Macrocyclic ligand design. X-Ray, DFT and solution studies of the effect of N-methylation and N-benzylation of 1,4,10,13-tetraoxa-7,16-diazacyclooctadecane on its affinity for selected transition and post-transition metal ions
Hambley, Trevor W.; Lindoy, Leonard F.; Reimers, Jeffrey R.; Turner, Peter; Wei, Gang; Widmer-Cooper, Asaph N.; Journal of the Chemical Society, Dalton Transactions  (2001) 614–; doi:10.1039/b008789k

data_7010417
_publ_section_title
;
 Macrocyclic ligand design. X-Ray, DFT and solution studies of the
 effect of N-methylation and N-benzylation of
 1,4,10,13-tetraoxa-7,16-diazacyclooctadecane on its affinity for
 selected transition and post-transition metal ions
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              614
_journal_paper_doi               10.1039/b008789k
_journal_year                    2001
_chemical_formula_sum            'C12 H26 N4 O10 Pb'
_chemical_formula_weight         593.56
_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'
_cell_angle_alpha                90
_cell_angle_beta                 110.668(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2659(4)
_cell_length_b                   12.2862(6)
_cell_length_c                   10.6536(5)
_cell_measurement_reflns_used    5527
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      28.173
_cell_measurement_theta_min      2.631
_cell_volume                     1012.31(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'teXsan (MSC, 1992-1997)'
_computing_structure_refinement  'teXsan (MSC, 1992-1997)'
_computing_structure_solution
;
SHELXS86 (Sheldrick, 1985)
;
_diffrn_ambient_temperature      294(2)
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.00000
_diffrn_orient_matrix_UB_12      0.00000
_diffrn_orient_matrix_UB_13      0.00000
_diffrn_orient_matrix_UB_21      0.00000
_diffrn_orient_matrix_UB_22      0.00000
_diffrn_orient_matrix_UB_23      0.00000
_diffrn_orient_matrix_UB_31      0.00000
_diffrn_orient_matrix_UB_32      0.00000
_diffrn_orient_matrix_UB_33      0.00000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10860
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0.11
_diffrn_standards_number         170
_exptl_absorpt_coefficient_mu    8.431
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.646
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.65
_refine_ls_extinction_coef       0.00000044(4)
_refine_ls_extinction_expression
;
equ(3) Acta Cryst.(1968) A24, p213.
;
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.869
_refine_ls_goodness_of_fit_ref   2.110
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.0140
_refine_ls_shift/su_mean         0.0110
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w =3D 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.0245
_refine_ls_wR_factor_ref         0.0223
_reflns_number_gt                1640
_reflns_number_total             2561
_reflns_threshold_expression     I>3.00\s(I)
_cod_data_source_file            b008789k.txt
_cod_data_source_block           '[Pb(1)](NO3)2'
_cod_original_sg_symbol_H-M      'P 21/c     '
_cod_original_formula_sum        'C12 H26 N4 O10 Pb1'
_cod_database_code               7010417