Crystal Engineering of “Porphyrin Sieves” Based on Coordination Polymers of Pd- and Pt-tetra(4-carboxyphenyl)porphyrin
Shmilovits, Michaela; Diskin-Posner, Yael; Vinodu, Mikki; Goldberg, Israel; Crystal Growth & Design 3 (2003) 855–; doi:10.1021/cg034071w

data_4505733
_publ_section_title
;
 Crystal Engineering of &#x201C;Porphyrin Sieves&#x201D; Based on
 Coordination Polymers of Pd- and Pt-tetra(4-carboxyphenyl)porphyrin
;
_journal_issue                   5
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              855
_journal_paper_doi               10.1021/cg034071w
_journal_volume                  3
_journal_year                    2003
_chemical_formula_moiety
'(C48 H24 N4 O8 Pd), Cu1.50, Na1.50, 3.5(C5 H5 N), (H2 O)'
_chemical_formula_sum            'C65.5 H43.5 Cu1.5 N7.5 Na1.5 O9 Pd'
_chemical_formula_weight         1315.77
_chemical_name_systematic
; 
 ? 
;
_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                86.1930(6)
_cell_angle_beta                 85.9540(6)
_cell_angle_gamma                80.8150(7)
_cell_formula_units_Z            2
_cell_length_a                   12.8740(2)
_cell_length_b                   13.0790(2)
_cell_length_c                   16.4710(4)
_cell_measurement_reflns_used    9058
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.06
_cell_volume                     2726.70(9)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & Omega 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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.1043
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20640
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.992
_exptl_absorpt_correction_T_max  0.8655
_exptl_absorpt_correction_T_min  0.7896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.924
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         12739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0913
_refine_ls_R_factor_gt           0.0532
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+3.8379P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1194
_reflns_number_gt                9058
_reflns_number_total             12739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg034071wsi20030504_115923.cif
_cod_data_source_block           Compound-3
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C65.50 H43.50 Cu1.50 N7.50 Na1.50 O9 Pd'
_cod_database_code               4505733