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#$Date: 2016-03-25 11:18:54 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179784 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/80/7008065.cif $
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#
# 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_7008065
loop_
_publ_author_name
'Pedrido, Rosa'
'Bermejo, Manuel R.'
'Romero, M José'
'Vázquez, Miguel'
'González-Noya, Ana M'
'Maneiro, Marcelino'
'Rodríguez, M Jesús'
'Fernández, M Isabel'
_publ_section_title
;
 Syntheses and X-ray characterization of metal complexes with the
 pentadentate thiosemicarbazone ligand
 bis(4-N-methylthiosemicarbazone)-2,6-diacetylpyridine. The first
 pentacoordinate lead(II) complex with a pentagonal geometry.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              572
_journal_page_last               579
_journal_paper_doi               10.1039/b416296j
_journal_year                    2005
_chemical_formula_sum            'C17 H29 Mn N7 O2 S2'
_chemical_formula_weight         482.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(4)
_cell_angle_beta                 100.32(2)
_cell_angle_gamma                90.00(2)
_cell_formula_units_Z            4
_cell_length_a                   14.981(6)
_cell_length_b                   10.466(4)
_cell_length_c                   14.281(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2202.9(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    0.0091
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5038
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    0.817
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1004
_refine_diff_density_max         0.006
_refine_diff_density_min         -0.008
_refine_diff_density_rms         0.001
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.246
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2519
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.246
_refine_ls_R_factor_all          0.0011
_refine_ls_R_factor_gt           0.0008
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0022
_refine_ls_wR_factor_ref         0.0033
_reflns_number_gt                2450
_reflns_number_total             2519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b416296j.txt
_cod_data_source_block           mndaptszme
_cod_database_code               7008065
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.0000 0.476570(2) 0.2500 0.03154(1) Uani 1 2 d S . .
S1 S -0.079872(2) 0.286829(2) 0.152843(2) 0.04578(1) Uani 1 1 d . . .
N4 N 0.0000 0.692800(9) 0.2500 0.03133(2) Uani 1 2 d S . .
N3 N -0.071205(5) 0.555992(7) 0.099544(5) 0.03156(2) Uani 1 1 d . . .
N2 N -0.104903(6) 0.481205(7) 0.021958(5) 0.03368(2) Uani 1 1 d . . .
N1 N -0.133912(7) 0.281004(8) -0.033707(6) 0.04447(2) Uani 1 1 d . . .
C5 C -0.037689(6) 0.757091(8) 0.171106(7) 0.03338(2) Uani 1 1 d . . .
C6 C -0.038908(8) 0.890729(9) 0.169503(8) 0.04406(2) Uani 1 1 d . . .
C7 C 0.0000 0.956100(13) 0.2500 0.04890(4) Uani 1 2 d S . .
C4 C -0.076904(6) 0.678904(8) 0.087298(7) 0.03346(2) Uani 1 1 d . . .
C3 C -0.120302(10) 0.742115(12) -0.003807(9) 0.05090(3) Uani 1 1 d . . .
C2 C -0.106712(6) 0.356097(9) 0.043090(6) 0.03318(2) Uani 1 1 d . . .
C1 C -0.146606(10) 0.144600(11) -0.032100(9) 0.05117(3) Uani 1 1 d . . .
O1S O 0.122895(5) 0.498897(7) 0.172710(5) 0.04107(2) Uani 1 1 d . . .
C1S C 0.218091(8) 0.480685(12) 0.207197(9) 0.04995(3) Uani 1 1 d . . .
C2S C 0.256634(10) 0.584503(15) 0.272902(11) 0.05974(3) Uani 1 1 d . . .
H1N H -0.14463(8) 0.31796(11) -0.08851(9) 0.0529(3) Uiso 1 1 d . . .
H6A H -0.06574(8) 0.93445(11) 0.11491(9) 0.0529(3) Uiso 1 1 d . . .
H7A H 0.0000 1.04499(17) 0.2500 0.0589(5) Uiso 1 2 d S . .
H3A H -0.14206(10) 0.67793(14) -0.05044(11) 0.0766(5) Uiso 1 1 d . . .
H3B H -0.07645(10) 0.79487(14) -0.02694(11) 0.0769(5) Uiso 1 1 d . . .
H3C H -0.17025(10) 0.79391(14) 0.00730(10) 0.0764(4) Uiso 1 1 d . . .
H1A H -0.16618(10) 0.11412(14) -0.09586(11) 0.0774(4) Uiso 1 1 d . . .
H1C H -0.19163(10) 0.12462(14) 0.00563(11) 0.0771(5) Uiso 1 1 d . . .
H1B H -0.09020(10) 0.10429(14) -0.00491(11) 0.0759(5) Uiso 1 1 d . . .
H1SA H 0.24974(8) 0.47808(12) 0.15373(10) 0.0599(4) Uiso 1 1 d . . .
H1SB H 0.22758(8) 0.39945(12) 0.24025(9) 0.0601(4) Uiso 1 1 d . . .
H2SA H 0.32022(11) 0.56936(15) 0.29447(11) 0.0891(5) Uiso 1 1 d . . .
H2SB H 0.22606(11) 0.58657(15) 0.32634(12) 0.0880(5) Uiso 1 1 d . . .
H2SC H 0.24852(10) 0.66503(15) 0.24013(12) 0.0896(5) Uiso 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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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'
S S 0.1246 0.1234 '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
N4 Mn1 O1S 84.224(16) . 2 ?
N4 Mn1 O1S 84.224(16) . . ?
O1S Mn1 O1S 168.447(7) 2 . ?
N4 Mn1 N3 69.482(13) . 2 ?
O1S Mn1 N3 78.48(3) 2 2 ?
O1S Mn1 N3 97.42(2) . 2 ?
N4 Mn1 N3 69.482(13) . . ?
O1S Mn1 N3 97.42(2) 2 . ?
O1S Mn1 N3 78.48(3) . . ?
N3 Mn1 N3 138.964(19) 2 . ?
N4 Mn1 S1 140.074(15) . . ?
O1S Mn1 S1 90.13(2) 2 . ?
O1S Mn1 S1 98.75(2) . . ?
N3 Mn1 S1 147.555(6) 2 . ?
N3 Mn1 S1 72.16(2) . . ?
N4 Mn1 S1 140.074(15) . 2 ?
O1S Mn1 S1 98.75(2) 2 2 ?
O1S Mn1 S1 90.13(2) . 2 ?
N3 Mn1 S1 72.16(2) 2 2 ?
N3 Mn1 S1 147.555(7) . 2 ?
S1 Mn1 S1 79.85(3) . 2 ?
C2 S1 Mn1 100.16(2) . . ?
C5 N4 C5 120.04(3) 2 . ?
C5 N4 Mn1 119.981(15) 2 . ?
C5 N4 Mn1 119.981(15) . . ?
C4 N3 N2 116.677(19) . . ?
C4 N3 Mn1 118.498(12) . . ?
N2 N3 Mn1 124.79(2) . . ?
C2 N2 N3 113.09(2) . . ?
C2 N1 C1 125.781(17) . . ?
N4 C5 C6 121.038(17) . . ?
N4 C5 C4 116.49(3) . . ?
C6 C5 C4 122.469(17) . . ?
C7 C6 C5 118.792(18) . . ?
C6 C7 C6 120.30(3) . 2 ?
N3 C4 C5 115.54(2) . . ?
N3 C4 C3 124.150(14) . . ?
C5 C4 C3 120.30(3) . . ?
N2 C2 N1 113.53(2) . . ?
N2 C2 S1 127.452(10) . . ?
N1 C2 S1 119.01(2) . . ?
C1S O1S Mn1 130.33(2) . . ?
O1S C1S C2S 111.71(2) . . ?
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
Mn1 N4 2.2631(9) . ?
Mn1 O1S 2.3218(7) 2 ?
Mn1 O1S 2.3218(7) . ?
Mn1 N3 2.3716(6) 2 ?
Mn1 N3 2.3716(6) . ?
Mn1 S1 2.5895(7) . ?
Mn1 S1 2.5895(7) 2 ?
S1 C2 1.7083(4) . ?
N4 C5 1.3465(4) 2 ?
N4 C5 1.3465(4) . ?
N3 C4 1.2990(5) . ?
N3 N2 1.3765(4) . ?
N2 C2 1.3451(5) . ?
N1 C2 1.3515(3) . ?
N1 C1 1.4409(6) . ?
C5 C6 1.3989(5) . ?
C5 C4 1.4817(4) . ?
C6 C7 1.3745(4) . ?
C7 C6 1.3745(4) 2 ?
C4 C3 1.5000(4) . ?
O1S C1S 1.4357(6) . ?
C1S C2S 1.4834(4) . ?
