Preparation of Mercury(II) Complexes of Tris[(2-pyridyl)methyl]amine and Characterization by X-ray Crystallography and NMR Spectroscopy
Deborah C. Bebout; David E. Ehmann; Jonathan C. Trinidad; Kathleen K. Crahan; Margaret E. Kastner; Damon A. Parrish; Inorganic Chemistry 36 (1997) 4257–4264; doi:10.1021/ic9702779

data_4324028
_publ_section_title
;
 Preparation of Mercury(II) Complexes of Tris[(2-pyridyl)methyl]amine and
 Characterization by X-ray Crystallography and NMR Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4257
_journal_page_last               4264
_journal_paper_doi               10.1021/ic9702779
_journal_volume                  36
_journal_year                    1997
_chemical_formula_moiety         '(C18 H18 Cl Hg N4 1+)2, Cl4 Hg 2-'
_chemical_formula_sum            'C36 H36 Cl6 Hg3 N8'
_chemical_formula_weight         1395.20
_chemical_name_systematic
; 
tris[(2-pyridyl)methyl]aminechloromercury(II) tetrachloromercurate(II) 
;
_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                112.27(2)
_cell_angle_beta                 109.39(2)
_cell_angle_gamma                90.670(10)
_cell_formula_units_Z            2
_cell_length_a                   11.887(2)
_cell_length_b                   13.260(2)
_cell_length_c                   15.278(4)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.77
_cell_measurement_theta_min      10.66
_cell_volume                     2075.9(9)
_computing_cell_refinement       SHELXL-93
_computing_data_collection       'Siemens SHELXL PLUS (VMS)'
_computing_data_reduction        'Siemens SHELXL PLUS (VMS)'
_computing_molecular_graphics    'Siemens SHELXL PLUS (VMS)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens R3m/V'
_diffrn_measurement_method       'theta 2 theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            9587
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        'none observed'
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    11.490
_exptl_absorpt_correction_T_max  0.0801
_exptl_absorpt_correction_T_min  0.0253
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_density_meas      2.289
_exptl_crystal_density_method    'floatation in bromoform/hexane solution'
_exptl_crystal_description       'cloudy plate'
_exptl_crystal_F_000             1300
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.092
_refine_diff_density_min         -3.771
_refine_diff_density_rms         0.377
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.919
_refine_ls_goodness_of_fit_obs   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9585
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_restrained_S_obs      0.943
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_obs          0.0468
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1411
_refine_ls_wR_factor_obs         0.1085
_reflns_number_observed          5941
_reflns_number_total             9587
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9702779_1.cif
_cod_data_source_block           bebo2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.0000P] 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^)+(0.0799P)^2^+0.0000P] 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        2075.9(7)
_cod_database_code               4324028