Oligocyclization of 2-(hydroxymethyl)pyrroles with electron-withdrawing groups at β-positions: formation and structural elucidation of porphyrinogens and hexaphyrinogens
Uno, Hidemitsu; Inoue, Kentarou; Inoue, Takashi; Ono, Noboru; Organic & Biomolecular Chemistry 1 (2003) 3857–3865; doi:10.1039/b307132d

data_7151528
_publ_section_title
;
 Oligocyclization of 2-(hydroxymethyl)pyrroles with electron-withdrawing
 groups at \b-positions: formation and structural elucidation of
 porphyrinogens and hexaphyrinogens
;
_journal_coden_ASTM              OBCRAK
_journal_issue                   21
_journal_name_full               'Organic & Biomolecular Chemistry'
_journal_page_first              3857
_journal_page_last               3865
_journal_paper_doi               10.1039/b307132d
_journal_volume                  1
_journal_year                    2003
_chemical_formula_moiety
;
C68 H12 F40 N4, 2(C3 H7 N O), 2(C0.85 H0.85 Cl2.55), 2(C0.15 H0.15 Cl0.45)
;
_chemical_formula_sum            'C76 H28 Cl6 F40 N6 O2'
_chemical_formula_weight         2029.75
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 100.47(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.679(3)
_cell_length_b                   10.995(4)
_cell_length_c                   23.426(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.2
_cell_measurement_theta_max      12.4
_cell_measurement_theta_min      10.5
_cell_volume                     3971.2(17)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    'Ortep-3 and Mercury '
_computing_publication_material  'teXsan Ver. 1.11'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       w-2q
_diffrn_radiation_type           'Mo Ka'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9956
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_decay_%        0.15
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.878
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.79
_refine_ls_goodness_of_fit_ref   1.327
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     609
_refine_ls_number_reflns         9111
_refine_ls_R_factor_gt           0.0769
_refine_ls_shift/su_max          0.0007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2003
_reflns_number_gt                4033
_reflns_number_total             9129
_reflns_threshold_expression     F^2^>2.0s(F^2^)
_cod_data_source_file            b307132d.txt
_cod_data_source_block           3g-2DMF-2CHCl3
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_geom_hbond_site_distance_dh' replaced with
'_geom_hbond_distance_DH' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_hbond_site_distance_ha' replaced with
'_geom_hbond_distance_HA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

data
name '_geom_hbond_site_distance_da' replaced with
'_geom_hbond_distance_DA' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 5005 2017-03-03 11:38:54Z antanas 
;
_cod_original_cell_volume        3971(1)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C76 H28 Cl6 F40 N6 O2 '
_cod_database_code               7151528