11B NMR Sensing of d-Block Metal Ions in Vitro and in Cells Based on the Carbon-Boron Bond Cleavage of Phenylboronic Acid-Pendant Cyclen (Cyclen = 1,4,7,10-Tetraazacyclododecane)
Masanori Kitamura; Toshihiro Suzuki; Ryo Abe; Takeru Ueno; Shin Aoki; Inorganic Chemistry 50 (2011) 11568–11580; doi:10.1021/ic201507q

data_4326873
_publ_contact_author_address
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Faculty of Pharmaceutical Sciences Tokyo University of Science,
2641 Yamazaki, Noda 278-8510 Japan
;
_publ_contact_author_email       shinaoki@rs.noda.tus.ac.jp
_publ_contact_author_fax         +81-4-7121-3670
_publ_contact_author_name        'Shin Aoki'
_publ_contact_author_phone       +81-4-7121-3670
_publ_section_title
;
 11B NMR Sensing of d-Block Metal Ions in Vitro and in Cells Based on the
 Carbon-Boron Bond Cleavage of Phenylboronic Acid-Pendant Cyclen (Cyclen =
 1,4,7,10-Tetraazacyclododecane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11568
_journal_page_last               11580
_journal_paper_doi               10.1021/ic201507q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C19 H29 B F6 N4 O6 '
_chemical_formula_sum            'C19 H29 B F6 N4 O6'
_chemical_formula_weight         534.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.892(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.392(5)
_cell_length_b                   12.179(7)
_cell_length_c                   21.872(12)
_cell_measurement_reflns_used    5205
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      123.1
_cell_measurement_theta_min      27.5
_cell_volume                     2493(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_sigmaI/netI    0.0691
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17564
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.22
_diffrn_standards_number         17564
_exptl_absorpt_coefficient_mu    0.132
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_correction_T_min  0.953
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
    Higashi, T. (1999). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         5601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_gt           0.0724
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1958
_reflns_number_gt                3898
_reflns_number_total             5601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201507q_si_002_1.cif
_cod_data_source_block           Compound5
_cod_database_code               4326873
_verf_plat306_alert_2_a
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PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......     O12
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......     O13      
RESPONSE: O atoms of waters, see _publ_section_exptl_refinement
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_verf_plat430_alert_2_b
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PROBLEM: Short Inter D...A Contact  O8 ..  O13     ..     2.81 Ang.   
RESPONSE: Hydrogen bonds formed between them.
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