A chemosensor for dihydrogenphosphate based on an oxoazamacrocycle possessing three thiourea arms.
Aldrey, Anxela; Macías, Alejandro; Bastida, Rufina; Zaragoza, Guillermo; Rama, Gustavo; López, Miguel Vázquez; Organic & biomolecular chemistry 10 (2012) 5379–5384; doi:10.1039/c2ob25498k

data_7152419
_publ_section_title
;
 A chemosensor for dihydrogenphosphate based on an oxoazamacrocycle
 possessing three thiourea arms.
;
_journal_issue                   28
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5379
_journal_page_last               5384
_journal_paper_doi               10.1039/c2ob25498k
_journal_volume                  10
_journal_year                    2012
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C43 H45 N10 O8 S3, C2 F3 O2, 2(C2 H3 N)'
_chemical_formula_sum            'C49 H51 F3 N12 O10 S3'
_chemical_formula_weight         1121.2
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2012-01-13T11:26:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.826(4)
_cell_angle_beta                 84.575(4)
_cell_angle_gamma                89.938(4)
_cell_formula_units_Z            2
_cell_length_a                   10.6022(7)
_cell_length_b                   13.4737(10)
_cell_length_c                   18.5141(14)
_cell_measurement_reflns_used    1984
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.47
_cell_measurement_theta_min      2.45
_cell_measurement_wavelength     0.71073
_cell_volume                     2591.2(3)
_computing_cell_refinement       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_collection       'APPEX2 (BRUKER AXS, 2005)'
_computing_data_reduction        'APPEX2 (BRUKER AXS, 2005)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'BRUKER APPEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_unetI/netI     0.072
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34955
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.9230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         7427
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+2.9862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1416
_reflns_number_gt                4666
_reflns_number_total             7427
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2ob25498k.txt
_cod_data_source_block           mig12n
_cod_database_code               7152419