# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_bn_nicfeni
_database_code_depnum_ccdc_archive 'CCDC 1054375'
_audit_update_record             
;
2015-03-17 deposited with the CCDC.
2015-06-09 downloaded from the CCDC.
;

_audit_creation_date             2015-03-17T14:34:24-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
'hydronium catena(bis(2-cyanido)-tetracyanido-(1,4,8,11-tetraazacyclotetradecane)-nickel(III)-iron(II)) pentahydrate'
_chemical_formula_moiety         'C16 H37 Fe N10 Ni O6'
_chemical_formula_sum            'C16 H37 Fe N10 Ni O6'
_chemical_formula_weight         579.8

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/m'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_Int_Tables_number      12
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.8630(4)
_cell_length_b                   12.5020(4)
_cell_length_c                   10.0930(4)
_cell_angle_alpha                90
_cell_angle_beta                 133.020(2)
_cell_angle_gamma                90
_cell_volume                     1278.92(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2829
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      27.485

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_F_000             610
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_type   none
_shelx_estimated_absorpt_T_min   0.687
_shelx_estimated_absorpt_T_max   0.935

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_detector_area_resol_mean 9
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_ub_11      -0.0239727
_diffrn_orient_matrix_ub_12      0.0604579
_diffrn_orient_matrix_ub_13      0.0968043
_diffrn_orient_matrix_ub_21      -0.12517
_diffrn_orient_matrix_ub_22      -0.0602596
_diffrn_orient_matrix_ub_23      -0.0917388
_diffrn_orient_matrix_ub_31      0.003284
_diffrn_orient_matrix_ub_32      -0.094036
_diffrn_orient_matrix_ub_33      0.0240376
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_number            5355
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.259
_diffrn_reflns_theta_max         27.539
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_reflns_number_total             1530
_reflns_number_gt                1116
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0395P)²+0.3742P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0047(8)
_refine_ls_number_reflns         1530
_refine_ls_number_parameters     105
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0808
_refine_ls_wR_factor_gt          0.0736
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.31
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.064

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002 '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'
Fe Fe 0.346 0.844 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.339 1.112 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 1 0.5 1 0.02284(19) Uani 1 d . .
Fe1 Fe 0.5 0.5 0.5 0.02235(19) Uani 1 d . .
C11 C 0.5 0.3473(3) 0.5 0.0312(8) Uani 1 d . .
N11 N 0.5 0.2549(3) 0.5 0.0525(9) Uani 1 d . .
C12 C 0.6840(3) 0.5 0.7162(4) 0.0251(7) Uani 1 d . .
N12 N 0.7962(3) 0.5 0.8422(4) 0.0297(6) Uani 1 d . .
C13 C 0.4565(3) 0.5 0.6419(4) 0.0285(7) Uani 1 d . .
N13 N 0.4292(3) 0.5 0.7279(4) 0.0449(8) Uani 1 d . .
N21 N 1.0190(2) 0.61530(18) 1.1498(3) 0.0341(5) Uani 1 d . .
C22 C 1.1143(3) 0.6005(3) 1.3496(3) 0.0477(8) Uani 1 d . .
H22A H 1.1089 0.6614 1.4039 0.057 Uiso 1 calc . .
H22B H 1.2032 0.5979 1.3973 0.057 Uiso 1 calc . .
C23 C 1.0877(4) 0.5 1.4011(5) 0.0546(13) Uani 1 d . .
H23A H 0.9961 0.5 1.3432 0.066 Uiso 1 calc . .
H23B H 1.142 0.5 1.5311 0.066 Uiso 1 calc . .
C24 C 1.0435(3) 0.7165(2) 1.1001(4) 0.0496(8) Uani 1 d . .
H24A H 1.1353 0.7209 1.1596 0.06 Uiso 1 calc . .
H24B H 1.0234 0.7773 1.1374 0.06 Uiso 1 calc . .
O1 O 0.6720(3) 0.5 1.1162(4) 0.0586(9) Uani 1 d . .
O2 O 0.8049(2) 0.6754(2) 1.1341(3) 0.0551(6) Uani 1 d . .
H21 H 0.946(3) 0.616(3) 1.115(5) 0.066 Uiso 1 d . .
H1B H 0.635(4) 0.5 1.167(6) 0.083 Uiso 1 d . .
H1A H 0.602(4) 0.5 0.993(3) 0.083 Uiso 1 d . .
H2A H 0.852(3) 0.707(3) 1.245(3) 0.083 Uiso 1 d . .
H2B H 0.754(3) 0.624(2) 1.125(5) 0.083 Uiso 1 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ni2 N21 1.972(2) 5_767 ?
Ni2 N21 1.972(2) 6_565 ?
Ni2 N21 1.972(2) 2_757 ?
Ni2 N21 1.972(2) . ?
Ni2 N12 2.092(3) . ?
Ni2 N12 2.092(3) 5_767 ?
Ni2 H21 2.28(3) . ?
Fe1 C13 1.895(3) 5_666 ?
Fe1 C13 1.895(3) . ?
Fe1 C11 1.909(4) . ?
Fe1 C11 1.909(4) 5_666 ?
Fe1 C12 1.916(3) 5_666 ?
Fe1 C12 1.916(3) . ?
C11 N11 1.155(5) . ?
C12 N12 1.157(4) . ?
C13 N13 1.160(4) . ?
N21 C24 1.482(4) . ?
N21 C22 1.487(3) . ?
N21 H21 0.82(4) . ?
C22 C23 1.499(4) . ?
C22 H22A 0.97 . ?
C22 H22B 0.97 . ?
C23 C22 1.499(4) 6_565 ?
C23 H23A 0.97 . ?
C23 H23B 0.97 . ?
C24 C24 1.488(6) 2_757 ?
C24 H24A 0.97 . ?
C24 H24B 0.97 . ?
O1 H1B 0.941(19) . ?
O1 H1A 0.915(19) . ?
O2 H2A 0.912(18) . ?
O2 H2B 0.909(18) . ?

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
N21 Ni2 N21 86.06(14) 5_767 6_565 ?
N21 Ni2 N21 93.94(14) 5_767 2_757 ?
N21 Ni2 N21 180 6_565 2_757 ?
N21 Ni2 N21 180.00(15) 5_767 . ?
N21 Ni2 N21 93.94(14) 6_565 . ?
N21 Ni2 N21 86.06(14) 2_757 . ?
N21 Ni2 N12 90.65(8) 5_767 . ?
N21 Ni2 N12 89.35(8) 6_565 . ?
N21 Ni2 N12 90.65(8) 2_757 . ?
N21 Ni2 N12 89.35(8) . . ?
N21 Ni2 N12 89.35(8) 5_767 5_767 ?
N21 Ni2 N12 90.65(8) 6_565 5_767 ?
N21 Ni2 N12 89.35(8) 2_757 5_767 ?
N21 Ni2 N12 90.65(8) . 5_767 ?
N12 Ni2 N12 180.00(11) . 5_767 ?
N21 Ni2 H21 159.5(9) 5_767 . ?
N21 Ni2 H21 89.6(9) 6_565 . ?
N21 Ni2 H21 90.4(9) 2_757 . ?
N21 Ni2 H21 20.5(9) . . ?
N12 Ni2 H21 69.3(9) . . ?
N12 Ni2 H21 110.7(9) 5_767 . ?
C13 Fe1 C13 180.00(14) 5_666 . ?
C13 Fe1 C11 90 5_666 . ?
C13 Fe1 C11 90.0000(10) . . ?
C13 Fe1 C11 90.0000(10) 5_666 5_666 ?
C13 Fe1 C11 90.0000(10) . 5_666 ?
C11 Fe1 C11 180 . 5_666 ?
C13 Fe1 C12 90.11(13) 5_666 5_666 ?
C13 Fe1 C12 89.89(13) . 5_666 ?
C11 Fe1 C12 90.000(2) . 5_666 ?
C11 Fe1 C12 90 5_666 5_666 ?
C13 Fe1 C12 89.89(13) 5_666 . ?
C13 Fe1 C12 90.11(13) . . ?
C11 Fe1 C12 90.0000(10) . . ?
C11 Fe1 C12 90.0000(10) 5_666 . ?
C12 Fe1 C12 180 5_666 . ?
N11 C11 Fe1 180 . . ?
N12 C12 Fe1 177.1(3) . . ?
C12 N12 Ni2 160.3(3) . . ?
N13 C13 Fe1 179.6(3) . . ?
C24 N21 C22 111.6(2) . . ?
C24 N21 Ni2 107.85(17) . . ?
C22 N21 Ni2 118.65(18) . . ?
C24 N21 H21 110(2) . . ?
C22 N21 H21 106(2) . . ?
Ni2 N21 H21 102(2) . . ?
N21 C22 C23 111.9(3) . . ?
N21 C22 H22A 109.2 . . ?
C23 C22 H22A 109.2 . . ?
N21 C22 H22B 109.2 . . ?
C23 C22 H22B 109.2 . . ?
H22A C22 H22B 107.9 . . ?
C22 C23 C22 113.9(3) . 6_565 ?
C22 C23 H23A 108.8 . . ?
C22 C23 H23A 108.8 6_565 . ?
C22 C23 H23B 108.8 . . ?
C22 C23 H23B 108.8 6_565 . ?
H23A C23 H23B 107.7 . . ?
N21 C24 C24 107.40(18) . 2_757 ?
N21 C24 H24A 110.2 . . ?
C24 C24 H24A 110.2 2_757 . ?
N21 C24 H24B 110.2 . . ?
C24 C24 H24B 110.2 2_757 . ?
H24A C24 H24B 108.5 . . ?
H1B O1 H1A 106(3) . . ?
H2A O2 H2B 107(3) . . ?

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
C24 N21 C22 C23 178.3(2) . . . . ?
Ni2 N21 C22 C23 -55.4(3) . . . . ?
N21 C22 C23 C22 68.1(4) . . . 6_565 ?
C22 N21 C24 C24 172.2(3) . . . 2_757 ?
Ni2 N21 C24 C24 40.2(3) . . . 2_757 ?

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
N21 H21 O2 0.82(4) 2.22(4) 2.960(3) 151(3) .
O1 H1B N13 0.941(19) 1.791(19) 2.731(4) 178(4) 5_667
O1 H1A N13 0.915(19) 2.04(2) 2.948(4) 171(4) .
O2 H2A N11 0.912(18) 2.00(2) 2.883(3) 163(4) 3_556
O2 H2B O1 0.909(18) 1.890(19) 2.789(3) 170(4) .

_shelxl_version_number           2012-9

