Azacalix[2]arene[2]triazine-based receptors bearing carboxymethyl pendant arms on nitrogen bridges: synthesis and evaluation of their coordination ability towards copper(II).
Caio, João M; Esteves, Teresa; Carvalho, Silvia; Moiteiro, Cristina; Félix, Vítor; Organic & biomolecular chemistry 12 (2014) 589–599; doi:10.1039/c3ob42047g

data_7153568
_publ_section_title
;
 Azacalix[2]arene[2]triazine-based receptors bearing carboxymethyl pendant
 arms on nitrogen bridges: synthesis and evaluation of their coordination
 ability towards copper(II).
;
_journal_issue                   4
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              589
_journal_page_last               599
_journal_paper_doi               10.1039/c3ob42047g
_journal_volume                  12
_journal_year                    2014
_chemical_formula_moiety         'C30 H28 Cl2 N10 O8, C6 H10 O5'
_chemical_formula_sum            'C36 H38 Cl2 N10 O13'
_chemical_formula_weight         889.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2013-10-13
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.734(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2611(11)
_cell_length_b                   18.2064(13)
_cell_length_c                   17.7004(19)
_cell_measurement_reflns_used    526
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.94
_cell_volume                     3882.1(6)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '4-circle KAPPA Goniometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            23350
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.551
_diffrn_reflns_theta_min         2.027
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_target            Mo
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.522
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.314
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         5940
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0465P)^2^+2.7270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4218
_reflns_number_total             5940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ob42047g.txt
_cod_data_source_block           compound_1
_cod_database_code               7153568
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.957
_olex2_refinement_description
;
1. Others
 Fixed U12: O100(0)
 Fixed U23: O100(0)
 Fixed Uiso: H6(0.024) H12A(0.026) H12B(0.026) H14(0.031) H19A(0.028)
 H19B(0.028) H20(0.032) H25(0.038) H29A(0.044) H29B(0.044) H29C(0.044)
 H30A(0.048) H30B(0.048) H30C(0.048) H10C(0.039) H10D(0.039) H10E(0.058)
 H10F(0.058) H10G(0.058)
 Fixed X: H6(1.069) H12A(0.8288) H12B(0.9259) H14(0.892) H19A(1.3115)
 H19B(1.3965) H20(1.2115) H25(1.046) H29A(0.6035) H29B(0.6608) H29C(0.7067)
 H30A(1.5151) H30B(1.6057) H30C(1.6) O100(1) H10C(0.8391) H10D(0.9107)
 H10E(0.7383) H10F(0.6829) H10G(0.8108)
 Fixed Y: H6(0.5389) H12A(0.5092) H12B(0.5643) H14(0.7234) H19A(0.5725)
 H19B(0.5504) H20(0.7392) H25(0.7947) H29A(0.6367) H29B(0.6091) H29C(0.6807)
 H30A(0.7523) H30B(0.6935) H30C(0.718) H10C(0.4333) H10D(0.3597) H10E(0.3879)
 H10F(0.3129) H10G(0.3144)
 Fixed Z: H6(0.141) H12A(-0.0167) H12B(-0.0286) H14(0.0727) H19A(0.1062)
 H19B(0.1828) H20(0.1837) H25(0.124) H29A(-0.1672) H29B(-0.2362) H29C(-0.1882)
 H30A(0.0775) H30B(0.0624) H30C(0.1484) O100(0.25) H10C(0.2406) H10D(0.2587)
 H10E(0.0121) H10F(0.0333) H10G(0.0253)
;
_shelx_res_checksum              13537
_shelx_hkl_checksum              71306