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_4326874
_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
'2(C17 H26 F3 N4 O2 Zn), 2(C2 F3 O2), B H3 O3, 2(O)'
_chemical_formula_sum            'C38 H55 B F12 N8 O13 Zn2'
_chemical_formula_weight         1201.45
_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_creation_method           SHELXL-97
_cell_angle_alpha                71.955(18)
_cell_angle_beta                 89.71(2)
_cell_angle_gamma                77.420(19)
_cell_formula_units_Z            2
_cell_length_a                   9.968(6)
_cell_length_b                   16.226(8)
_cell_length_c                   16.718(9)
_cell_measurement_reflns_used    7798
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      3.0
_cell_volume                     2504(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 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0721
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16602
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    1.070
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.740
_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    1.594
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         8975
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                6634
_reflns_number_total             8975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201507q_si_002_2.cif
_cod_data_source_block           Compound9a
_cod_database_code               4326874