Characterization of Mercury(II) Complexes of Bis[(2-pyridyl)methyl]amine by X-ray Crystallography and NMR Spectroscopy
Deborah C. Bebout; Anne E. DeLanoy; David E. Ehmann; Margaret E. Kastner; Damon A. Parrish; Raymond J. Butcher; Inorganic Chemistry 37 (1998) 2952–2959; doi:10.1021/ic971499+

data_4327680
_publ_section_title
;
 Characterization of Mercury(II) Complexes of Bis[(2-pyridyl)methyl]amine
 by X-ray Crystallography and NMR Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2952
_journal_page_last               2959
_journal_paper_doi               10.1021/ic971499+
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C27.5 H30 Cl2 Hg N6 O8'
_chemical_formula_weight         844.07
_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                67.50(3)
_cell_angle_beta                 82.74(3)
_cell_angle_gamma                67.88(3)
_cell_formula_units_Z            2
_cell_length_a                   10.953(5)
_cell_length_b                   12.812(5)
_cell_length_c                   13.006(5)
_cell_measurement_reflns_used    19
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      20
_cell_volume                     1561.8(12)
_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    0.0249
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7221
_diffrn_reflns_theta_max         27.65
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.157
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_meas      1.77
_exptl_crystal_density_method    flotation
_exptl_crystal_description       'cloudy plate'
_exptl_crystal_F_000             830
_exptl_crystal_size_max          .50
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .13
_refine_diff_density_max         2.465
_refine_diff_density_min         -2.453
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.983
_refine_ls_goodness_of_fit_obs   1.035
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.983
_refine_ls_restrained_S_obs      1.036
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_obs          0.0390
_refine_ls_shift/esd_max         0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1019
_refine_ls_wR_factor_obs         0.0996
_reflns_number_observed          6270
_reflns_number_total             7221
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9714992B_1.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0795P)^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^)+(0.0795P)^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        1561.8(11)
_cod_original_formula_sum        'C27.50 H30 Cl2 Hg N6 O8'
_cod_database_code               4327680