Supramolecular hydrogen bonding of [5,10,15,20-tetrakis(4-carboxyphenyl)porphyrinato]palladium(II) in the presence of competing solvents
Sophia Lipstman; Israel Goldberg; Acta Crystallographica Section C 64 (2008) m53–m57; doi:10.1107/S0108270107063524

data_2016380
_publ_section_title
;
 Supramolecular hydrogen bonding of
 [5,10,15,20-tetrakis(4-carboxyphenyl)porphyrinato]palladium(II) in the
 presence of competing solvents
;
_journal_coeditor_code           GD3172
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m53
_journal_page_last               m57
_journal_paper_doi               10.1107/S0108270107063524
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Pd (C48 H28 N4 O8)], 4C3 H7 N O, 4H2 O'
_chemical_formula_moiety         'C48 H28 N4 O8 Pd, 4(C3 H7 N O), 4(H2 O)'
_chemical_formula_sum            'C60 H64 N8 O16 Pd'
_chemical_formula_weight         1259.61
_chemical_name_systematic
;
[5,10,15,20-tetrakis(4-carboxyphenyl)porphyrinato]palladium(II)--
<i>N</i>,<i>N</i>'-dimethylformamide--water (1/4/4)
;
_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                81.3820(16)
_cell_angle_beta                 87.3282(17)
_cell_angle_gamma                87.0384(17)
_cell_formula_units_Z            1
_cell_length_a                   7.7243(2)
_cell_length_b                   13.2668(4)
_cell_length_c                   14.5878(5)
_cell_measurement_reflns_used    5044
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      1.41
_cell_volume                     1474.91(8)
_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, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. \f and \w scans'
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12855
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.25
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             654
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.724
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     437
_refine_ls_number_reflns         5498
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+1.3991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0825
_reflns_number_gt                4868
_reflns_number_total             5498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gd3172.cif
_cod_data_source_block           II
_cod_database_code               2016380
_cod_database_fobs_code          2016380