Synthesis of [28]Heptaphyrin(1.0.0.1.0.0.0) and [32]Octaphyrin(1.0.0.0.1.0.0.0) via a Directed Oxidative Ring Closure: The First Expanded Porphyrins Containing a Quaterpyrrole Subunit
Jonathan L. Sessler; Daniel Seidel; Vincent Lynch; Journal of the American Chemical Society 121 (1999) 11257–11258; doi:10.1021/ja992934x

data_4116625
_publ_section_title
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 Synthesis of [28]Heptaphyrin(1.0.0.1.0.0.0) and
 [32]Octaphyrin(1.0.0.0.1.0.0.0) via a Directed Oxidative Ring Closure:
 The First Expanded Porphyrins Containing a Quaterpyrrole Subunit
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11257
_journal_page_last               11258
_journal_paper_doi               10.1021/ja992934x
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C48 H52 Cl2 N8 O2'
_chemical_formula_weight         843.88
_chemical_name_systematic
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 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                92.146(2)
_cell_angle_beta                 103.2450(15)
_cell_angle_gamma                104.125(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7120(3)
_cell_length_b                   13.3270(3)
_cell_length_c                   18.1620(6)
_cell_measurement_temperature    153(2)
_cell_volume                     2435.51(12)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Nonius Kappa CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0933
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20143
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.178
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_F_000             892
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0029(11)
_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   1.601
_refine_ls_goodness_of_fit_obs   1.934
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         11961
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.601
_refine_ls_restrained_S_obs      1.934
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_obs          0.1013
_refine_ls_shift/esd_max         -0.080
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+2.4581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2416
_refine_ls_wR_factor_obs         0.2263
_reflns_number_observed          7373
_reflns_number_total             11961
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja992934x_2.cif
_cod_data_source_block           JA992934X-63_[32]Octaphyrin
_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^)+(0.0426P)^2^+2.4581P] 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^)+(0.0426P)^2^+2.4581P] 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               4116625