#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:53:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179710 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/13/7001391.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_7001391
loop_
_publ_author_name
'Kabir, S. E.'
'Alam, J.'
'Ghosh, S.'
'Kundu, K.'
'Hogarth, G.'
'Tocher, D. A.'
'Hossain, G. M. G.'
'Roesky, H. W.'
_publ_section_title
;
 Synthesis, structure and reactivity of tetranuclear square-type
 complexes of rhenium and manganese bearing pyrimidine-2-thiolate
 (pymS) ligands: versatile and efficient precursors for mono- and
 polynuclear compounds containing M(CO)3 (M = Re, Mn) fragments
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              4458
_journal_page_last               4467
_journal_paper_doi               10.1039/b815337j
_journal_year                    2009
_chemical_formula_moiety         'C19 H11 Mn N4 O3 S'
_chemical_formula_sum            'C19 H11 Mn N4 O3 S'
_chemical_formula_weight         430.32
_chemical_name_systematic
;
?
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.237(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0795(3)
_cell_length_b                   10.4855(3)
_cell_length_c                   12.2960(2)
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1814.84(7)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'ORTEP3 for windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'ω scans'
_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  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13680
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.871
_exptl_absorpt_correction_T_max  0.8450
_exptl_absorpt_correction_T_min  0.8116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[Blessing, Acta Cryst. (1995)]
;
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.271
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4147
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0507P)²+0.1070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                2947
_reflns_number_total             4147
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b815337j.txt
_cod_data_source_block           comp6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7001391
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.69636(2) 0.07693(3) 0.16488(2) 0.03887(13) Uani 1 1 d . . .
S1 S 0.78432(4) 0.25603(5) 0.10414(5) 0.04638(17) Uani 1 1 d . . .
O1 O 0.60514(15) -0.15361(19) 0.25158(18) 0.0861(6) Uani 1 1 d . . .
O2 O 0.63637(15) 0.22226(19) 0.35669(14) 0.0799(6) Uani 1 1 d . . .
O3 O 0.51343(12) 0.14565(17) 0.05898(17) 0.0743(6) Uani 1 1 d . . .
N1 N 0.62803(13) 0.39627(18) 0.12765(16) 0.0509(5) Uani 1 1 d . . .
N2 N 0.76337(15) 0.4953(2) 0.05236(17) 0.0594(5) Uani 1 1 d . . .
N3 N 0.82775(13) 0.02075(17) 0.22254(14) 0.0434(4) Uani 1 1 d . . .
N4 N 0.74724(11) -0.01646(16) 0.03118(13) 0.0376(4) Uani 1 1 d . . .
C1 C 0.64125(18) -0.0650(2) 0.2164(2) 0.0520(6) Uani 1 1 d . . .
C2 C 0.66155(17) 0.1662(2) 0.2831(2) 0.0528(6) Uani 1 1 d . . .
C3 C 0.58608(16) 0.1234(2) 0.0994(2) 0.0501(6) Uani 1 1 d . . .
C4 C 0.71774(15) 0.3953(2) 0.09467(15) 0.0387(5) Uani 1 1 d . . .
C5 C 0.58047(19) 0.5046(2) 0.1110(2) 0.0628(7) Uani 1 1 d . . .
H5 H 0.5161 0.5080 0.1326 0.075 Uiso 1 1 calc R . .
C6 C 0.6180(2) 0.6098(3) 0.0654(2) 0.0668(7) Uani 1 1 d . . .
H6 H 0.5821 0.6853 0.0531 0.080 Uiso 1 1 calc R . .
C7 C 0.7110(2) 0.5998(3) 0.0382(2) 0.0731(8) Uani 1 1 d . . .
H7 H 0.7404 0.6723 0.0071 0.088 Uiso 1 1 calc R . .
C8 C 0.86954(19) 0.0465(2) 0.31844(19) 0.0570(6) Uani 1 1 d . . .
H8 H 0.8349 0.0919 0.3714 0.068 Uiso 1 1 calc R . .
C9 C 0.9626(2) 0.0088(3) 0.3436(2) 0.0713(8) Uani 1 1 d . . .
H9 H 0.9904 0.0306 0.4122 0.086 Uiso 1 1 calc R . .
C10 C 1.01356(19) -0.0584(3) 0.2712(3) 0.0672(8) Uani 1 1 d . . .
H10 H 1.0764 -0.0851 0.2892 0.081 Uiso 1 1 calc R . .
C11 C 0.97267(17) -0.0881(2) 0.1697(2) 0.0528(6) Uani 1 1 d . . .
C12 C 1.01988(18) -0.1545(2) 0.0853(3) 0.0649(7) Uani 1 1 d . . .
H12 H 1.0830 -0.1839 0.0982 0.078 Uiso 1 1 calc R . .
C13 C 0.97796(18) -0.1766(2) -0.0112(3) 0.0653(7) Uani 1 1 d . . .
H13 H 1.0114 -0.2225 -0.0649 0.078 Uiso 1 1 calc R . .
C14 C 0.88400(16) -0.1328(2) -0.03558(19) 0.0487(6) Uani 1 1 d . . .
C15 C 0.8368(2) -0.1469(2) -0.1362(2) 0.0603(7) Uani 1 1 d . . .
H15 H 0.8661 -0.1917 -0.1937 0.072 Uiso 1 1 calc R . .
C16 C 0.7493(2) -0.0961(3) -0.1508(2) 0.0625(7) Uani 1 1 d . . .
H16 H 0.7169 -0.1051 -0.2190 0.075 Uiso 1 1 calc R . .
C17 C 0.70650(17) -0.0310(2) -0.06688(18) 0.0499(6) Uani 1 1 d . . .
H17 H 0.6453 0.0048 -0.0798 0.060 Uiso 1 1 calc R . .
C18 C 0.83582(14) -0.06669(18) 0.04552(17) 0.0377(5) Uani 1 1 d . . .
C19 C 0.87985(15) -0.0460(2) 0.14942(18) 0.0400(5) 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 0.0000 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'
S S 0.1246 0.1234 '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'
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
C1 Mn1 C3 90.39(11) . . ?
C1 Mn1 C2 91.07(11) . . ?
C3 Mn1 C2 88.47(11) . . ?
C1 Mn1 N3 91.91(9) . . ?
C3 Mn1 N3 173.64(9) . . ?
C2 Mn1 N3 97.41(9) . . ?
C1 Mn1 N4 92.76(8) . . ?
C3 Mn1 N4 94.77(9) . . ?
C2 Mn1 N4 174.96(9) . . ?
N3 Mn1 N4 79.19(7) . . ?
C1 Mn1 S1 174.07(8) . . ?
C3 Mn1 S1 95.51(7) . . ?
C2 Mn1 S1 89.74(8) . . ?
N3 Mn1 S1 82.16(5) . . ?
N4 Mn1 S1 86.11(5) . . ?
C4 S1 Mn1 113.61(7) . . ?
C5 N1 C4 115.8(2) . . ?
C7 N2 C4 115.3(2) . . ?
C8 N3 C19 116.9(2) . . ?
C8 N3 Mn1 128.62(17) . . ?
C19 N3 Mn1 114.36(13) . . ?
C17 N4 C18 116.60(19) . . ?
C17 N4 Mn1 128.87(15) . . ?
C18 N4 Mn1 114.50(13) . . ?
O1 C1 Mn1 178.2(2) . . ?
O2 C2 Mn1 177.7(2) . . ?
O3 C3 Mn1 175.8(2) . . ?
N1 C4 N2 125.2(2) . . ?
N1 C4 S1 119.93(16) . . ?
N2 C4 S1 114.90(17) . . ?
N1 C5 C6 124.1(3) . . ?
N1 C5 H5 118.0 . . ?
C6 C5 H5 118.0 . . ?
C5 C6 C7 115.2(3) . . ?
C5 C6 H6 122.4 . . ?
C7 C6 H6 122.4 . . ?
N2 C7 C6 124.3(3) . . ?
N2 C7 H7 117.8 . . ?
C6 C7 H7 117.8 . . ?
N3 C8 C9 122.1(3) . . ?
N3 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C10 C9 C8 120.6(2) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 119.3(2) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C19 C11 C10 117.0(3) . . ?
C19 C11 C12 118.3(2) . . ?
C10 C11 C12 124.7(2) . . ?
C13 C12 C11 121.8(2) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 121.5(2) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C15 C14 C18 117.0(2) . . ?
C15 C14 C13 124.9(2) . . ?
C18 C14 C13 118.1(2) . . ?
C16 C15 C14 119.3(2) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 120.3(2) . . ?
C15 C16 H16 119.8 . . ?
C17 C16 H16 119.8 . . ?
N4 C17 C16 123.0(2) . . ?
N4 C17 H17 118.5 . . ?
C16 C17 H17 118.5 . . ?
N4 C18 C14 123.7(2) . . ?
N4 C18 C19 115.90(18) . . ?
C14 C18 C19 120.4(2) . . ?
N3 C19 C11 124.0(2) . . ?
N3 C19 C18 116.04(18) . . ?
C11 C19 C18 119.9(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 C1 1.800(3) . ?
Mn1 C3 1.801(2) . ?
Mn1 C2 1.806(3) . ?
Mn1 N3 2.0531(18) . ?
Mn1 N4 2.0556(17) . ?
Mn1 S1 2.3788(6) . ?
S1 C4 1.738(2) . ?
O1 C1 1.148(3) . ?
O2 C2 1.142(3) . ?
O3 C3 1.152(3) . ?
N1 C5 1.332(3) . ?
N1 C4 1.335(3) . ?
N2 C7 1.330(3) . ?
N2 C4 1.341(3) . ?
N3 C8 1.334(3) . ?
N3 C19 1.365(3) . ?
N4 C17 1.333(3) . ?
N4 C18 1.362(3) . ?
C5 C6 1.350(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.363(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.397(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.352(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.399(4) . ?
C10 H10 0.9500 . ?
C11 C19 1.397(3) . ?
C11 C12 1.426(4) . ?
C12 C13 1.334(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.426(3) . ?
C13 H13 0.9500 . ?
C14 C15 1.399(3) . ?
C14 C18 1.402(3) . ?
C15 C16 1.351(4) . ?
C15 H15 0.9500 . ?
C16 C17 1.386(4) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
C18 C19 1.425(3) . ?
