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_7010418
_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 Ag F6 N2 O4 P'
_chemical_formula_weight         515.18
_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'
_audit_creation_date             1999-09-04
_audit_creation_method           'by teXsan v1.8'
_audit_update_record
;
?
;
_cell_angle_alpha                90
_cell_angle_beta                 97.427(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3255(5)
_cell_length_b                   8.5474(3)
_cell_length_c                   14.5016(5)
_cell_measurement_reflns_used    7953
_cell_measurement_temperature    273.2
_cell_measurement_theta_max      27.987
_cell_measurement_theta_min      2.131
_cell_volume                     1883.67(11)
_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  0.02224
_diffrn_reflns_av_sigmaI/netI    0.020
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9764
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        0.22
_diffrn_standards_interval_count 0
_diffrn_standards_number         261
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.757
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 1996)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.143
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.62
_refine_ls_extinction_coef       0.00000178(7)
_refine_ls_extinction_expression
;
equ(3) Acta Cryst.(1968) A24, p213.
;
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   3.815
_refine_ls_goodness_of_fit_ref   3.976
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2027
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_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         0.0376
_refine_ls_wR_factor_ref         0.0375
_reflns_number_gt                2027
_reflns_number_total             2356
_reflns_threshold_expression     I>2.50\s(I)
_cod_data_source_file            b008789k.txt
_cod_data_source_block           '[Ag(1)]PF6'
_cod_original_cell_volume        1883.7(1)
_cod_original_sg_symbol_H-M      'C 2/c      '
_cod_original_formula_sum        'C12 H26 Ag1 F6 N2 O4 P1 '
_cod_database_code               7010418