Regioselective phosphorylation and thiophosphorylation of N-confused porphyrin: a route to hybrid carbaporphyrinoids.
Grzegorzek, Norbert; Latos-Grażyński, Lechosław; Szterenberg, Ludmiła; Organic & biomolecular chemistry 10 (2012) 8064–8075; doi:10.1039/c2ob26019k

data_7152645
_publ_section_title
;
 Regioselective phosphorylation and thiophosphorylation of N-confused
 porphyrin: a route to hybrid carbaporphyrinoids.
;
_journal_issue                   40
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              8064
_journal_page_last               8075
_journal_paper_doi               10.1039/c2ob26019k
_journal_volume                  10
_journal_year                    2012
_chemical_formula_sum            'C60 H47 N4 P S2'
_chemical_formula_weight         919.11
_chemical_name_systematic
;
5,10,15,20-Tetratolyl-2-aza-21-carbaporphiryno-21-diphenylphosphinodithioate
;
_space_group_IT_number           14
_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
_audit_update_record
;
2012-03-16 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.53(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.678(4)
_cell_length_b                   15.687(4)
_cell_length_c                   20.796(6)
_cell_measurement_temperature    100(2)
_cell_volume                     4708(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.923
_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  0.0532
_diffrn_reflns_av_sigmaI/netI    0.1117
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            57874
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         4.65
_exptl_absorpt_coefficient_mu    0.193
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         19138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1111
_refine_ls_wR_factor_ref         0.1174
_reflns_number_gt                9965
_reflns_number_total             19138
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ob26019k.txt
_cod_data_source_block           ng08
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7152645