#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:42:11 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179985 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/79/7027919.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027919
loop_
_publ_author_name
'Lü, Jian'
'Gao, Shui-Ying'
'Lin, Jing-Xiang'
'Shi, Lin-Xi'
'Cao, Rong'
'Batten, Stuart R.'
_publ_section_title
;
 Systematic investigation on the coordination chemistry of a sulfonated
 monoazo dye: Ligand-dominated d- and f-block derivatives
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              1944
_journal_page_last               1953
_journal_paper_doi               10.1039/b814774d
_journal_year                    2009
_chemical_formula_sum            'C24 H24 Mn N6 O8 S2'
_chemical_formula_weight         643.55
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_method           SHELXL-97
_cell_angle_alpha                100.329(9)
_cell_angle_beta                 100.032(15)
_cell_angle_gamma                96.299(12)
_cell_formula_units_Z            1
_cell_length_a                   6.0026(18)
_cell_length_b                   7.049(2)
_cell_length_c                   15.438(5)
_cell_measurement_reflns_used    2782
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.97
_cell_volume                     626.1(3)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type
;
Mercury70 (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0279
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4849
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_correction_T_min  0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.707
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       trunk
_exptl_crystal_F_000             331
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.976
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2782
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0800P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.0991
_reflns_number_gt                2401
_reflns_number_total             2782
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7000729
_cod_data_source_file            B814774dsup1.cif
_cod_data_source_block           Compd3a
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7027919
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
Mn1 Mn 1.0000 0.0000 1.0000 0.01908(13) Uani 1 2 d S
S1 S 1.18170(7) 0.28137(5) 0.86087(2) 0.02008(13) Uani 1 1 d .
O1W O 0.7286(2) 0.18764(19) 1.00006(9) 0.0274(3) Uani 1 1 d .
O1 O 1.0941(2) 0.09866(17) 0.88415(8) 0.0271(3) Uani 1 1 d .
O3 O 1.4289(2) 0.3142(2) 0.87479(9) 0.0355(3) Uani 1 1 d .
O2 O 1.0878(3) 0.44456(19) 0.90610(9) 0.0366(3) Uani 1 1 d .
N1 N 0.7455(3) -0.2591(2) 0.90817(10) 0.0247(3) Uani 1 1 d .
C2 C 1.2205(3) 0.3040(3) 0.68892(12) 0.0249(4) Uani 1 1 d .
C1 C 1.0752(3) 0.2556(2) 0.74496(10) 0.0188(3) Uani 1 1 d .
C6 C 0.8425(3) 0.1939(3) 0.71170(12) 0.0255(4) Uani 1 1 d .
C4 C 0.8988(3) 0.2369(2) 0.56569(11) 0.0233(3) Uani 1 1 d .
C5 C 0.7544(3) 0.1853(3) 0.62180(12) 0.0262(4) Uani 1 1 d .
C3 C 1.1328(3) 0.2902(3) 0.59871(12) 0.0287(4) Uani 1 1 d .
H2A H 1.365(4) 0.343(3) 0.7143(15) 0.031(5) Uiso 1 1 d .
H5A H 0.605(5) 0.134(4) 0.6005(18) 0.049(7) Uiso 1 1 d .
H1D H 0.644(4) -0.267(3) 0.9346(17) 0.039(7) Uiso 1 1 d .
H6A H 0.743(4) 0.154(3) 0.7474(16) 0.035(6) Uiso 1 1 d .
H1C H 0.826(4) -0.361(4) 0.9060(17) 0.045(7) Uiso 1 1 d .
H3A H 1.231(4) 0.309(4) 0.5540(17) 0.051(7) Uiso 1 1 d .
H1B H 0.768(4) 0.310(4) 1.0276(18) 0.040(6) Uiso 1 1 d .
H1A H 0.636(5) 0.186(4) 0.9499(19) 0.046(7) Uiso 1 1 d .
C10 C 0.3469(3) 0.2549(2) 0.18329(11) 0.0207(3) Uani 1 1 d .
N3 N 0.6130(3) 0.2533(2) 0.45342(10) 0.0264(3) Uani 1 1 d .
N2 N 0.8214(3) 0.2365(2) 0.47264(10) 0.0280(3) Uani 1 1 d .
C11 C 0.2275(3) 0.3119(2) 0.25067(12) 0.0248(3) Uani 1 1 d .
C8 C 0.6488(3) 0.1861(2) 0.29297(11) 0.0242(3) Uani 1 1 d .
C7 C 0.5315(3) 0.2487(2) 0.36062(11) 0.0230(3) Uani 1 1 d .
C9 C 0.5561(3) 0.1886(2) 0.20469(11) 0.0238(3) Uani 1 1 d .
C12 C 0.3186(3) 0.3082(3) 0.33884(12) 0.0266(4) Uani 1 1 d .
H11A H 0.079(4) 0.365(3) 0.2412(16) 0.038(6) Uiso 1 1 d .
H12A H 0.246(4) 0.353(3) 0.3850(15) 0.030(5) Uiso 1 1 d .
H8A H 0.807(4) 0.141(3) 0.3088(16) 0.035(6) Uiso 1 1 d .
H9A H 0.631(4) 0.151(3) 0.1613(15) 0.026(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'
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
O1 Mn1 O1 180.000(1) 2_757 .
O1 Mn1 O1W 90.52(5) 2_757 2_757
O1 Mn1 O1W 89.48(5) . 2_757
O1 Mn1 O1W 89.48(5) 2_757 .
O1 Mn1 O1W 90.52(5) . .
O1W Mn1 O1W 180.000(1) 2_757 .
O1 Mn1 N1 88.71(5) 2_757 .
O1 Mn1 N1 91.29(5) . .
O1W Mn1 N1 88.89(6) 2_757 .
O1W Mn1 N1 91.11(6) . .
O1 Mn1 N1 91.29(5) 2_757 2_757
O1 Mn1 N1 88.71(5) . 2_757
O1W Mn1 N1 91.11(6) 2_757 2_757
O1W Mn1 N1 88.89(6) . 2_757
N1 Mn1 N1 180.0 . 2_757
O3 S1 O2 113.05(9) . .
O3 S1 O1 112.63(8) . .
O2 S1 O1 110.90(8) . .
O3 S1 C1 107.36(8) . .
O2 S1 C1 106.65(8) . .
O1 S1 C1 105.72(7) . .
S1 O1 Mn1 138.22(8) . .
C10 N1 Mn1 121.22(10) 2_656 .
C3 C2 C1 119.43(16) . .
C2 C1 C6 121.03(15) . .
C2 C1 S1 120.10(13) . .
C6 C1 S1 118.82(12) . .
C5 C6 C1 119.30(15) . .
C5 C4 C3 120.38(16) . .
C5 C4 N2 123.50(16) . .
C3 C4 N2 116.11(15) . .
C6 C5 C4 119.85(17) . .
C2 C3 C4 119.89(15) . .
C11 C10 C9 119.68(15) . .
C11 C10 N1 120.58(16) . 2_656
C9 C10 N1 119.72(15) . 2_656
N2 N3 C7 113.91(14) . .
N3 N2 C4 113.10(14) . .
C12 C11 C10 120.16(16) . .
C9 C8 C7 119.77(16) . .
C12 C7 C8 119.90(15) . .
C12 C7 N3 115.99(14) . .
C8 C7 N3 124.10(15) . .
C8 C9 C10 120.32(15) . .
C11 C12 C7 120.11(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.1710(12) 2_757
Mn1 O1 2.1710(12) .
Mn1 O1W 2.2083(14) 2_757
Mn1 O1W 2.2083(14) .
Mn1 N1 2.3204(16) .
Mn1 N1 2.3204(16) 2_757
S1 O3 1.4482(14) .
S1 O2 1.4561(13) .
S1 O1 1.4655(12) .
S1 C1 1.7615(17) .
N1 C10 1.431(2) 2_656
C2 C3 1.382(2) .
C2 C1 1.389(2) .
C1 C6 1.393(2) .
C6 C5 1.384(2) .
C4 C5 1.393(2) .
C4 C3 1.393(3) .
C4 N2 1.430(2) .
C10 C11 1.390(2) .
C10 C9 1.394(2) .
C10 N1 1.431(2) 2_656
N3 N2 1.258(2) .
N3 C7 1.424(2) .
C11 C12 1.382(2) .
C8 C9 1.383(2) .
C8 C7 1.393(2) .
C7 C12 1.393(2) .
