Structural Effects of the Lone Pair on Lead(II), and Parallels with the Coordination Geometry of Mercury(II). Does the Lone Pair on Lead(II) Form H-Bonds? Structures of the Lead(II) and Mercury(II) Complexes of the Pendant-Donor Macrocycle DOTAM (1,4,7,10-Tetrakis(carbamoylmethyl)-1,4,7,10-tetraazacyclododecane)
Robert D. Hancock; Joseph H. Reibenspies; Hulisani Maumela; Inorganic Chemistry 43 (2004) 2981–2987; doi:10.1021/ic030277a

data_4310895
_publ_section_title
;
 Structural Effects of the Lone Pair on Lead(II), and Parallels with the
 Coordination Geometry of Mercury(II). Does the Lone Pair on Lead(II) Form
 H-Bonds? Structures of the Lead(II) and Mercury(II) Complexes of the
 Pendant-Donor Macrocycle DOTAM
 (1,4,7,10-Tetrakis(carbamoylmethyl)-1,4,7,10-tetraazacyclododecane)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2981
_journal_page_last               2987
_journal_paper_doi               10.1021/ic030277a
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C16 H41 Cl2 N8 O16.5 Pb'
_chemical_formula_weight         887.66
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                101.45(2)
_cell_angle_beta                 93.32(2)
_cell_angle_gamma                90.53(2)
_cell_formula_units_Z            4
_cell_length_a                   12.767(3)
_cell_length_b                   13.528(4)
_cell_length_c                   18.385(5)
_cell_measurement_temperature    293(2)
_cell_volume                     3106.2(15)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0733
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11304
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    5.687
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       plate
_exptl_crystal_F_000             1764
_refine_diff_density_max         1.649
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.097
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_matrix_type           full
_refine_ls_number_parameters     765
_refine_ls_number_reflns         10875
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.156
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_obs          0.0500
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0310P)^2^+31.4774P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1240
_refine_ls_wR_factor_obs         0.0984
_reflns_number_observed          7755
_reflns_number_total             10932
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic030277a_s_2.cif
_cod_data_source_block           rh23
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0310P)^2^+31.4774P] where P=(Fo^2^+2Fc^2^)/3' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/[s^2^(Fo^2^)+( 0.0310P)^2^+31.4774P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3106.2(14)
_cod_original_formula_sum        'C16 H41 Cl2 N8 O16.50 Pb'
_cod_database_code               4310895