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_7107151
_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
'C48 H54 Fe2 O4 P4, 2(C16 H30 K N2 O6), 2(C2 H3 N)'
_chemical_formula_sum            'C84 H120 Fe2 K2 N6 O16 P4'
_chemical_formula_weight         1783.64
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                108.305(1)
_cell_angle_beta                 106.230(1)
_cell_angle_gamma                109.092(1)
_cell_formula_units_Z            1
_cell_length_a                   13.995(1)
_cell_length_b                   14.050(1)
_cell_length_c                   14.447(1)
_cell_measurement_reflns_used    7960
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     2305.8(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28523
_diffrn_reflns_theta_full        29.97
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.8728
_exptl_absorpt_correction_T_min  0.8137
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         13331
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+0.1565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                10339
_reflns_number_total             13331
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15421d.txt
_cod_data_source_block           em485
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7107151