Phosphorus Complexes of N-Fused Porphyrin and Its Reduced Derivatives: New Isomers of Porphyrin Stabilized via Coordination
Anna Młodzianowska; Lechosław Latos-Grażyński; Ludmiła Szterenberg; Inorganic Chemistry 47 (2008) 6364–6374; doi:10.1021/ic800437y

data_4305455
_publ_section_title
;
Phosphorus Complexes of N-Fused Porphyrin and Its Reduced Derivatives: New
Isomers of Porphyrin Stabilized via Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6364
_journal_page_last               6374
_journal_paper_doi               10.1021/ic800437y
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C44 H27 N4 O P, C Cl2'
_chemical_formula_sum            'C45 H27 Cl2 N4 O P'
_chemical_formula_weight         741.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 106.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.968(5)
_cell_length_b                   10.148(3)
_cell_length_c                   22.786(7)
_cell_measurement_reflns_used    23521
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.4
_cell_measurement_theta_min      4.0
_cell_volume                     3533(2)
_computing_cell_refinement       'CrysalisRED (Oxford Diffraction,2006)'
_computing_data_collection       'CrysalisRED (Oxford Diffraction,2006)'
_computing_data_reduction        'CrysalisRED (Oxford Diffraction,2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Xcalibur PX kappa-geometry diffractometer with CCD Onyx camera'
_diffrn_measurement_method       '\f and \w'
_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  0.0830
_diffrn_reflns_av_sigmaI/netI    0.0884
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            54082
_diffrn_reflns_theta_full        27.0
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    0.273
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.827
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         7663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1288
_reflns_number_gt                4283
_reflns_number_total             7663
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800437y-file001.cif
_cod_data_source_block           aml1
_cod_original_cell_volume        3532.7(19)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4305455