Photochemistry of p-Benzoquinone Diazide Carboxylic Acids: Formation of 2,4-Didehydrophenols
Wolfram W. Sander; Götz Bucher; Holger Wandel; Elfi Kraka; Dieter Cremer; William S. Sheldrick; Journal of the American Chemical Society 119 (1997) 10660–10672; doi:10.1021/ja971731a

data_4117058
_publ_contact_author
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        Wolfram W. Sander 
        Lehrstuhl f\"ur Organische Chemie II
        Ruhr-Universit\"at Bochum
        Universit\"atsstrasse 150
        44780 Bochum
        Bundesrepublik Deutschland
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_publ_contact_author_email       sander@neon.orch.ruhr-uni-bochum.de
_publ_contact_author_fax         '049 234 709-353'
_publ_contact_author_phone       '049 234 700-4593'
_publ_section_title
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 Photochemistry of p-Benzoquinone Diazide Carboxylic Acids: Formation of
 2,4-Didehydrophenols
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_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10660
_journal_page_last               10672
_journal_paper_doi               10.1021/ja971731a
_journal_volume                  119
_journal_year                    1997
_chemical_formula_sum            'C11 H11 N2 O3'
_chemical_formula_weight         219.22
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.154(2)
_cell_length_b                   10.377(2)
_cell_length_c                   11.362(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      7.3
_cell_volume                     1077.1(4)
_computing_cell_refinement       'Siemens R3m/V'
_computing_data_collection       'Siemens R3m/V'
_computing_data_reduction        XDISK
_computing_molecular_graphics    'Siemens SHELXTL-PLUS(VMS)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      218(2)
_diffrn_measurement_device       'Siemens P4 4-circle-diffractometer'
_diffrn_measurement_method       'Profile fitted'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_sigmaI/netI    0.1156
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1498
_diffrn_reflns_theta_max         22.56
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        20
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.100
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       prism
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.78
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.200
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.907
_refine_ls_goodness_of_fit_obs   1.143
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         1401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_restrained_S_obs      1.143
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_obs          0.0609
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1596
_refine_ls_wR_factor_obs         0.1274
_reflns_number_observed          646
_reflns_number_total             1401
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja971731a.cif
_cod_data_source_block           sand2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0753P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4117058