Stabilization of Calcium- and Terbium-Carboxylate Bonds by NH...O Hydrogen Bonds in a Mononuclear Complex: A Functional Model of the Active Site of Calcium-Binding Proteins
Akira Onoda; Yusuke Yamada; Yoshiki Nakayama; Kazuyuki Takahashi; Hiroshi Adachi; Taka-aki Okamura; Akira Nakamura; Hitoshi Yamamoto; Norikazu Ueyama; Drahomir Vyprachticky; Yoshi Okamoto; Inorganic Chemistry 43 (2004) 4447–4455; doi:10.1021/ic035075t

data_4311215
_publ_section_title
;
 Stabilization of Calcium- and Terbium-Carboxylate Bonds by NH...O
 Hydrogen Bonds in a Mononuclear Complex: A Functional Model of the Active
 Site of Calcium-Binding Proteins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4447
_journal_page_last               4455
_journal_paper_doi               10.1021/ic035075t
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C90 H140 N9 O20.50 Tb '
_chemical_formula_sum            'C90 H140 N9 O20.5 Tb'
_chemical_formula_weight         1835.03
_chemical_name_systematic
; 
(NMe4)[Tb{OCOC6H3(NHCO-t-Bu)3}4(thf)]-3.5(THF) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Wed Jan 28 17:19:18 2004'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.1880(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1181(4)
_cell_length_b                   25.0087(7)
_cell_length_c                   27.8505(7)
_cell_measurement_reflns_used    66536
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     9678.3(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1440
_diffrn_reflns_av_sigmaI/netI    0.2065
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            77771
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.800
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             3888
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.774
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1029
_refine_ls_number_reflns         21784
_refine_ls_number_restraints     741
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1598
_refine_ls_R_factor_gt           0.0627
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                10274
_reflns_number_total             21784
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic035075tsi20040225_084922_3.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C90 H140 N9 O20.50 Tb'
_cod_database_code               4311215