Hydrogen-bonded three-dimensional network of a lanthanum(III) exocyclic complex with 5,10,15,20-tetra-4-pyridylporphyrin
Lipstman, Sophia; Goldberg, Israel; Acta Crystallographica Section C 65 (2009) m371–m373; doi:10.1107/S0108270109034532

data_2017326
_publ_section_title
;
 Hydrogen-bonded three-dimensional network of a lanthanum(III)
 exocyclic complex with 5,10,15,20-tetra-4-pyridylporphyrin
;
_journal_coeditor_code           FA3203
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m371
_journal_page_last               m373
_journal_paper_doi               10.1107/S0108270109034532
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[La (N O3)4 (C40 H27 N8) (H2 O)2] , 3C6 H4 Cl2'
_chemical_formula_moiety         'C40 H31 La N12 O14 , 3C6 H4 Cl2'
_chemical_formula_sum            'C58 H43 Cl6 La N12 O14'
_chemical_formula_weight         1483.65
_chemical_name_systematic
;
diaquatetranitrato[5-(pyridinium-4-yl)-10,15,20-tri-4-
pyridylporphyrin]lanthanum(III) 1,2-dichlorobenzene trisolvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.9840(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1527(3)
_cell_length_b                   28.5415(6)
_cell_length_c                   13.5331(2)
_cell_measurement_reflns_used    10292
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      1.41
_cell_volume                     6099.36(19)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and Mercury (Macrae <i>et al.</i>,
2006)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '1\% \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  0.0910
_diffrn_reflns_av_sigmaI/netI    0.1117
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            36533
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.17
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  0.9113
_exptl_absorpt_correction_T_min  0.7979
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.772
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         10767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0704P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1478
_reflns_number_gt                6137
_reflns_number_total             10767
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3203.cif
_cod_data_source_block           I
_cod_original_cell_volume        6099.34(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017326
_cod_database_fobs_code          2017326