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_4301220
_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         'C68 H40 N8 O8 Co3, (N O3)'
_chemical_formula_sum            'C68 H40 Co3 N9 O11'
_chemical_formula_weight         1335.88
_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            2
_cell_length_a                   16.6007(2)
_cell_length_b                   16.6007(2)
_cell_length_c                   24.6892(5)
_cell_measurement_reflns_used    8330
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.87
_cell_measurement_theta_min      2.39
_cell_volume                     6803.93(18)
_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      100(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_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  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0179
_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       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            45975
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.393
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_correction_T_min  0.9155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    0.652
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.07
_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           0.1490 
_refine_ls_R_factor_gt            0.1314 
_refine_ls_wR_factor_ref          0.3827 
_refine_ls_wR_factor_gt           0.3711 
;
_refine_diff_density_max         .927
_refine_diff_density_min         -.638
_refine_diff_density_rms         .109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1759
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0974
_refine_ls_R_factor_gt           0.0801
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1828P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2432
_refine_ls_wR_factor_ref         0.2657
_reflns_number_gt                1451
_reflns_number_total             1759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801677y_si_001.cif
_cod_data_source_block           c6ch16-8703sq
_cod_original_sg_symbol_Hall     '-I 4 2 '
_cod_database_code               4301220