#------------------------------------------------------------------------------
#$Date: 2018-09-04 16:16:39 +0300 (Tue, 04 Sep 2018) $
#$Revision: 210409 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/11/35/7113542.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_7113542
loop_
_publ_author_name
'Grirrane, Abdessamad'
'Pastor, Antonio'
'Galindo, Agustín'
'Ienco, Andrea'
'Mealli, Carlo'
'Rosa, Patrick'
_publ_section_title
;
 First example of a tetra-carboxylate bridged dimanganese species
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   4
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              512
_journal_page_last               513
_journal_paper_doi               10.1039/b211886f
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C14 H12 Mn1 N2 O4 S1'
_chemical_formula_sum            'C14 H12 Mn N2 O4 S'
_chemical_formula_weight         359.26
_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_creation_date             2002-10-31T16:09:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                73.86(2)
_cell_angle_beta                 72.86(3)
_cell_angle_gamma                80.71(3)
_cell_formula_units_Z            2
_cell_length_a                   8.018(3)
_cell_length_b                   9.104(3)
_cell_length_c                   10.484(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      9
_cell_measurement_wavelength     0.71073
_cell_volume                     699.8(5)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      -0.078018
_diffrn_orient_matrix_UB_12      0.095035
_diffrn_orient_matrix_UB_13      0.013436
_diffrn_orient_matrix_UB_21      0.047449
_diffrn_orient_matrix_UB_22      0.051222
_diffrn_orient_matrix_UB_23      -0.09933
_diffrn_orient_matrix_UB_31      -0.093839
_diffrn_orient_matrix_UB_32      -0.038928
_diffrn_orient_matrix_UB_33      -0.023565
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2612
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.1
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.4571
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was   2
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0451
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0836P)²+0.4370P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1186
_refine_ls_wR_factor_ref         0.1221
_reflns_number_gt                2294
_reflns_number_total             2463
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103974
_cod_data_source_file            198988.txt
_cod_data_source_block           79b
_cod_original_formula_sum        'C14 H12 Mn1 N2 O4 S1'
_cod_database_code               7113542
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_factor_mur        0.275
_exptl_absorpt_correction_t_ave  0.5786
_diffrn_standards_decay_corr_max 1.041
_diffrn_standards_decay_corr_min 0.97
#END Tags that were not found in dictionaries
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
Mn Mn 0.40707(5) 0.49142(4) 0.17518(3) 0.02049(18) Uani 1 1 d .
S S -0.01850(9) 0.16652(9) 0.15798(7) 0.0318(2) Uani 1 1 d .
O1 O 0.2228(3) 0.3859(3) 0.1229(2) 0.0410(6) Uani 1 1 d .
O2 O 0.3369(3) 0.4230(3) -0.1031(2) 0.0383(5) Uani 1 1 d .
O3 O -0.3126(3) 0.3040(2) -0.0434(2) 0.0366(5) Uani 1 1 d .
O4 O -0.4385(3) 0.2716(2) 0.1812(2) 0.0379(5) Uani 1 1 d .
N1 N 0.2583(3) 0.3771(3) 0.3963(2) 0.0257(5) Uani 1 1 d .
N2 N 0.3691(3) 0.6532(3) 0.3195(2) 0.0289(5) Uani 1 1 d .
C1 C 0.2285(3) 0.3713(3) 0.0070(3) 0.0257(6) Uani 1 1 d .
C2 C 0.0868(4) 0.2875(3) -0.0048(3) 0.0262(6) Uani 1 1 d .
H2A H 0.1383 0.2252 -0.0705 0.031 Uiso 1 1 calc R
H2B H -0.0003 0.3621 -0.0395 0.031 Uiso 1 1 calc R
C3 C -0.1896(3) 0.1059(3) 0.1087(3) 0.0261(6) Uani 1 1 d .
H3A H -0.1385 0.067 0.0271 0.031 Uiso 1 1 calc R
H3B H -0.2453 0.0233 0.1821 0.031 Uiso 1 1 calc R
C4 C -0.3265(3) 0.2379(3) 0.0797(3) 0.0243(6) Uani 1 1 d .
C5 C 0.1874(4) 0.2449(3) 0.4265(3) 0.0320(6) Uani 1 1 d .
H5 H 0.2061 0.1944 0.3569 0.038 Uiso 1 1 calc R
C6 C 0.0871(4) 0.1787(4) 0.5567(3) 0.0355(7) Uani 1 1 d .
H6 H 0.0393 0.0863 0.5744 0.043 Uiso 1 1 calc R
C7 C 0.0603(4) 0.2544(4) 0.6590(3) 0.0376(7) Uani 1 1 d .
H7 H -0.0076 0.214 0.7472 0.045 Uiso 1 1 calc R
C8 C 0.1342(4) 0.3895(4) 0.6302(3) 0.0344(7) Uani 1 1 d .
H8 H 0.1182 0.441 0.6987 0.041 Uiso 1 1 calc R
C9 C 0.2333(3) 0.4487(3) 0.4972(3) 0.0242(6) Uani 1 1 d .
C10 C 0.3087(3) 0.5976(3) 0.4558(3) 0.0249(6) Uani 1 1 d .
C11 C 0.3122(4) 0.6784(4) 0.5491(3) 0.0348(7) Uani 1 1 d .
H11 H 0.2745 0.6362 0.6433 0.042 Uiso 1 1 calc R
C12 C 0.3724(4) 0.8218(4) 0.4997(4) 0.0399(7) Uani 1 1 d .
H12 H 0.3767 0.8776 0.5606 0.048 Uiso 1 1 calc R
C13 C 0.4264(4) 0.8830(4) 0.3599(4) 0.0395(7) Uani 1 1 d .
H13 H 0.4623 0.9818 0.3246 0.047 Uiso 1 1 calc R
C14 C 0.4254(4) 0.7933(4) 0.2741(3) 0.0366(7) Uani 1 1 d .
H14 H 0.4661 0.8323 0.1796 0.044 Uiso 1 1 calc R
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'
O O 0.0106 0.006 '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_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
-2 2 -4
-1 4 0
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
O1 Mn O2 144.61(9) . 2_665
O1 Mn O3 82.98(9) . 2_565
O2 Mn O3 88.71(10) 2_665 2_565
O1 Mn O4 85.04(10) . 1_655
O2 Mn O4 82.36(9) 2_665 1_655
O3 Mn O4 145.04(8) 2_565 1_655
O1 Mn N1 82.50(9) . .
O2 Mn N1 128.78(9) 2_665 .
O3 Mn N1 125.57(9) 2_565 .
O4 Mn N1 84.91(8) 1_655 .
O1 Mn N2 131.94(9) . .
O2 Mn N2 80.46(9) 2_665 .
O3 Mn N2 82.95(9) 2_565 .
O4 Mn N2 128.09(9) 1_655 .
N1 Mn N2 69.41(8) . .
C2 S C3 99.51(13) . .
C1 O1 Mn 127.1(2) . .
C1 O2 Mn 139.6(2) . 2_665
C4 O3 Mn 142.09(19) . 2_565
C4 O4 Mn 124.10(19) . 1_455
C5 N1 C9 118.4(2) . .
C5 N1 Mn 121.95(18) . .
C9 N1 Mn 119.60(19) . .
C14 N2 C10 118.3(2) . .
C14 N2 Mn 122.28(19) . .
C10 N2 Mn 118.85(18) . .
O1 C1 O2 126.5(3) . .
O1 C1 C2 118.0(2) . .
O2 C1 C2 115.5(2) . .
C1 C2 S 112.11(19) . .
C1 C2 H2A 109.2 . .
S C2 H2A 109.2 . .
C1 C2 H2B 109.2 . .
S C2 H2B 109.2 . .
H2A C2 H2B 107.9 . .
C4 C3 S 111.23(18) . .
C4 C3 H3A 109.4 . .
S C3 H3A 109.4 . .
C4 C3 H3B 109.4 . .
S C3 H3B 109.4 . .
H3A C3 H3B 108 . .
O3 C4 O4 126.6(3) . .
O3 C4 C3 116.2(2) . .
O4 C4 C3 117.2(2) . .
N1 C5 C6 123.2(3) . .
N1 C5 H5 118.4 . .
C6 C5 H5 118.4 . .
C7 C6 C5 117.9(3) . .
C7 C6 H6 121.1 . .
C5 C6 H6 121.1 . .
C8 C7 C6 119.7(3) . .
C8 C7 H7 120.2 . .
C6 C7 H7 120.2 . .
C7 C8 C9 119.1(3) . .
C7 C8 H8 120.4 . .
C9 C8 H8 120.4 . .
N1 C9 C8 121.7(3) . .
N1 C9 C10 115.7(2) . .
C8 C9 C10 122.5(2) . .
N2 C10 C11 121.7(3) . .
N2 C10 C9 115.1(2) . .
C11 C10 C9 123.1(3) . .
C12 C11 C10 118.7(3) . .
C12 C11 H11 120.6 . .
C10 C11 H11 120.6 . .
C11 C12 C13 119.9(3) . .
C11 C12 H12 120.1 . .
C13 C12 H12 120.1 . .
C12 C13 C14 117.9(3) . .
C12 C13 H13 121.1 . .
C14 C13 H13 121.1 . .
N2 C14 C13 123.3(3) . .
N2 C14 H14 118.3 . .
C13 C14 H14 118.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn O1 2.153(2) .
Mn O2 2.160(2) 2_665
Mn O3 2.164(2) 2_565
Mn O4 2.172(2) 1_655
Mn N1 2.304(2) .
Mn N2 2.318(2) .
S C2 1.802(3) .
S C3 1.809(3) .
O1 C1 1.246(4) .
O2 C1 1.244(4) .
O2 Mn 2.160(2) 2_665
O3 C4 1.243(3) .
O3 Mn 2.164(2) 2_565
O4 C4 1.250(3) .
O4 Mn 2.172(2) 1_455
N1 C5 1.333(4) .
N1 C9 1.341(3) .
N2 C14 1.334(4) .
N2 C10 1.342(4) .
C1 C2 1.517(4) .
C2 H2A 0.97 .
C2 H2B 0.97 .
C3 C4 1.520(4) .
C3 H3A 0.97 .
C3 H3B 0.97 .
C5 C6 1.387(4) .
C5 H5 0.93 .
C6 C7 1.378(5) .
C6 H6 0.93 .
C7 C8 1.370(5) .
C7 H7 0.93 .
C8 C9 1.391(4) .
C8 H8 0.93 .
C9 C10 1.474(4) .
C10 C11 1.386(4) .
C11 C12 1.374(5) .
C11 H11 0.93 .
C12 C13 1.376(5) .
C12 H12 0.93 .
C13 C14 1.375(4) .
C13 H13 0.93 .
C14 H14 0.93 .
