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_7152418
_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, N O3, 4(C2 H3 N)'
_chemical_formula_sum            'C51 H57 N15 O11 S3'
_chemical_formula_weight         1152.3
_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             2012-01-13T13:19:32-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                95.902(14)
_cell_angle_beta                 105.791(13)
_cell_angle_gamma                91.983(13)
_cell_formula_units_Z            2
_cell_length_a                   12.535(4)
_cell_length_b                   14.086(5)
_cell_length_c                   16.533(6)
_cell_measurement_reflns_used    1935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.67
_cell_measurement_wavelength     0.71073
_cell_volume                     2788.2(17)
_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    'SIR-97 (Giacovazzo et all, 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.1100
_diffrn_reflns_av_unetI/netI     0.1904
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            30269
_diffrn_reflns_theta_full        18.86
_diffrn_reflns_theta_max         18.86
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.206
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     754
_refine_ls_number_reflns         4281
_refine_ls_number_restraints     553
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.1011
_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^)+(0.1773P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2647
_refine_ls_wR_factor_ref         0.2891
_reflns_number_gt                2364
_reflns_number_total             4281
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2ob25498k.txt
_cod_data_source_block           ba01yra2n
_cod_original_cell_volume        2788.1(16)
_cod_database_code               7152418