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_4109390
_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            'C52 H36 Cl2 F12 N4 O'
_chemical_formula_weight         1031.75
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 107.201(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.678(3)
_cell_length_b                   14.800(3)
_cell_length_c                   21.393(4)
_cell_measurement_reflns_used    1010
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.476
_cell_measurement_theta_min      4.844
_cell_volume                     4741.9(16)
_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  0.1508
_diffrn_reflns_av_sigmaI/netI    0.2343
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24524
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64756
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.846
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8796
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.2682
_refine_ls_R_factor_gt           0.0993
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2409
_refine_ls_wR_factor_ref         0.3135
_reflns_number_gt                3426
_reflns_number_total             8796
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070855csi20070206_123946.cif
_cod_data_source_block           cd26369
_cod_original_cell_volume        4741.8(15)
_cod_database_code               4109390