#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:32:23 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179333 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/30/4323001.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_4323001
loop_
_publ_author_name
'Deborah C. Bebout'
'James F. Bush'
'Kathleen K. Crahan'
'Margaret E. Kastner'
'Damon A. Parrish'
_publ_section_title
;
 Correlation of a Solution-State Conformational Change between Mercuric
 Chloride Complexes of Tris[(2-(6-methylpyridyl))methyl]amine with X-ray
 Crystallographic Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4641
_journal_page_last               4646
_journal_paper_doi               10.1021/ic980296y
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C21 H24 Cl2 Hg N4'
_chemical_formula_sum            'C21 H24 Cl2 Hg N4'
_chemical_formula_weight         603.93
_chemical_name_systematic
; 
tris[(2-methylpyridyl)methyl]aminedichloromercury(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                80.81(2)
_cell_angle_beta                 75.84(2)
_cell_angle_gamma                80.97(3)
_cell_formula_units_Z            2
_cell_length_a                   8.663(3)
_cell_length_b                   11.539(4)
_cell_length_c                   13.739(3)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.51
_cell_measurement_theta_min      9.04
_cell_volume                     1304.6(7)
_computing_cell_refinement       'Siemens 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       omega
_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  0.3286
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6486
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        5%
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.116
_exptl_absorpt_correction_T_max  0.0650
_exptl_absorpt_correction_T_min  0.0181
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_meas      1.57
_exptl_crystal_density_method    'flotation in bromofrom/hexane solution'
_exptl_crystal_description       'semi-clear plate'
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.218
_refine_diff_density_min         -2.337
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.140
_refine_ls_goodness_of_fit_obs   1.252
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         5998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_restrained_S_obs      1.252
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_obs          0.0516
_refine_ls_shift/esd_max         -0.181
_refine_ls_shift/esd_mean        0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1043P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1639
_refine_ls_wR_factor_obs         0.1599
_reflns_number_observed          4767
_reflns_number_total             5998
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980296y_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (32 times).

'_geom_angle_publ_flag' value 'Y'
changed to 'y' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (53
times).

Automatic conversion script
Id: cif_fix_values 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1043P)^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^)+(0.1043P)^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_database_code               4323001
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.21760(4) 0.59545(3) 0.25568(2) 0.05168(14) Uani 1 d . .
N N 0.2391(8) 0.3751(6) 0.2654(5) 0.0468(13) Uani 1 d . .
N1 N 0.4418(7) 0.4994(6) 0.3344(5) 0.0476(14) Uani 1 d . .
N2 N 0.0008(8) 0.5373(7) 0.1875(6) 0.055(2) Uani 1 d . .
N3 N 0.2679(12) 0.1638(8) 0.1472(7) 0.077(2) Uani 1 d . .
C1A C 0.5584(10) 0.5560(9) 0.3499(6) 0.055(2) Uani 1 d . .
C1B C 0.6784(10) 0.4958(10) 0.3954(7) 0.063(2) Uani 1 d . .
H1B H 0.7606(10) 0.5364(10) 0.4058(7) 0.080 Uiso 1 d R .
C1C C 0.6791(11) 0.3771(12) 0.4258(7) 0.070(3) Uani 1 d . .
H1C H 0.7590(11) 0.3347(12) 0.4602(7) 0.080 Uiso 1 d R .
C1D C 0.5623(11) 0.3187(9) 0.4087(6) 0.058(2) Uani 1 d . .
H1D H 0.5662(11) 0.2344(9) 0.4253(6) 0.080 Uiso 1 d R .
C1E C 0.4426(9) 0.3831(7) 0.3649(6) 0.048(2) Uani 1 d . .
C1F C 0.3048(10) 0.3250(8) 0.3557(6) 0.053(2) Uani 1 d . .
H1FB H 0.3380(10) 0.2418(8) 0.3540(6) 0.080 Uiso 1 d R .
H1FA H 0.2204(10) 0.3342(8) 0.4150(6) 0.080 Uiso 1 d R .
C1G C 0.5463(14) 0.6866(10) 0.3137(9) 0.074(3) Uani 1 d . .
H1GC H 0.4544(14) 0.7096(10) 0.2845(9) 0.080 Uiso 1 d R .
H1GB H 0.5356(14) 0.7299(10) 0.3696(9) 0.080 Uiso 1 d R .
H1GA H 0.6415(14) 0.7034(10) 0.2635(9) 0.080 Uiso 1 d R .
C2A C -0.0871(10) 0.6103(10) 0.1283(7) 0.062(2) Uani 1 d . .
C2B C -0.1887(11) 0.5672(12) 0.0841(8) 0.072(3) Uani 1 d . .
H2B H -0.2504(11) 0.6205(12) 0.0428(8) 0.080 Uiso 1 d R .
C2C C -0.1984(11) 0.4523(12) 0.0952(8) 0.072(3) Uani 1 d . .
H2C H -0.2660(11) 0.4212(12) 0.0624(8) 0.080 Uiso 1 d R .
C2D C -0.1071(11) 0.3742(11) 0.1583(8) 0.070(3) Uani 1 d . .
H2D H -0.1106(11) 0.2903(11) 0.1682(8) 0.080 Uiso 1 d R .
C2E C -0.0111(10) 0.4224(9) 0.2032(6) 0.056(2) Uani 1 d . .
C2F C 0.0769(10) 0.3487(8) 0.2797(7) 0.055(2) Uani 1 d . .
H2FB H 0.0189(10) 0.3636(8) 0.3465(7) 0.080 Uiso 1 d R .
H2FA H 0.0796(10) 0.2661(8) 0.2754(7) 0.080 Uiso 1 d R .
C2G C -0.0669(14) 0.7361(10) 0.1123(10) 0.080(3) Uani 1 d . .
H2GC H 0.0054(14) 0.7508(10) 0.1506(10) 0.080 Uiso 1 d R .
H2GB H -0.0242(14) 0.7585(10) 0.0416(10) 0.080 Uiso 1 d R .
H2GA H -0.1693(14) 0.7817(10) 0.1330(10) 0.080 Uiso 1 d R .
C3A C 0.2984(20) 0.0469(11) 0.1320(10) 0.094(4) Uani 1 d . .
C3B C 0.4501(22) -0.0178(12) 0.1294(10) 0.102(5) Uani 1 d . .
H3B H 0.4663(22) -0.1006(12) 0.1225(10) 0.080 Uiso 1 d R .
C3C C 0.5703(21) 0.0412(13) 0.1384(11) 0.105(5) Uani 1 d . .
H3C H 0.6773(21) 0.0013(13) 0.1334(11) 0.080 Uiso 1 d R .
C3D C 0.5366(14) 0.1574(10) 0.1562(9) 0.076(3) Uani 1 d . .
H3D H 0.6191(14) 0.1981(10) 0.1661(9) 0.080 Uiso 1 d R .
C3E C 0.3879(12) 0.2161(8) 0.1579(6) 0.057(2) Uani 1 d . .
C3F C 0.3477(10) 0.3427(7) 0.1711(6) 0.051(2) Uani 1 d . .
H3FB H 0.4466(10) 0.3736(7) 0.1656(6) 0.080 Uiso 1 d R .
H3FA H 0.3026(10) 0.3830(7) 0.1158(6) 0.080 Uiso 1 d R .
C3G C 0.1543(27) -0.0063(15) 0.1190(17) 0.156(8) Uani 1 d . .
H3GC H 0.1884(27) -0.0879(15) 0.1099(17) 0.080 Uiso 1 d R .
H3GB H 0.0690(27) -0.0012(15) 0.1784(17) 0.080 Uiso 1 d R .
H3GA H 0.1170(27) 0.0346(15) 0.0610(17) 0.080 Uiso 1 d R .
Cl1 Cl 0.3786(3) 0.6664(2) 0.0913(2) 0.0648(5) Uani 1 d . .
Cl2 Cl 0.0420(4) 0.6870(4) 0.3948(2) 0.0936(10) 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'
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
Cl2 Hg Cl1 135.32(13) . . y
Cl2 Hg N1 100.8(2) . . y
Cl1 Hg N1 97.6(2) . . y
Cl2 Hg N 117.6(2) . . y
Cl1 Hg N 106.9(2) . . y
N1 Hg N 69.6(2) . . y
Cl2 Hg N2 96.5(2) . . y
Cl1 Hg N2 95.7(2) . . y
N1 Hg N2 138.9(2) . . y
N Hg N2 69.3(2) . . y
C2F N C3F 114.7(6) . . y
C2F N C1F 110.7(7) . . y
C3F N C1F 112.2(6) . . y
C2F N Hg 105.5(5) . . y
C3F N Hg 106.7(5) . . y
C1F N Hg 106.4(5) . . y
C1E N1 C1A 119.2(7) . . y
C1E N1 Hg 115.7(5) . . y
C1A N1 Hg 125.1(6) . . y
C2E N2 C2A 119.7(8) . . y
C2E N2 Hg 114.5(5) . . y
C2A N2 Hg 125.3(7) . . y
C3E N3 C3A 118.1(11) . . y
N1 C1A C1B 121.3(9) . . y
N1 C1A C1G 115.2(8) . . y
C1B C1A C1G 123.5(9) . . y
C1C C1B C1A 119.1(9) . . y
C1B C1C C1D 119.8(9) . . y
C1C C1D C1E 119.0(9) . . y
N1 C1E C1D 121.5(8) . . y
N1 C1E C1F 118.2(7) . . y
C1D C1E C1F 120.2(8) . . y
N C1F C1E 113.9(7) . . y
N2 C2A C2B 121.0(10) . . y
N2 C2A C2G 117.2(9) . . y
C2B C2A C2G 121.8(10) . . y
C2C C2B C2A 120.7(10) . . y
C2B C2C C2D 118.8(9) . . y
C2E C2D C2C 118.1(11) . . y
N2 C2E C2D 121.7(9) . . y
N2 C2E C2F 116.3(7) . . y
C2D C2E C2F 121.9(9) . . y
N C2F C2E 112.9(7) . . y
N3 C3A C3B 121.8(13) . . y
N3 C3A C3G 114.9(14) . . y
C3B C3A C3G 123.3(13) . . y
C3C C3B C3A 117.5(12) . . y
C3B C3C C3D 119.8(14) . . y
C3E C3D C3C 120.3(13) . . y
N3 C3E C3D 122.3(9) . . y
N3 C3E C3F 115.2(8) . . y
C3D C3E C3F 122.5(9) . . y
N C3F C3E 118.4(7) . . 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 Cl2 2.408(3) . y
Hg Cl1 2.438(2) . y
Hg N1 2.478(7) . y
Hg N 2.505(7) . y
Hg N2 2.513(6) . y
N C2F 1.444(10) . y
N C3F 1.467(10) . y
N C1F 1.487(10) . y
N1 C1E 1.340(11) . y
N1 C1A 1.359(10) . y
N2 C2E 1.325(12) . y
N2 C2A 1.354(12) . y
N3 C3E 1.329(13) . y
N3 C3A 1.373(15) . y
C1A C1B 1.381(13) . y
C1A C1G 1.505(15) . y
C1B C1C 1.37(2) . y
C1C C1D 1.384(15) . y
C1D C1E 1.382(11) . y
C1E C1F 1.498(11) . y
C2A C2B 1.373(14) . y
C2A C2G 1.46(2) . y
C2B C2C 1.32(2) . y
C2C C2D 1.43(2) . y
C2D C2E 1.373(12) . y
C2E C2F 1.521(13) . y
C3A C3B 1.40(2) . y
C3A C3G 1.53(2) . y
C3B C3C 1.37(2) . y
C3C C3D 1.38(2) . y
C3D C3E 1.355(14) . y
C3E C3F 1.478(12) . y
