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_2016379
_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)], C H4 O'
_chemical_formula_moiety         'C48 H28 N4 O8 Pd, C H4 O'
_chemical_formula_sum            'C49 H32 N4 O9 Pd'
_chemical_formula_weight         927.21
_chemical_name_systematic
;
[5,10,15,20-tetrakis(4-carboxyphenyl)porphyrinato]palladium(II)
methanol solvate
;
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.0347(6)
_cell_length_b                   15.9441(11)
_cell_length_c                   18.3824(7)
_cell_measurement_reflns_used    4588
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.60
_cell_measurement_theta_min      2.55
_cell_volume                     9096.0(7)
_computing_cell_refinement       'Denzo (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius, 1999)'
_computing_data_reduction
'Denzo and Scalepack (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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '0.5 deg. \f 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  0.0980
_diffrn_reflns_av_sigmaI/netI    0.1178
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20365
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         2.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhomb
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.773
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         4344
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1191
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0724P)^2^+2.4049P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                2688
_reflns_number_total             4344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gd3172.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               2016379
_cod_database_fobs_code          2016379