volume                     1814.31(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
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_diffrn_reflns_av_R_equivalents  0.0257
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_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23035
_diffrn_reflns_theta_full        32.52
_diffrn_reflns_theta_max         32.52
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9774
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             760
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_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_parameters     323
_refine_ls_number_reflns         6407
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_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0846P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1542
_reflns_number_gt                4842
_reflns_number_total             6407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo034813ssi20030613_020353.cif
_cod_data_source_block           tomg918
_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 21/c'
_cod_database_code               4022529