Design and Synthesis of a Fluorescent Probe for Zn2+, 5,7-Bis(N,N-dimethylaminosulfonyl)-8-hydroxyquinoline-Pendant 1,4,7,10-Tetraazacyclododecane and Zn2±Dependent Hydrolytic and Zn2±Independent Photochemical Reactivation of Its Benzenesulfonyl-Caged Derivative
Ryosuke Ohshima; Masanori Kitamura; Akinori Morita; Motoo Shiro; Yasuyuki Yamada; Masahiko Ikekita; Eiichi Kimura; Shin Aoki; Inorganic Chemistry 49 (2010) 888–899; doi:10.1021/ic901279t

data_4314627
_publ_section_title
;
 Design and Synthesis of a Fluorescent Probe for Zn2+,
 5,7-Bis(N,N-dimethylaminosulfonyl)-8-hydroxyquinoline-Pendant
 1,4,7,10-Tetraazacyclododecane and Zn2+-Dependent Hydrolytic and
 Zn2+-Independent Photochemical Reactivation of Its Benzenesulfonyl-Caged
 Derivative
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              888
_journal_page_last               899
_journal_paper_doi               10.1021/ic901279t
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C22 H38 N7 O5 S2, 6.2(H2 O), Cl '
_chemical_formula_sum            'C22 H50.4 Cl N7 O11.2 S2'
_chemical_formula_weight         691.85
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 118.8100(7)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            16
_cell_length_a                   35.8779(7)
_cell_length_b                   19.7401(4)
_cell_length_c                   21.4880(7)
_cell_measurement_reflns_used    57169
_cell_measurement_temperature    93.1
_cell_measurement_theta_max      68.3
_cell_measurement_theta_min      4.0
_cell_volume                     13334.8(6)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku & RAC 2007)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'CrystalStructure (Rigaku & RAC 2007)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Rigaku VariMax-RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            91503
_diffrn_reflns_theta_full        68.25
_diffrn_reflns_theta_max         68.25
_exptl_absorpt_coefficient_mu    2.738
_exptl_absorpt_correction_T_max  0.682
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5920.00
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.86
_refine_diff_density_min         -0.79
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     817
_refine_ls_number_reflns         11999
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1002P)^2^+63.1538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1966
_reflns_number_gt                9056
_reflns_number_total             11999
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic901279t_si_002_2.cif
_cod_data_source_block           10
_cod_original_cell_volume        13334.9(6)
_cod_original_formula_sum        'C22 H50.40 Cl N7 O11.20 S2 '
_cod_database_code               4314627
_verf_plat306_alert_2_a
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......     O9      
RESPONSE: O atoms of waters, see _publ_section_exptl_refinement
;