Efficient microwave-assisted synthesis of amine-substituted tetrakis(pentafluorophenyl)porphyrin.
Samaroo, Diana; Soll, Clifford E.; Todaro, Louis J.; Drain, Charles M.; Organic letters 8 (2006) 4985–4988; doi:10.1021/ol060946z

data_1506043
_publ_section_title
;
 Efficient microwave-assisted synthesis of amine-substituted
 tetrakis(pentafluorophenyl)porphyrin.
;
_journal_issue                   22
_journal_name_full               'Organic letters'
_journal_page_first              4985
_journal_page_last               4988
_journal_paper_doi               10.1021/ol060946z
_journal_volume                  8
_journal_year                    2006
_chemical_formula_sum            'C39.5 H39 F8 N6 O4'
_chemical_formula_weight         813.77
_chemical_name_systematic
;
 ?
;
_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-97
_cell_angle_alpha                91.03(3)
_cell_angle_beta                 104.31(3)
_cell_angle_gamma                107.76(3)
_cell_formula_units_Z            2
_cell_length_a                   10.750(2)
_cell_length_b                   10.912(2)
_cell_length_c                   17.685(4)
_cell_measurement_temperature    373(2)
_cell_volume                     1904.5(8)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\w scans'
_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  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0772
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16118
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.120
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.9765
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.279
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         8724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1233
_refine_ls_R_factor_gt           0.0680
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+1.9897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                5349
_reflns_number_total             8724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol060946zsi20060419_020047.cif
_cod_data_source_block           x1536l
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        1904.5(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C39.50 H39 F8 N6 O4'
_cod_database_code               1506043