Metal ion recognition. Interaction of a series of successively N-benzylated derivatives of 1,4,8,11-tetraazacyclotetradecane (cyclam) with selected transition and post-transition metal ions
Dong, Ying; Farquhar, Sandra; Gloe, Karsten; Lindoy, Leonard F.; Rumbel, Brendan R.; Turner, Peter; Wichmann, Kathrin; Dalton Transactions  (2003) 1558–; doi:10.1039/b300002h

data_7012676
_publ_section_title
;
 Metal ion recognition. Interaction of a series of successively
 N-benzylated derivatives of 1,4,8,11-tetraazacyclotetradecane (cyclam)
 with selected transition and post-transition metal ions
;
_journal_issue                   8
_journal_name_full               'Dalton Transactions'
_journal_page_first              1558
_journal_paper_doi               10.1039/b300002h
_journal_year                    2003
_chemical_formula_sum            'C24 H38 N6 O7 Pb'
_chemical_formula_weight         729.79
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1228(13)
_cell_length_b                   9.4321(7)
_cell_length_c                   18.4865(15)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.081
_cell_measurement_theta_min      2.540
_cell_volume                     2811.3(4)
_computing_cell_refinement       'SAINT (Bruker,1995)'
_computing_data_collection       'SMART (Bruker,1995)'
_computing_data_reduction        'SAINT and XPREP (Bruker 1995)'
_computing_molecular_graphics
;
teXsan for Windows (MSC, 1997) 
xtal 3.6 (Hall,du Boulay, D.J. & Olthof-Hazekamp, R. 1999)
ORTEPII  (Johnson,C.K., 1976). 
WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, et. al. 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_crystal_treatment
;
attached to a thin glass fibre
;
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0134
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            27909
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.20
_diffrn_standards_decay_%        0.54
_diffrn_standards_number         211
_exptl_absorpt_coefficient_mu    6.053
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.792
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.264
_refine_diff_density_max         0.744
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00043(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.350
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3412
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.350
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+1.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0553
_reflns_number_gt                2361
_reflns_number_total             3412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b300002h.txt
_cod_data_source_block           lfl62
_cod_original_sg_symbol_H-M      'P b c n    '
_cod_database_code               7012676