Stepwise syntheses of tri- and tetraphosphaporphyrinogens
Duncan Carmichael; Aurelie Escalle-Lewis; Xavier Le Goff; Gilles Frison; Eric Muller; Chem.Commun. 48 (2012) 302–304; doi:10.1039/c1cc15421d

data_7107152
_publ_section_title
;
 Stepwise syntheses of tri- and tetraphosphaporphyrinogens
;
_journal_name_full               Chem.Commun.
_journal_page_first              302
_journal_page_last               304
_journal_paper_doi               10.1039/c1cc15421d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C61 H84 Fe K2 N O16 P3, C2 H3 N'
_chemical_formula_sum            'C63 H87 Fe K2 N2 O16 P3'
_chemical_formula_weight         1355.31
_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                 125.457(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.606(1)
_cell_length_b                   16.733(1)
_cell_length_c                   27.421(1)
_cell_measurement_reflns_used    797
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      0.998
_cell_volume                     6580.2(6)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Kappa APEX II'
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0897
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            58153
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_T_max  0.9902
_exptl_absorpt_correction_T_min  0.8987
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.641
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         11464
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.1279
_refine_ls_R_factor_gt           0.0968
_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^)+(0.0105P)^2^+32.3497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1767
_reflns_number_gt                8811
_reflns_number_total             11464
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15421d.txt
_cod_data_source_block           ae490
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7107152