#------------------------------------------------------------------------------
#$Date: 2016-02-05 00:25:18 +0200 (Fri, 05 Feb 2016) $
#$Revision: 175960 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/37/7223734.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_7223734
loop_
_publ_author_name
'Mahmoudi, Ghodrat'
'Castiñeiras, Alfonso'
'Garczarek, Piotr'
'Bauzá, Antonio'
'Rheingold, Arnold L.'
'Kinzhybalo, Vasyl'
'Frontera, Antonio'
_publ_section_title
;
 Synthesis, X-ray characterization, DFT calculations and Hirshfeld surface
 analysis of thiosemicarbazone complexes of Mn+ions (n = 2, 3; M = Ni, Cd,
 Mn, Co and Cu)
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1009
_journal_paper_doi               10.1039/C5CE02371H
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C26 H20 Cl8 Hg4 N6'
_chemical_formula_sum            'C26 H20 Cl8 Hg4 N6'
_chemical_formula_weight         1502.44
_chemical_name_common            1
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_update_record
;
2015-03-19 deposited with the CCDC.
2016-01-05 downloaded from the CCDC.
;
_cell_angle_alpha                104.8910(10)
_cell_angle_beta                 101.344(2)
_cell_angle_gamma                99.190(4)
_cell_formula_units_Z            2
_cell_length_a                   7.6970(3)
_cell_length_b                   15.9190(5)
_cell_length_c                   16.0270(7)
_cell_measurement_reflns_used    443
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1814.35(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'maXus, Zortep'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1547
_diffrn_reflns_av_unetI/netI     0.1717
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12858
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.489
_exptl_absorpt_correction_T_max  0.2737
_exptl_absorpt_correction_T_min  0.0773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   HKL2008
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.75
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.695
_refine_diff_density_min         -3.586
_refine_diff_density_rms         0.366
_refine_ls_extinction_coef       0.0015(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         8150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0787
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1081P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1929
_refine_ls_wR_factor_ref         0.2325
_reflns_number_gt                4352
_reflns_number_total             8150
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            c5ce02371h2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7223734--7223741.cif.'
_cod_original_cell_volume        1814.35(12)
_cod_database_code               7223734
_audit_block_doi                 10.5517/cc143g7y
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.406(2) 0.8566(13) 0.8490(13) 0.054(5) Uani 1 1 d .
H1 H 0.3003 0.8193 0.8096 0.065 Uiso 1 1 calc R
C2 C 0.499(3) 0.8295(15) 0.9205(14) 0.069(6) Uani 1 1 d .
H2 H 0.4576 0.773 0.9248 0.083 Uiso 1 1 calc R
C3 C 0.644(3) 0.8842(17) 0.9809(15) 0.076(7) Uani 1 1 d .
H3 H 0.6979 0.8694 1.0307 0.091 Uiso 1 1 calc R
C4 C 0.711(2) 0.9652(12) 0.9665(14) 0.055(5) Uani 1 1 d .
H4 H 0.8167 1.0029 1.0056 0.066 Uiso 1 1 calc R
C5 C 0.626(2) 0.9903(11) 0.8968(11) 0.043(4) Uani 1 1 d .
C6 C 0.696(2) 1.0700(11) 0.8804(13) 0.048(4) Uani 1 1 d .
H6 H 0.8026 1.1074 0.9189 0.058 Uiso 1 1 calc R
C7 C 0.279(3) 0.9173(13) 0.5228(13) 0.064(6) Uani 1 1 d .
H7 H 0.3031 0.8654 0.5344 0.077 Uiso 1 1 calc R
C8 C 0.248(3) 0.9206(12) 0.4337(12) 0.056(5) Uani 1 1 d .
H8 H 0.2474 0.8711 0.3876 0.067 Uiso 1 1 calc R
C9 C 0.218(2) 0.9977(12) 0.4163(12) 0.054(5) Uani 1 1 d .
H9 H 0.1984 1.0017 0.3584 0.065 Uiso 1 1 calc R
C10 C 0.218(3) 1.0695(14) 0.4867(13) 0.063(6) Uani 1 1 d .
H10 H 0.1954 1.122 0.476 0.075 Uiso 1 1 calc R
C11 C 0.251(2) 1.0636(11) 0.5759(11) 0.045(4) Uani 1 1 d .
C12 C 0.264(2) 1.1406(12) 0.6508(11) 0.051(5) Uani 1 1 d .
H12 H 0.2433 1.1942 0.6425 0.061 Uiso 1 1 calc R
C13 C 0.477(2) 1.2443(11) 0.8431(12) 0.048(4) Uani 1 1 d .
C14 C 0.648(2) 1.2355(11) 0.8094(11) 0.048(4) Uani 1 1 d .
C15 C 0.508(2) 1.3092(11) 0.9278(11) 0.048(4) Uani 1 1 d .
C16 C 0.363(4) 1.3346(15) 0.9625(15) 0.080(7) Uani 1 1 d .
H16 H 0.2455 1.309 0.928 0.096 Uiso 1 1 calc R
C17 C 0.388(4) 1.3973(17) 1.0478(18) 0.095(8) Uani 1 1 d .
H17 H 0.2896 1.4153 1.0668 0.114 Uiso 1 1 calc R
C18 C 0.554(3) 1.4287(15) 1.0986(15) 0.087(8) Uani 1 1 d .
H18 H 0.5712 1.4674 1.1554 0.104 Uiso 1 1 calc R
C19 C 0.700(4) 1.4077(16) 1.0726(16) 0.089(8) Uani 1 1 d .
H19 H 0.8156 1.4328 1.1102 0.106 Uiso 1 1 calc R
C20 C 0.678(3) 1.3468(13) 0.9869(12) 0.064(6) Uani 1 1 d .
H20 H 0.7808 1.3317 0.9699 0.077 Uiso 1 1 calc R
C21 C 0.741(3) 1.3106(14) 0.7868(15) 0.065(6) Uani 1 1 d .
C22 C 0.651(3) 1.3816(13) 0.7789(12) 0.061(5) Uani 1 1 d .
H22 H 0.5343 1.3789 0.7869 0.074 Uiso 1 1 calc R
C23 C 0.740(4) 1.4547(14) 0.7591(13) 0.072(6) Uani 1 1 d .
H23 H 0.6803 1.4993 0.75 0.086 Uiso 1 1 calc R
C24 C 0.911(4) 1.4595(17) 0.7534(13) 0.089(9) Uani 1 1 d .
H24 H 0.9715 1.5105 0.7442 0.107 Uiso 1 1 calc R
C25 C 1.009(3) 1.3903(17) 0.7605(13) 0.081(8) Uani 1 1 d .
H25 H 1.1282 1.3964 0.7546 0.097 Uiso 1 1 calc R
C26 C 0.923(3) 1.3151(18) 0.7764(12) 0.079(7) Uani 1 1 d .
H26 H 0.9809 1.2688 0.7803 0.094 Uiso 1 1 calc R
N1 N 0.4693(16) 0.9345(9) 0.8384(9) 0.038(3) Uani 1 1 d .
N2 N 0.6182(17) 1.0926(9) 0.8149(10) 0.048(3) Uani 1 1 d .
N3 N 0.2760(18) 0.9856(9) 0.5905(9) 0.044(3) Uani 1 1 d .
N4 N 0.3057(18) 1.1317(10) 0.7270(9) 0.051(4) Uani 1 1 d .
N5 N 0.315(2) 1.1998(10) 0.8021(10) 0.059(4) Uani 1 1 d .
N6 N 0.7086(18) 1.1663(10) 0.7975(11) 0.050(4) Uani 1 1 d .
Hg1 Hg 0.31403(10) 0.97794(5) 0.73156(4) 0.0523(3) Uani 1 1 d .
Hg2 Hg -0.13033(11) 0.82359(6) 0.76347(6) 0.0694(3) Uani 1 1 d .
Hg3 Hg -0.02474(9) 0.63150(5) 0.52500(6) 0.0575(3) Uani 1 1 d .
Hg4 Hg 0.48215(10) 0.64272(6) 0.53740(6) 0.0621(3) Uani 1 1 d .
Cl1 Cl 0.0411(6) 0.9964(3) 0.8074(3) 0.0608(12) Uani 1 1 d .
Cl2 Cl 0.0789(6) 0.8041(3) 0.6476(3) 0.0585(12) Uani 1 1 d .
Cl3 Cl -0.4048(6) 0.8246(4) 0.6630(4) 0.0666(13) Uani 1 1 d .
Cl4 Cl -0.0213(9) 0.7743(5) 0.8847(5) 0.097(2) Uani 1 1 d .
Cl5 Cl -0.2466(7) 0.6640(3) 0.4248(4) 0.0630(13) Uani 1 1 d .
Cl6 Cl 0.2784(6) 0.6923(3) 0.4480(3) 0.0559(11) Uani 1 1 d .
Cl7 Cl 0.6787(7) 0.5793(5) 0.6152(5) 0.092(2) Uani 1 1 d .
Cl8 Cl 0.1715(7) 0.5701(4) 0.6099(4) 0.0675(14) Uani 1 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 0 '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'
Hg Hg -2.3894 9.2266 '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'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C5CE00382B 2015
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_3
N1 C1 C2 120.5(17) .
N1 C1 H1 119.7 .
C2 C1 H1 119.7 .
C3 C2 C1 120.7(19) .
C3 C2 H2 119.6 .
C1 C2 H2 119.6 .
C2 C3 C4 117.3(18) .
C2 C3 H3 121.3 .
C4 C3 H3 121.3 .
C5 C4 C3 122.0(18) .
C5 C4 H4 119 .
C3 C4 H4 119 .
C4 C5 N1 119.2(15) .
C4 C5 C6 122.3(16) .
N1 C5 C6 118.5(14) .
N2 C6 C5 122.2(16) .
N2 C6 H6 118.9 .
C5 C6 H6 118.9 .
N3 C7 C8 122.5(17) .
N3 C7 H7 118.7 .
C8 C7 H7 118.7 .
C9 C8 C7 119.1(17) .
C9 C8 H8 120.4 .
C7 C8 H8 120.4 .
C8 C9 C10 118.6(16) .
C8 C9 H9 120.7 .
C10 C9 H9 120.7 .
C9 C10 C11 120.6(17) .
C9 C10 H10 119.7 .
C11 C10 H10 119.7 .
N3 C11 C10 119.3(17) .
N3 C11 C12 119.8(15) .
C10 C11 C12 120.9(15) .
N4 C12 C11 117.0(16) .
N4 C12 H12 121.5 .
C11 C12 H12 121.5 .
N5 C13 C15 119.4(18) .
N5 C13 C14 126.0(17) .
C15 C13 C14 114.6(15) .
N6 C14 C21 118.5(18) .
N6 C14 C13 123.3(15) .
C21 C14 C13 118.2(15) .
C20 C15 C16 113.6(18) .
C20 C15 C13 124.4(18) .
C16 C15 C13 121.7(18) .
C15 C16 C17 124(2) .
C15 C16 H16 118.2 .
C17 C16 H16 118.2 .
C18 C17 C16 118(2) .
C18 C17 H17 121.1 .
C16 C17 H17 121.1 .
C17 C18 C19 123(2) .
C17 C18 H18 118.4 .
C19 C18 H18 118.4 .
C18 C19 C20 120(2) .
C18 C19 H19 120.1 .
C20 C19 H19 120.1 .
C15 C20 C19 122(2) .
C15 C20 H20 119 .
C19 C20 H20 119 .
C22 C21 C26 120.5(19) .
C22 C21 C14 119.4(17) .
C26 C21 C14 120(2) .
C23 C22 C21 120(2) .
C23 C22 H22 120 .
C21 C22 H22 120 .
C24 C23 C22 119(2) .
C24 C23 H23 120.6 .
C22 C23 H23 120.6 .
C23 C24 C25 124(2) .
C23 C24 H24 117.9 .
C25 C24 H24 117.9 .
C26 C25 C24 119(2) .
C26 C25 H25 120.7 .
C24 C25 H25 120.7 .
C25 C26 C21 118(3) .
C25 C26 H26 121 .
C21 C26 H26 121 .
C1 N1 C5 120.0(13) .
C1 N1 Hg1 119.6(10) .
C5 N1 Hg1 120.2(10) .
C6 N2 N6 118.0(14) .
C6 N2 Hg1 109.5(11) .
N6 N2 Hg1 132.4(10) .
C7 N3 C11 119.8(15) .
C7 N3 Hg1 122.4(11) .
C11 N3 Hg1 117.8(12) .
C12 N4 N5 121.3(15) .
C12 N4 Hg1 115.5(12) .
N5 N4 Hg1 122.3(10) .
C13 N5 N4 113.8(16) .
C14 N6 N2 119.4(15) .
N1 Hg1 N3 146.8(5) .
N1 Hg1 N4 128.6(5) .
N3 Hg1 N4 69.2(5) .
N1 Hg1 N2 69.0(5) .
N3 Hg1 N2 102.9(5) .
N4 Hg1 N2 66.5(4) .
N1 Hg1 Cl1 94.0(3) .
N3 Hg1 Cl1 117.7(4) .
N4 Hg1 Cl1 82.9(4) .
N2 Hg1 Cl1 115.3(3) .
N1 Hg1 Cl2 92.9(4) .
N3 Hg1 Cl2 83.9(4) .
N4 Hg1 Cl2 136.0(3) .
N2 Hg1 Cl2 156.4(3) .
Cl1 Hg1 Cl2 79.77(15) .
Cl4 Hg2 Cl3 142.6(2) .
Cl4 Hg2 Cl2 111.6(2) .
Cl3 Hg2 Cl2 98.13(17) .
Cl4 Hg2 Cl1 106.0(2) .
Cl3 Hg2 Cl1 99.84(17) .
Cl2 Hg2 Cl1 82.47(15) .
Cl5 Hg3 Cl8 168.82(19) .
Cl5 Hg3 Cl2 95.51(17) .
Cl8 Hg3 Cl2 95.33(18) .
Cl5 Hg3 Cl6 94.52(15) .
Cl8 Hg3 Cl6 88.98(15) .
Cl2 Hg3 Cl6 85.77(14) .
Cl6 Hg4 Cl7 174.0(2) .
Cl6 Hg4 Cl3 88.50(16) 1_655
Cl7 Hg4 Cl3 97.4(2) 1_655
Hg1 Cl1 Hg2 99.53(16) .
Hg2 Cl2 Hg3 111.33(16) .
Hg2 Cl2 Hg1 94.44(15) .
Hg3 Cl2 Hg1 153.92(19) .
Hg2 Cl3 Hg4 104.37(19) 1_455
Hg4 Cl6 Hg3 92.47(16) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.32(2) .
C1 C2 1.43(2) .
C1 H1 0.93 .
C2 C3 1.33(3) .
C2 H2 0.93 .
C3 C4 1.40(3) .
C3 H3 0.93 .
C4 C5 1.36(2) .
C4 H4 0.93 .
C5 N1 1.38(2) .
C5 C6 1.41(2) .
C6 N2 1.27(2) .
C6 H6 0.93 .
C7 N3 1.33(2) .
C7 C8 1.42(3) .
C7 H7 0.93 .
C8 C9 1.37(3) .
C8 H8 0.93 .
C9 C10 1.39(3) .
C9 H9 0.93 .
C10 C11 1.43(2) .
C10 H10 0.93 .
C11 N3 1.36(2) .
C11 C12 1.45(3) .
C12 N4 1.25(2) .
C12 H12 0.93 .
C13 N5 1.29(2) .
C13 C15 1.43(2) .
C13 C14 1.53(3) .
C14 N6 1.25(2) .
C14 C21 1.46(2) .
C15 C20 1.39(3) .
C15 C16 1.41(3) .
C16 C17 1.43(3) .
C16 H16 0.93 .
C17 C18 1.32(3) .
C17 H17 0.93 .
C18 C19 1.33(3) .
C18 H18 0.93 .
C19 C20 1.42(3) .
C19 H19 0.93 .
C20 H20 0.93 .
C21 C22 1.43(3) .
C21 C26 1.44(3) .
C22 C23 1.39(3) .
C22 H22 0.93 .
C23 C24 1.33(4) .
C23 H23 0.93 .
C24 C25 1.45(4) .
C24 H24 0.93 .
C25 C26 1.38(3) .
C25 H25 0.93 .
C26 H26 0.93 .
N1 Hg1 2.216(11) .
N2 N6 1.387(19) .
N2 Hg1 2.598(14) .
N3 Hg1 2.259(13) .
N4 N5 1.38(2) .
N4 Hg1 2.478(15) .
Hg1 Cl1 2.645(5) .
Hg1 Cl2 2.877(5) .
Hg2 Cl4 2.333(6) .
Hg2 Cl3 2.396(5) .
Hg2 Cl2 2.679(5) .
Hg2 Cl1 2.699(5) .
Hg3 Cl5 2.322(5) .
Hg3 Cl8 2.331(5) .
Hg3 Cl2 2.820(5) .
Hg3 Cl6 2.989(5) .
Hg4 Cl6 2.286(4) .
Hg4 Cl7 2.293(5) .
Hg4 Cl3 2.951(6) 1_655
Cl3 Hg4 2.951(6) 1_455
