# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_an232
#============================================================================== 
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H38 Cl2 N8 O11 S4 Zn'
_chemical_formula_weight         1071.35

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   P41212

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, -z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'-y, -x, -z+1/2'
'y, x, -z'
'y+1/2, -x+1/2, z+3/4'
'-y+1/2, x+1/2, z+1/4'

_cell_length_a                   16.529(2)
_cell_length_b                   16.529(2)
_cell_length_c                   16.604(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4536.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.0021
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.569
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2200
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28832
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         28.20
_reflns_number_total             5315
_reflns_number_gt                4875
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0707P)²+3.2047P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.026(16)
_refine_ls_number_reflns         5315
_refine_ls_number_parameters     311
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1195
_refine_ls_wR_factor_gt          0.1156
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_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
Zn1 Zn 0.005164(19) 1.005164(19) 0.5000 0.02195(12) Uani 1 2 d S . .
S2 S -0.00233(6) 0.60227(5) 0.46181(6) 0.0381(2) Uani 1 1 d . . .
S1 S 0.07535(6) 1.40411(5) 0.53448(7) 0.0386(2) Uani 1 1 d . . .
Cl1 Cl 0.19625(5) 1.22252(5) 0.22747(5) 0.0360(2) Uani 1 1 d . . .
O5 O 0.05611(15) 0.94389(15) 0.2500 0.0378(8) Uani 1 2 d S . .
N1 N 0.01281(16) 1.13453(15) 0.52581(16) 0.0249(5) Uani 1 1 d . . .
N2 N 0.00601(15) 0.87642(15) 0.48762(14) 0.0229(5) Uani 1 1 d . . .
N4 N 0.33092(17) 1.41948(17) 0.42795(16) 0.0289(6) Uani 1 1 d . . .
O1W O -0.01499(15) 1.03107(15) 0.37456(13) 0.0276(5) Uani 1 1 d . . .
C6 C 0.05129(19) 0.7545(2) 0.4248(2) 0.0282(6) Uani 1 1 d . . .
H6 H 0.0842 0.7295 0.3868 0.034 Uiso 1 1 calc R . .
C7 C 0.0002(2) 0.70891(18) 0.4735(2) 0.0283(6) Uani 1 1 d . . .
C8 C -0.04194(19) 0.83174(19) 0.53599(19) 0.0250(6) Uani 1 1 d . . .
H8 H -0.0736 0.8580 0.5742 0.030 Uiso 1 1 calc R . .
C9 C 0.1748(2) 1.4055(2) 0.4935(2) 0.0297(7) Uani 1 1 d . . .
C10 C 0.05245(19) 0.8372(2) 0.43390(19) 0.0264(6) Uani 1 1 d . . .
H10 H 0.0869 0.8674 0.4014 0.032 Uiso 1 1 calc R . .
C11 C 0.0755(2) 1.1623(2) 0.5701(2) 0.0278(7) Uani 1 1 d . . .
H11 H 0.1055 1.1253 0.5999 0.033 Uiso 1 1 calc R . .
C12 C 0.0974(2) 1.2439(2) 0.5734(2) 0.0303(7) Uani 1 1 d . . .
H12 H 0.1418 1.2606 0.6036 0.036 Uiso 1 1 calc R . .
O1 O 0.28106(18) 1.2247(3) 0.2451(2) 0.0684(10) Uani 1 1 d . . .
N3 N -0.2750(2) 0.5540(2) 0.4648(2) 0.0457(8) Uani 1 1 d . . .
O4 O 0.17592(19) 1.1529(2) 0.1821(2) 0.0664(10) Uani 1 1 d . . .
C16 C 0.2033(2) 1.3498(2) 0.4386(2) 0.0328(7) Uani 1 1 d . . .
H16 H 0.1709 1.3068 0.4225 0.039 Uiso 1 1 calc R . .
C17 C -0.0459(2) 0.7481(2) 0.5308(2) 0.0289(7) Uani 1 1 d . . .
H17 H -0.0790 0.7188 0.5655 0.035 Uiso 1 1 calc R . .
C18 C -0.0155(2) 1.2725(2) 0.4887(2) 0.0329(7) Uani 1 1 d . . .
H18 H -0.0489 1.3090 0.4621 0.039 Uiso 1 1 calc R . .
C19 C 0.2802(2) 1.3584(2) 0.4080(2) 0.0329(7) Uani 1 1 d . . .
H19 H 0.2984 1.3200 0.3714 0.039 Uiso 1 1 calc R . .
C20 C 0.0517(2) 1.29920(19) 0.5308(2) 0.0305(7) Uani 1 1 d . . .
C21 C -0.0320(2) 1.1898(2) 0.4872(2) 0.0299(7) Uani 1 1 d . . .
H21 H -0.0765 1.1721 0.4578 0.036 Uiso 1 1 calc R . .
C22 C -0.1085(2) 0.5850(2) 0.4616(2) 0.0337(7) Uani 1 1 d . . .
O3 O 0.1542(2) 1.2156(3) 0.3033(2) 0.0689(10) Uani 1 1 d . . .
C24 C 0.3018(2) 1.4740(2) 0.4804(2) 0.0351(8) Uani 1 1 d . . .
H24 H 0.3349 1.5171 0.4947 0.042 Uiso 1 1 calc R . .
C25 C 0.2249(2) 1.4697(2) 0.5148(2) 0.0316(7) Uani 1 1 d . . .
H25 H 0.2075 1.5089 0.5511 0.038 Uiso 1 1 calc R . .
C26 C -0.2206(3) 0.4995(2) 0.4906(2) 0.0463(10) Uani 1 1 d . . .
H26 H -0.2398 0.4504 0.5103 0.056 Uiso 1 1 calc R . .
C27 C -0.1383(2) 0.5118(2) 0.4899(2) 0.0390(8) Uani 1 1 d . . .
H27 H -0.1032 0.4718 0.5080 0.047 Uiso 1 1 calc R . .
C28 C -0.1641(2) 0.6409(2) 0.4315(2) 0.0387(8) Uani 1 1 d . . .
H28 H -0.1466 0.6895 0.4092 0.046 Uiso 1 1 calc R . .
C29 C -0.2457(2) 0.6228(2) 0.4355(2) 0.0389(8) Uani 1 1 d . . .
H29 H -0.2823 0.6611 0.4166 0.047 Uiso 1 1 calc R . .
O2 O 0.1669(3) 1.2925(2) 0.1888(3) 0.1008(17) Uani 1 1 d . . .
H12W H 0.007(2) 1.001(3) 0.346(3) 0.037(11) Uiso 1 1 d . . .
H11W H -0.058(3) 1.049(3) 0.364(3) 0.058(15) Uiso 1 1 d . . .
H51 H 0.111(2) 0.947(2) 0.263(2) 0.039(11) Uiso 1 1 d . . .


_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
Zn1 N2 2.138(2) 6_466 ?
Zn1 N2 2.138(2) . ?
Zn1 O1W 2.152(2) . ?
Zn1 O1W 2.152(2) 6_466 ?
Zn1 N1 2.184(2) . ?
Zn1 N1 2.184(3) 6_466 ?
S2 C7 1.774(3) . ?
S2 C22 1.779(4) . ?
S1 C20 1.779(3) . ?
S1 C9 1.779(3) . ?
Cl1 O2 1.408(4) . ?
Cl1 O4 1.416(3) . ?
Cl1 O1 1.433(3) . ?
Cl1 O3 1.443(3) . ?
N1 C21 1.340(4) . ?
N1 C11 1.351(4) . ?
N2 C10 1.343(4) . ?
N2 C8 1.349(4) . ?
N4 C24 1.342(4) . ?
N4 C19 1.353(4) . ?
C6 C10 1.376(5) . ?
C6 C7 1.391(5) . ?
C7 C17 1.380(5) . ?
C8 C17 1.387(5) . ?
C9 C16 1.377(5) . ?
C9 C25 1.393(5) . ?
C11 C12 1.398(4) . ?
C12 C20 1.381(5) . ?
N3 C29 1.328(5) . ?
N3 C26 1.343(6) . ?
C16 C19 1.377(5) . ?
C18 C20 1.384(5) . ?
C18 C21 1.394(5) . ?
C22 C27 1.387(5) . ?
C22 C28 1.396(5) . ?
C24 C25 1.396(5) . ?
C26 C27 1.375(6) . ?
C28 C29 1.384(5) . ?

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
N2 Zn1 N2 91.27(14) 6_466 . ?
N2 Zn1 O1W 86.43(9) 6_466 . ?
N2 Zn1 O1W 96.08(9) . . ?
N2 Zn1 O1W 96.08(9) 6_466 6_466 ?
N2 Zn1 O1W 86.43(9) . 6_466 ?
O1W Zn1 O1W 176.42(13) . 6_466 ?
N2 Zn1 N1 91.85(9) 6_466 . ?
N2 Zn1 N1 173.11(10) . . ?
O1W Zn1 N1 90.24(10) . . ?
O1W Zn1 N1 87.14(10) 6_466 . ?
N2 Zn1 N1 173.11(10) 6_466 6_466 ?
N2 Zn1 N1 91.85(9) . 6_466 ?
O1W Zn1 N1 87.14(10) . 6_466 ?
O1W Zn1 N1 90.24(10) 6_466 6_466 ?
N1 Zn1 N1 85.71(14) . 6_466 ?
C7 S2 C22 100.52(17) . . ?
C20 S1 C9 101.65(16) . . ?
O2 Cl1 O4 110.1(2) . . ?
O2 Cl1 O1 114.2(3) . . ?
O4 Cl1 O1 111.2(2) . . ?
O2 Cl1 O3 107.3(3) . . ?
O4 Cl1 O3 106.6(2) . . ?
O1 Cl1 O3 107.1(2) . . ?
C21 N1 C11 116.9(3) . . ?
C21 N1 Zn1 122.8(2) . . ?
C11 N1 Zn1 118.9(2) . . ?
C10 N2 C8 117.9(3) . . ?
C10 N2 Zn1 123.2(2) . . ?
C8 N2 Zn1 118.9(2) . . ?
C24 N4 C19 115.9(3) . . ?
C10 C6 C7 118.9(3) . . ?
C17 C7 C6 118.8(3) . . ?
C17 C7 S2 121.9(3) . . ?
C6 C7 S2 119.3(3) . . ?
N2 C8 C17 122.5(3) . . ?
C16 C9 C25 118.3(3) . . ?
C16 C9 S1 124.1(3) . . ?
C25 C9 S1 117.5(3) . . ?
N2 C10 C6 123.0(3) . . ?
N1 C11 C12 123.2(3) . . ?
C20 C12 C11 118.5(3) . . ?
C29 N3 C26 116.5(4) . . ?
C19 C16 C9 119.4(3) . . ?
C7 C17 C8 119.0(3) . . ?
C20 C18 C21 118.7(3) . . ?
N4 C19 C16 124.0(3) . . ?
C12 C20 C18 119.1(3) . . ?
C12 C20 S1 120.5(3) . . ?
C18 C20 S1 120.3(3) . . ?
N1 C21 C18 123.5(3) . . ?
C27 C22 C28 117.7(4) . . ?
C27 C22 S2 119.3(3) . . ?
C28 C22 S2 123.0(3) . . ?
N4 C24 C25 124.0(3) . . ?
C9 C25 C24 118.4(3) . . ?
N3 C26 C27 124.0(4) . . ?
C26 C27 C22 118.9(4) . . ?
C29 C28 C22 118.7(4) . . ?
N3 C29 C28 124.0(4) . . ?

_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_theta_full        28.20
_diffrn_measured_fraction_theta_full 0.973
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.084
_database_code_depnum_ccdc_archive 'CCDC 885878'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_274mnbps

_audit_creation_date             2011-12-01T10:49:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C42 H32 Mn N10 S6'
_chemical_formula_moiety         'C42 H32 Mn N10 S6'
_chemical_formula_weight         924.08

#==============================================================================

# CRYSTAL DATA

_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.694(3)
_cell_length_b                   11.143(4)
_cell_length_c                   11.326(3)
_cell_angle_alpha                87.71(4)
_cell_angle_beta                 76.90(3)
_cell_angle_gamma                67.65(4)
_cell_volume                     1100.5(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1354
_cell_measurement_theta_max      26.08
_cell_measurement_theta_min      1.98
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             475
_exptl_crystal_size_max          0.319
_exptl_crystal_size_mid          0.198
_exptl_crystal_size_min          0.072
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        a grid of  8 x  8 x  8 =   512 sampling points was used
;
_exptl_absorpt_correction_T_min  0.8748
_exptl_absorpt_correction_T_max  0.9646

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_number            8602
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.118
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measured_fraction_theta_full 0.941
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13

#==============================================================================

# STRUCTURE SOLUTION

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total             4003
_reflns_number_gt                1803
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1201
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.094
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_restrained_S_all      0.787
_refine_ls_number_reflns         4003
_refine_ls_number_parameters     277
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0366P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
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'
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'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Mn1 0.5 0.5 0 0.0427(2) Uani d S 1 . . Mn
S1 0.87809(15) 0.70063(16) -0.10964(13) 0.1048(5) Uani d . 1 . . S
S2 1.1068(12) -0.0681(9) -0.2115(9) 0.081(2) Uani d P 0.5 . . S
S2' 1.1063(11) -0.0502(9) -0.2488(10) 0.122(3) Uani d P 0.5 . . S
S3 0.69799(11) 0.29961(11) 0.54318(10) 0.0649(3) Uani d . 1 . . S
N1 0.6511(3) 0.6045(3) -0.0340(3) 0.0577(9) Uani d . 1 . . N
N2 0.7024(3) 0.3129(3) -0.0769(3) 0.0480(7) Uani d . 1 . . N
N3 1.5304(5) 0.0324(5) -0.2567(6) 0.1177(16) Uani d . 1 . . N
N4 0.5549(3) 0.4526(3) 0.1922(2) 0.0434(7) Uani d . 1 . . N
N5 1.1525(4) 0.3355(4) 0.5400(4) 0.0829(12) Uani d . 1 . . N
C1 0.7457(4) 0.6446(3) -0.0651(3) 0.0460(9) Uani d . 1 . . C
C2 0.6890(4) 0.2187(4) -0.1381(4) 0.0574(10) Uani d . 1 . . C
H2 0.5924 0.23 -0.1485 0.086 Uiso calc R 1 . . H
C3 0.8103(4) 0.1063(4) -0.1861(4) 0.0678(12) Uani d . 1 . . C
H3 0.7956 0.0444 -0.2291 0.102 Uiso calc R 1 . . H
C4 0.9549(4) 0.0862(4) -0.1697(4) 0.0645(11) Uani d . 1 . . C
C5 0.9693(4) 0.1815(4) -0.1060(4) 0.0610(11) Uani d . 1 . . C
H5 1.0644 0.1715 -0.0933 0.091 Uiso calc R 1 . . H
C6 0.8439(4) 0.2910(4) -0.0614(3) 0.0537(10) Uani d . 1 . . C
H6 0.8566 0.3537 -0.018 0.081 Uiso calc R 1 . . H
C7 1.2707(4) -0.0223(4) -0.2365(5) 0.0665(12) Uani d . 1 . . C
C8 1.3117(6) 0.0483(5) -0.3249(5) 0.1058(18) Uani d . 1 . . C
H8 1.2527 0.08 -0.3819 0.159 Uiso calc R 1 . . H
C9 1.4396(8) 0.0743(7) -0.3320(6) 0.134(2) Uani d . 1 . . C
H9 1.464 0.1249 -0.3942 0.201 Uiso calc R 1 . . H
C10 1.4876(7) -0.0364(6) -0.1683(6) 0.1053(18) Uani d . 1 . . C
H10 1.5474 -0.0671 -0.1116 0.158 Uiso calc R 1 . . H
C11 1.3582(6) -0.0646(5) -0.1564(5) 0.0882(14) Uani d . 1 . . C
H11 1.3323 -0.1129 -0.0926 0.132 Uiso calc R 1 . . H
C12 0.4926(4) 0.3812(3) 0.2666(3) 0.0493(9) Uani d . 1 . . C
H12 0.4168 0.3608 0.2448 0.074 Uiso calc R 1 . . H
C13 0.5336(4) 0.3364(3) 0.3730(3) 0.0509(9) Uani d . 1 . . C
H13 0.4849 0.2884 0.4219 0.076 Uiso calc R 1 . . H
C14 0.6482(4) 0.3628(3) 0.4073(3) 0.0455(9) Uani d . 1 . . C
C15 0.7098(4) 0.4402(4) 0.3340(4) 0.0569(10) Uani d . 1 . . C
H15 0.7834 0.4641 0.3552 0.085 Uiso calc R 1 . . H
C16 0.6610(4) 0.4818(4) 0.2291(3) 0.0550(10) Uani d . 1 . . C
H16 0.7045 0.5335 0.1806 0.082 Uiso calc R 1 . . H
C17 0.8747(4) 0.3161(4) 0.5370(4) 0.0548(10) Uani d . 1 . . C
C18 1.0005(4) 0.2648(4) 0.4411(4) 0.0722(12) Uani d . 1 . . C
H18 0.9947 0.2225 0.3744 0.108 Uiso calc R 1 . . H
C19 1.1366(5) 0.2780(5) 0.4469(5) 0.0824(14) Uani d . 1 . . C
H19 1.2206 0.2445 0.3817 0.124 Uiso calc R 1 . . H
C20 1.0312(6) 0.3815(4) 0.6312(5) 0.0793(13) Uani d . 1 . . C
H20 1.0406 0.4208 0.6982 0.119 Uiso calc R 1 . . H
C21 0.8909(5) 0.3747(4) 0.6332(4) 0.0650(11) Uani d . 1 . . C
H21 0.8089 0.4098 0.6995 0.097 Uiso calc R 1 . . H



#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Mn1 N1 2_665 2.158(3) ?
Mn1 N1 . 2.158(3) ?
Mn1 N2 2_665 2.283(3) ?
Mn1 N2 . 2.283(3) ?
Mn1 N4 2_665 2.349(3) ?
Mn1 N4 . 2.349(3) ?
S1 C1 . 1.606(4) ?
S2 C4 . 1.780(11) ?
S2 C7 . 1.807(10) ?
S2' C4 . 1.755(11) ?
S2' C7 . 1.770(10) ?
S3 C14 . 1.757(4) ?
S3 C17 . 1.776(4) ?
N1 C1 . 1.148(4) ?
N2 C2 . 1.343(4) ?
N2 C6 . 1.350(4) ?
N3 C9 . 1.310(7) ?
N3 C10 . 1.325(7) ?
N4 C12 . 1.338(4) ?
N4 C16 . 1.341(4) ?
N5 C20 . 1.320(6) ?
N5 C19 . 1.323(6) ?
C2 C3 . 1.375(5) ?
C2 H2 . 0.93 ?
C3 C4 . 1.388(5) ?
C3 H3 . 0.93 ?
C4 C5 . 1.374(5) ?
C5 C6 . 1.365(5) ?
C5 H5 . 0.93 ?
C6 H6 . 0.93 ?
C7 C8 . 1.331(6) ?
C7 C11 . 1.333(6) ?
C8 C9 . 1.362(7) ?
C8 H8 . 0.93 ?
C9 H9 . 0.93 ?
C10 C11 . 1.382(7) ?
C10 H10 . 0.93 ?
C11 H11 . 0.93 ?
C12 C13 . 1.370(5) ?
C12 H12 . 0.93 ?
C13 C14 . 1.387(4) ?
C13 H13 . 0.93 ?
C14 C15 . 1.379(5) ?
C15 C16 . 1.376(5) ?
C15 H15 . 0.93 ?
C16 H16 . 0.93 ?
C17 C21 . 1.360(5) ?
C17 C18 . 1.383(5) ?
C18 C19 . 1.398(5) ?
C18 H18 . 0.93 ?
C19 H19 . 0.93 ?
C20 C21 . 1.386(5) ?
C20 H20 . 0.93 ?
C21 H21 . 0.93 ?

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
#S2' C4 S2 14.9(6) . . ?
#S2' C7 S2 14.7(6) . . ?
N1 Mn1 N1 180 2_665 . ?
N1 Mn1 N2 89.75(11) 2_665 2_665 ?
N1 Mn1 N2 90.25(11) . 2_665 ?
N1 Mn1 N2 90.25(11) 2_665 . ?
N1 Mn1 N2 89.75(11) . . ?
N2 Mn1 N2 180 2_665 . ?
N1 Mn1 N4 89.39(11) 2_665 2_665 ?
N1 Mn1 N4 90.61(11) . 2_665 ?
N2 Mn1 N4 88.58(10) 2_665 2_665 ?
N2 Mn1 N4 91.42(10) . 2_665 ?
N1 Mn1 N4 90.61(11) 2_665 . ?
N1 Mn1 N4 89.39(11) . . ?
N2 Mn1 N4 91.42(10) 2_665 . ?
N2 Mn1 N4 88.58(10) . . ?
N4 Mn1 N4 180.00(14) 2_665 . ?
C4 S2 C7 100.5(5) . . ?
C4 S2' C7 103.0(6) . . ?
C14 S3 C17 104.25(17) . . ?
C1 N1 Mn1 169.4(3) . . ?
C2 N2 C6 116.2(3) . . ?
C2 N2 Mn1 123.0(2) . . ?
C6 N2 Mn1 120.8(2) . . ?
C9 N3 C10 115.2(5) . . ?
C12 N4 C16 115.7(3) . . ?
C12 N4 Mn1 120.8(2) . . ?
C16 N4 Mn1 123.2(2) . . ?
C20 N5 C19 116.6(4) . . ?
N1 C1 S1 179.5(3) . . ?
N2 C2 C3 123.6(3) . . ?
N2 C2 H2 118.2 . . ?
C3 C2 H2 118.2 . . ?
C2 C3 C4 119.2(4) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 117.6(3) . . ?
C5 C4 S2' 125.9(4) . . ?
C3 C4 S2' 116.1(5) . . ?
C5 C4 S2 122.2(5) . . ?
C3 C4 S2 119.6(5) . . ?
C6 C5 C4 120.0(3) . . ?
C6 C5 H5 120 . . ?
C4 C5 H5 120 . . ?
N2 C6 C5 123.4(3) . . ?
N2 C6 H6 118.3 . . ?
C5 C6 H6 118.3 . . ?
C8 C7 C11 117.6(4) . . ?
C8 C7 S2' 112.6(5) . . ?
C11 C7 S2' 129.8(5) . . ?
C8 C7 S2 127.2(5) . . ?
C11 C7 S2 115.2(5) . . ?
C7 C8 C9 120.3(5) . . ?
C7 C8 H8 119.9 . . ?
C9 C8 H8 119.9 . . ?
N3 C9 C8 124.1(5) . . ?
N3 C9 H9 118 . . ?
C8 C9 H9 118 . . ?
N3 C10 C11 123.0(5) . . ?
N3 C10 H10 118.5 . . ?
C11 C10 H10 118.5 . . ?
C7 C11 C10 119.9(5) . . ?
C7 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
N4 C12 C13 123.9(3) . . ?
N4 C12 H12 118 . . ?
C13 C12 H12 118 . . ?
C12 C13 C14 119.7(3) . . ?
C12 C13 H13 120.1 . . ?
C14 C13 H13 120.1 . . ?
C15 C14 C13 117.1(3) . . ?
C15 C14 S3 125.4(3) . . ?
C13 C14 S3 117.4(3) . . ?
C16 C15 C14 119.2(3) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 120.4 . . ?
N4 C16 C15 124.3(3) . . ?
N4 C16 H16 117.9 . . ?
C15 C16 H16 117.9 . . ?
C21 C17 C18 118.1(4) . . ?
C21 C17 S3 119.1(3) . . ?
C18 C17 S3 122.6(3) . . ?
C17 C18 C19 118.5(4) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 H18 120.8 . . ?
N5 C19 C18 123.5(4) . . ?
N5 C19 H19 118.2 . . ?
C18 C19 H19 118.2 . . ?
N5 C20 C21 124.1(5) . . ?
N5 C20 H20 118 . . ?
C21 C20 H20 118 . . ?
C17 C21 C20 119.2(4) . . ?
C17 C21 H21 120.4 . . ?
C20 C21 H21 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
#N1 Mn1 N1 C1 17E1(10) 2_665 . . . ?
#N2 Mn1 N2 C2 17E1(10) 2_665 . . . ?
#N2 Mn1 N2 C6 -1E1(10) 2_665 . . . ?
#N4 Mn1 N4 C12 5E1(10) 2_665 . . . ?
#N4 Mn1 N4 C16 -14E1(10) 2_665 . . . ?
#Mn1 N1 C1 S1 5E1(4) . . . . ?
N2 Mn1 N1 C1 -157.5(15) 2_665 . . . ?
N2 Mn1 N1 C1 22.5(15) . . . . ?
N4 Mn1 N1 C1 -68.9(15) 2_665 . . . ?
N4 Mn1 N1 C1 111.1(15) . . . . ?
N1 Mn1 N2 C2 33.3(3) 2_665 . . . ?
N1 Mn1 N2 C2 -146.7(3) . . . . ?
N4 Mn1 N2 C2 -56.1(3) 2_665 . . . ?
N4 Mn1 N2 C2 123.9(3) . . . . ?
N1 Mn1 N2 C6 -145.9(3) 2_665 . . . ?
N1 Mn1 N2 C6 34.1(3) . . . . ?
N4 Mn1 N2 C6 124.7(3) 2_665 . . . ?
N4 Mn1 N2 C6 -55.3(3) . . . . ?
N1 Mn1 N4 C12 1.0(3) 2_665 . . . ?
N1 Mn1 N4 C12 -179.0(3) . . . . ?
N2 Mn1 N4 C12 90.8(2) 2_665 . . . ?
N2 Mn1 N4 C12 -89.2(2) . . . . ?
N1 Mn1 N4 C16 173.5(3) 2_665 . . . ?
N1 Mn1 N4 C16 -6.5(3) . . . . ?
N2 Mn1 N4 C16 -96.7(3) 2_665 . . . ?
N2 Mn1 N4 C16 83.3(3) . . . . ?
C6 N2 C2 C3 -1.6(6) . . . . ?
Mn1 N2 C2 C3 179.2(3) . . . . ?
N2 C2 C3 C4 1.2(6) . . . . ?
C2 C3 C4 C5 -0.3(6) . . . . ?
C2 C3 C4 S2' -172.8(4) . . . . ?
C2 C3 C4 S2 170.8(4) . . . . ?
C7 S2' C4 C5 -5.5(8) . . . . ?
C7 S2' C4 C3 166.3(4) . . . . ?
C7 S2' C4 S2 -86(3) . . . . ?
C7 S2 C4 C5 -33.6(7) . . . . ?
C7 S2 C4 C3 155.7(5) . . . . ?
C7 S2 C4 S2' 76(2) . . . . ?
C3 C4 C5 C6 0.0(6) . . . . ?
S2' C4 C5 C6 171.7(5) . . . . ?
S2 C4 C5 C6 -170.8(4) . . . . ?
C2 N2 C6 C5 1.2(5) . . . . ?
Mn1 N2 C6 C5 -179.5(3) . . . . ?
C4 C5 C6 N2 -0.5(6) . . . . ?
C4 S2' C7 C8 -87.6(6) . . . . ?
C4 S2' C7 C11 95.0(6) . . . . ?
C4 S2' C7 S2 85(3) . . . . ?
C4 S2 C7 C8 -67.9(8) . . . . ?
C4 S2 C7 C11 111.8(5) . . . . ?
C4 S2 C7 S2' -77(2) . . . . ?
C11 C7 C8 C9 0.5(9) . . . . ?
S2' C7 C8 C9 -177.3(6) . . . . ?
S2 C7 C8 C9 -179.7(6) . . . . ?
C10 N3 C9 C8 -1.6(11) . . . . ?
C7 C8 C9 N3 0.9(11) . . . . ?
C9 N3 C10 C11 1.1(9) . . . . ?
C8 C7 C11 C10 -1.1(7) . . . . ?
S2' C7 C11 C10 176.3(6) . . . . ?
S2 C7 C11 C10 179.1(5) . . . . ?
N3 C10 C11 C7 0.3(8) . . . . ?
C16 N4 C12 C13 -1.4(5) . . . . ?
Mn1 N4 C12 C13 171.6(3) . . . . ?
N4 C12 C13 C14 -1.2(6) . . . . ?
C12 C13 C14 C15 3.4(5) . . . . ?
C12 C13 C14 S3 -178.7(3) . . . . ?
C17 S3 C14 C15 -16.7(4) . . . . ?
C17 S3 C14 C13 165.6(3) . . . . ?
C13 C14 C15 C16 -3.0(5) . . . . ?
S3 C14 C15 C16 179.3(3) . . . . ?
C12 N4 C16 C15 1.9(5) . . . . ?
Mn1 N4 C16 C15 -171.0(3) . . . . ?
C14 C15 C16 N4 0.4(6) . . . . ?
C14 S3 C17 C21 128.8(3) . . . . ?
C14 S3 C17 C18 -55.2(4) . . . . ?
C21 C17 C18 C19 -1.2(6) . . . . ?
S3 C17 C18 C19 -177.3(3) . . . . ?
C20 N5 C19 C18 0.3(6) . . . . ?
C17 C18 C19 N5 0.9(7) . . . . ?
C19 N5 C20 C21 -1.2(6) . . . . ?
C18 C17 C21 C20 0.4(6) . . . . ?
S3 C17 C21 C20 176.6(3) . . . . ?
N5 C20 C21 C17 0.9(6) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 885879'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_r321

_audit_creation_date             2011-05-02T13:42:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C12 H8 N4 O2 S Zn'
_chemical_formula_moiety         'C12 H8 N4 O2 S Zn'
_chemical_formula_weight         337.65

#==============================================================================

# CRYSTAL DATA

_symmetry_space_group_name_H-M   'P c a b'
_symmetry_space_group_name_Hall  '-P 2bc 2ac'

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

_cell_length_a                   14.545(3)
_cell_length_b                   14.834(3)
_cell_length_c                   12.805(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2762.8(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9399
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      2.52
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    1.934
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6643
_exptl_absorpt_correction_T_max  0.8152
_exptl_absorpt_process_details   
;J. de Meulenaar and H. Tompa, Acta Crystallogr., Sect A 1965, 19, 1014-1018.
;

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_number            9399
_diffrn_reflns_av_R_equivalents  0.1025
_diffrn_reflns_av_unetI/netI     0.1957
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_full        25.99
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       15

#==============================================================================

# STRUCTURE SOLUTION

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total             2698
_reflns_number_gt                852
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.1409
_refine_ls_R_factor_gt           0.029
_refine_ls_wR_factor_ref         0.0613
_refine_ls_goodness_of_fit_ref   0.801
_refine_ls_restrained_S_all      0.801
_refine_ls_number_reflns         2698
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;calc w=[0.00000+1.00000exp(3.50(sinθ/λ)²)]/[σ²(Fo²)+
0.0000+0.0000*P+(0.0000P)²+0.0000sinθ/λ] 
where P = 0.33333Fo² + 0.66667Fc²
;

_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00076(9)
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Zn1 0.54519(5) 0.25867(4) 0.12262(4) 0.0566(2) Uani d . 1 . . Zn
S1 0.69116(12) 0.49513(11) 0.52506(11) 0.0648(5) Uani d . 1 . . S
N1 0.6318(3) 0.2673(4) 0.0100(4) 0.0751(14) Uani d . 1 . . N
N2 0.5037(4) 0.1459(3) 0.1754(4) 0.0777(18) Uani d . 1 . . N
N3 0.9340(3) 0.6683(3) 0.4251(3) 0.0504(12) Uani d . 1 . . N
N4 0.5950(3) 0.3318(3) 0.2457(3) 0.0551(12) Uani d . 1 . . N
O1 0.7106(4) 0.2156(2) -0.1382(3) 0.0925(14) Uani d . 1 . . O
O2 0.4498(4) 0.0286(3) 0.2824(3) 0.0985(15) Uani d . 1 . . O
C1 0.6706(4) 0.2426(5) -0.0646(4) 0.0614(15) Uani d . 1 . . C
C2 0.4759(5) 0.0879(4) 0.2292(4) 0.0619(17) Uani d . 1 . . C
C3 0.5432(5) 0.3446(4) 0.3318(4) 0.0706(17) Uani d . 1 . . C
H3 0.4856 0.3175 0.3348 0.106 Uiso calc R 1 . . H
C4 0.5716(4) 0.3957(4) 0.4155(4) 0.0681(18) Uani d . 1 . . C
H4 0.533 0.4046 0.4725 0.102 Uiso calc R 1 . . H
C5 0.6578(4) 0.4335(3) 0.4136(4) 0.0495(16) Uani d . 1 . . C
C6 0.7120(4) 0.4208(3) 0.3255(4) 0.0552(14) Uani d . 1 . . C
H6 0.7701 0.4468 0.3213 0.083 Uiso calc R 1 . . H
C7 0.6785(4) 0.3691(4) 0.2442(4) 0.0530(15) Uani d . 1 . . C
H7 0.7157 0.36 0.1861 0.08 Uiso calc R 1 . . H
C8 0.7858(4) 0.5598(3) 0.4812(4) 0.0493(14) Uani d . 1 . . C
C9 0.8671(4) 0.5578(4) 0.5379(4) 0.0578(17) Uani d . 1 . . C
H9 0.873 0.5197 0.5952 0.087 Uiso calc R 1 . . H
C10 0.9386(4) 0.6124(3) 0.5089(4) 0.0556(15) Uani d . 1 . . C
H10 0.9925 0.611 0.548 0.083 Uiso calc R 1 . . H
C11 0.8539(4) 0.6681(3) 0.3696(4) 0.0533(14) Uani d . 1 . . C
H11 0.8494 0.7055 0.3115 0.08 Uiso calc R 1 . . H
C12 0.7804(4) 0.6161(3) 0.3950(4) 0.0519(14) Uani d . 1 . . C
H12 0.7271 0.6182 0.3551 0.078 Uiso calc R 1 . . H



#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 N2 . 1.903(5) ?
Zn1 N1 . 1.920(5) ?
Zn1 N3 3_465 2.040(4) ?
Zn1 N4 . 2.046(4) ?
S1 C5 . 1.763(5) ?
S1 C8 . 1.769(6) ?
N1 C1 . 1.168(7) ?
N2 C2 . 1.173(7) ?
N3 C10 . 1.358(6) ?
N3 C11 . 1.365(6) ?
N3 Zn1 3_565 2.040(4) ?
N4 C7 . 1.335(6) ?
N4 C3 . 1.349(6) ?
O1 C1 . 1.178(7) ?
O2 C2 . 1.176(7) ?
C3 C4 . 1.376(6) ?
C3 H3 . 0.93 ?
C4 C5 . 1.373(7) ?
C4 H4 . 0.93 ?
C5 C6 . 1.390(7) ?
C6 C7 . 1.382(6) ?
C6 H6 . 0.93 ?
C7 H7 . 0.93 ?
C8 C9 . 1.389(7) ?
C8 C12 . 1.386(6) ?
C9 C10 . 1.369(7) ?
C9 H9 . 0.93 ?
C10 H10 . 0.93 ?
C11 C12 . 1.358(7) ?
C11 H11 . 0.93 ?
C12 H12 . 0.93 ?

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
N2 Zn1 N1 122.3(2) . . ?
N2 Zn1 N3 108.8(2) . 3_465 ?
N1 Zn1 N3 105.08(19) . 3_465 ?
N2 Zn1 N4 107.76(19) . . ?
N1 Zn1 N4 108.1(2) . . ?
N3 Zn1 N4 103.29(17) 3_465 . ?
C5 S1 C8 103.8(3) . . ?
C1 N1 Zn1 155.5(6) . . ?
C2 N2 Zn1 164.2(5) . . ?
C10 N3 C11 116.9(5) . . ?
C10 N3 Zn1 121.4(4) . 3_565 ?
C11 N3 Zn1 121.5(3) . 3_565 ?
C7 N4 C3 117.5(5) . . ?
C7 N4 Zn1 122.1(4) . . ?
C3 N4 Zn1 120.4(4) . . ?
N1 C1 O1 178.1(8) . . ?
O2 C2 N2 178.4(8) . . ?
N4 C3 C4 123.1(6) . . ?
N4 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C5 C4 C3 119.0(5) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 118.5(5) . . ?
C4 C5 S1 116.7(4) . . ?
C6 C5 S1 124.8(4) . . ?
C7 C6 C5 119.1(6) . . ?
C7 C6 H6 120.4 . . ?
C5 C6 H6 120.4 . . ?
N4 C7 C6 122.7(5) . . ?
N4 C7 H7 118.6 . . ?
C6 C7 H7 118.6 . . ?
C9 C8 C12 118.5(5) . . ?
C9 C8 S1 119.0(4) . . ?
C12 C8 S1 122.4(5) . . ?
C10 C9 C8 119.5(5) . . ?
C10 C9 H9 120.2 . . ?
C8 C9 H9 120.2 . . ?
N3 C10 C9 122.5(5) . . ?
N3 C10 H10 118.7 . . ?
C9 C10 H10 118.7 . . ?
C12 C11 N3 123.2(5) . . ?
C12 C11 H11 118.4 . . ?
N3 C11 H11 118.4 . . ?
C11 C12 C8 119.3(5) . . ?
C11 C12 H12 120.4 . . ?
C8 C12 H12 120.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
#Zn1 N1 C1 O1 -6E1(2) . . . . ?
#Zn1 N2 C2 O2 -13E1(3) . . . . ?
N2 Zn1 N1 C1 24.6(12) . . . . ?
N3 Zn1 N1 C1 -99.7(11) 3_465 . . . ?
N4 Zn1 N1 C1 150.5(11) . . . . ?
N1 Zn1 N2 C2 151.2(19) . . . . ?
N3 Zn1 N2 C2 -86.1(19) 3_465 . . . ?
N4 Zn1 N2 C2 25(2) . . . . ?
N2 Zn1 N4 C7 128.0(4) . . . . ?
N1 Zn1 N4 C7 -6.0(5) . . . . ?
N3 Zn1 N4 C7 -117.0(4) 3_465 . . . ?
N2 Zn1 N4 C3 -52.6(5) . . . . ?
N1 Zn1 N4 C3 173.4(4) . . . . ?
N3 Zn1 N4 C3 62.4(4) 3_465 . . . ?
C7 N4 C3 C4 1.8(8) . . . . ?
Zn1 N4 C3 C4 -177.6(4) . . . . ?
N4 C3 C4 C5 -2.2(9) . . . . ?
C3 C4 C5 C6 2.0(8) . . . . ?
C3 C4 C5 S1 -178.0(4) . . . . ?
C8 S1 C5 C4 -163.0(4) . . . . ?
C8 S1 C5 C6 17.0(5) . . . . ?
C4 C5 C6 C7 -1.5(8) . . . . ?
S1 C5 C6 C7 178.5(4) . . . . ?
C3 N4 C7 C6 -1.3(8) . . . . ?
Zn1 N4 C7 C6 178.1(4) . . . . ?
C5 C6 C7 N4 1.2(8) . . . . ?
C5 S1 C8 C9 -128.7(4) . . . . ?
C5 S1 C8 C12 54.6(5) . . . . ?
C12 C8 C9 C10 1.3(8) . . . . ?
S1 C8 C9 C10 -175.5(4) . . . . ?
C11 N3 C10 C9 -0.1(7) . . . . ?
Zn1 N3 C10 C9 -175.2(4) 3_565 . . . ?
C8 C9 C10 N3 -0.9(8) . . . . ?
C10 N3 C11 C12 0.7(7) . . . . ?
Zn1 N3 C11 C12 175.7(4) 3_565 . . . ?
N3 C11 C12 C8 -0.2(8) . . . . ?
C9 C8 C12 C11 -0.8(7) . . . . ?
S1 C8 C12 C11 175.9(4) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 885880'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_275febpsns

_audit_creation_date             2011-12-07T13:37:37-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#==============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'C22 H20 Fe N6 O2 S4'
_chemical_formula_moiety         'C22 H16 Fe N6 S4, 2(H2 O)'

_chemical_formula_weight         584.53

#==============================================================================

# CRYSTAL DATA

_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'


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

_cell_length_a                   17.001(6)
_cell_length_b                   10.288(4)
_cell_length_c                   16.629(6)
#_cell_angle_alpha                       89.99(4)
_cell_angle_alpha                90
_cell_angle_beta                 118.53(4)
#_cell_angle_gamma                       90.14(4)
_cell_angle_gamma                90
#_cell_volume                            2555.3(16)
_cell_volume                     2555.3(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1049
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.4
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    0.95
_exptl_absorpt_correction_type   none

#==============================================================================

# EXPERIMENTAL DATA

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_number            9614
_diffrn_reflns_av_R_equivalents  0.2777
_diffrn_reflns_av_unetI/netI     0.4306
_diffrn_reflns_theta_min         2.4
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_full        26.12
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measured_fraction_theta_full 0.98
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20

#==============================================================================

# STRUCTURE SOLUTION

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#==============================================================================

# REFINEMENT DATA

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_reflns_number_total             2490
_reflns_number_gt                564
_reflns_threshold_expression     >2σ(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.2429
_refine_ls_R_factor_gt           0.0446
_refine_ls_wR_factor_ref         0.1051
_refine_ls_goodness_of_fit_ref   0.625
_refine_ls_restrained_S_all      0.625
_refine_ls_number_reflns         2490
_refine_ls_number_parameters     174
_refine_ls_number_restraints     3
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0155P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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'

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'

#==============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.5 0.16206(18) 0.75 0.0436(5) Uani d S 1 . . Fe
S1 0.65336(13) 0.6637(2) 1.05256(13) 0.0530(6) Uani d . 1 . . S
S3 0.2054(12) 0.1300(19) 0.7264(13) 0.138(7) Uani d P 0.5 . . S
S3' 0.2246(12) 0.0762(16) 0.7555(13) 0.090(4) Uani d P 0.5 . . S
N1 0.5544(4) 0.3201(7) 0.8541(4) 0.0429(18) Uani d . 1 . . N
N2 0.4326(4) 0.0088(6) 0.6431(5) 0.0467(18) Uani d . 1 . . N
N3 0.3830(4) 0.1581(7) 0.7627(4) 0.0523(17) Uani d . 1 . . N
C3 0.3141(6) 0.1338(8) 0.7550(5) 0.062(3) Uani d . 1 . . C
C11 0.6415(5) 0.3339(8) 0.9140(5) 0.061(2) Uani d . 1 . . C
H11 0.6815 0.2715 0.915 0.092 Uiso calc R 1 . . H
C12 0.4288(5) 0.0167(7) 0.5627(6) 0.054(2) Uani d . 1 . . C
H12 0.4452 0.0946 0.5464 0.081 Uiso calc R 1 . . H
C21 0.6742(5) 0.4369(7) 0.9741(5) 0.052(2) Uani d . 1 . . C
H21 0.7351 0.4427 1.0149 0.078 Uiso calc R 1 . . H
C22 0.4014(5) -0.0864(8) 0.5000(6) 0.054(2) Uani d . 1 . . C
H22 0.3978 -0.076 0.4428 0.082 Uiso calc R 1 . . H
C31 0.6166(5) 0.5317(7) 0.9740(5) 0.039(2) Uani d . 1 . . C
C32 0.3797(5) -0.2050(7) 0.5252(6) 0.039(2) Uani d . 1 . . C
C41 0.5254(5) 0.5151(7) 0.9128(5) 0.048(2) Uani d . 1 . . C
H41 0.4836 0.5747 0.9111 0.071 Uiso calc R 1 . . H
C42 0.3784(5) -0.2075(7) 0.6081(5) 0.044(2) Uani d . 1 . . C
H42 0.3594 -0.2822 0.6253 0.066 Uiso calc R 1 . . H
C51 0.4984(5) 0.4089(7) 0.8548(5) 0.048(2) Uani d . 1 . . C
H51 0.4377 0.3993 0.8142 0.071 Uiso calc R 1 . . H
C52 0.4050(5) -0.1011(7) 0.6651(5) 0.048(2) Uani d . 1 . . C
H52 0.4037 -0.1055 0.7203 0.072 Uiso calc R 1 . . H
O1 0.149(3) 0.332(6) 0.629(3) 0.65(2) Uani d D 1 . . O
H1O1 0.20(2) 0.35(9) 0.66(4) 0.98 Uiso d D 1 . . H
H2O1 0.14(4) 0.28(7) 0.66(4) 0.98 Uiso d D 1 . . H



#==============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
#O1 H1O1 . 0.850(10) ?
#O1 H2O1 . 0.850(5) ?
Fe1 N3 . 2.099(6) ?
Fe1 N3 2_656 2.099(6) ?
Fe1 N1 . 2.227(7) ?
Fe1 N1 2_656 2.230(7) ?
Fe1 N2 . 2.238(7) ?
Fe1 N2 2_656 2.241(7) ?
S1 C32 2_666 1.766(8) ?
S1 C31 . 1.777(8) ?
S3 S3' . 0.71(2) ?
S3 C3 . 1.67(2) ?
S3' C3 . 1.64(2) ?
N2 C12 . 1.311(9) ?
N2 C52 . 1.339(8) ?
N1 C51 . 1.325(8) ?
N1 C11 . 1.341(8) ?
C22 C32 . 1.395(9) ?
C22 C12 . 1.400(10) ?
C22 H22 . 0.93 ?
C31 C21 . 1.382(9) ?
C31 C41 . 1.401(8) ?
C21 C11 . 1.378(9) ?
C21 H21 . 0.93 ?
C12 H12 . 0.93 ?
C42 C52 . 1.375(8) ?
C42 C32 . 1.390(9) ?
C42 H42 . 0.93 ?
C32 S1 2_646 1.765(8) ?
C52 H52 . 0.93 ?
C11 H11 . 0.93 ?
C41 C51 . 1.381(9) ?
C41 H41 . 0.93 ?
C3 N3 . 1.142(8) ?
C51 H51 . 0.93 ?
O1 H1O1 . 0.8(8) ?
O1 H2O1 . 0.8(5) ?

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
#S3' C3 S3 24.6(8) . . ?
#H1O1 O1 H2O1 107.3(9) . . ?
N3 Fe1 N3 177.8(4) . 2_656 ?
N3 Fe1 N1 89.7(2) . . ?
N3 Fe1 N1 91.9(2) 2_656 . ?
N3 Fe1 N1 91.7(2) . 2_656 ?
N3 Fe1 N1 89.9(2) 2_656 2_656 ?
N1 Fe1 N1 86.3(3) . 2_656 ?
N3 Fe1 N2 85.3(2) . . ?
N3 Fe1 N2 93.2(3) 2_656 . ?
N1 Fe1 N2 174.6(2) . . ?
N1 Fe1 N2 91.8(2) 2_656 . ?
N3 Fe1 N2 93.4(3) . 2_656 ?
N3 Fe1 N2 85.1(2) 2_656 2_656 ?
N1 Fe1 N2 91.8(2) . 2_656 ?
N1 Fe1 N2 174.6(2) 2_656 2_656 ?
N2 Fe1 N2 90.5(4) . 2_656 ?
C32 S1 C31 99.7(3) 2_666 . ?
S3' S3 C3 75(3) . . ?
S3 S3' C3 81(3) . . ?
C12 N2 C52 118.6(7) . . ?
C12 N2 Fe1 121.6(6) . . ?
C52 N2 Fe1 119.3(6) . . ?
C51 N1 C11 117.7(7) . . ?
C51 N1 Fe1 118.6(5) . . ?
C11 N1 Fe1 123.7(6) . . ?
C32 C22 C12 118.7(8) . . ?
C32 C22 H22 120.7 . . ?
C12 C22 H22 120.7 . . ?
C21 C31 C41 117.0(7) . . ?
C21 C31 S1 122.6(6) . . ?
C41 C31 S1 120.2(6) . . ?
C11 C21 C31 120.2(7) . . ?
C11 C21 H21 119.9 . . ?
C31 C21 H21 119.9 . . ?
N2 C12 C22 123.3(8) . . ?
N2 C12 H12 118.3 . . ?
C22 C12 H12 118.3 . . ?
C52 C42 C32 121.0(7) . . ?
C52 C42 H42 119.5 . . ?
C32 C42 H42 119.5 . . ?
C42 C32 C22 116.4(7) . . ?
C42 C32 S1 124.3(6) . 2_646 ?
C22 C32 S1 119.1(7) . 2_646 ?
N2 C52 C42 121.6(7) . . ?
N2 C52 H52 119.2 . . ?
C42 C52 H52 119.2 . . ?
N1 C11 C21 122.6(8) . . ?
N1 C11 H11 118.7 . . ?
C21 C11 H11 118.7 . . ?
C51 C41 C31 119.0(7) . . ?
C51 C41 H41 120.5 . . ?
C31 C41 H41 120.5 . . ?
N3 C3 S3' 169.6(10) . . ?
N3 C3 S3 165.8(10) . . ?
C3 N3 Fe1 164.2(7) . . ?
N1 C51 C41 123.5(7) . . ?
N1 C51 H51 118.2 . . ?
C41 C51 H51 118.2 . . ?
H1O1 O1 H2O1 103.00 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
#N1 Fe1 N2 C12 109(3) . . . . ?
#N1 Fe1 N2 C52 -79(3) . . . . ?
#N2 Fe1 N1 C51 -15(3) . . . . ?
#N2 Fe1 N1 C11 168(3) . . . . ?
#N3 Fe1 N3 C3 -43(3) 2_656 . . . ?
N3 Fe1 N2 C12 131.3(6) . . . . ?
N3 Fe1 N2 C12 -50.2(6) 2_656 . . . ?
N1 Fe1 N2 C12 39.8(6) 2_656 . . . ?
N2 Fe1 N2 C12 -135.3(7) 2_656 . . . ?
N3 Fe1 N2 C52 -56.9(6) . . . . ?
N3 Fe1 N2 C52 121.5(6) 2_656 . . . ?
N1 Fe1 N2 C52 -148.5(6) 2_656 . . . ?
N2 Fe1 N2 C52 36.4(5) 2_656 . . . ?
N3 Fe1 N1 C51 -36.5(6) . . . . ?
N3 Fe1 N1 C51 145.0(6) 2_656 . . . ?
N1 Fe1 N1 C51 55.2(5) 2_656 . . . ?
N2 Fe1 N1 C51 -129.8(6) 2_656 . . . ?
N3 Fe1 N1 C11 146.5(6) . . . . ?
N3 Fe1 N1 C11 -32.0(7) 2_656 . . . ?
N1 Fe1 N1 C11 -121.8(7) 2_656 . . . ?
N2 Fe1 N1 C11 53.1(6) 2_656 . . . ?
C32 S1 C31 C21 121.1(7) 2_666 . . . ?
C32 S1 C31 C41 -63.4(7) 2_666 . . . ?
C41 C31 C21 C11 1.8(12) . . . . ?
S1 C31 C21 C11 177.5(6) . . . . ?
C52 N2 C12 C22 -3.2(12) . . . . ?
Fe1 N2 C12 C22 168.6(6) . . . . ?
C32 C22 C12 N2 -2.2(12) . . . . ?
C52 C42 C32 C22 -5.5(11) . . . . ?
C52 C42 C32 S1 -179.8(6) . . . 2_646 ?
C12 C22 C32 C42 6.3(11) . . . . ?
C12 C22 C32 S1 -179.1(6) . . . 2_646 ?
C12 N2 C52 C42 4.2(11) . . . . ?
Fe1 N2 C52 C42 -167.8(5) . . . . ?
C32 C42 C52 N2 0.3(11) . . . . ?
C51 N1 C11 C21 -1.1(12) . . . . ?
Fe1 N1 C11 C21 176.0(6) . . . . ?
C31 C21 C11 N1 -0.4(13) . . . . ?
C21 C31 C41 C51 -1.9(11) . . . . ?
S1 C31 C41 C51 -177.6(6) . . . . ?
S3 S3' C3 N3 -177(5) . . . . ?
S3' S3 C3 N3 178(3) . . . . ?
S3' C3 N3 Fe1 77(7) . . . . ?
S3 C3 N3 Fe1 -98(5) . . . . ?
N1 Fe1 N3 C3 -179(3) . . . . ?
N1 Fe1 N3 C3 94(3) 2_656 . . . ?
N2 Fe1 N3 C3 3(3) . . . . ?
N2 Fe1 N3 C3 -88(3) 2_656 . . . ?
C11 N1 C51 C41 1.0(11) . . . . ?
Fe1 N1 C51 C41 -176.2(6) . . . . ?
C31 C41 C51 N1 0.5(11) . . . . ?

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
#O1 H1O1 S3' 0.850(10) 2.7(8) 3.26(7) 13E1(9) 4_556
#O1 H2O1 S3 0.850(5) 1.9(7) 2.52(4) 13E1(7) .
O1 H1O1 S3' 0.8(8) 2.7(8) 3.26(7) 130(9) 4_556
O1 H2O1 S3 0.8(5) 1.9(7) 2.52(4) 132(7) .

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_database_code_depnum_ccdc_archive 'CCDC 996526'
