Cyclen-based bismacrocycles for biological anion recognition. A potentiometric and NMR study of AMP, ADP and ATP nucleotide complexation
Delépine, Anne-Sophie; Tripier, Raphaël; Handel, Henri; Organic & Biomolecular Chemistry 6 (2008) 1743–1750; doi:10.1039/b719514a

data_7150870
_publ_section_title
;
 Cyclen-based bismacrocycles for biological anion recognition. A
 potentiometric and NMR study of AMP, ADP and ATP nucleotide
 complexation
;
_journal_issue                   10
_journal_name_full               'Organic &amp;  Biomolecular Chemistry'
_journal_page_first              1743
_journal_page_last               1750
_journal_paper_doi               10.1039/b719514a
_journal_volume                  6
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety
;
C23 H52 N9 7+, 7(Cl 1-), 6(H2 O)
;
_chemical_formula_sum            'C23 H64 Cl7 N9 O6'
_chemical_formula_weight         810.98
_chemical_name_common            Bis2,6pyr-cyclen
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
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_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5917(5)
_cell_length_b                   17.7280(11)
_cell_length_c                   14.9620(10)
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      27.4224
_cell_measurement_theta_min      2.7456
_cell_volume                     1993.3(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_collection
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CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_data_reduction
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CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
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_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device       'Kappa-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR2'
_diffrn_measurement_method
;
4 stepped omega-scans over 115 deg with kappa -79 deg (chi -58.3 deg)
and phi 0, 90, 180, 270 deg;
step 0.75 deg, exposure time 30 s;
detector distance 50 mm;
detector angle 20 deg.
;
_diffrn_orient_matrix_UB_11      0.0295566989
_diffrn_orient_matrix_UB_12      -0.0342108703
_diffrn_orient_matrix_UB_13      0.0216966778
_diffrn_orient_matrix_UB_21      -0.0762816199
_diffrn_orient_matrix_UB_22      -0.0187302621
_diffrn_orient_matrix_UB_23      -0.0224017968
_diffrn_orient_matrix_UB_31      0.047051363
_diffrn_orient_matrix_UB_32      -0.0088927077
_diffrn_orient_matrix_UB_33      -0.0363583365
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_unetI/netI     0.0687
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
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_diffrn_reflns_limit_k_min       -22
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_diffrn_reflns_limit_l_min       -19
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_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.94
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.96145
_exptl_absorpt_correction_T_min  0.80055
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr 1 2005,17:53:34)
Scale3 Abspack program including interframe scaling, empirical
absorption correction (Blessing) and detector sensitivity correction.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.146
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7739
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                5927
_reflns_number_total             7739
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719514a.txt
_cod_data_source_block           bpyc
_cod_depositor_comments
;
The following automatic conversions were performed:
'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7150870