Entry point into new trimeric and tetrameric imide-based macrocyclic esters derived from isophthaloyl dichloride and methyl 6-aminonicotinate
Mocilac, Pavle; Gallagher, John F.; Acta Crystallographica Section B 69 (2013) 62–69; doi:10.1107/S0108768112047416

data_2105318
_publ_section_title
;
 Entry point into new trimeric and tetrameric imide-based macrocyclic
 esters derived from isophthaloyl dichloride and methyl 6-aminonicotinate
;
_journal_coeditor_code           GP5057
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              62
_journal_page_last               69
_journal_paper_doi               10.1107/S0108768112047416
_journal_volume                  69
_journal_year                    2013
_chemical_formula_moiety         'C60 H40 N8 O16'
_chemical_formula_sum            'C60 H40 N8 O16'
_chemical_formula_weight         1129.00
_chemical_melting_point          476
_chemical_name_common            (EsIO)4
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.7210(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.68700(10)
_cell_length_b                   22.4852(2)
_cell_length_c                   22.6756(2)
_cell_measurement_reflns_used    11636
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      63.13
_cell_measurement_theta_min      2.79
_cell_volume                     5335.31(9)
_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 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Xcalibur, Sapphire3, Gemini Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            31765
_diffrn_reflns_theta_full        63.13
_diffrn_reflns_theta_max         63.27
_diffrn_reflns_theta_min         2.80
_diffrn_standards_decay_%        1
_exptl_absorpt_coefficient_mu    0.875
_exptl_absorpt_correction_T_max  0.9576
_exptl_absorpt_correction_T_min  0.6309
_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_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.172
_refine_ls_extinction_coef       0.00038(5)
_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   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     762
_refine_ls_number_reflns         8619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0411
_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^)+(0.06P)^2^+1.1981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1195
_reflns_number_gt                6947
_reflns_number_total             8619
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gp5057.cif
_cod_data_source_block           EsIO4_I_12-001
_cod_original_cell_volume        5335.31(8)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2105318