An unusual ring expansion from the Zav’yalov pyrrole synthesis: formation of oxacino[2,3-c]pyrroles
Gabbutt, Christopher D.; Hepworth, John D.; Mark Heron, B.; Elsegood, Mark R. J.; Clegg, William; Chemical Communications  (1999) 289–; doi:10.1039/a809033e

data_7110414
_publ_section_title
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 An unusual ring expansion from the Zav&#x2019;yalov pyrrole synthesis:
 formation of oxacino[2,3-c]pyrroles
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_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              289
_journal_paper_doi               10.1039/a809033e
_journal_year                    1999
_chemical_formula_sum            'C17 H23 N O4'
_chemical_formula_weight         305.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL
_cell_angle_alpha                78.530(14)
_cell_angle_beta                 89.250(12)
_cell_angle_gamma                81.025(9)
_cell_formula_units_Z            2
_cell_length_a                   7.7540(11)
_cell_length_b                   8.8328(12)
_cell_length_c                   12.476(2)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.36
_cell_measurement_theta_min      25.23
_cell_volume                     827.0(2)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-93 and local programs'
_computing_structure_refinement  SHELXL-93
_computing_structure_solution    SHELXTL/PC
_diffrn_ambient_temperature      160(2)
_diffrn_measurement_device       'Stoe-Siemens diffractometer'
_diffrn_measurement_method       '\w/\q scans with on-line profile fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5549
_diffrn_reflns_theta_max         64.96
_diffrn_reflns_theta_min         3.62
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.226
_exptl_crystal_description       prism
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.17
_refine_diff_density_max         .320
_refine_diff_density_min         -.243
_refine_diff_density_rms         .052
_refine_ls_extinction_coef       0.0071(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         2777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.054
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_obs          0.0471
_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^)+(0.0531P)^2^+0.2831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1095
_refine_ls_wR_factor_obs         0.1072
_reflns_number_observed          2632
_reflns_number_total             2778
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809033esup1.cif
_cod_data_source_block           esr3
_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^)+(0.0531P)^2^+0.2831P] 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^)+(0.0531P)^2^+0.2831P] 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_original_sg_symbol_H-M      P-1
_cod_database_code               7110414