Structural Variation in Porphyrin Pillared Homologous Series: Influence of Distinct Coordination Centers for Pillars on Framework Topology
Chung, Haemi; Barron, Paul M.; Novotny, Richard W.; Son, Hyun-Tak; Hu, Chunhua; Choe, Wonyoung; Crystal Growth & Design 9 (2009) 3327–; doi:10.1021/cg900220g

data_4509521
_publ_section_title
;
 Structural Variation in Porphyrin Pillared Homologous Series: Influence
 of Distinct Coordination Centers for Pillars on Framework Topology
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3327
_journal_paper_doi               10.1021/cg900220g
_journal_volume                  9
_journal_year                    2009
_chemical_formula_moiety         'C66 H36 N13 O8 Zn3'
_chemical_formula_sum            'C66 H36 N13 O8 Zn3'
_chemical_formula_weight         1335.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           139
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2'
_symmetry_space_group_name_H-M   'I 4/m m m'
_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                   16.6790(4)
_cell_length_b                   16.6790(4)
_cell_length_c                   71.0521(18)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.30
_cell_measurement_theta_min      2.29
_cell_volume                     19765.9(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       84
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            85541
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  0.9556
_exptl_absorpt_correction_T_min  0.8203
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2708
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
Disordered, independent solvent molecules were eliminated from the refinement 
using SQUEEZE/PLATON [Spek, A.L. (2003), J. Appl. Cryst. 36, 7-13].

R factors before data are squeezed:
_refine_ls_R_factor_all           0.2738 
_refine_ls_R_factor_gt            0.2233 
_refine_ls_wR_factor_ref          0.6386 
_refine_ls_wR_factor_gt           0.6188 

;
_refine_diff_density_max         1.011
_refine_diff_density_min         -1.137
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         5061
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1468P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2208
_refine_ls_wR_factor_ref         0.2369
_reflns_number_gt                3216
_reflns_number_total             5061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg900220gsup5.cif
_cod_data_source_block           09wyc7hsq
_cod_original_sg_symbol_H-M      'I 4/mmm'
_cod_database_code               4509521