Synthesis and Reactions of 20 π-Electron β-Tetrakis(trifluoromethyl)-meso-tetraphenylporphyrins
Chao Liu; Dong-Mei Shen; Qing-Yun Chen; Journal of the American Chemical Society 129 (2007) 5814–5815; doi:10.1021/ja070855c

data_4109392
_publ_section_title
;
 Synthesis and Reactions of 20 \p-Electron
 \b-Tetrakis(trifluoromethyl)-meso-tetraphenylporphyrins
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5814
_journal_page_last               5815
_journal_paper_doi               10.1021/ja070855c
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C53 H38 Cl2 F12 N4'
_chemical_formula_weight         1029.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.61(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.440(15)
_cell_length_b                   22.28(2)
_cell_length_c                   15.994(16)
_cell_measurement_reflns_used    1673
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.155
_cell_measurement_theta_min      4.487
_cell_volume                     5040(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.1166
_diffrn_reflns_av_sigmaI/netI    0.1566
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26394
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8354
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.507
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.0019(6)
_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_ref   0.911
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         9383
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.2013
_refine_ls_R_factor_gt           0.0876
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.029
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1208P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2261
_refine_ls_wR_factor_ref         0.2780
_reflns_number_gt                3553
_reflns_number_total             9383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070855csi20070206_124023.cif
_cod_data_source_block           cd2708
_cod_database_code               4109392