#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:33:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179146 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/07/4310757.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_4310757
loop_
_publ_author_name
'Isabel García Santos'
'Ulrich Abram'
'Roger Alberto'
'Ezequiel Vázquez López'
'Agustín Sánchez'
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
 Tricarbonylrhenium(I) Complexes with Thiosemicarbazone Derivatives of
 2-Acetylpyridine and 2-Pyridine Formamide Showing Two Unusual
 Coordination Modes of Tridentate Thiosemicarbazone Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1834
_journal_page_last               1836
_journal_paper_doi               10.1021/ic035367u
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[Re(CO)3(APTPhtsc)]'
_chemical_formula_sum            'C17 H13 N4 O3 Re S'
_chemical_formula_weight         539.57
_chemical_name_systematic
'(Acetylpyridine phenylthiosemicarbazonato)tricarbonylrhenium(I)'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.31(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.705(1)
_cell_length_b                   13.552(1)
_cell_length_c                   11.389(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      15.28
_cell_volume                     1806.6(3)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'SCHAKAL, ZORTEP'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3878
_diffrn_reflns_theta_full        64.92
_diffrn_reflns_theta_max         64.92
_diffrn_reflns_theta_min         5.07
_diffrn_standards_decay_%        7.5
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.461
_exptl_absorpt_correction_T_max  0.6229
_exptl_absorpt_correction_T_min  0.3842
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0272P)²+2.4408P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                2751
_reflns_number_total             3063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035367usi20040130_124545_1.cif
_cod_data_source_block           tsc
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'PSI scan' changed to 'psi-scan'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+2.4408P] 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^)+(0.0272P)^2^+2.4408P] 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               4310757
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 0.257657(14) 0.406595(13) 0.239562(14) 0.03089(7) Uani 1 d . . .
C10 C 0.2686(4) 0.3501(3) 0.3929(4) 0.0379(10) Uani 1 d . . .
O10 O 0.2773(3) 0.3185(3) 0.4868(3) 0.0615(10) Uani 1 d . . .
C20 C 0.1242(4) 0.4746(3) 0.2907(4) 0.0366(9) Uani 1 d . . .
O20 O 0.0417(3) 0.5166(3) 0.3173(3) 0.0523(8) Uani 1 d . . .
C30 C 0.1592(4) 0.3016(4) 0.1912(4) 0.0427(10) Uani 1 d . . .
O30 O 0.1022(3) 0.2355(3) 0.1671(3) 0.0622(10) Uani 1 d . . .
N1 N 0.2544(3) 0.4548(3) 0.0559(3) 0.0375(8) Uani 1 d . . .
C2 C 0.1707(4) 0.5090(4) 0.0051(5) 0.0473(11) Uani 1 d . . .
C3 C 0.1578(5) 0.5160(4) -0.1150(5) 0.0568(14) Uani 1 d . . .
C4 C 0.2299(5) 0.4634(4) -0.1870(4) 0.0570(15) Uani 1 d . . .
C5 C 0.3193(5) 0.4106(4) -0.1372(4) 0.0490(12) Uani 1 d . . .
C6 C 0.3307(4) 0.4080(3) -0.0156(4) 0.0383(10) Uani 1 d . . .
C7 C 0.4267(4) 0.3619(3) 0.0468(3) 0.0366(9) Uani 1 d . . .
C8 C 0.5336(5) 0.3342(5) -0.0134(5) 0.0505(13) Uani 1 d . . .
N9 N 0.4127(3) 0.3591(3) 0.1602(3) 0.0327(7) Uani 1 d . . .
N10 N 0.5093(3) 0.3389(3) 0.2295(3) 0.0361(8) Uani 1 d . . .
C11 C 0.5189(3) 0.4085(3) 0.3081(3) 0.0313(8) Uani 1 d . . .
N12 N 0.6096(3) 0.4098(3) 0.3844(3) 0.0356(8) Uani 1 d . . .
S13 S 0.42189(8) 0.50865(7) 0.32084(8) 0.0335(2) Uani 1 d . . .
C14 C 0.7109(3) 0.3542(3) 0.3816(3) 0.0330(9) Uani 1 d . . .
C15 C 0.7927(4) 0.3758(4) 0.4670(4) 0.0474(12) Uani 1 d . . .
C16 C 0.8963(4) 0.3284(5) 0.4701(5) 0.0540(13) Uani 1 d . . .
C17 C 0.9213(4) 0.2575(4) 0.3871(4) 0.0480(12) Uani 1 d . . .
C18 C 0.8417(4) 0.2368(4) 0.3021(4) 0.0497(12) Uani 1 d . . .
C19 C 0.7368(4) 0.2831(4) 0.2990(4) 0.0437(11) Uani 1 d . . .
H2 H 0.132(5) 0.544(4) 0.052(5) 0.065(18) Uiso 1 d . . .
H3 H 0.099(5) 0.549(5) -0.156(5) 0.071(18) Uiso 1 d . . .
H4 H 0.228(5) 0.462(5) -0.266(5) 0.071(18) Uiso 1 d . . .
H5 H 0.376(4) 0.373(4) -0.179(4) 0.048(14) Uiso 1 d . . .
H8A H 0.554(6) 0.376(6) -0.077(7) 0.11(3) Uiso 1 d . . .
H8B H 0.523(5) 0.286(5) -0.071(6) 0.077(19) Uiso 1 d . . .
H8C H 0.591(5) 0.326(5) 0.035(5) 0.072(19) Uiso 1 d . . .
H12 H 0.597(4) 0.450(3) 0.444(4) 0.032(11) Uiso 1 d . . .
H15 H 0.778(4) 0.427(4) 0.516(4) 0.046(14) Uiso 1 d . . .
H16 H 0.951(6) 0.342(5) 0.523(6) 0.09(2) Uiso 1 d . . .
H17 H 0.994(4) 0.228(3) 0.390(4) 0.039(12) Uiso 1 d . . .
H18 H 0.855(4) 0.188(4) 0.249(4) 0.057(15) Uiso 1 d . . .
H19 H 0.686(4) 0.264(4) 0.247(4) 0.039(13) Uiso 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -5.2083 5.8923 '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
C20 Re C30 87.37(18) . . ?
C20 Re C10 88.04(18) . . ?
C30 Re C10 90.14(19) . . ?
C20 Re N9 167.42(16) . . ?
C30 Re N9 99.59(15) . . ?
C10 Re N9 102.32(15) . . ?
C20 Re N1 97.89(16) . . ?
C30 Re N1 86.54(17) . . ?
C10 Re N1 173.06(16) . . ?
N9 Re N1 72.29(13) . . ?
C20 Re S13 104.18(13) . . ?
C30 Re S13 164.87(14) . . ?
C10 Re S13 80.68(13) . . ?
N9 Re S13 71.00(9) . . ?
N1 Re S13 101.23(9) . . ?
O10 C10 Re 177.8(4) . . ?
O20 C20 Re 177.3(4) . . ?
O30 C30 Re 176.3(4) . . ?
C2 N1 C6 118.1(4) . . ?
C2 N1 Re 125.4(3) . . ?
C6 N1 Re 115.0(3) . . ?
N1 C2 C3 122.5(5) . . ?
C4 C3 C2 119.4(5) . . ?
C3 C4 C5 119.1(5) . . ?
C4 C5 C6 119.3(5) . . ?
N1 C6 C5 121.4(4) . . ?
N1 C6 C7 114.2(3) . . ?
C5 C6 C7 124.3(4) . . ?
N9 C7 C6 113.1(4) . . ?
N9 C7 C8 124.3(4) . . ?
C6 C7 C8 122.1(4) . . ?
C7 N9 N10 117.3(3) . . ?
C7 N9 Re 121.5(3) . . ?
N10 N9 Re 120.4(2) . . ?
C11 N10 N9 108.1(3) . . ?
N10 C11 N12 120.5(4) . . ?
N10 C11 S13 123.8(3) . . ?
N12 C11 S13 115.7(3) . . ?
C11 N12 C14 129.1(3) . . ?
C11 S13 Re 92.14(13) . . ?
C19 C14 C15 117.9(4) . . ?
C19 C14 N12 125.3(4) . . ?
C15 C14 N12 116.7(4) . . ?
C16 C15 C14 121.6(5) . . ?
C15 C16 C17 119.9(5) . . ?
C18 C17 C16 118.8(4) . . ?
C17 C18 C19 121.8(5) . . ?
C18 C19 C14 120.0(4) . . ?
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
Re C20 1.908(4) . ?
Re C30 1.910(5) . ?
Re C10 1.911(5) . ?
Re N9 2.131(3) . ?
Re N1 2.192(3) . ?
Re S13 2.5389(10) . ?
C10 O10 1.156(5) . ?
C20 O20 1.162(5) . ?
C30 O30 1.150(5) . ?
N1 C2 1.351(6) . ?
N1 C6 1.368(6) . ?
C2 C3 1.379(7) . ?
C3 C4 1.378(8) . ?
C4 C5 1.386(8) . ?
C5 C6 1.390(6) . ?
C6 C7 1.466(6) . ?
C7 N9 1.303(5) . ?
C7 C8 1.478(6) . ?
N9 N10 1.403(5) . ?
N10 C11 1.305(5) . ?
C11 N12 1.369(5) . ?
C11 S13 1.776(4) . ?
N12 C14 1.404(5) . ?
C14 C19 1.381(6) . ?
C14 C15 1.393(6) . ?
C15 C16 1.373(7) . ?
C16 C17 1.380(7) . ?
C17 C18 1.370(7) . ?
C18 C19 1.379(6) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N12 H12 S13 0.88(4) 2.75(4) 3.555(4) 153(4) 3_666
