#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:42:34 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179343 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/40/4324029.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4324029
loop_
_publ_author_name
'Deborah C. Bebout'
'David E. Ehmann'
'Jonathan C. Trinidad'
'Kathleen K. Crahan'
'Margaret E. Kastner'
'Damon A. Parrish'
_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/[σ²(Fo²)+(0.0555P)²+0.0000P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Hg Hg 0.0000 0.5000 0.5000 0.04063(7) Uani 1 d S .
N N 0.0713(2) 0.7121(2) 0.55375(14) 0.0436(6) Uani 1 d . .
N1 N -0.1969(3) 0.6135(2) 0.5425(2) 0.0512(7) Uani 1 d . .
N2 N 0.0789(3) 0.6520(2) 0.41052(15) 0.0498(6) Uani 1 d . .
N3 N 0.2074(4) 0.5000(2) 0.6174(2) 0.0519(7) Uani 1 d . .
C1A C -0.3125(4) 0.5604(4) 0.5560(2) 0.0643(10) Uani 1 d . .
H1A H -0.3214(4) 0.4734(4) 0.5512(2) 0.080 Uiso 1 d R .
C1B C -0.4172(4) 0.6260(4) 0.5771(2) 0.0739(12) Uani 1 d . .
H1B H -0.5004(4) 0.5851(4) 0.5838(2) 0.080 Uiso 1 d R .
C1C C -0.4026(4) 0.7486(4) 0.5837(2) 0.0783(13) Uani 1 d . .
H1C H -0.4713(4) 0.7949(4) 0.6017(2) 0.080 Uiso 1 d R .
C1D C -0.2856(4) 0.8052(4) 0.5701(2) 0.0667(11) Uani 1 d . .
H1D H -0.2760(4) 0.8923(4) 0.5728(2) 0.080 Uiso 1 d R .
C1E C -0.1829(3) 0.7336(3) 0.5498(2) 0.0474(7) Uani 1 d . .
C1F C -0.0542(3) 0.7907(3) 0.5324(2) 0.0499(8) Uani 1 d . .
H1FB H -0.0736(3) 0.8051(3) 0.4799(2) 0.080 Uiso 1 d R .
H1FA H -0.0353(3) 0.8679(3) 0.5572(2) 0.080 Uiso 1 d R .
C2A C 0.0696(4) 0.6277(4) 0.3395(2) 0.0614(9) Uani 1 d . .
H2A H 0.0025(4) 0.5674(4) 0.3156(2) 0.080 Uiso 1 d R .
C2B C 0.1510(4) 0.6844(4) 0.2980(2) 0.0716(11) Uani 1 d . .
H2B H 0.1417(4) 0.6647(4) 0.2467(2) 0.080 Uiso 1 d R .
C2C C 0.2439(4) 0.7725(4) 0.3313(2) 0.0733(11) Uani 1 d . .
H2C H 0.3026(4) 0.8138(4) 0.3041(2) 0.080 Uiso 1 d R .
C2D C 0.2539(4) 0.8007(4) 0.4048(2) 0.0611(10) Uani 1 d . .
H2D H 0.3180(4) 0.8628(4) 0.4290(2) 0.080 Uiso 1 d R .
C2E C 0.1696(3) 0.7381(3) 0.4429(2) 0.0461(7) Uani 1 d . .
C2F C 0.1869(3) 0.7608(3) 0.5237(2) 0.0514(8) Uani 1 d . .
H2FB H 0.2739(3) 0.7236(3) 0.5498(2) 0.080 Uiso 1 d R .
H2FA H 0.1948(3) 0.8470(3) 0.5328(2) 0.080 Uiso 1 d R .
C3A C 0.2956(4) 0.4073(3) 0.6396(2) 0.0609(9) Uani 1 d . .
H3A H 0.2788(4) 0.3322(3) 0.6123(2) 0.080 Uiso 1 d R .
C3B C 0.4079(4) 0.4123(4) 0.7007(3) 0.0697(11) Uani 1 d . .
H3B H 0.4712(4) 0.3446(4) 0.7144(3) 0.080 Uiso 1 d R .
C3C C 0.4286(6) 0.5178(4) 0.7409(3) 0.0722(13) Uani 1 d . .
H3C H 0.5064(6) 0.5250(4) 0.7836(3) 0.080 Uiso 1 d R .
C3D C 0.3362(4) 0.6148(4) 0.7192(2) 0.0596(9) Uani 1 d . .
H3D H 0.3483(4) 0.6898(4) 0.7467(2) 0.080 Uiso 1 d R .
C3E C 0.2255(3) 0.6026(3) 0.6575(2) 0.0442(7) Uani 1 d . .
C3F C 0.1167(3) 0.7009(3) 0.6344(2) 0.0472(7) Uani 1 d . .
H3FB H 0.0365(3) 0.6835(3) 0.6543(2) 0.080 Uiso 1 d R .
H3FA H 0.1561(3) 0.7774(3) 0.6545(2) 0.080 Uiso 1 d R .
Cl Cl 0.12023(12) 0.53577(10) 0.85608(6) 0.0591(2) Uani 1 d . .
O1 O 0.1311(4) 0.4186(3) 0.8275(2) 0.0804(9) Uani 1 d . .
O2 O 0.0436(8) 0.5276(4) 0.9116(3) 0.131(2) Uani 1 d . .
O3 O 0.0512(4) 0.6138(3) 0.7969(2) 0.0997(11) Uani 1 d . .
O4 O 0.2582(4) 0.5789(4) 0.8873(2) 0.133(2) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N Hg N 180.0 3_566 . y
N Hg N1 114.07(9) 3_566 . y
N Hg N1 65.93(9) . . y
N Hg N1 65.93(9) 3_566 3_566 y
N Hg N1 114.07(9) . 3_566 y
N1 Hg N1 180.0 . 3_566 y
N Hg N3 65.69(9) 3_566 3_566 y
N Hg N3 114.31(9) . 3_566 y
N1 Hg N3 76.62(14) . 3_566 y
N1 Hg N3 103.38(14) 3_566 3_566 y
N Hg N3 114.31(9) 3_566 . y
N Hg N3 65.69(9) . . y
N1 Hg N3 103.38(14) . . y
N1 Hg N3 76.62(14) 3_566 . y
N3 Hg N3 180.0 3_566 . y
N Hg N2 64.63(12) 3_566 3_566 y
N Hg N2 115.37(12) . 3_566 y
N1 Hg N2 75.99(12) . 3_566 y
N1 Hg N2 104.01(12) 3_566 3_566 y
N3 Hg N2 104.32(13) 3_566 3_566 y
N3 Hg N2 75.68(13) . 3_566 y
N Hg N2 115.37(12) 3_566 . y
N Hg N2 64.63(12) . . y
N1 Hg N2 104.01(12) . . y
N1 Hg N2 75.99(12) 3_566 . y
N3 Hg N2 75.68(13) 3_566 . y
N3 Hg N2 104.32(13) . . y
N2 Hg N2 180.0 3_566 . y
C3F N C1F 110.8(3) . . y
C3F N C2F 110.3(3) . . y
C1F N C2F 110.3(3) . . y
C3F N Hg 108.1(2) . . y
C1F N Hg 107.3(2) . . y
C2F N Hg 110.0(2) . . y
C1E N1 C1A 118.7(3) . . y
C1E N1 Hg 116.6(2) . . y
C1A N1 Hg 124.7(2) . . y
C2A N2 C2E 118.1(3) . . y
C2A N2 Hg 123.1(2) . . y
C2E N2 Hg 115.6(2) . . y
C3A N3 C3E 118.8(4) . . y
C3A N3 Hg 125.1(3) . . y
C3E N3 Hg 116.1(2) . . y
N1 C1A C1B 122.4(4) . . y
C1C C1B C1A 118.4(4) . . y
C1B C1C C1D 120.4(4) . . y
C1C C1D C1E 118.4(4) . . y
N1 C1E C1D 121.6(3) . . y
N1 C1E C1F 117.4(3) . . y
C1D C1E C1F 120.9(3) . . y
N C1F C1E 112.3(3) . . y
N2 C2A C2B 123.5(4) . . y
C2C C2B C2A 118.3(4) . . y
C2B C2C C2D 119.2(3) . . y
C2C C2D C2E 118.9(4) . . y
N2 C2E C2D 122.0(3) . . y
N2 C2E C2F 118.4(3) . . y
C2D C2E C2F 119.5(3) . . y
N C2F C2E 114.1(3) . . y
N3 C3A C3B 123.5(4) . . y
C3C C3B C3A 118.0(4) . . y
C3B C3C C3D 119.3(4) . . y
C3E C3D C3C 119.3(4) . . y
N3 C3E C3D 121.1(3) . . y
N3 C3E C3F 117.1(3) . . y
C3D C3E C3F 121.8(3) . . y
N C3F C3E 112.0(3) . . y
O1 Cl O2 108.6(3) . . y
O1 Cl O4 108.1(2) . . y
O2 Cl O4 109.8(4) . . y
O1 Cl O3 108.8(2) . . y
O2 Cl O3 111.4(3) . . y
O4 Cl O3 110.0(3) . . y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Hg N 2.560(3) 3_566 y
Hg N 2.560(3) . y
Hg N1 2.562(3) . y
Hg N1 2.562(3) 3_566 y
Hg N3 2.593(6) 3_566 y
Hg N3 2.593(6) . y
Hg N2 2.595(4) 3_566 y
Hg N2 2.595(4) . y
N C3F 1.460(5) . y
N C1F 1.469(4) . y
N C2F 1.471(4) . y
N1 C1E 1.328(4) . y
N1 C1A 1.343(4) . y
N2 C2A 1.327(5) . y
N2 C2E 1.334(4) . y
N3 C3A 1.331(5) . y
N3 C3E 1.336(4) . y
C1A C1B 1.379(5) . y
C1B C1C 1.354(6) . y
C1C C1D 1.372(6) . y
C1D C1E 1.391(5) . y
C1E C1F 1.504(5) . y
C2A C2B 1.377(5) . y
C2B C2C 1.366(6) . y
C2C C2D 1.379(6) . y
C2D C2E 1.386(5) . y
C2E C2F 1.489(5) . y
C3A C3B 1.375(6) . y
C3B C3C 1.365(6) . y
C3C C3D 1.389(6) . y
C3D C3E 1.379(5) . y
C3E C3F 1.500(4) . y
Cl O1 1.403(3) . y
Cl O2 1.411(5) . y
Cl O4 1.412(4) . y
Cl O3 1.428(4) . y
