Model porphyrin precursors: 1,2,4,5-tetrakis(cyanomethyl)benzene, methyl 3,4,5-triacetoxybenzoate and 2-(<i>N</i>-phthalimidomethyl)benzoic acid
Jene, Paul G.; Ibers, James A.; Acta Crystallographica Section C 56 (2000) 246–249; doi:10.1107/S0108270199014663

data_2010592
_publ_section_title
;
 Model porphyrin precursors: 1,2,4,5-tetrakis(cyanomethyl)benzene,
 methyl 3,4,5-triacetoxybenzoate and
 2-(<i>N</i>-phthalimidomethyl)benzoic acid
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              246
_journal_page_last               249
_journal_paper_doi               10.1107/S0108270199014663
_journal_volume                  56
_journal_year                    2000
_chemical_formula_sum            'C16 H11 N O4'
_chemical_formula_weight         281.26
_chemical_melting_point          263.0(10)
_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'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 96.722(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1250(10)
_cell_length_b                   13.7200(10)
_cell_length_c                   7.7247(8)
_cell_measurement_reflns_used    2323
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.69
_cell_volume                     1276.21(19)
_computing_cell_refinement       'SMART version 5.054 (Bruker, 1999)'
_computing_data_collection       'SMART version 5.054 (Bruker, 1999)'
_computing_data_reduction        'SAINT-Plus version 6.0 (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL-99 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL-99 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-99 (Sheldrick, 1999)'
_computing_structure_solution    'SHELXS-99 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .026
_diffrn_reflns_av_sigmaI/netI    .0314
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6929
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.69
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    .107
_exptl_absorpt_correction_T_max  .992
_exptl_absorpt_correction_T_min  .974
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed (Sheldrick, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             584
_exptl_crystal_size_max          .33
_exptl_crystal_size_mid          .17
_exptl_crystal_size_min          .08
_refine_diff_density_max         .158
_refine_diff_density_min         -.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    'H atoms; see below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          .0539
_refine_ls_R_factor_gt           .036
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
w = 1/[\s^2^(Fo^2^)+(0.04Fo^2^)^2^]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .089
_reflns_number_gt                1722
_reflns_number_total             2365
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk1493.cif
_cod_data_source_block           III
_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 '262.0-264.0' was changed to
'263.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '262.0-264.0' was changed to
'263.0(10)' - the average value was taken and precision was
estimated.

'_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1276.2(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2010592