Pillared Porphyrin Homologous Series: Intergrowth in Metal-Organic Frameworks
Eun-Young Choi; Paul M. Barron; Richard W. Novotny; Hyun-Tak Son; Chunhua Hu; Wonyoung Choe; Inorganic Chemistry 48 (2009) 426–428; doi:10.1021/ic801677y

data_4301221
_publ_section_title
;
Pillared Porphyrin Homologous Series: Intergrowth in Metal-Organic
Frameworks
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              426
_journal_page_last               428
_journal_paper_doi               10.1021/ic801677y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C63 H36 N7 O8 Zn3'
_chemical_formula_sum            'C63 H36 N7 O8 Zn3'
_chemical_formula_weight         1215.10
_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           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7122(2)
_cell_length_b                   16.7122(2)
_cell_length_c                   54.2436(14)
_cell_measurement_reflns_used    9431
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.13
_cell_measurement_theta_min      2.24
_cell_volume                     15150.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full .998
_diffrn_measured_fraction_theta_max .998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '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  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0120
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       72
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            180349
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.494
_exptl_absorpt_correction_T_max  0.9163
_exptl_absorpt_correction_T_min  0.7693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2468
_exptl_crystal_size_max          0.560
_exptl_crystal_size_mid          0.464
_exptl_crystal_size_min          0.180
_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           0.0967 
_refine_ls_R_factor_gt            0.0838 
_refine_ls_wR_factor_ref          0.2960 
_refine_ls_wR_factor_gt           0.2715 
;
_refine_diff_density_max         .894
_refine_diff_density_min         -.349
_refine_diff_density_rms         .036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         5311
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0517P)^2^+1.8280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0898
_reflns_number_gt                4613
_reflns_number_total             5311
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic801677y_si_002.cif
_cod_data_source_block           c8ch2sq
_cod_original_sg_symbol_Hall     '-I 4 2 '
_cod_database_code               4301221