The effects of strong Lewis-base reagents on supramolecular hydrogen bonding of meso-tetra(carboxyphenyl)porphyrins
Lipstman, Sophia; Muniappan, Sankar; George, Sumod; Goldberg, Israel; CrystEngComm 8 (2006) 601–; doi:10.1039/b608852j

data_7203542
_publ_section_title
;
 The effects of strong Lewis-base reagents on supramolecular hydrogen
 bonding of meso-tetra(carboxyphenyl)porphyrins
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              601
_journal_paper_doi               10.1039/b608852j
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C48 H28 N4 O8 Pd, 4(C2 H6 O S)'
_chemical_formula_sum            'C56 H52 N4 O12 Pd S4'
_chemical_formula_weight         1207.66
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b 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            4
_cell_length_a                   17.3027(2)
_cell_length_b                   14.0365(2)
_cell_length_c                   22.2494(3)
_cell_measurement_reflns_used    7172
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.18
_cell_volume                     5403.70(12)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        'Denzo & Scalepack'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi 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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43072
_diffrn_reflns_theta_full        28.24
_diffrn_reflns_theta_max         28.24
_diffrn_reflns_theta_min         2.18
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  0.8716
_exptl_absorpt_correction_T_min  0.7851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.767
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     384
_refine_ls_number_reflns         6608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0679P)^2^+6.1136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                4833
_reflns_number_total             6608
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B608852J.txt
_cod_data_source_block           Compound-4
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               7203542