Synthesis and Reactions of Phosphaporphyrins: Reconstruction of π-Skeleton Triggered by Oxygenation of a Core Phosphorus Atom
Takashi Nakabuchi; Makoto Nakashima; Shinya Fujishige; Haruyuki Nakano; Yoshihiro Matano; Hiroshi Imahori; Journal of Organic Chemistry 75 (2010) 375–389; doi:10.1021/jo902060b

data_4025155
_publ_section_title
;
 Synthesis and Reactions of Phosphaporphyrins: Reconstruction of
 \p-Skeleton Triggered by Oxygenation of a Core Phosphorus Atom
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              375
_journal_page_last               389
_journal_paper_doi               10.1021/jo902060b
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C42.50 H34 Cl3 N2 O P S'
_chemical_formula_sum            'C42.5 H34 Cl3 N2 O P S'
_chemical_formula_weight         758.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                73.315(14)
_cell_angle_beta                 68.206(9)
_cell_angle_gamma                83.527(13)
_cell_formula_units_Z            2
_cell_length_a                   9.4207(19)
_cell_length_b                   13.290(3)
_cell_length_c                   16.037(4)
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.25
_cell_volume                     1785.8(7)
_computing_cell_refinement       HKL2000
_computing_data_collection       'Crystal Clear'
_computing_data_reduction        HKL2000
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0898
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14291
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.9804
_exptl_absorpt_correction_T_min  0.9246
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            platelet
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       red
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         5964
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1583
_refine_ls_R_factor_gt           0.0878
_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^)+(0.1356P)^2^+2.4115P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2310
_refine_ls_wR_factor_ref         0.2804
_reflns_number_gt                3109
_reflns_number_total             5964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo902060b_si_001.cif
_cod_data_source_block           2
_cod_original_sg_symbol_Hall     '    -P 1'
_cod_original_formula_sum        'C42.50 H34 Cl3 N2 O P S'
_cod_database_code               4025155