Recognition of bio-relevant dicarboxylate anions by an azacalix[2]arene[2]triazine derivative decorated with urea moieties.
Santos, Miguel M.; Marques, Igor; Carvalho, Sílvia; Moiteiro, Cristina; Félix, Vítor; Organic & biomolecular chemistry 13 (2015) 3070–3085; doi:10.1039/c4ob02283a

data_7154275
_publ_section_title
;
 Recognition of bio-relevant dicarboxylate anions by an
 azacalix[2]arene[2]triazine derivative decorated with urea moieties.
;
_journal_issue                   10
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3070
_journal_page_last               3085
_journal_paper_doi               10.1039/c4ob02283a
_journal_volume                  13
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C46 H48 Cl2 N14 O6'
_chemical_formula_weight         963.88
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-10-23 deposited with the CCDC.
2015-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                86.107(2)
_cell_angle_beta                 81.276(2)
_cell_angle_gamma                67.781(2)
_cell_formula_units_Z            4
_cell_length_a                   14.9779(6)
_cell_length_b                   15.1104(6)
_cell_length_c                   23.1992(8)
_cell_measurement_reflns_used    388
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      4.88
_cell_volume                     4804.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'OLEX2 (J. Appl. Cryst., 2009, 42, 339-341)'
_computing_publication_material  'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      150(2)
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_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.942
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_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55221
_diffrn_reflns_point_group_measured_fraction_full 0.745
_diffrn_reflns_point_group_measured_fraction_max 0.759
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.830
_diffrn_reflns_theta_min         2.464
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker AXS Inc.)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       needle
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.963
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 6811 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2473
_refine_ls_number_reflns         28172
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+1.5652P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.581
_reflns_Friedel_fraction_full    0.548
_reflns_Friedel_fraction_max     0.558
_reflns_number_gt                21085
_reflns_number_total             28172
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4ob02283a2.cif
_cod_data_source_block           urea_aza_calix_derivative_1
_cod_depositor_comments          'Adding full bibliography for 7154275.cif.'
_cod_database_code               7154275
_shelx_estimated_absorpt_t_min   0.947
_shelx_estimated_absorpt_t_max   0.994
_shelxl_version_number           2013-4
_shelx_res_checksum              50919