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_4310894
_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 H36 Cl2 Hg N8 O14'
_chemical_formula_weight         836.02
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.91(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.849(5)
_cell_length_b                   21.292(7)
_cell_length_c                   11.349(2)
_cell_measurement_temperature    293(2)
_cell_volume                     2801.6(16)
_computing_cell_refinement       'MSC CTR (4:1:0)'
_computing_data_collection       'MSC CTR (4:1:0)'
_computing_data_reduction        'MSC TEXSAN PROCESS'
_computing_molecular_graphics    'Siemens XP SHELXTL-PLUS'
_computing_publication_material  'SHELXL-93 CIFTAB'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      167(2)
_diffrn_measurement_device       'Rigaku AFC5'
_diffrn_measurement_method       theta-2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0765
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2612
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.764
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_description       plate
_exptl_crystal_F_000             1656
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.314
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.021
_refine_ls_goodness_of_fit_obs   1.028
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         2603
_refine_ls_number_restraints     583
_refine_ls_restrained_S_all      1.037
_refine_ls_restrained_S_obs      0.954
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_obs          0.0381
_refine_ls_shift/esd_max         0.026
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0348P)^2^+17.0953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1033
_refine_ls_wR_factor_obs         0.0878
_reflns_number_observed          2267
_reflns_number_total             2612
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic030277a_s_1.cif
_cod_data_source_block           rh13
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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^)+(
0.0348P)^2^+17.0953P] 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^)+( 0.0348P)^2^+17.0953P]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4310894