# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 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
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#  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.
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data_100

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '[Zn{MnN(CN)4(OH2)}](H2O)2(CH3OH)'
_chemical_formula_sum            'C5 H10 Mn N5 O4 Zn'
_chemical_formula_weight         324.49

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'
Mn Mn 0.3368 0.7283 '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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/m m c'
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_Int_Tables_number      131

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

_cell_length_a                   7.51110(10)
_cell_length_b                   7.51110(10)
_cell_length_c                   13.4593(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     759.33(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5377
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      29.35

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             324
_exptl_absorpt_coefficient_mu    2.416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6985
_exptl_absorpt_correction_T_max  0.8302
_exptl_absorpt_process_details   
;
 CrysAlisPro, Agilent Technologies
 Version 1.171.35.21
;

_diffrn_crystal_treatment        
;
attached with Exxon Paratone N, to a short length 
of fibre supported on a thin piece of copper wire 
inserted in a copper mounting pin.  The crystal was 
quenched in a cold nitrogen gas stream from an 
Oxford Cryosystems Cryostream. 
;

_exptl_special_details           
;  
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean 10.5861
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11832
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0117
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         4.89
_diffrn_reflns_theta_max         26.34
_reflns_number_total             469
_reflns_number_gt                451
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;

_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^)+(0.0667P)^2^+1.3721P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         469
_refine_ls_number_parameters     27
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1233
_refine_ls_wR_factor_gt          0.1218
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_restrained_S_all      1.109
_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
Zn1 Zn 0.5000 0.5000 0.2500 0.0312(4) Uani 1 8 d S . .
Mn1 Mn 0.0000 0.4384(3) 0.0000 0.0351(6) Uani 0.50 4 d SP . .
N2 N 0.0000 0.221(5) 0.0000 0.040(5) Uani 0.50 4 d SP . .
O1 O 0.0000 0.731(3) 0.0000 0.040(5) Uani 0.50 4 d SP . .
C1 C 0.1861(7) 0.4683(7) 0.1030(4) 0.0319(13) Uiso 0.50 1 d P . .
N1 N 0.2912(5) 0.4766(9) 0.1628(3) 0.0337(11) Uiso 0.50 1 d P . .
O11 O 0.0000 0.177(10) 0.224(7) 0.36(4) Uiso 0.25 2 d SPD . .
H11 H -0.0395 0.1879 0.1660 0.547 Uiso 0.125 1 calc PR . .
C11 C 0.0000 0.0000 0.2500 0.36(4) Uiso 1 8 d SD . .
H11A H 0.1159 -0.0525 0.2340 0.541 Uiso 0.125 1 calc PR . .
H11B H -0.0936 -0.0624 0.2131 0.541 Uiso 0.125 1 calc PR . .
H11C H -0.0224 -0.0113 0.3215 0.541 Uiso 0.125 1 calc PR . .
O21 O 0.0000 0.591(4) 0.407(3) 0.34(2) Uiso 0.50 2 d SP . .

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
Zn1 0.0386(5) 0.0386(5) 0.0165(5) 0.000 0.000 0.000
Mn1 0.0295(9) 0.0520(14) 0.0237(8) 0.000 0.000 0.000
N2 0.047(3) 0.015(15) 0.056(3) 0.000 0.000 0.000
O1 0.047(3) 0.015(15) 0.056(3) 0.000 0.000 0.000

_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 N1 1.967(4) 8_665 ?
Zn1 N1 1.967(4) . ?
Zn1 N1 1.967(4) 13_565 ?
Zn1 N1 1.967(4) 11_566 ?
Zn1 N1 1.967(4) 2_665 ?
Zn1 N1 1.967(4) 14_655 ?
Zn1 N1 1.967(4) 12_656 ?
Zn1 N1 1.967(4) 7 ?
Mn1 N2 1.64(3) . ?
Mn1 C1 1.981(5) . ?
Mn1 C1 1.981(5) 5 ?
Mn1 C1 1.981(5) 10 ?
Mn1 C1 1.981(5) 14 ?
Mn1 O1 2.20(2) . ?
C1 N1 1.129(6) . ?
O11 C11 1.37(7) . ?
O21 O21 1.37(7) 2_565 ?

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
N1 Zn1 N1 119.9(3) 8_665 . ?
N1 Zn1 N1 110.87(12) 8_665 13_565 ?
N1 Zn1 N1 10.2(4) . 13_565 ?
N1 Zn1 N1 10.2(4) 8_665 11_566 ?
N1 Zn1 N1 110.87(12) . 11_566 ?
N1 Zn1 N1 102.3(3) 13_565 11_566 ?
N1 Zn1 N1 102.3(3) 8_665 2_665 ?
N1 Zn1 N1 106.7(2) . 2_665 ?
N1 Zn1 N1 105.8(2) 13_565 2_665 ?
N1 Zn1 N1 110.87(12) 11_566 2_665 ?
N1 Zn1 N1 110.87(12) 8_665 14_655 ?
N1 Zn1 N1 105.8(2) . 14_655 ?
N1 Zn1 N1 106.7(2) 13_565 14_655 ?
N1 Zn1 N1 119.9(4) 11_566 14_655 ?
N1 Zn1 N1 10.2(4) 2_665 14_655 ?
N1 Zn1 N1 105.8(2) 8_665 12_656 ?
N1 Zn1 N1 110.87(12) . 12_656 ?
N1 Zn1 N1 119.9(4) 13_565 12_656 ?
N1 Zn1 N1 106.7(2) 11_566 12_656 ?
N1 Zn1 N1 110.87(12) 2_665 12_656 ?
N1 Zn1 N1 102.3(3) 14_655 12_656 ?
N1 Zn1 N1 106.7(2) 8_665 7 ?
N1 Zn1 N1 102.3(3) . 7 ?
N1 Zn1 N1 110.87(12) 13_565 7 ?
N1 Zn1 N1 105.8(2) 11_566 7 ?
N1 Zn1 N1 119.9(3) 2_665 7 ?
N1 Zn1 N1 110.87(12) 14_655 7 ?
N1 Zn1 N1 10.2(4) 12_656 7 ?
N2 Mn1 C1 96.50(17) . . ?
N2 Mn1 C1 96.50(17) . 5 ?
C1 Mn1 C1 167.0(3) . 5 ?
N2 Mn1 C1 96.50(17) . 10 ?
C1 Mn1 C1 88.8(3) . 10 ?
C1 Mn1 C1 89.8(3) 5 10 ?
N2 Mn1 C1 96.50(17) . 14 ?
C1 Mn1 C1 89.8(3) . 14 ?
C1 Mn1 C1 88.8(3) 5 14 ?
C1 Mn1 C1 167.0(3) 10 14 ?
N2 Mn1 O1 180.000(3) . . ?
C1 Mn1 O1 83.50(17) . . ?
C1 Mn1 O1 83.50(17) 5 . ?
C1 Mn1 O1 83.50(17) 10 . ?
C1 Mn1 O1 83.50(17) 14 . ?
N1 C1 Mn1 176.6(6) . . ?
C1 N1 Zn1 171.1(4) . . ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        29.35
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         1.081
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.087
_database_code_depnum_ccdc_archive 'CCDC 933557'