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_4324029
_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         'C36 H36 Hg N8 2+,(Cl O4 1-)2'
_chemical_formula_sum            'C36 H36 Cl2 Hg N8 O8'
_chemical_formula_weight         980.22
_chemical_name_systematic
; 
bis-tris[(2-pyridyl)methyl]aminemercury(II) perchlorate 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.81(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.735(10)
_cell_length_b                   10.963(2)
_cell_length_c                   18.553(34)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.43
_cell_measurement_theta_min      5.69
_cell_volume                     1923(4)
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7507
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.203
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      1.689
_exptl_crystal_density_method    'floatation in bromoform/hexane solution'
_exptl_crystal_description       'cloudy needle'
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.304
_refine_diff_density_min         -2.003
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.901
_refine_ls_goodness_of_fit_obs   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_restrained_S_obs      1.004
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_obs          0.0277
_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^)+(0.0555P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0823
_refine_ls_wR_factor_obs         0.0700
_reflns_number_observed          3194
_reflns_number_total             4420
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9702779_2.cif
_cod_data_source_block           hg1d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0555P)^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^)+(0.0555P)^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        1922.8(41)
_cod_database_code               4324029