Trezimides and Tennimides: New Imide-Based Macrocycles
Pavle Mocilac; John F. Gallagher; Journal of Organic Chemistry 78 (2013) 2355–2361; doi:10.1021/jo302448h

data_4028020
_publ_contact_author_address
;
School of Chemical Sciences,
Dublin City University, Dublin 9, Ireland
;
_publ_contact_author_email       john.gallagher@dcu.ie
_publ_contact_author_fax         '353 1 7005503'
_publ_contact_author_name
;
Dr. John F. Gallagher
;
_publ_contact_author_phone       '353 1 7005114'
_publ_section_title
;
 Trezimides and Tennimides: New Imide-Based Macrocycles
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2355
_journal_page_last               2361
_journal_paper_doi               10.1021/jo302448h
_journal_volume                  78
_journal_year                    2013
_chemical_formula_moiety         '2(C48 H28 N12 O8), C3 H5 Cl7'
_chemical_formula_sum            'C99 H61 Cl7 N24 O16'
_chemical_formula_weight         2090.87
_chemical_name_common            (26IO)4_OC
_chemical_name_systematic        ' ? '
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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                   22.7814(1)
_cell_length_b                   22.7814(1)
_cell_length_c                   19.0308(1)
_cell_measurement_reflns_used    25938
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      63.19
_cell_measurement_theta_min      2.74
_cell_volume                     9876.84(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  SHELXL97
_computing_structure_refinement
'SHELXL97 (Sheldrick, 2008) and SORTX (McArdle, 1995)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Sapphire3, Gemini Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            65749
_diffrn_reflns_theta_full        63.29
_diffrn_reflns_theta_max         63.29
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         65749
_exptl_absorpt_coefficient_mu    2.496
_exptl_absorpt_correction_T_max  0.7884
_exptl_absorpt_correction_T_min  0.5975
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(ABSFAC, Clark and Reid, 1998)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       Block
_exptl_crystal_F_000             4280
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details '(Flack, 1983)'
_refine_ls_abs_structure_Flack   0.00(6)
_refine_ls_extinction_coef       0.00010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         8025
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0458
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.096P)^2^+1.41P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                7474
_reflns_number_total             8025
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo302448h_si_002_5.cif
_cod_data_source_block           11-103-[(26IO)4_OC]
_cod_original_cell_volume        9876.84(10)
_cod_database_code               4028020