Supplementary Material (ESI) for Dalton Transactions
This journal is (C) The Royal Society of Chemistry 2007

data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_Cambridge         0222

_publ_contact_author_name        'Prof Jie Zhang'
_publ_contact_author_address     
;
The State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
the Chinese Academy of Sciences,
Fuzhou, Fujian 350002,
P. R. China
;
_publ_contact_author_email       zhangjie@fjirsm.ac.cn
_publ_contact_author_phone       86-591-83792871
_publ_contact_author_fax         86-591-83710051
_publ_requested_category         ?
_publ_requested_coeditor_name    ?

_publ_contact_letter             
;
This CIF will submit for publication as a full paper
in 'Dalton Trans.'
;

# 2.AUTHOR LIST

loop_
_publ_author_name
_publ_author_address

'Zhan-Feng Ju'
;
The State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
the Chinese Academy of Sciences,
Fuzhou, Fujian 350002,
P. R. China
;
'Qing-Xia Yao'
;
The State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
the Chinese Academy of Sciences,
Fuzhou, Fujian 350002,
P. R. China
;
'Wei Wu'
;
The State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
the Chinese Academy of Sciences,
Fuzhou, Fujian 350002,
P. R. China
;
'Jie Zhang'
;
The State Key Laboratory of Structural Chemistry,
Fujian Institute of Research on the Structure of Matter,
the Chinese Academy of Sciences,
Fuzhou, Fujian 350002,
P. R. China
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 653490'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H32 Cl N9 Ni O2 S5'
_chemical_formula_weight         793.10

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   6.4118(2)
_cell_length_b                   23.7160(6)
_cell_length_c                   12.1682(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.5790(10)
_cell_angle_gamma                90.00
_cell_volume                     1838.14(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             820
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7085
_exptl_absorpt_correction_T_max  0.8737
_exptl_absorpt_process_details   'Siemens SMART'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            10093
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.73
_reflns_number_total             3573
_reflns_number_gt                3206
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Siemens SMART'
_computing_cell_refinement       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+3.5000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3573
_refine_ls_number_parameters     240
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1566
_refine_ls_wR_factor_gt          0.1419
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
Ni1 Ni 0.23627(10) 0.2500 0.95551(5) 0.0387(2) Uani 1 2 d S . .
Cl1 Cl 0.0000 0.0000 0.5000 0.1320(12) Uani 1 2 d S . .
S1 S 0.2627(3) 0.04740(6) 0.94924(13) 0.0948(5) Uani 1 1 d . . .
S2 S -0.1784(2) 0.2500 0.59771(11) 0.0512(4) Uani 1 2 d S . .
S3 S -0.0905(2) 0.2500 1.04969(12) 0.0568(4) Uani 1 2 d S . .
S4 S 0.4852(3) 0.2500 1.34650(12) 0.0620(4) Uani 1 2 d S . .
O1W O -0.2008(7) -0.00916(16) 0.3318(4) 0.0297(9) Uani 0.50 1 d P . .
O1W' O -0.3537(14) 0.0028(3) 0.2964(6) 0.076(2) Uani 0.50 1 d P . .
N1 N -0.0826(7) 0.11456(16) 0.2013(3) 0.0608(9) Uani 1 1 d . . .
N2 N 0.6041(5) 0.12229(15) 0.6894(3) 0.0523(8) Uani 1 1 d . . .
N3 N 0.0856(7) 0.2500 0.7968(4) 0.0475(10) Uani 1 2 d S . .
N4 N -0.4558(8) 0.2500 0.9009(4) 0.0604(13) Uani 1 2 d S . .
N5 N 0.3646(7) 0.2500 1.1194(4) 0.0551(12) Uani 1 2 d S . .
N6 N 0.2407(6) 0.16379(16) 0.9519(3) 0.0558(9) Uani 1 1 d . . .
C1 C 0.7383(8) 0.1191(2) 0.7961(4) 0.0745(14) Uani 1 1 d . . .
H1A H 0.6722 0.0944 0.8467 0.112 Uiso 1 1 calc R . .
H1B H 0.7558 0.1569 0.8283 0.112 Uiso 1 1 calc R . .
H1C H 0.8759 0.1038 0.7843 0.112 Uiso 1 1 calc R . .
C2 C 0.4303(7) 0.1531(2) 0.6800(4) 0.0598(11) Uani 1 1 d . . .
H2 H 0.3961 0.1743 0.7417 0.072 Uiso 1 1 calc R . .
C3 C 0.2996(7) 0.1551(2) 0.5833(4) 0.0583(11) Uani 1 1 d . . .
H3 H 0.1759 0.1774 0.5785 0.070 Uiso 1 1 calc R . .
C4 C 0.3462(6) 0.12476(17) 0.4923(3) 0.0475(9) Uani 1 1 d . . .
C5 C 0.2001(6) 0.12319(17) 0.3887(3) 0.0490(9) Uani 1 1 d . . .
C6 C 0.0235(8) 0.1563(2) 0.3729(4) 0.0642(12) Uani 1 1 d . . .
H6 H -0.0030 0.1829 0.4281 0.077 Uiso 1 1 calc R . .
C7 C -0.1141(8) 0.1517(2) 0.2796(4) 0.0693(13) Uani 1 1 d . . .
H7 H -0.2345 0.1753 0.2703 0.083 Uiso 1 1 calc R . .
C8 C -0.2408(10) 0.1077(3) 0.1046(4) 0.0856(17) Uani 1 1 d . . .
H8A H -0.1782 0.0877 0.0460 0.128 Uiso 1 1 calc R . .
H8B H -0.2899 0.1448 0.0776 0.128 Uiso 1 1 calc R . .
H8C H -0.3597 0.0859 0.1259 0.128 Uiso 1 1 calc R . .
C9 C 0.0878(9) 0.0833(2) 0.2122(4) 0.0731(14) Uani 1 1 d . . .
H9 H 0.1110 0.0576 0.1548 0.088 Uiso 1 1 calc R . .
C10 C 0.2323(8) 0.0865(2) 0.3033(4) 0.0671(12) Uani 1 1 d . . .
H10 H 0.3547 0.0636 0.3085 0.081 Uiso 1 1 calc R . .
C11 C 0.5320(7) 0.0946(2) 0.5039(4) 0.0645(12) Uani 1 1 d . . .
H11 H 0.5731 0.0742 0.4427 0.077 Uiso 1 1 calc R . .
C12 C 0.6564(8) 0.0938(2) 0.6025(4) 0.0678(12) Uani 1 1 d . . .
H12 H 0.7826 0.0724 0.6093 0.081 Uiso 1 1 calc R . .
C13 C -0.0250(8) 0.2500 0.7149(4) 0.0401(11) Uani 1 2 d S . .
C14 C -0.3009(8) 0.2500 0.9602(5) 0.0456(12) Uani 1 2 d S . .
C15 C 0.4112(8) 0.2500 1.2141(4) 0.0430(11) Uani 1 2 d S . .
C16 C 0.2491(6) 0.11586(19) 0.9500(3) 0.0487(9) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0356(4) 0.0449(4) 0.0341(4) 0.000 -0.0026(2) 0.000
Cl1 0.132(2) 0.0822(15) 0.201(3) 0.0185(17) 0.101(2) 0.0148(15)
S1 0.1526(16) 0.0477(7) 0.0860(10) -0.0071(6) 0.0214(10) 0.0107(8)
S2 0.0457(7) 0.0659(9) 0.0390(7) 0.000 -0.0077(6) 0.000
S3 0.0396(7) 0.0822(11) 0.0483(8) 0.000 0.0032(6) 0.000
S4 0.0691(10) 0.0761(11) 0.0379(7) 0.000 -0.0065(7) 0.000
O1W 0.038(2) 0.0157(19) 0.038(2) 0.0027(17) 0.0147(19) -0.0033(17)
O1W' 0.107(6) 0.070(4) 0.059(4) -0.006(3) 0.039(4) 0.016(4)
N1 0.079(3) 0.053(2) 0.0470(19) 0.0051(16) -0.0073(17) -0.0085(19)
N2 0.0529(19) 0.055(2) 0.0477(18) 0.0010(15) -0.0007(15) -0.0043(16)
N3 0.046(2) 0.057(3) 0.039(2) 0.000 0.000(2) 0.000
N4 0.038(3) 0.081(4) 0.062(3) 0.000 0.001(2) 0.000
N5 0.040(2) 0.081(4) 0.042(3) 0.000 -0.002(2) 0.000
N6 0.060(2) 0.049(2) 0.057(2) 0.0006(16) 0.0006(16) 0.0070(16)
C1 0.072(3) 0.089(4) 0.057(3) 0.000(3) -0.017(2) -0.002(3)
C2 0.066(3) 0.069(3) 0.043(2) -0.011(2) 0.0044(19) 0.008(2)
C3 0.058(2) 0.067(3) 0.049(2) -0.010(2) 0.0025(19) 0.013(2)
C4 0.052(2) 0.048(2) 0.0428(19) -0.0011(16) 0.0097(16) -0.0009(17)
C5 0.056(2) 0.051(2) 0.041(2) -0.0029(17) 0.0105(17) -0.0016(18)
C6 0.075(3) 0.066(3) 0.049(2) -0.014(2) -0.005(2) 0.016(2)
C7 0.075(3) 0.066(3) 0.063(3) -0.006(2) -0.009(2) 0.013(2)
C8 0.107(4) 0.080(4) 0.061(3) 0.000(3) -0.028(3) -0.014(3)
C9 0.100(4) 0.071(3) 0.047(2) -0.013(2) 0.002(2) 0.004(3)
C10 0.073(3) 0.076(3) 0.052(2) -0.013(2) 0.005(2) 0.014(2)
C11 0.065(3) 0.079(3) 0.050(2) -0.013(2) 0.009(2) 0.017(2)
C12 0.061(3) 0.076(3) 0.065(3) -0.005(2) 0.002(2) 0.015(2)
C13 0.037(3) 0.047(3) 0.036(3) 0.000 0.003(2) 0.000
C14 0.043(3) 0.045(3) 0.050(3) 0.000 0.014(2) 0.000
C15 0.035(3) 0.049(3) 0.044(3) 0.000 0.002(2) 0.000
C16 0.048(2) 0.056(3) 0.041(2) -0.0017(17) 0.0002(16) 0.0043(17)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ni1 N6 2.045(4) 4_565 ?
Ni1 N6 2.045(4) . ?
Ni1 N3 2.058(4) . ?
Ni1 N5 2.069(5) . ?
Ni1 N4 2.154(5) 1_655 ?
Ni1 S3 2.5006(16) . ?
S1 C16 1.626(5) . ?
S2 C13 1.637(5) . ?
S3 C14 1.634(6) . ?
S4 C15 1.627(5) . ?
O1W O1W' 1.064(8) . ?
N1 C9 1.315(7) . ?
N1 C7 1.329(6) . ?
N1 C8 1.472(6) . ?
N2 C2 1.327(6) . ?
N2 C12 1.330(6) . ?
N2 C1 1.475(5) . ?
N3 C13 1.155(6) . ?
N4 C14 1.159(7) . ?
N4 Ni1 2.154(5) 1_455 ?
N5 C15 1.156(7) . ?
N6 C16 1.138(6) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.365(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.381(6) . ?
C3 H3 0.9500 . ?
C4 C11 1.383(6) . ?
C4 C5 1.482(6) . ?
C5 C6 1.374(6) . ?
C5 C10 1.388(6) . ?
C6 C7 1.360(6) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.363(7) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
C11 C12 1.363(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?

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
N6 Ni1 N6 176.9(2) 4_565 . ?
N6 Ni1 N3 89.20(10) 4_565 . ?
N6 Ni1 N3 89.20(10) . . ?
N6 Ni1 N5 90.90(10) 4_565 . ?
N6 Ni1 N5 90.90(10) . . ?
N3 Ni1 N5 175.48(18) . . ?
N6 Ni1 N4 88.74(10) 4_565 1_655 ?
N6 Ni1 N4 88.74(10) . 1_655 ?
N3 Ni1 N4 93.37(19) . 1_655 ?
N5 Ni1 N4 91.1(2) . 1_655 ?
N6 Ni1 S3 91.38(10) 4_565 . ?
N6 Ni1 S3 91.38(10) . . ?
N3 Ni1 S3 95.88(14) . . ?
N5 Ni1 S3 79.60(14) . . ?
N4 Ni1 S3 170.75(15) 1_655 . ?
C14 S3 Ni1 111.44(19) . . ?
C9 N1 C7 119.6(4) . . ?
C9 N1 C8 120.4(4) . . ?
C7 N1 C8 120.0(5) . . ?
C2 N2 C12 119.8(4) . . ?
C2 N2 C1 120.2(4) . . ?
C12 N2 C1 119.9(4) . . ?
C13 N3 Ni1 170.2(4) . . ?
C14 N4 Ni1 124.0(5) . 1_455 ?
C15 N5 Ni1 171.6(4) . . ?
C16 N6 Ni1 178.1(4) . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C2 C3 121.3(4) . . ?
N2 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C11 116.8(4) . . ?
C3 C4 C5 121.4(4) . . ?
C11 C4 C5 121.8(4) . . ?
C6 C5 C10 116.5(4) . . ?
C6 C5 C4 122.3(4) . . ?
C10 C5 C4 121.2(4) . . ?
C7 C6 C5 121.0(4) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N1 C7 C6 121.0(5) . . ?
N1 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
N1 C8 H8A 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 122.0(4) . . ?
N1 C9 H9 119.0 . . ?
C10 C9 H9 119.0 . . ?
C9 C10 C5 119.9(5) . . ?
C9 C10 H10 120.1 . . ?
C5 C10 H10 120.1 . . ?
C12 C11 C4 120.5(4) . . ?
C12 C11 H11 119.7 . . ?
C4 C11 H11 119.7 . . ?
N2 C12 C11 121.2(4) . . ?
N2 C12 H12 119.4 . . ?
C11 C12 H12 119.4 . . ?
N3 C13 S2 179.0(5) . . ?
N4 C14 S3 176.7(5) . . ?
N5 C15 S4 178.0(5) . . ?
N6 C16 S1 179.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.73
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.098

data_1
_database_code_depnum_ccdc_archive 'CCDC 653491'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 Mn N8 S2, 2(C6 H7 N)'
_chemical_formula_sum            'C14 H14 Mn N10 S2'
_chemical_formula_weight         441.41

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'
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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2/c
_symmetry_space_group_name_Hall  '-P 2yc'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   11.9679(13)
_cell_length_b                   6.3012(6)
_cell_length_c                   12.4917(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.092(7)
_cell_angle_gamma                90.00
_cell_volume                     941.40(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1424
_cell_measurement_theta_min      2.3143
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.0800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             450
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8335
_exptl_absorpt_correction_T_max  0.9282
_exptl_absorpt_process_details   'CrystalClear (Rigaku Corp., 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Mercury70 (2x2 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_diffrn_detector_area_resol_mean 14.6306
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6976
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.23
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2162
_reflns_number_gt                1675
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2162
_refine_ls_number_parameters     126
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0658
_refine_ls_wR_factor_ref         0.1229
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.5000 0.5000 0.0000 0.0392(2) Uani 1 2 d S . .
S1 S 0.87399(9) 0.6402(2) 0.16539(9) 0.0596(3) Uani 1 1 d . . .
N1 N 0.2430(3) 0.0294(6) 0.1632(3) 0.0565(9) Uani 1 1 d . . .
N2 N 0.4464(3) 0.5362(7) 0.1694(3) 0.0687(11) Uani 1 1 d . . .
N3 N 0.5000 0.5379(8) 0.2500 0.0521(12) Uani 1 2 d S . .
N4 N 0.5380(3) 0.1603(6) 0.0280(4) 0.0731(12) Uani 1 1 d . . .
N5 N 0.5000 0.0000 0.0000 0.0536(12) Uani 1 2 d S . .
N6 N 0.6722(3) 0.5757(6) 0.0519(3) 0.0623(10) Uani 1 1 d . . .
C1 C 0.3427(4) 0.0419(9) 0.2370(4) 0.0764(15) Uani 1 1 d . . .
H1B H 0.3410 0.1754 0.2772 0.115 Uiso 1 1 calc R . .
H1A H 0.4106 0.0365 0.1955 0.115 Uiso 1 1 calc R . .
H1C H 0.3423 -0.0778 0.2870 0.115 Uiso 1 1 calc R . .
C2 C 0.1686(5) 0.1844(9) 0.1647(4) 0.0793(15) Uani 1 1 d . . .
H2 H 0.1818 0.3032 0.2103 0.095 Uiso 1 1 calc R . .
C3 C 0.0733(4) 0.1760(8) 0.1019(4) 0.0758(15) Uani 1 1 d . . .
H3 H 0.0210 0.2890 0.1045 0.091 Uiso 1 1 calc R . .
C4 C 0.0514(3) 0.0060(7) 0.0343(3) 0.0497(9) Uani 1 1 d . . .
C5 C 0.1317(4) -0.1503(8) 0.0341(4) 0.0626(12) Uani 1 1 d . . .
H5 H 0.1215 -0.2697 -0.0117 0.075 Uiso 1 1 calc R . .
C6 C 0.2259(4) -0.1360(8) 0.0989(4) 0.0653(12) Uani 1 1 d . . .
H6 H 0.2799 -0.2463 0.0979 0.078 Uiso 1 1 calc R . .
C7 C 0.7555(3) 0.6035(6) 0.1003(3) 0.0463(9) Uani 1 1 d . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Mn1 0.0419(4) 0.0396(4) 0.0357(4) -0.0030(4) -0.0059(3) -0.0022(4)
S1 0.0457(6) 0.0719(8) 0.0603(7) -0.0015(6) -0.0103(5) -0.0051(6)
N1 0.0495(19) 0.063(2) 0.056(2) 0.0088(18) -0.0032(15) -0.0030(19)
N2 0.068(2) 0.103(3) 0.0350(18) -0.006(2) -0.0041(17) 0.012(2)
N3 0.057(3) 0.056(3) 0.044(3) 0.000 0.005(2) 0.000
N4 0.084(3) 0.034(2) 0.100(3) 0.002(2) -0.023(2) -0.004(2)
N5 0.061(3) 0.049(3) 0.051(3) 0.016(3) -0.003(2) 0.010(3)
N6 0.051(2) 0.068(2) 0.067(2) -0.0103(19) -0.0105(18) -0.0053(19)
C1 0.066(3) 0.091(4) 0.071(3) 0.008(3) -0.013(2) -0.010(3)
C2 0.091(4) 0.071(3) 0.074(3) -0.017(3) -0.026(3) 0.016(3)
C3 0.086(4) 0.065(3) 0.074(3) -0.014(3) -0.018(3) 0.031(3)
C4 0.051(2) 0.053(2) 0.045(2) 0.000(2) 0.0038(16) 0.008(2)
C5 0.054(3) 0.065(3) 0.068(3) -0.015(2) -0.002(2) 0.014(2)
C6 0.051(3) 0.073(3) 0.072(3) -0.012(3) 0.003(2) 0.015(2)
C7 0.047(2) 0.045(2) 0.046(2) -0.0027(18) 0.0017(17) -0.0006(19)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 N6 2.190(3) . ?
Mn1 N6 2.190(3) 3_665 ?
Mn1 N4 2.213(4) 3_665 ?
Mn1 N4 2.213(4) . ?
Mn1 N2 2.245(3) . ?
Mn1 N2 2.245(3) 3_665 ?
S1 C7 1.625(4) . ?
N1 C2 1.323(6) . ?
N1 C6 1.328(6) . ?
N1 C1 1.482(5) . ?
N2 N3 1.174(3) . ?
N3 N2 1.174(3) 2_655 ?
N4 N5 1.157(4) . ?
N5 N4 1.157(4) 3_655 ?
N6 C7 1.161(5) . ?
C1 H1B 0.9800 . ?
C1 H1A 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.361(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.376(6) . ?
C4 C4 1.475(7) 3 ?
C5 C6 1.366(6) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?

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
N6 Mn1 N6 180.0 . 3_665 ?
N6 Mn1 N4 91.26(14) . 3_665 ?
N6 Mn1 N4 88.74(14) 3_665 3_665 ?
N6 Mn1 N4 88.74(14) . . ?
N6 Mn1 N4 91.26(14) 3_665 . ?
N4 Mn1 N4 180.0(2) 3_665 . ?
N6 Mn1 N2 89.82(14) . . ?
N6 Mn1 N2 90.18(14) 3_665 . ?
N4 Mn1 N2 89.22(16) 3_665 . ?
N4 Mn1 N2 90.78(16) . . ?
N6 Mn1 N2 90.18(14) . 3_665 ?
N6 Mn1 N2 89.82(14) 3_665 3_665 ?
N4 Mn1 N2 90.78(16) 3_665 3_665 ?
N4 Mn1 N2 89.22(16) . 3_665 ?
N2 Mn1 N2 180.0(2) . 3_665 ?
C2 N1 C6 119.9(4) . . ?
C2 N1 C1 118.6(4) . . ?
C6 N1 C1 121.4(4) . . ?
N3 N2 Mn1 130.0(3) . . ?
N2 N3 N2 178.9(7) . 2_655 ?
N5 N4 Mn1 136.1(3) . . ?
N4 N5 N4 180.0(6) . 3_655 ?
C7 N6 Mn1 165.5(4) . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1A 109.5 . . ?
H1B C1 H1A 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
N1 C2 C3 120.9(5) . . ?
N1 C2 H2 119.6 . . ?
C3 C2 H2 119.6 . . ?
C2 C3 C4 121.2(4) . . ?
C2 C3 H3 119.4 . . ?
C4 C3 H3 119.4 . . ?
C5 C4 C3 116.0(4) . . ?
C5 C4 C4 122.0(5) . 3 ?
C3 C4 C4 122.0(5) . 3 ?
C6 C5 C4 120.8(4) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
N1 C6 C5 121.1(4) . . ?
N1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
N6 C7 S1 178.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.062