Synthesis and anion binding studies of o-phenylenevinylene-bridged tetrapyrrolic macrocycle as an expanded analogue of calix[4]pyrrole
Sudip Kumar Ghosh; Masatoshi Ishida; Jiazhu Li; Won-Young Cha; Vincent M. Lynch; Dongho Kim; Jonathan L. Sessler; Chem.Commun. 50 (2014) 3753–; doi:10.1039/c4cc00686k

data_7112160
_publ_section_title
;
 Synthesis and anion binding studies of o-phenylenevinylene-bridged
 tetrapyrrolic macrocycle as an expanded analogue of calix[4]pyrrole
;
_journal_name_full               Chem.Commun.
_journal_page_first              3753
_journal_paper_doi               10.1039/c4cc00686k
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C56 H44 N4, 4 C2 H3 N, 2 C4 H8 O'
_chemical_formula_sum            'C72 H72 N8 O2'
_chemical_formula_weight         1081.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.182(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3594(12)
_cell_length_b                   16.2083(13)
_cell_length_c                   24.658(2)
_cell_measurement_reflns_used    9560
_cell_measurement_temperature    100
_cell_measurement_theta_max      74.12
_cell_measurement_theta_min      2.70
_cell_volume                     6538.2(9)
_computing_cell_refinement       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_collection       'Apex II release 2010, Bruker AXS, Inc.'
_computing_data_reduction        'Apex II release 2010, Bruker AXS, Inc.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/Plus, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M. 2013'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.991
_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       28
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            61513
_diffrn_reflns_point_group_measured_fraction_full 0.929
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         64.991
_diffrn_reflns_theta_min         2.701
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0963 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.8961.
The \l/2 correction factor is 0.0015.

;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.099
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.690
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         11009
_refine_ls_number_restraints     322
_refine_ls_restrained_S_all      1.686
_refine_ls_R_factor_all          0.1582
_refine_ls_R_factor_gt           0.1225
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1500P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3419
_refine_ls_wR_factor_ref         0.3655
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7274
_reflns_number_total             11009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc00686k2.cif
_cod_data_source_block           shelx
_cod_database_code               7112160
_shelxl_version_number           2013-4
_shelx_res_checksum              21696
_shelx_hkl_checksum              31769
_shelx_fab_checksum              96922