# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_fac-nil1_schmidt20
_database_code_depnum_ccdc_archive 'CCDC 1008832'
_audit_update_record             
;
2014-06-17 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;

_audit_creation_date             2014-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;[6-methyl-6-(pyridin-2-yl)-1,4-bis(pyridin-2-ylmethyl)-
        1,4-diazepane]nickel(II) perchlorate--methanol(1/1)
;
_chemical_formula_iupac          '[Ni (C23 H27 N5)](Cl O4)2.C H3 O H'
_chemical_formula_moiety         'C23 H27 N5 Ni 2+, 2(Cl O4 1-), C H4 O'
_chemical_formula_sum            'C24 H31 Cl2 N5 Ni O9'
_chemical_formula_weight         663.15

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

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.6432(6)
_cell_length_b                   15.5442(13)
_cell_length_c                   19.6209(15)
_cell_angle_alpha                90
_cell_angle_beta                 108.042(5)
_cell_angle_gamma                90
_cell_volume                     2796.5(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1629
_cell_measurement_theta_min      3.384
_cell_measurement_theta_max      32.4831

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

_exptl_crystal_description       coloumn
_exptl_crystal_colour            'light violet'
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method 
'precipitation: wet methanol, diethyl ether, vapour diffusion, r.t., 1 d'

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

_exptl_absorpt_coefficient_mu    0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.91485
_exptl_absorpt_correction_T_max  1.00000

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

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0864
_diffrn_reflns_av_unetI/netI     0.1405
_diffrn_reflns_number            11741
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             5481
_reflns_number_gt                3561
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

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

_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.
 One perchlorate moiety (at Cl2) exhibits strong rotational disorder and was
 modelled in two discrete positions using SAME and tight DELU as well as ISOR
 restraints (for the oxygen atoms). S.o.f. refined to 57(3) % and 43(3) %,
 respectively.
;
_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)+(0.0232P)²+1.9037P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5481
_refine_ls_number_parameters     409
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0659
_refine_ls_wR_factor_ref         0.1309
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.109

#----------------------------------------------------------------------------#
#                   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 0.0033 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'
Cl Cl 0.1484 0.1585 '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 0.006 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.74266(6) 0.74355(4) 0.77818(3) 0.01810(17) Uani 1 1 d . . .
N1 N 0.7900(4) 0.6808(3) 0.8785(2) 0.0204(9) Uani 1 1 d . A .
N4 N 0.9659(4) 0.7480(3) 0.8140(2) 0.0198(9) Uani 1 1 d . A .
N10 N 0.6916(4) 0.8500(3) 0.8237(2) 0.0224(10) Uani 1 1 d . A .
N17 N 0.5458(4) 0.6847(3) 0.7592(2) 0.0207(9) Uani 1 1 d . A .
N24 N 0.7715(4) 0.8089(3) 0.6917(2) 0.0198(9) Uani 1 1 d . A .
C2 C 0.8907(5) 0.6148(3) 0.8644(3) 0.0264(12) Uani 1 1 d . . .
H2A H 0.838 0.5783 0.8232 0.032 Uiso 1 1 calc R A .
H2B H 0.9297 0.5775 0.9069 0.032 Uiso 1 1 calc R . .
C3 C 1.0156(5) 0.6627(3) 0.8479(3) 0.0243(12) Uani 1 1 d . A .
H3A H 1.0966 0.6713 0.8929 0.029 Uiso 1 1 calc R . .
H3B H 1.0526 0.6274 0.8152 0.029 Uiso 1 1 calc R . .
C5 C 1.0055(5) 0.8185(4) 0.8676(3) 0.0299(13) Uani 1 1 d . . .
H5A H 0.9948 0.8738 0.8415 0.036 Uiso 1 1 calc R A .
H5B H 1.1097 0.8121 0.8956 0.036 Uiso 1 1 calc R . .
C6 C 0.9153(5) 0.8236(3) 0.9211(2) 0.0226(11) Uani 1 1 d . A .
C7 C 0.8706(5) 0.7335(3) 0.9415(3) 0.0242(12) Uani 1 1 d . . .
H7A H 0.9596 0.702 0.969 0.029 Uiso 1 1 calc R A .
H7B H 0.8089 0.741 0.973 0.029 Uiso 1 1 calc R . .
C8 C 1.0151(6) 0.8654(4) 0.9894(3) 0.0393(15) Uani 1 1 d . . .
H8A H 1.0445 0.9226 0.978 0.059 Uiso 1 1 calc R A .
H8B H 1.102 0.8296 1.0091 0.059 Uiso 1 1 calc R . .
H8C H 0.9628 0.8707 1.0248 0.059 Uiso 1 1 calc R . .
C9 C 0.7759(5) 0.8750(3) 0.8890(3) 0.0252(12) Uani 1 1 d . . .
C11 C 0.5614(5) 0.8899(3) 0.7926(3) 0.0260(12) Uani 1 1 d . . .
H11 H 0.5039 0.8731 0.7458 0.031 Uiso 1 1 calc R A .
C12 C 0.5118(6) 0.9534(4) 0.8273(3) 0.0357(15) Uani 1 1 d . A .
H12 H 0.4203 0.98 0.8049 0.043 Uiso 1 1 calc R . .
C13 C 0.5943(6) 0.9785(4) 0.8940(3) 0.0399(15) Uani 1 1 d . . .
H13 H 0.5604 1.0225 0.9184 0.048 Uiso 1 1 calc R A .
C14 C 0.7279(6) 0.9395(4) 0.9260(3) 0.0365(14) Uani 1 1 d . A .
H14 H 0.7862 0.9564 0.9726 0.044 Uiso 1 1 calc R . .
C15 C 0.6542(5) 0.6422(4) 0.8848(3) 0.0259(12) Uani 1 1 d . . .
H15A H 0.6202 0.6767 0.919 0.031 Uiso 1 1 calc R A .
H15B H 0.6757 0.5835 0.9047 0.031 Uiso 1 1 calc R . .
C16 C 0.5347(5) 0.6375(3) 0.8152(3) 0.0216(11) Uani 1 1 d . A .
C18 C 0.4314(5) 0.6867(3) 0.6989(2) 0.0201(11) Uani 1 1 d . . .
H18 H 0.4384 0.7206 0.6598 0.024 Uiso 1 1 calc R A .
C19 C 0.3040(5) 0.6413(4) 0.6912(3) 0.0284(13) Uani 1 1 d . A .
H19 H 0.2248 0.6447 0.648 0.034 Uiso 1 1 calc R . .
C20 C 0.2944(5) 0.5911(4) 0.7475(3) 0.0330(14) Uani 1 1 d . . .
H20 H 0.2088 0.5587 0.7438 0.04 Uiso 1 1 calc R A .
C21 C 0.4105(5) 0.5888(3) 0.8089(3) 0.0266(12) Uani 1 1 d . A .
H21 H 0.4062 0.5535 0.8477 0.032 Uiso 1 1 calc R . .
C22 C 1.0212(5) 0.7672(3) 0.7533(3) 0.0235(12) Uani 1 1 d . . .
H22A H 1.0416 0.7127 0.7322 0.028 Uiso 1 1 calc R A .
H22B H 1.1138 0.7997 0.771 0.028 Uiso 1 1 calc R . .
C23 C 0.9123(5) 0.8192(3) 0.6964(3) 0.0205(11) Uani 1 1 d . A .
C25 C 0.6704(5) 0.8491(3) 0.6380(3) 0.0236(12) Uani 1 1 d . . .
H25 H 0.5704 0.8416 0.634 0.028 Uiso 1 1 calc R A .
C26 C 0.7055(5) 0.9008(3) 0.5887(3) 0.0269(12) Uani 1 1 d . A .
H26 H 0.6312 0.9281 0.5515 0.032 Uiso 1 1 calc R . .
C27 C 0.8513(5) 0.9121(3) 0.5944(3) 0.0290(13) Uani 1 1 d . . .
H27 H 0.8789 0.9478 0.5615 0.035 Uiso 1 1 calc R A .
C28 C 0.9554(5) 0.8706(4) 0.6489(3) 0.0295(13) Uani 1 1 d . A .
H28 H 1.0559 0.8771 0.6537 0.035 Uiso 1 1 calc R . .
Cl2 Cl 0.83626(14) 0.55912(11) 0.65967(8) 0.0391(4) Uani 1 1 d DU . .
O5A O 0.9350(19) 0.5072(11) 0.7160(6) 0.066(4) Uani 0.57(3) 1 d PDU A 1
O6A O 0.7441(18) 0.6082(10) 0.6900(10) 0.030(3) Uani 0.57(3) 1 d PDU A 1
O7A O 0.7543(17) 0.5055(9) 0.6026(6) 0.033(3) Uani 0.57(3) 1 d PDU A 1
O8A O 0.930(2) 0.6205(12) 0.6376(8) 0.067(4) Uani 0.57(3) 1 d PDU A 1
O5B O 0.865(3) 0.4859(9) 0.7137(7) 0.049(4) Uani 0.43(3) 1 d PDU A 2
O6B O 0.766(2) 0.6244(12) 0.6876(13) 0.028(4) Uani 0.43(3) 1 d PDU A 2
O7B O 0.734(2) 0.5282(14) 0.5938(9) 0.038(4) Uani 0.43(3) 1 d PDU A 2
O8B O 0.9694(11) 0.5782(17) 0.6511(8) 0.052(4) Uani 0.43(3) 1 d PDU A 2
Cl1 Cl 0.26272(12) 0.89571(9) 0.56003(7) 0.0259(3) Uani 1 1 d . . .
O1 O 0.3244(4) 0.9191(3) 0.6344(2) 0.0512(12) Uani 1 1 d . . .
O2 O 0.2503(4) 0.8045(3) 0.5551(2) 0.0520(12) Uani 1 1 d . . .
O3 O 0.1226(3) 0.9349(2) 0.53037(19) 0.0312(9) Uani 1 1 d . . .
O4 O 0.3560(4) 0.9243(3) 0.5204(2) 0.0626(15) Uani 1 1 d . . .
O9 O 0.4114(6) 0.7439(4) 0.9441(3) 0.0871(18) Uani 1 1 d . . .
H9 H 0.402 0.7018 0.9691 0.131 Uiso 1 1 d R . .
C1 C 0.4514(8) 0.8178(5) 0.9878(5) 0.077(3) Uani 1 1 d . . .
H1A H 0.3913 0.8215 1.0198 0.116 Uiso 1 1 calc R . .
H1B H 0.4362 0.8692 0.9575 0.116 Uiso 1 1 calc R . .
H1C H 0.5545 0.8138 1.0163 0.116 Uiso 1 1 calc R . .


#----------------------------------------------------------------------------#
#                   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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N10 2.012(4) . ?
Ni1 N17 2.035(4) . ?
Ni1 N4 2.049(4) . ?
Ni1 N24 2.069(4) . ?
Ni1 N1 2.115(4) . ?
Ni1 O6B 2.624(15) . ?
Ni1 O6A 2.726(13) . ?
N1 C15 1.480(5) . ?
N1 C7 1.486(6) . ?
N1 C2 1.497(6) . ?
N4 C22 1.477(6) . ?
N4 C5 1.484(6) . ?
N4 C3 1.494(6) . ?
N10 C9 1.345(6) . ?
N10 C11 1.363(6) . ?
N17 C18 1.345(6) . ?
N17 C16 1.352(6) . ?
N24 C23 1.342(5) . ?
N24 C25 1.347(6) . ?
C2 C3 1.533(6) . ?
C5 C6 1.560(6) . ?
C6 C9 1.523(7) . ?
C6 C8 1.531(7) . ?
C6 C7 1.554(7) . ?
C9 C14 1.398(7) . ?
C11 C12 1.368(7) . ?
C12 C13 1.361(8) . ?
C13 C14 1.386(8) . ?
C15 C16 1.491(7) . ?
C16 C21 1.389(6) . ?
C18 C19 1.383(6) . ?
C19 C20 1.380(7) . ?
C20 C21 1.367(7) . ?
C22 C23 1.509(6) . ?
C23 C28 1.386(7) . ?
C25 C26 1.377(7) . ?
C26 C27 1.387(6) . ?
C27 C28 1.379(7) . ?
Cl2 O8B 1.378(10) . ?
Cl2 O6B 1.422(11) . ?
Cl2 O7A 1.423(8) . ?
Cl2 O6A 1.434(9) . ?
Cl2 O7B 1.444(11) . ?
Cl2 O5A 1.459(8) . ?
Cl2 O8A 1.467(9) . ?
Cl2 O5B 1.522(10) . ?
Cl1 O2 1.424(4) . ?
Cl1 O4 1.429(4) . ?
Cl1 O3 1.431(3) . ?
Cl1 O1 1.441(4) . ?
O9 C1 1.413(9) . ?

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
N10 Ni1 N17 96.21(15) . . ?
N10 Ni1 N4 101.30(16) . . ?
N17 Ni1 N4 154.12(17) . . ?
N10 Ni1 N24 94.23(16) . . ?
N17 Ni1 N24 115.16(16) . . ?
N4 Ni1 N24 82.57(15) . . ?
N10 Ni1 N1 88.76(16) . . ?
N17 Ni1 N1 83.29(15) . . ?
N4 Ni1 N1 78.22(14) . . ?
N24 Ni1 N1 160.77(14) . . ?
N10 Ni1 O6B 164.7(5) . . ?
N17 Ni1 O6B 80.1(5) . . ?
N4 Ni1 O6B 87.4(5) . . ?
N24 Ni1 O6B 74.3(5) . . ?
N1 Ni1 O6B 105.4(5) . . ?
N10 Ni1 O6A 165.0(4) . . ?
N17 Ni1 O6A 74.0(4) . . ?
N4 Ni1 O6A 91.8(4) . . ?
N24 Ni1 O6A 80.2(4) . . ?
N1 Ni1 O6A 101.1(4) . . ?
O6B Ni1 O6A 6.9(7) . . ?
C15 N1 C7 113.7(4) . . ?
C15 N1 C2 112.3(4) . . ?
C7 N1 C2 109.2(4) . . ?
C15 N1 Ni1 108.9(3) . . ?
C7 N1 Ni1 115.3(3) . . ?
C2 N1 Ni1 96.3(3) . . ?
C22 N4 C5 110.1(4) . . ?
C22 N4 C3 113.1(4) . . ?
C5 N4 C3 111.3(4) . . ?
C22 N4 Ni1 109.5(3) . . ?
C5 N4 Ni1 106.2(3) . . ?
C3 N4 Ni1 106.3(3) . . ?
C9 N10 C11 119.7(4) . . ?
C9 N10 Ni1 120.1(3) . . ?
C11 N10 Ni1 119.6(3) . . ?
C18 N17 C16 118.5(4) . . ?
C18 N17 Ni1 128.0(3) . . ?
C16 N17 Ni1 113.5(3) . . ?
C23 N24 C25 118.1(4) . . ?
C23 N24 Ni1 113.1(3) . . ?
C25 N24 Ni1 128.3(3) . . ?
N1 C2 C3 107.7(4) . . ?
N4 C3 C2 111.1(4) . . ?
N4 C5 C6 116.2(4) . . ?
C9 C6 C8 112.0(4) . . ?
C9 C6 C7 107.5(4) . . ?
C8 C6 C7 107.8(4) . . ?
C9 C6 C5 110.7(4) . . ?
C8 C6 C5 106.3(4) . . ?
C7 C6 C5 112.6(4) . . ?
N1 C7 C6 113.4(4) . . ?
N10 C9 C14 120.2(5) . . ?
N10 C9 C6 116.0(4) . . ?
C14 C9 C6 123.6(5) . . ?
N10 C11 C12 121.4(5) . . ?
C13 C12 C11 119.7(5) . . ?
C12 C13 C14 119.7(5) . . ?
C13 C14 C9 119.2(6) . . ?
N1 C15 C16 113.3(4) . . ?
N17 C16 C21 120.4(5) . . ?
N17 C16 C15 119.0(4) . . ?
C21 C16 C15 120.6(4) . . ?
N17 C18 C19 122.9(5) . . ?
C20 C19 C18 118.6(5) . . ?
C21 C20 C19 118.7(5) . . ?
C20 C21 C16 120.9(5) . . ?
N4 C22 C23 111.3(4) . . ?
N24 C23 C28 122.0(5) . . ?
N24 C23 C22 116.4(4) . . ?
C28 C23 C22 121.4(4) . . ?
N24 C25 C26 122.9(4) . . ?
C25 C26 C27 118.7(5) . . ?
C28 C27 C26 118.7(5) . . ?
C27 C28 C23 119.5(5) . . ?
O8B Cl2 O6B 117.9(11) . . ?
O7A Cl2 O6A 112.0(9) . . ?
O8B Cl2 O7B 111.5(11) . . ?
O6B Cl2 O7B 107.8(11) . . ?
O7A Cl2 O5A 110.2(7) . . ?
O6A Cl2 O5A 108.8(9) . . ?
O7A Cl2 O8A 113.0(8) . . ?
O6A Cl2 O8A 107.0(8) . . ?
O5A Cl2 O8A 105.5(6) . . ?
O8B Cl2 O5B 105.8(7) . . ?
O6B Cl2 O5B 105.6(10) . . ?
O7B Cl2 O5B 107.5(9) . . ?
Cl2 O6A Ni1 143.1(11) . . ?
Cl2 O6B Ni1 156.3(15) . . ?
O2 Cl1 O4 109.0(3) . . ?
O2 Cl1 O3 110.3(2) . . ?
O4 Cl1 O3 108.7(2) . . ?
O2 Cl1 O1 108.7(3) . . ?
O4 Cl1 O1 109.9(3) . . ?
O3 Cl1 O1 110.2(2) . . ?

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
N10 Ni1 N1 C15 87.5(3) . . . . ?
N17 Ni1 N1 C15 -8.9(3) . . . . ?
N4 Ni1 N1 C15 -170.7(3) . . . . ?
N24 Ni1 N1 C15 -173.2(4) . . . . ?
O6B Ni1 N1 C15 -86.7(6) . . . . ?
O6A Ni1 N1 C15 -81.1(5) . . . . ?
N10 Ni1 N1 C7 -41.6(3) . . . . ?
N17 Ni1 N1 C7 -138.0(3) . . . . ?
N4 Ni1 N1 C7 60.2(3) . . . . ?
N24 Ni1 N1 C7 57.7(6) . . . . ?
O6B Ni1 N1 C7 144.2(6) . . . . ?
O6A Ni1 N1 C7 149.7(4) . . . . ?
N10 Ni1 N1 C2 -156.3(3) . . . . ?
N17 Ni1 N1 C2 107.3(3) . . . . ?
N4 Ni1 N1 C2 -54.5(3) . . . . ?
N24 Ni1 N1 C2 -57.0(6) . . . . ?
O6B Ni1 N1 C2 29.5(6) . . . . ?
O6A Ni1 N1 C2 35.1(4) . . . . ?
N10 Ni1 N4 C22 -110.5(3) . . . . ?
N17 Ni1 N4 C22 117.8(4) . . . . ?
N24 Ni1 N4 C22 -17.7(3) . . . . ?
N1 Ni1 N4 C22 163.2(4) . . . . ?
O6B Ni1 N4 C22 56.8(6) . . . . ?
O6A Ni1 N4 C22 62.2(5) . . . . ?
N10 Ni1 N4 C5 8.4(3) . . . . ?
N17 Ni1 N4 C5 -123.3(4) . . . . ?
N24 Ni1 N4 C5 101.2(3) . . . . ?
N1 Ni1 N4 C5 -78.0(3) . . . . ?
O6B Ni1 N4 C5 175.7(6) . . . . ?
O6A Ni1 N4 C5 -178.9(5) . . . . ?
N10 Ni1 N4 C3 127.0(3) . . . . ?
N17 Ni1 N4 C3 -4.7(5) . . . . ?
N24 Ni1 N4 C3 -140.2(3) . . . . ?
N1 Ni1 N4 C3 40.6(3) . . . . ?
O6B Ni1 N4 C3 -65.7(6) . . . . ?
O6A Ni1 N4 C3 -60.3(5) . . . . ?
N17 Ni1 N10 C9 125.9(3) . . . . ?
N4 Ni1 N10 C9 -35.0(4) . . . . ?
N24 Ni1 N10 C9 -118.2(4) . . . . ?
N1 Ni1 N10 C9 42.8(3) . . . . ?
O6B Ni1 N10 C9 -158.9(19) . . . . ?
O6A Ni1 N10 C9 174.3(15) . . . . ?
N17 Ni1 N10 C11 -45.2(4) . . . . ?
N4 Ni1 N10 C11 153.9(3) . . . . ?
N24 Ni1 N10 C11 70.7(4) . . . . ?
N1 Ni1 N10 C11 -128.3(4) . . . . ?
O6B Ni1 N10 C11 30(2) . . . . ?
O6A Ni1 N10 C11 3.2(16) . . . . ?
N10 Ni1 N17 C18 94.3(4) . . . . ?
N4 Ni1 N17 C18 -133.2(4) . . . . ?
N24 Ni1 N17 C18 -3.3(5) . . . . ?
N1 Ni1 N17 C18 -177.7(4) . . . . ?
O6B Ni1 N17 C18 -70.7(7) . . . . ?
O6A Ni1 N17 C18 -74.1(6) . . . . ?
N10 Ni1 N17 C16 -87.0(3) . . . . ?
N4 Ni1 N17 C16 45.6(5) . . . . ?
N24 Ni1 N17 C16 175.4(3) . . . . ?
N1 Ni1 N17 C16 1.1(3) . . . . ?
O6B Ni1 N17 C16 108.0(6) . . . . ?
O6A Ni1 N17 C16 104.7(5) . . . . ?
N10 Ni1 N24 C23 104.1(3) . . . . ?
N17 Ni1 N24 C23 -157.0(3) . . . . ?
N4 Ni1 N24 C23 3.2(3) . . . . ?
N1 Ni1 N24 C23 5.7(7) . . . . ?
O6B Ni1 N24 C23 -86.2(6) . . . . ?
O6A Ni1 N24 C23 -90.0(5) . . . . ?
N10 Ni1 N24 C25 -67.6(4) . . . . ?
N17 Ni1 N24 C25 31.3(5) . . . . ?
N4 Ni1 N24 C25 -168.4(5) . . . . ?
N1 Ni1 N24 C25 -166.0(5) . . . . ?
O6B Ni1 N24 C25 102.2(7) . . . . ?
O6A Ni1 N24 C25 98.4(6) . . . . ?
C15 N1 C2 C3 171.8(4) . . . . ?
C7 N1 C2 C3 -61.1(5) . . . . ?
Ni1 N1 C2 C3 58.4(4) . . . . ?
C22 N4 C3 C2 -137.2(4) . . . . ?
C5 N4 C3 C2 98.2(4) . . . . ?
Ni1 N4 C3 C2 -17.0(4) . . . . ?
N1 C2 C3 N4 -29.7(5) . . . . ?
C22 N4 C5 C6 160.8(4) . . . . ?
C3 N4 C5 C6 -72.9(5) . . . . ?
Ni1 N4 C5 C6 42.4(5) . . . . ?
N4 C5 C6 C9 -85.8(5) . . . . ?
N4 C5 C6 C8 152.4(4) . . . . ?
N4 C5 C6 C7 34.5(6) . . . . ?
C15 N1 C7 C6 -130.9(4) . . . . ?
C2 N1 C7 C6 102.8(4) . . . . ?
Ni1 N1 C7 C6 -4.2(5) . . . . ?
C9 C6 C7 N1 67.0(5) . . . . ?
C8 C6 C7 N1 -172.1(4) . . . . ?
C5 C6 C7 N1 -55.2(5) . . . . ?
C11 N10 C9 C14 2.3(7) . . . . ?
Ni1 N10 C9 C14 -168.8(4) . . . . ?
C11 N10 C9 C6 176.7(4) . . . . ?
Ni1 N10 C9 C6 5.7(5) . . . . ?
C8 C6 C9 N10 170.8(4) . . . . ?
C7 C6 C9 N10 -70.9(5) . . . . ?
C5 C6 C9 N10 52.4(6) . . . . ?
C8 C6 C9 C14 -14.9(7) . . . . ?
C7 C6 C9 C14 103.4(5) . . . . ?
C5 C6 C9 C14 -133.3(5) . . . . ?
C9 N10 C11 C12 -2.0(7) . . . . ?
Ni1 N10 C11 C12 169.2(4) . . . . ?
N10 C11 C12 C13 0.7(8) . . . . ?
C11 C12 C13 C14 0.1(8) . . . . ?
C12 C13 C14 C9 0.2(8) . . . . ?
N10 C9 C14 C13 -1.4(8) . . . . ?
C6 C9 C14 C13 -175.5(5) . . . . ?
C7 N1 C15 C16 144.8(4) . . . . ?
C2 N1 C15 C16 -90.6(5) . . . . ?
Ni1 N1 C15 C16 14.8(5) . . . . ?
C18 N17 C16 C21 3.2(7) . . . . ?
Ni1 N17 C16 C21 -175.7(4) . . . . ?
C18 N17 C16 C15 -173.6(4) . . . . ?
Ni1 N17 C16 C15 7.6(6) . . . . ?
N1 C15 C16 N17 -15.6(7) . . . . ?
N1 C15 C16 C21 167.7(4) . . . . ?
C16 N17 C18 C19 -1.1(7) . . . . ?
Ni1 N17 C18 C19 177.6(4) . . . . ?
N17 C18 C19 C20 -0.8(8) . . . . ?
C18 C19 C20 C21 0.6(8) . . . . ?
C19 C20 C21 C16 1.4(8) . . . . ?
N17 C16 C21 C20 -3.4(8) . . . . ?
C15 C16 C21 C20 173.3(5) . . . . ?
C5 N4 C22 C23 -88.1(5) . . . . ?
C3 N4 C22 C23 146.7(4) . . . . ?
Ni1 N4 C22 C23 28.3(5) . . . . ?
C25 N24 C23 C28 1.0(7) . . . . ?
Ni1 N24 C23 C28 -171.5(4) . . . . ?
C25 N24 C23 C22 -175.0(4) . . . . ?
Ni1 N24 C23 C22 12.4(5) . . . . ?
N4 C22 C23 N24 -27.6(6) . . . . ?
N4 C22 C23 C28 156.3(5) . . . . ?
C23 N24 C25 C26 -0.7(7) . . . . ?
Ni1 N24 C25 C26 170.6(4) . . . . ?
N24 C25 C26 C27 -0.1(8) . . . . ?
C25 C26 C27 C28 0.6(8) . . . . ?
C26 C27 C28 C23 -0.3(8) . . . . ?
N24 C23 C28 C27 -0.5(8) . . . . ?
C22 C23 C28 C27 175.3(5) . . . . ?
O8B Cl2 O6A Ni1 -19(2) . . . . ?
O6B Cl2 O6A Ni1 -36(6) . . . . ?
O7A Cl2 O6A Ni1 -166.5(15) . . . . ?
O7B Cl2 O6A Ni1 -152.5(18) . . . . ?
O5A Cl2 O6A Ni1 71.4(18) . . . . ?
O8A Cl2 O6A Ni1 -42.2(19) . . . . ?
O5B Cl2 O6A Ni1 98.0(17) . . . . ?
N10 Ni1 O6A Cl2 139.2(12) . . . . ?
N17 Ni1 O6A Cl2 -170(2) . . . . ?
N4 Ni1 O6A Cl2 -12.1(19) . . . . ?
N24 Ni1 O6A Cl2 70.0(18) . . . . ?
N1 Ni1 O6A Cl2 -90.5(19) . . . . ?
O6B Ni1 O6A Cl2 39(6) . . . . ?
O8B Cl2 O6B Ni1 -52(4) . . . . ?
O7A Cl2 O6B Ni1 169(3) . . . . ?
O6A Cl2 O6B Ni1 114(9) . . . . ?
O7B Cl2 O6B Ni1 -179(3) . . . . ?
O5A Cl2 O6B Ni1 37(4) . . . . ?
O8A Cl2 O6B Ni1 -72(3) . . . . ?
O5B Cl2 O6B Ni1 66(3) . . . . ?
N10 Ni1 O6B Cl2 144(2) . . . . ?
N17 Ni1 O6B Cl2 -138(4) . . . . ?
N4 Ni1 O6B Cl2 19(4) . . . . ?
N24 Ni1 O6B Cl2 102(4) . . . . ?
N1 Ni1 O6B Cl2 -58(4) . . . . ?
O6A Ni1 O6B Cl2 -110(9) . . . . ?

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
O9 H9 O4 0.84 2.31 3.141(7) 170.8 4_576

# 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
####################################################################### 
# 
# 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_mer-1-mecn_cu-478
_database_code_depnum_ccdc_archive 'CCDC 1008833'
_audit_update_record             
;
2014-06-17 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;

_audit_creation_date             2014-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;acetonitrile[6-methyl-6-(pyridin-2-yl)-1,4-bis(pyridin-2-ylmethyl)-
        1,4-diazepane]iron(II) tetraphenylborate
;
_chemical_formula_iupac          '[Fe(C H3 C N)(C23 H27 N5)](B{C6 H5}4)2'
_chemical_formula_moiety         'C25 H30 Fe N6 2+, 2(C24 H20 B 1-)'
_chemical_formula_sum            'C73 H70 B2 Fe N6'
_chemical_formula_weight         1108.82

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

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/n'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.0919(2)
_cell_length_b                   33.6364(5)
_cell_length_c                   14.6502(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.4960(10)
_cell_angle_gamma                90
_cell_volume                     5958.42(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    11196
_cell_measurement_theta_min      3.276
_cell_measurement_theta_max      73.287

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

_exptl_crystal_description       rod
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             2344
_exptl_crystal_recrystallization_method 
'precipitation: acetonitrile, diethyl ether, layering, r.t., 7 d'

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

_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.6084
_exptl_absorpt_correction_T_max  0.8131

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

_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Agilent Nova'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Atlas'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova (Single Source)'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_number            46761
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.63
_diffrn_reflns_theta_max         67.5
_diffrn_reflns_theta_full        67.5
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.00
_reflns_number_total             10755
_reflns_number_gt                8845
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
        (compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

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

_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)+(0.0374P)²+1.4804P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         10755
_refine_ls_number_parameters     739
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.0927
_refine_ls_wR_factor_gt          0.0845
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.041

#----------------------------------------------------------------------------#
#                   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 0.0181 0.0091 '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'
B B 0.009 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.76949(2) 0.127650(8) 0.707950(19) 0.01864(8) Uani 1 1 d . . .
N1 N 0.94598(12) 0.13530(4) 0.69432(10) 0.0220(3) Uani 1 1 d . . .
C2 C 1.00076(15) 0.09528(6) 0.68964(13) 0.0255(4) Uani 1 1 d . . .
H2A H 1.0379 0.0894 0.7486 0.031 Uiso 1 1 calc R . .
H2B H 1.0576 0.0955 0.6414 0.031 Uiso 1 1 calc R . .
C3 C 0.91538(15) 0.06305(5) 0.66873(13) 0.0241(4) Uani 1 1 d . . .
H3A H 0.9511 0.0402 0.6383 0.029 Uiso 1 1 calc R . .
H3B H 0.8813 0.0536 0.7259 0.029 Uiso 1 1 calc R . .
N4 N 0.83053(12) 0.08058(4) 0.60832(10) 0.0208(3) Uani 1 1 d . . .
C5 C 0.88284(16) 0.09564(6) 0.52394(13) 0.0243(4) Uani 1 1 d . . .
H5A H 0.8348 0.0888 0.4712 0.029 Uiso 1 1 calc R . .
H5B H 0.9543 0.0818 0.5157 0.029 Uiso 1 1 calc R . .
C6 C 0.90388(16) 0.14140(6) 0.52364(13) 0.0244(4) Uani 1 1 d . . .
C7 C 0.96518(16) 0.15798(6) 0.60950(13) 0.0270(4) Uani 1 1 d . . .
H7A H 1.0456 0.1583 0.5973 0.032 Uiso 1 1 calc R . .
H7B H 0.9415 0.1858 0.6193 0.032 Uiso 1 1 calc R . .
C8 C 0.97836(17) 0.14981(7) 0.44135(14) 0.0341(5) Uani 1 1 d . . .
H8A H 0.9941 0.1784 0.4381 0.051 Uiso 1 1 calc R . .
H8B H 0.9406 0.1414 0.3852 0.051 Uiso 1 1 calc R . .
H8C H 1.0479 0.1351 0.4483 0.051 Uiso 1 1 calc R . .
N10 N 0.72045(13) 0.15576(5) 0.58259(10) 0.0236(3) Uani 1 1 d . . .
C11 C 0.61351(16) 0.16596(6) 0.57130(13) 0.0262(4) Uani 1 1 d . . .
H11A H 0.5649 0.1627 0.6213 0.031 Uiso 1 1 calc R . .
C12 C 0.57132(17) 0.18085(6) 0.49064(14) 0.0284(4) Uani 1 1 d . . .
H12A H 0.4948 0.1866 0.484 0.034 Uiso 1 1 calc R . .
C13 C 0.64360(18) 0.18714(6) 0.42004(14) 0.0323(5) Uani 1 1 d . . .
H13A H 0.6178 0.1985 0.3644 0.039 Uiso 1 1 calc R . .
C14 C 0.75361(17) 0.17697(6) 0.43030(14) 0.0303(5) Uani 1 1 d . . .
H14A H 0.804 0.1815 0.382 0.036 Uiso 1 1 calc R . .
C15 C 0.79015(16) 0.16006(5) 0.51165(13) 0.0235(4) Uani 1 1 d . . .
N20 N 0.84912(13) 0.11384(5) 0.84663(11) 0.0245(3) Uani 1 1 d . . .
C21 C 0.81683(17) 0.08907(6) 0.91292(13) 0.0281(4) Uani 1 1 d . . .
H21A H 0.7483 0.0756 0.9056 0.034 Uiso 1 1 calc R . .
C22 C 0.87791(18) 0.08206(6) 0.99129(13) 0.0310(5) Uani 1 1 d . . .
H22A H 0.853 0.0636 1.0357 0.037 Uiso 1 1 calc R . .
C23 C 0.97583(18) 0.10241(6) 1.00364(14) 0.0336(5) Uani 1 1 d . . .
H23A H 1.0194 0.0985 1.0572 0.04 Uiso 1 1 calc R . .
C24 C 1.00984(17) 0.12878(6) 0.93655(14) 0.0318(5) Uani 1 1 d . . .
H24A H 1.0761 0.1437 0.9442 0.038 Uiso 1 1 calc R . .
C25 C 0.94593(16) 0.13305(6) 0.85867(13) 0.0255(4) Uani 1 1 d . . .
C26 C 0.98306(17) 0.15704(6) 0.77717(13) 0.0290(4) Uani 1 1 d . . .
H26A H 0.9497 0.1839 0.7786 0.035 Uiso 1 1 calc R . .
H26B H 1.0646 0.1598 0.7777 0.035 Uiso 1 1 calc R . .
N30 N 0.64901(12) 0.08284(4) 0.72018(10) 0.0210(3) Uani 1 1 d . . .
C31 C 0.57723(15) 0.08198(6) 0.79004(12) 0.0239(4) Uani 1 1 d . . .
H31A H 0.5638 0.1059 0.8227 0.029 Uiso 1 1 calc R . .
C32 C 0.52258(16) 0.04798(6) 0.81603(13) 0.0277(4) Uani 1 1 d . . .
H32A H 0.4724 0.0484 0.8655 0.033 Uiso 1 1 calc R . .
C33 C 0.54245(16) 0.01315(6) 0.76832(14) 0.0303(5) Uani 1 1 d . . .
H33A H 0.5072 -0.0109 0.7856 0.036 Uiso 1 1 calc R . .
C34 C 0.61417(16) 0.01385(6) 0.69530(14) 0.0280(4) Uani 1 1 d . . .
H34A H 0.6282 -0.0097 0.6615 0.034 Uiso 1 1 calc R . .
C35 C 0.66542(15) 0.04923(5) 0.67192(12) 0.0224(4) Uani 1 1 d . . .
C36 C 0.73892(16) 0.05281(6) 0.59004(13) 0.0259(4) Uani 1 1 d . . .
H36A H 0.7692 0.0263 0.5745 0.031 Uiso 1 1 calc R . .
H36B H 0.695 0.0624 0.5371 0.031 Uiso 1 1 calc R . .
N40 N 0.68531(14) 0.17502(5) 0.77644(11) 0.0278(4) Uani 1 1 d . . .
C41 C 0.63533(16) 0.20136(6) 0.80324(13) 0.0252(4) Uani 1 1 d . . .
C42 C 0.57094(18) 0.23464(6) 0.83630(14) 0.0322(5) Uani 1 1 d . . .
H42A H 0.6114 0.2594 0.8256 0.048 Uiso 1 1 calc R . .
H42B H 0.558 0.2314 0.9018 0.048 Uiso 1 1 calc R . .
H42C H 0.4998 0.2356 0.8038 0.048 Uiso 1 1 calc R . .
B50 B 0.79708(19) 0.24238(6) 1.08770(14) 0.0239(5) Uani 1 1 d . . .
C51 C 0.68224(17) 0.21677(6) 1.07581(12) 0.0264(4) Uani 1 1 d . . .
C52 C 0.6801(2) 0.17933(6) 1.03332(14) 0.0335(5) Uani 1 1 d . . .
H52A H 0.7478 0.168 1.0135 0.04 Uiso 1 1 calc R . .
C53 C 0.5829(2) 0.15824(7) 1.01916(15) 0.0460(6) Uani 1 1 d . . .
H53A H 0.5852 0.1328 0.9912 0.055 Uiso 1 1 calc R . .
C54 C 0.4827(2) 0.17398(9) 1.04545(16) 0.0529(7) Uani 1 1 d . . .
H54A H 0.4161 0.1595 1.0361 0.063 Uiso 1 1 calc R . .
C55 C 0.4807(2) 0.21117(8) 1.08556(16) 0.0480(6) Uani 1 1 d . . .
H55A H 0.4123 0.2226 1.103 0.058 Uiso 1 1 calc R . .
C56 C 0.57916(18) 0.23182(7) 1.10040(14) 0.0355(5) Uani 1 1 d . . .
H56A H 0.576 0.2572 1.1285 0.043 Uiso 1 1 calc R . .
C57 C 0.81362(15) 0.26440(5) 0.98864(12) 0.0213(4) Uani 1 1 d . . .
C58 C 0.87521(16) 0.24765(6) 0.91744(13) 0.0256(4) Uani 1 1 d . . .
H58A H 0.9104 0.2228 0.9276 0.031 Uiso 1 1 calc R . .
C59 C 0.88700(17) 0.26575(6) 0.83288(13) 0.0279(4) Uani 1 1 d . . .
H59A H 0.9303 0.2534 0.7872 0.034 Uiso 1 1 calc R . .
C60 C 0.83596(17) 0.30177(6) 0.81487(13) 0.0283(4) Uani 1 1 d . . .
H60A H 0.8448 0.3145 0.7576 0.034 Uiso 1 1 calc R . .
C61 C 0.77162(17) 0.31883(6) 0.88224(13) 0.0284(4) Uani 1 1 d . . .
H61A H 0.7347 0.3433 0.8707 0.034 Uiso 1 1 calc R . .
C62 C 0.76091(15) 0.30037(5) 0.96658(13) 0.0238(4) Uani 1 1 d . . .
H62A H 0.7159 0.3126 1.0113 0.029 Uiso 1 1 calc R . .
C63 C 0.79002(16) 0.27367(6) 1.17382(13) 0.0246(4) Uani 1 1 d . . .
C64 C 0.74882(19) 0.26064(6) 1.25795(14) 0.0335(5) Uani 1 1 d . . .
H64A H 0.7184 0.2346 1.2614 0.04 Uiso 1 1 calc R . .
C65 C 0.7502(2) 0.28381(7) 1.33616(15) 0.0391(5) Uani 1 1 d . . .
H65A H 0.7212 0.2736 1.3915 0.047 Uiso 1 1 calc R . .
C66 C 0.79384(19) 0.32174(6) 1.33377(15) 0.0367(5) Uani 1 1 d . . .
H66A H 0.7952 0.3378 1.3871 0.044 Uiso 1 1 calc R . .
C67 C 0.83536(18) 0.33590(6) 1.25266(15) 0.0349(5) Uani 1 1 d . . .
H67A H 0.8655 0.362 1.2499 0.042 Uiso 1 1 calc R . .
C68 C 0.83336(17) 0.31211(6) 1.17472(14) 0.0284(4) Uani 1 1 d . . .
H68A H 0.8628 0.3225 1.1198 0.034 Uiso 1 1 calc R . .
C69 C 0.90320(17) 0.21376(6) 1.11454(12) 0.0259(4) Uani 1 1 d . . .
C70 C 0.89165(19) 0.17891(6) 1.16557(13) 0.0318(5) Uani 1 1 d . . .
H70A H 0.8194 0.1705 1.1816 0.038 Uiso 1 1 calc R . .
C71 C 0.9813(2) 0.15612(6) 1.19377(14) 0.0393(5) Uani 1 1 d . . .
H71A H 0.9693 0.1325 1.2277 0.047 Uiso 1 1 calc R . .
C72 C 1.0878(2) 0.16755(7) 1.17285(16) 0.0429(6) Uani 1 1 d . . .
H72A H 1.1493 0.1519 1.1918 0.051 Uiso 1 1 calc R . .
C73 C 1.1034(2) 0.20217(7) 1.12379(17) 0.0428(6) Uani 1 1 d . . .
H73A H 1.176 0.2107 1.1092 0.051 Uiso 1 1 calc R . .
C74 C 1.01220(18) 0.22457(6) 1.09580(15) 0.0332(5) Uani 1 1 d . . .
H74A H 1.0248 0.2483 1.0624 0.04 Uiso 1 1 calc R . .
B80 B 0.78911(17) 0.00662(6) 0.25172(14) 0.0218(4) Uani 1 1 d . . .
C81 C 0.73990(15) -0.01342(6) 0.15678(12) 0.0227(4) Uani 1 1 d . . .
C82 C 0.76175(16) -0.05305(6) 0.13239(13) 0.0278(4) Uani 1 1 d . . .
H82A H 0.8027 -0.0692 0.1739 0.033 Uiso 1 1 calc R . .
C83 C 0.72625(17) -0.06986(7) 0.05026(14) 0.0322(5) Uani 1 1 d . . .
H83A H 0.7432 -0.0968 0.037 0.039 Uiso 1 1 calc R . .
C84 C 0.66655(17) -0.04747(7) -0.01181(13) 0.0329(5) Uani 1 1 d . . .
H84A H 0.6407 -0.0589 -0.0674 0.04 Uiso 1 1 calc R . .
C85 C 0.64517(17) -0.00813(7) 0.00866(14) 0.0319(5) Uani 1 1 d . . .
H85A H 0.6058 0.0079 -0.034 0.038 Uiso 1 1 calc R . .
C86 C 0.68072(15) 0.00825(6) 0.09115(13) 0.0256(4) Uani 1 1 d . . .
H86A H 0.664 0.0353 0.1034 0.031 Uiso 1 1 calc R . .
C87 C 0.71101(15) 0.04477(6) 0.28146(12) 0.0232(4) Uani 1 1 d . . .
C88 C 0.71223(17) 0.08125(6) 0.23445(14) 0.0304(5) Uani 1 1 d . . .
H88A H 0.7683 0.0856 0.1906 0.036 Uiso 1 1 calc R . .
C89 C 0.63546(19) 0.11102(6) 0.24927(16) 0.0367(5) Uani 1 1 d . . .
H89A H 0.6379 0.1347 0.214 0.044 Uiso 1 1 calc R . .
C90 C 0.55491(18) 0.10651(6) 0.31530(16) 0.0363(5) Uani 1 1 d . . .
H90A H 0.501 0.1266 0.3247 0.044 Uiso 1 1 calc R . .
C91 C 0.55472(17) 0.07203(6) 0.36739(14) 0.0317(5) Uani 1 1 d . . .
H91A H 0.5025 0.0689 0.4149 0.038 Uiso 1 1 calc R . .
C92 C 0.63076(16) 0.04197(6) 0.35019(13) 0.0256(4) Uani 1 1 d . . .
H92A H 0.6284 0.0186 0.3864 0.031 Uiso 1 1 calc R . .
C93 C 0.78623(15) -0.02480(5) 0.33831(12) 0.0209(4) Uani 1 1 d . . .
C94 C 0.85028(15) -0.01836(5) 0.41753(12) 0.0216(4) Uani 1 1 d . . .
H94A H 0.9028 0.0026 0.4175 0.026 Uiso 1 1 calc R . .
C95 C 0.84027(16) -0.04132(6) 0.49580(13) 0.0258(4) Uani 1 1 d . . .
H95A H 0.8861 -0.036 0.5474 0.031 Uiso 1 1 calc R . .
C96 C 0.76367(17) -0.07195(6) 0.49903(14) 0.0301(5) Uani 1 1 d . . .
H96A H 0.7558 -0.0875 0.5527 0.036 Uiso 1 1 calc R . .
C97 C 0.69877(18) -0.07952(6) 0.42256(14) 0.0326(5) Uani 1 1 d . . .
H97A H 0.6464 -0.1006 0.4233 0.039 Uiso 1 1 calc R . .
C98 C 0.71050(16) -0.05625(6) 0.34461(13) 0.0271(4) Uani 1 1 d . . .
H98A H 0.6649 -0.062 0.2931 0.032 Uiso 1 1 calc R . .
C99 C 0.91692(15) 0.02088(5) 0.23162(12) 0.0218(4) Uani 1 1 d . . .
C100 C 0.96912(16) 0.05044(6) 0.28458(13) 0.0247(4) Uani 1 1 d . . .
H10A H 0.9279 0.0631 0.3312 0.03 Uiso 1 1 calc R . .
C101 C 1.07837(17) 0.06187(6) 0.27166(14) 0.0282(4) Uani 1 1 d . . .
H10B H 1.1104 0.0816 0.3099 0.034 Uiso 1 1 calc R . .
C102 C 1.14061(17) 0.04471(6) 0.20369(14) 0.0317(5) Uani 1 1 d . . .
H10C H 1.2154 0.0524 0.1949 0.038 Uiso 1 1 calc R . .
C103 C 1.09191(17) 0.01596(6) 0.14834(14) 0.0321(5) Uani 1 1 d . . .
H10D H 1.1331 0.0041 0.1006 0.039 Uiso 1 1 calc R . .
C104 C 0.98302(16) 0.00448(6) 0.16276(13) 0.0264(4) Uani 1 1 d . . .
H10E H 0.9518 -0.0154 0.1243 0.032 Uiso 1 1 calc R . .


#----------------------------------------------------------------------------#
#                   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
Fe1 N30 2.1050(15) . ?
Fe1 N40 2.1445(16) . ?
Fe1 N10 2.1447(15) . ?
Fe1 N1 2.1605(15) . ?
Fe1 N4 2.2805(15) . ?
Fe1 N20 2.2884(16) . ?
N1 C7 1.478(2) . ?
N1 C26 1.483(2) . ?
N1 C2 1.502(2) . ?
C2 C3 1.526(3) . ?
C3 N4 1.472(2) . ?
N4 C36 1.472(2) . ?
N4 C5 1.483(2) . ?
C5 C6 1.560(3) . ?
C6 C15 1.521(3) . ?
C6 C8 1.537(2) . ?
C6 C7 1.558(3) . ?
N10 C11 1.347(2) . ?
N10 C15 1.352(2) . ?
C11 C12 1.377(3) . ?
C12 C13 1.376(3) . ?
C13 C14 1.380(3) . ?
C14 C15 1.389(3) . ?
N20 C21 1.340(2) . ?
N20 C25 1.347(3) . ?
C21 C22 1.380(3) . ?
C22 C23 1.378(3) . ?
C23 C24 1.389(3) . ?
C24 C25 1.380(3) . ?
C25 C26 1.512(3) . ?
N30 C31 1.348(2) . ?
N30 C35 1.349(2) . ?
C31 C32 1.376(3) . ?
C32 C33 1.386(3) . ?
C33 C34 1.383(3) . ?
C34 C35 1.386(3) . ?
C35 C36 1.504(2) . ?
N40 C41 1.144(2) . ?
C41 C42 1.449(3) . ?
B50 C51 1.642(3) . ?
B50 C57 1.643(3) . ?
B50 C63 1.646(3) . ?
B50 C69 1.649(3) . ?
C51 C56 1.396(3) . ?
C51 C52 1.405(3) . ?
C52 C53 1.387(3) . ?
C53 C54 1.380(4) . ?
C54 C55 1.382(4) . ?
C55 C56 1.394(3) . ?
C57 C62 1.404(3) . ?
C57 C58 1.405(3) . ?
C58 C59 1.389(3) . ?
C59 C60 1.384(3) . ?
C60 C61 1.386(3) . ?
C61 C62 1.390(3) . ?
C63 C68 1.395(3) . ?
C63 C64 1.403(3) . ?
C64 C65 1.386(3) . ?
C65 C66 1.381(3) . ?
C66 C67 1.379(3) . ?
C67 C68 1.394(3) . ?
C69 C74 1.397(3) . ?
C69 C70 1.398(3) . ?
C70 C71 1.387(3) . ?
C71 C72 1.382(4) . ?
C72 C73 1.382(3) . ?
C73 C74 1.394(3) . ?
B80 C99 1.647(3) . ?
B80 C93 1.652(3) . ?
B80 C81 1.652(3) . ?
B80 C87 1.654(3) . ?
C81 C86 1.398(3) . ?
C81 C82 1.406(3) . ?
C82 C83 1.394(3) . ?
C83 C84 1.380(3) . ?
C84 C85 1.382(3) . ?
C85 C86 1.393(3) . ?
C87 C88 1.407(3) . ?
C87 C92 1.408(3) . ?
C88 C89 1.384(3) . ?
C89 C90 1.387(3) . ?
C90 C91 1.388(3) . ?
C91 C92 1.391(3) . ?
C93 C98 1.403(3) . ?
C93 C94 1.406(3) . ?
C94 C95 1.389(3) . ?
C95 C96 1.386(3) . ?
C96 C97 1.386(3) . ?
C97 C98 1.393(3) . ?
C99 C104 1.405(3) . ?
C99 C100 1.407(3) . ?
C100 C101 1.390(3) . ?
C101 C102 1.380(3) . ?
C102 C103 1.390(3) . ?
C103 C104 1.390(3) . ?

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
N30 Fe1 N40 99.24(6) . . ?
N30 Fe1 N10 101.66(6) . . ?
N40 Fe1 N10 86.81(6) . . ?
N30 Fe1 N1 141.08(6) . . ?
N40 Fe1 N1 115.34(6) . . ?
N10 Fe1 N1 97.72(6) . . ?
N30 Fe1 N4 77.61(6) . . ?
N40 Fe1 N4 166.61(6) . . ?
N10 Fe1 N4 81.18(6) . . ?
N1 Fe1 N4 72.43(6) . . ?
N30 Fe1 N20 93.74(6) . . ?
N40 Fe1 N20 86.17(6) . . ?
N10 Fe1 N20 163.91(6) . . ?
N1 Fe1 N20 72.41(6) . . ?
N4 Fe1 N20 106.93(5) . . ?
C7 N1 C26 112.63(15) . . ?
C7 N1 C2 110.59(15) . . ?
C26 N1 C2 110.42(15) . . ?
C7 N1 Fe1 107.56(11) . . ?
C26 N1 Fe1 105.96(11) . . ?
C2 N1 Fe1 109.50(11) . . ?
N1 C2 C3 110.36(15) . . ?
N4 C3 C2 107.62(15) . . ?
C36 N4 C3 112.00(15) . . ?
C36 N4 C5 113.01(14) . . ?
C3 N4 C5 109.75(14) . . ?
C36 N4 Fe1 108.05(11) . . ?
C3 N4 Fe1 96.96(10) . . ?
C5 N4 Fe1 116.05(11) . . ?
N4 C5 C6 114.21(15) . . ?
C15 C6 C8 111.64(16) . . ?
C15 C6 C7 111.65(16) . . ?
C8 C6 C7 106.82(16) . . ?
C15 C6 C5 105.09(15) . . ?
C8 C6 C5 106.29(15) . . ?
C7 C6 C5 115.31(16) . . ?
N1 C7 C6 114.63(15) . . ?
C11 N10 C15 118.87(16) . . ?
C11 N10 Fe1 118.40(13) . . ?
C15 N10 Fe1 122.42(13) . . ?
N10 C11 C12 123.11(18) . . ?
C13 C12 C11 117.89(19) . . ?
C12 C13 C14 119.85(19) . . ?
C13 C14 C15 119.60(19) . . ?
N10 C15 C14 120.51(18) . . ?
N10 C15 C6 115.87(16) . . ?
C14 C15 C6 123.28(17) . . ?
C21 N20 C25 117.48(17) . . ?
C21 N20 Fe1 130.28(13) . . ?
C25 N20 Fe1 112.17(12) . . ?
N20 C21 C22 123.5(2) . . ?
C23 C22 C21 118.5(2) . . ?
C22 C23 C24 118.92(19) . . ?
C25 C24 C23 119.0(2) . . ?
N20 C25 C24 122.55(19) . . ?
N20 C25 C26 114.58(17) . . ?
C24 C25 C26 122.70(18) . . ?
N1 C26 C25 107.06(15) . . ?
C31 N30 C35 118.59(16) . . ?
C31 N30 Fe1 122.06(12) . . ?
C35 N30 Fe1 116.77(12) . . ?
N30 C31 C32 122.82(18) . . ?
C31 C32 C33 118.49(18) . . ?
C34 C33 C32 119.22(18) . . ?
C33 C34 C35 119.36(19) . . ?
N30 C35 C34 121.46(17) . . ?
N30 C35 C36 116.21(16) . . ?
C34 C35 C36 122.30(17) . . ?
N4 C36 C35 110.78(15) . . ?
C41 N40 Fe1 172.03(16) . . ?
N40 C41 C42 179.3(2) . . ?
C51 B50 C57 104.60(15) . . ?
C51 B50 C63 111.55(16) . . ?
C57 B50 C63 113.36(15) . . ?
C51 B50 C69 111.99(16) . . ?
C57 B50 C69 111.93(16) . . ?
C63 B50 C69 103.64(15) . . ?
C56 C51 C52 115.2(2) . . ?
C56 C51 B50 122.59(18) . . ?
C52 C51 B50 122.00(19) . . ?
C53 C52 C51 122.5(2) . . ?
C54 C53 C52 120.5(2) . . ?
C53 C54 C55 119.0(2) . . ?
C54 C55 C56 119.9(2) . . ?
C55 C56 C51 122.9(2) . . ?
C62 C57 C58 114.66(17) . . ?
C62 C57 B50 122.23(16) . . ?
C58 C57 B50 122.98(17) . . ?
C59 C58 C57 123.06(18) . . ?
C60 C59 C58 120.32(18) . . ?
C59 C60 C61 118.61(18) . . ?
C60 C61 C62 120.33(18) . . ?
C61 C62 C57 122.97(18) . . ?
C68 C63 C64 114.66(18) . . ?
C68 C63 B50 125.30(17) . . ?
C64 C63 B50 119.66(17) . . ?
C65 C64 C63 123.3(2) . . ?
C66 C65 C64 120.0(2) . . ?
C67 C66 C65 118.9(2) . . ?
C66 C67 C68 120.3(2) . . ?
C67 C68 C63 122.9(2) . . ?
C74 C69 C70 114.98(19) . . ?
C74 C69 B50 122.32(17) . . ?
C70 C69 B50 122.41(18) . . ?
C71 C70 C69 122.8(2) . . ?
C72 C71 C70 120.5(2) . . ?
C71 C72 C73 118.7(2) . . ?
C72 C73 C74 119.8(2) . . ?
C73 C74 C69 123.1(2) . . ?
C99 B80 C93 110.47(15) . . ?
C99 B80 C81 107.46(15) . . ?
C93 B80 C81 112.07(15) . . ?
C99 B80 C87 111.09(15) . . ?
C93 B80 C87 106.16(15) . . ?
C81 B80 C87 109.64(15) . . ?
C86 C81 C82 114.55(18) . . ?
C86 C81 B80 123.00(17) . . ?
C82 C81 B80 122.27(16) . . ?
C83 C82 C81 123.16(19) . . ?
C84 C83 C82 120.2(2) . . ?
C83 C84 C85 118.51(19) . . ?
C84 C85 C86 120.68(19) . . ?
C85 C86 C81 122.87(19) . . ?
C88 C87 C92 114.74(17) . . ?
C88 C87 B80 122.63(17) . . ?
C92 C87 B80 122.37(16) . . ?
C89 C88 C87 122.98(19) . . ?
C88 C89 C90 120.4(2) . . ?
C89 C90 C91 118.65(19) . . ?
C90 C91 C92 120.21(19) . . ?
C91 C92 C87 122.82(18) . . ?
C98 C93 C94 114.64(17) . . ?
C98 C93 B80 123.44(17) . . ?
C94 C93 B80 121.35(16) . . ?
C95 C94 C93 123.00(18) . . ?
C96 C95 C94 120.29(18) . . ?
C97 C96 C95 118.87(18) . . ?
C96 C97 C98 119.91(19) . . ?
C97 C98 C93 123.29(19) . . ?
C104 C99 C100 114.71(17) . . ?
C104 C99 B80 123.67(17) . . ?
C100 C99 B80 121.61(16) . . ?
C101 C100 C99 122.85(18) . . ?
C102 C101 C100 120.48(19) . . ?
C101 C102 C103 118.77(19) . . ?
C102 C103 C104 120.12(19) . . ?
C103 C104 C99 123.05(19) . . ?

# 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
####################################################################### 
# 
# 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_mer-1-otf
_database_code_depnum_ccdc_archive 'CCDC 1008834'
_audit_update_record             
;
2014-06-17 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;

_audit_creation_date             2014-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;(trifluoromethanesulfonato)[6-methyl-6-(pyridin-2-yl)-
1,4-bis(pyridin-2-ylmethyl)-1,4-diazepane]iron(II) trifluoromethanesulfonate
;
_chemical_formula_iupac          '[Fe(C F3 S O3)(C23 H27 N5)](C F3 S O3)'
_chemical_formula_moiety         'C24 H27 F3 Fe N5 O3 S 1+, C F3 O3 S 1-'
_chemical_formula_sum            'C25 H27 F6 Fe N5 O6 S2'
_chemical_formula_weight         727.49

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

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.8155(3)
_cell_length_b                   17.6019(5)
_cell_length_c                   14.8106(4)
_cell_angle_alpha                90
_cell_angle_beta                 96.124(3)
_cell_angle_gamma                90
_cell_volume                     3062.66(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    5907
_cell_measurement_theta_min      3.4117
_cell_measurement_theta_max      32.5041

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

_exptl_crystal_description       cube
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1488
_exptl_crystal_recrystallization_method 
'precipitation: dichloromethane, diethyl ether, vapour diffusion, r.t., 5 d'

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

_exptl_absorpt_coefficient_mu    0.713
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.92072
_exptl_absorpt_correction_T_max  1.00000

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

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_number            13451
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             6006
_reflns_number_gt                4989
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

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

_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

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

_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.
 The triflato ligand exhibits disorder and was modelled in two discrete
 positions using tight DELU und ISOR restraints. The s.o.f refined to
 0.51(2) and 0.49(2), respectively.
;
_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)+(0.0327P)²+2.8354P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6006
_refine_ls_number_parameters     480
_refine_ls_number_restraints     155
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.046
_refine_ls_wR_factor_ref         0.098
_refine_ls_wR_factor_gt          0.0925
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.058

#----------------------------------------------------------------------------#
#                   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 0.0033 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'
F F 0.0171 0.0103 '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'

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
C2 C 0.8561(3) 0.32533(17) 0.3235(2) 0.0272(7) Uani 1 1 d . . .
H2A H 0.7825 0.2979 0.3171 0.033 Uiso 1 1 calc R . .
H2B H 0.8877 0.324 0.3881 0.033 Uiso 1 1 calc R . .
C3 C 0.9389(2) 0.28777(17) 0.2644(2) 0.0266(7) Uani 1 1 d . . .
H3A H 1.0178 0.2952 0.2927 0.032 Uiso 1 1 calc R . .
H3B H 0.9237 0.2325 0.2608 0.032 Uiso 1 1 calc R . .
C5 C 1.0179(2) 0.37700(16) 0.1602(2) 0.0261(6) Uani 1 1 d . . .
H5A H 1.0185 0.3884 0.0948 0.031 Uiso 1 1 calc R . .
H5B H 1.0921 0.3537 0.1819 0.031 Uiso 1 1 calc R . .
C6 C 1.0063(2) 0.45290(16) 0.2119(2) 0.0244(6) Uani 1 1 d . . .
C7 C 0.9505(2) 0.44520(17) 0.3015(2) 0.0259(6) Uani 1 1 d . . .
H7A H 1.0039 0.4178 0.3463 0.031 Uiso 1 1 calc R . .
H7B H 0.9394 0.4967 0.3259 0.031 Uiso 1 1 calc R . .
C8 C 1.1273(2) 0.48264(19) 0.2381(2) 0.0365(8) Uani 1 1 d . . .
H8A H 1.1666 0.4878 0.1834 0.055 Uiso 1 1 calc R . .
H8B H 1.169 0.4468 0.2801 0.055 Uiso 1 1 calc R . .
H8C H 1.1236 0.5323 0.2676 0.055 Uiso 1 1 calc R . .
C9 C 0.9347(2) 0.51016(16) 0.1525(2) 0.0244(6) Uani 1 1 d . . .
C11 C 0.7587(3) 0.53977(17) 0.0752(2) 0.0326(7) Uani 1 1 d . . .
H11 H 0.6834 0.5246 0.0539 0.039 Uiso 1 1 calc R . .
C12 C 0.7924(3) 0.61252(18) 0.0572(2) 0.0376(8) Uani 1 1 d . . .
H12 H 0.7411 0.6472 0.0253 0.045 Uiso 1 1 calc R . .
C13 C 0.9022(3) 0.63369(18) 0.0864(2) 0.0375(8) Uani 1 1 d . . .
H13 H 0.9282 0.6833 0.0741 0.045 Uiso 1 1 calc R . .
C14 C 0.9741(3) 0.58259(17) 0.1336(2) 0.0314(7) Uani 1 1 d . . .
H14 H 1.0504 0.5966 0.1532 0.038 Uiso 1 1 calc R . .
C15 C 0.7532(2) 0.44428(18) 0.3408(2) 0.0299(7) Uani 1 1 d . . .
H15A H 0.7627 0.4998 0.3342 0.036 Uiso 1 1 calc R . .
H15B H 0.766 0.432 0.4063 0.036 Uiso 1 1 calc R . .
C16 C 0.6335(2) 0.42264(16) 0.3052(2) 0.0255(6) Uani 1 1 d . . .
C18 C 0.5088(2) 0.38853(17) 0.1809(2) 0.0308(7) Uani 1 1 d . . .
H18 H 0.4957 0.3754 0.1184 0.037 Uiso 1 1 calc R . .
C19 C 0.4167(3) 0.39215(19) 0.2308(2) 0.0371(8) Uani 1 1 d . . .
H19 H 0.3419 0.382 0.2033 0.044 Uiso 1 1 calc R . .
C20 C 0.4356(3) 0.4107(2) 0.3215(3) 0.0423(9) Uani 1 1 d . . .
H20 H 0.374 0.4124 0.3578 0.051 Uiso 1 1 calc R . .
C21 C 0.5439(3) 0.42681(19) 0.3587(2) 0.0364(8) Uani 1 1 d . . .
H21 H 0.5578 0.4408 0.4209 0.044 Uiso 1 1 calc R . .
C22 C 0.9241(2) 0.25994(16) 0.1019(2) 0.0264(6) Uani 1 1 d . . .
H22A H 0.992 0.2271 0.114 0.032 Uiso 1 1 calc R . .
H22B H 0.9245 0.2823 0.0406 0.032 Uiso 1 1 calc R . .
C23 C 0.8174(2) 0.21373(16) 0.10650(18) 0.0214(6) Uani 1 1 d . . .
C25 C 0.6314(2) 0.21304(17) 0.1385(2) 0.0279(7) Uani 1 1 d . . .
H25 H 0.5675 0.2394 0.1568 0.034 Uiso 1 1 calc R . .
C26 C 0.6201(3) 0.13669(17) 0.1193(2) 0.0308(7) Uani 1 1 d . . .
H26 H 0.5502 0.1112 0.1244 0.037 Uiso 1 1 calc R . .
C27 C 0.7123(3) 0.09809(16) 0.0925(2) 0.0280(7) Uani 1 1 d . . .
H27 H 0.707 0.0454 0.0786 0.034 Uiso 1 1 calc R . .
C28 C 0.8125(2) 0.13703(16) 0.0862(2) 0.0262(6) Uani 1 1 d . . .
H28 H 0.8772 0.1115 0.0681 0.031 Uiso 1 1 calc R . .
N1 N 0.83912(19) 0.40473(13) 0.29297(16) 0.0225(5) Uani 1 1 d . A .
N4 N 0.92680(18) 0.32082(13) 0.17056(16) 0.0210(5) Uani 1 1 d . A .
N10 N 0.8277(2) 0.48899(13) 0.12178(16) 0.0245(5) Uani 1 1 d . A .
N17 N 0.61626(19) 0.40278(13) 0.21684(16) 0.0238(5) Uani 1 1 d . A .
N24 N 0.72741(19) 0.25187(13) 0.13289(16) 0.0226(5) Uani 1 1 d . A .
Fe1 Fe 0.76233(3) 0.37781(2) 0.14917(3) 0.01843(11) Uani 1 1 d D . .
O1A O 0.6687(9) 0.3840(7) 0.0174(5) 0.038(2) Uani 0.515(17) 1 d PDU A 1
O2A O 0.7569(7) 0.3481(6) -0.1373(8) 0.055(2) Uani 0.515(17) 1 d PDU A 1
O3A O 0.6284(15) 0.4524(7) -0.1188(13) 0.097(5) Uani 0.515(17) 1 d PDU A 1
S1A S 0.6776(3) 0.38005(14) -0.0817(3) 0.0210(10) Uani 0.515(17) 1 d PDU A 1
C29A C 0.5487(10) 0.3261(8) -0.1095(8) 0.056(3) Uani 0.515(17) 1 d PDU A 1
F1A F 0.4645(10) 0.3540(8) -0.0730(10) 0.106(4) Uani 0.515(17) 1 d PDU A 1
F2A F 0.5645(10) 0.2527(6) -0.0794(10) 0.089(3) Uani 0.515(17) 1 d PDU A 1
F3A F 0.5058(7) 0.3291(9) -0.1912(6) 0.086(3) Uani 0.515(17) 1 d PDU A 1
O1B O 0.7089(12) 0.3752(8) 0.0132(5) 0.052(3) Uani 0.485(17) 1 d PDU A 2
O2B O 0.7746(8) 0.3313(6) -0.0970(9) 0.061(3) Uani 0.485(17) 1 d PDU A 2
O3B O 0.6545(12) 0.4428(7) -0.1259(10) 0.060(3) Uani 0.485(17) 1 d PDU A 2
S1B S 0.6761(5) 0.3700(5) -0.0794(5) 0.0722(19) Uani 0.485(17) 1 d PDU A 2
C29B C 0.5583(9) 0.3084(7) -0.1028(8) 0.040(3) Uani 0.485(17) 1 d PDU A 2
F1B F 0.4771(10) 0.3263(8) -0.0537(8) 0.085(3) Uani 0.485(17) 1 d PDU A 2
F2B F 0.5998(13) 0.2406(6) -0.0694(9) 0.096(4) Uani 0.485(17) 1 d PDU A 2
F3B F 0.5371(13) 0.2951(7) -0.1886(6) 0.085(3) Uani 0.485(17) 1 d PDU A 2
C30 C 0.2761(3) 0.1877(2) 0.0928(3) 0.0418(9) Uani 1 1 d . . .
O4 O 0.2563(2) 0.07297(14) -0.01157(18) 0.0522(7) Uani 1 1 d . . .
O5 O 0.1376(3) 0.18301(14) -0.05115(19) 0.0624(8) Uani 1 1 d . . .
O6 O 0.09983(19) 0.10321(13) 0.07417(18) 0.0446(6) Uani 1 1 d . . .
F4 F 0.2207(2) 0.24533(14) 0.1265(2) 0.0777(8) Uani 1 1 d . . .
F5 F 0.35893(18) 0.21888(14) 0.0511(2) 0.0735(8) Uani 1 1 d . . .
F6 F 0.3259(2) 0.14703(15) 0.16151(17) 0.0735(8) Uani 1 1 d . . .
S2 S 0.18135(7) 0.13001(4) 0.01672(5) 0.02867(18) Uani 1 1 d . . .


#----------------------------------------------------------------------------#
#                   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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 N1 1.476(4) . ?
C2 C3 1.530(4) . ?
C3 N4 1.500(4) . ?
C5 N4 1.481(3) . ?
C5 C6 1.553(4) . ?
C6 C9 1.532(4) . ?
C6 C8 1.533(4) . ?
C6 C7 1.550(4) . ?
C7 N1 1.490(4) . ?
C9 N10 1.350(4) . ?
C9 C14 1.396(4) . ?
C11 N10 1.349(4) . ?
C11 C12 1.376(4) . ?
C12 C13 1.374(5) . ?
C13 C14 1.376(5) . ?
C15 N1 1.473(4) . ?
C15 C16 1.506(4) . ?
C16 N17 1.349(4) . ?
C16 C21 1.391(4) . ?
C18 N17 1.347(4) . ?
C18 C19 1.381(4) . ?
C19 C20 1.377(5) . ?
C20 C21 1.368(5) . ?
C22 N4 1.476(4) . ?
C22 C23 1.508(4) . ?
C23 N24 1.350(3) . ?
C23 C28 1.383(4) . ?
C25 N24 1.334(4) . ?
C25 C26 1.377(4) . ?
C26 C27 1.378(4) . ?
C27 C28 1.379(4) . ?
N1 Fe1 2.274(2) . ?
N4 Fe1 2.180(2) . ?
N10 Fe1 2.158(2) . ?
N17 Fe1 2.132(2) . ?
N24 Fe1 2.263(2) . ?
Fe1 O1B 2.045(8) . ?
Fe1 O1A 2.141(7) . ?
O1A S1A 1.484(8) . ?
O2A S1A 1.427(8) . ?
O3A S1A 1.481(9) . ?
S1A C29A 1.805(10) . ?
C29A F3A 1.262(11) . ?
C29A F1A 1.279(11) . ?
C29A F2A 1.372(12) . ?
O1B S1B 1.388(9) . ?
O2B S1B 1.397(9) . ?
O3B S1B 1.465(9) . ?
S1B C29B 1.769(10) . ?
C29B F3B 1.290(11) . ?
C29B F1B 1.303(11) . ?
C29B F2B 1.363(12) . ?
C30 F6 1.329(4) . ?
C30 F5 1.330(4) . ?
C30 F4 1.333(4) . ?
C30 S2 1.813(4) . ?
O4 S2 1.431(2) . ?
O5 S2 1.427(2) . ?
O6 S2 1.431(2) . ?

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 C2 C3 108.0(2) . . ?
N4 C3 C2 111.0(2) . . ?
N4 C5 C6 114.9(2) . . ?
C9 C6 C8 111.4(2) . . ?
C9 C6 C7 106.8(2) . . ?
C8 C6 C7 106.4(2) . . ?
C9 C6 C5 110.8(2) . . ?
C8 C6 C5 106.9(2) . . ?
C7 C6 C5 114.5(2) . . ?
N1 C7 C6 114.9(2) . . ?
N10 C9 C14 120.3(3) . . ?
N10 C9 C6 116.9(2) . . ?
C14 C9 C6 122.7(3) . . ?
N10 C11 C12 123.0(3) . . ?
C13 C12 C11 118.3(3) . . ?
C12 C13 C14 119.6(3) . . ?
C13 C14 C9 119.8(3) . . ?
N1 C15 C16 112.4(2) . . ?
N17 C16 C21 121.4(3) . . ?
N17 C16 C15 116.4(2) . . ?
C21 C16 C15 122.1(3) . . ?
N17 C18 C19 122.9(3) . . ?
C20 C19 C18 118.6(3) . . ?
C21 C20 C19 119.3(3) . . ?
C20 C21 C16 119.7(3) . . ?
N4 C22 C23 108.5(2) . . ?
N24 C23 C28 122.1(3) . . ?
N24 C23 C22 115.7(2) . . ?
C28 C23 C22 122.2(3) . . ?
N24 C25 C26 123.5(3) . . ?
C27 C26 C25 118.6(3) . . ?
C26 C27 C28 119.0(3) . . ?
C27 C28 C23 119.1(3) . . ?
C15 N1 C2 112.2(2) . . ?
C15 N1 C7 112.4(2) . . ?
C2 N1 C7 109.7(2) . . ?
C15 N1 Fe1 108.82(17) . . ?
C2 N1 Fe1 96.70(16) . . ?
C7 N1 Fe1 116.08(17) . . ?
C22 N4 C5 112.1(2) . . ?
C22 N4 C3 110.5(2) . . ?
C5 N4 C3 110.9(2) . . ?
C22 N4 Fe1 106.29(16) . . ?
C5 N4 Fe1 108.90(16) . . ?
C3 N4 Fe1 107.95(16) . . ?
C11 N10 C9 118.9(3) . . ?
C11 N10 Fe1 119.23(19) . . ?
C9 N10 Fe1 121.87(19) . . ?
C18 N17 C16 118.0(2) . . ?
C18 N17 Fe1 123.5(2) . . ?
C16 N17 Fe1 117.62(18) . . ?
C25 N24 C23 117.7(2) . . ?
C25 N24 Fe1 129.91(19) . . ?
C23 N24 Fe1 112.18(18) . . ?
O1B Fe1 N17 106.7(4) . . ?
O1B Fe1 O1A 13.7(4) . . ?
N17 Fe1 O1A 93.0(3) . . ?
O1B Fe1 N10 85.1(4) . . ?
N17 Fe1 N10 103.01(9) . . ?
O1A Fe1 N10 86.7(4) . . ?
O1B Fe1 N4 108.0(4) . . ?
N17 Fe1 N4 141.30(9) . . ?
O1A Fe1 N4 121.5(3) . . ?
N10 Fe1 N4 96.52(9) . . ?
O1B Fe1 N24 80.7(4) . . ?
N17 Fe1 N24 96.00(9) . . ?
O1A Fe1 N24 83.2(4) . . ?
N10 Fe1 N24 158.92(9) . . ?
N4 Fe1 N24 73.40(8) . . ?
O1B Fe1 N1 167.7(4) . . ?
N17 Fe1 N1 77.23(9) . . ?
O1A Fe1 N1 163.5(3) . . ?
N10 Fe1 N1 82.65(9) . . ?
N4 Fe1 N1 72.50(8) . . ?
N24 Fe1 N1 110.73(8) . . ?
S1A O1A Fe1 144.6(7) . . ?
O2A S1A O3A 112.4(8) . . ?
O2A S1A O1A 135.2(8) . . ?
O3A S1A O1A 105.1(9) . . ?
O2A S1A C29A 104.5(6) . . ?
O3A S1A C29A 94.6(9) . . ?
O1A S1A C29A 95.9(6) . . ?
F3A C29A F1A 97.9(12) . . ?
F3A C29A F2A 112.2(11) . . ?
F1A C29A F2A 108.1(10) . . ?
F3A C29A S1A 116.0(9) . . ?
F1A C29A S1A 112.2(10) . . ?
F2A C29A S1A 109.8(8) . . ?
S1B O1B Fe1 177.0(10) . . ?
O1B S1B O2B 93.8(10) . . ?
O1B S1B O3B 115.1(9) . . ?
O2B S1B O3B 116.5(8) . . ?
O1B S1B C29B 111.4(9) . . ?
O2B S1B C29B 108.6(7) . . ?
O3B S1B C29B 110.5(7) . . ?
F3B C29B F1B 121.1(12) . . ?
F3B C29B F2B 102.9(10) . . ?
F1B C29B F2B 105.4(10) . . ?
F3B C29B S1B 111.8(9) . . ?
F1B C29B S1B 110.7(9) . . ?
F2B C29B S1B 102.7(9) . . ?
F6 C30 F5 106.9(3) . . ?
F6 C30 F4 108.5(3) . . ?
F5 C30 F4 106.0(3) . . ?
F6 C30 S2 111.6(3) . . ?
F5 C30 S2 112.2(3) . . ?
F4 C30 S2 111.3(2) . . ?
O5 S2 O6 114.69(17) . . ?
O5 S2 O4 116.20(18) . . ?
O6 S2 O4 114.81(14) . . ?
O5 S2 C30 103.00(16) . . ?
O6 S2 C30 103.02(17) . . ?
O4 S2 C30 102.39(16) . . ?

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 C2 C3 N4 -31.4(3) . . . . ?
N4 C5 C6 C9 -89.1(3) . . . . ?
N4 C5 C6 C8 149.4(3) . . . . ?
N4 C5 C6 C7 31.9(3) . . . . ?
C9 C6 C7 N1 70.8(3) . . . . ?
C8 C6 C7 N1 -170.1(2) . . . . ?
C5 C6 C7 N1 -52.3(3) . . . . ?
C8 C6 C9 N10 177.3(3) . . . . ?
C7 C6 C9 N10 -66.8(3) . . . . ?
C5 C6 C9 N10 58.5(3) . . . . ?
C8 C6 C9 C14 -5.8(4) . . . . ?
C7 C6 C9 C14 110.1(3) . . . . ?
C5 C6 C9 C14 -124.6(3) . . . . ?
N10 C11 C12 C13 1.4(5) . . . . ?
C11 C12 C13 C14 -1.0(5) . . . . ?
C12 C13 C14 C9 -0.9(5) . . . . ?
N10 C9 C14 C13 2.5(5) . . . . ?
C6 C9 C14 C13 -174.3(3) . . . . ?
N1 C15 C16 N17 -29.8(4) . . . . ?
N1 C15 C16 C21 153.7(3) . . . . ?
N17 C18 C19 C20 -0.3(5) . . . . ?
C18 C19 C20 C21 1.6(5) . . . . ?
C19 C20 C21 C16 -1.3(5) . . . . ?
N17 C16 C21 C20 -0.2(5) . . . . ?
C15 C16 C21 C20 176.2(3) . . . . ?
N4 C22 C23 N24 30.3(3) . . . . ?
N4 C22 C23 C28 -148.9(3) . . . . ?
N24 C25 C26 C27 -0.2(5) . . . . ?
C25 C26 C27 C28 0.2(5) . . . . ?
C26 C27 C28 C23 -0.3(4) . . . . ?
N24 C23 C28 C27 0.3(4) . . . . ?
C22 C23 C28 C27 179.5(3) . . . . ?
C16 C15 N1 C2 -77.5(3) . . . . ?
C16 C15 N1 C7 158.3(2) . . . . ?
C16 C15 N1 Fe1 28.3(3) . . . . ?
C3 C2 N1 C15 175.4(2) . . . . ?
C3 C2 N1 C7 -59.0(3) . . . . ?
C3 C2 N1 Fe1 61.9(2) . . . . ?
C6 C7 N1 C15 -134.5(3) . . . . ?
C6 C7 N1 C2 99.9(3) . . . . ?
C6 C7 N1 Fe1 -8.4(3) . . . . ?
C23 C22 N4 C5 -170.0(2) . . . . ?
C23 C22 N4 C3 65.7(3) . . . . ?
C23 C22 N4 Fe1 -51.2(2) . . . . ?
C6 C5 N4 C22 164.4(2) . . . . ?
C6 C5 N4 C3 -71.6(3) . . . . ?
C6 C5 N4 Fe1 47.1(3) . . . . ?
C2 C3 N4 C22 -134.6(2) . . . . ?
C2 C3 N4 C5 100.5(3) . . . . ?
C2 C3 N4 Fe1 -18.7(3) . . . . ?
C12 C11 N10 C9 0.1(5) . . . . ?
C12 C11 N10 Fe1 178.0(3) . . . . ?
C14 C9 N10 C11 -2.1(4) . . . . ?
C6 C9 N10 C11 174.9(3) . . . . ?
C14 C9 N10 Fe1 -179.9(2) . . . . ?
C6 C9 N10 Fe1 -2.9(3) . . . . ?
C19 C18 N17 C16 -1.2(4) . . . . ?
C19 C18 N17 Fe1 168.1(2) . . . . ?
C21 C16 N17 C18 1.4(4) . . . . ?
C15 C16 N17 C18 -175.2(3) . . . . ?
C21 C16 N17 Fe1 -168.5(2) . . . . ?
C15 C16 N17 Fe1 14.9(3) . . . . ?
C26 C25 N24 C23 0.3(4) . . . . ?
C26 C25 N24 Fe1 174.2(2) . . . . ?
C28 C23 N24 C25 -0.3(4) . . . . ?
C22 C23 N24 C25 -179.6(3) . . . . ?
C28 C23 N24 Fe1 -175.3(2) . . . . ?
C22 C23 N24 Fe1 5.4(3) . . . . ?
C18 N17 Fe1 O1B 23.8(5) . . . . ?
C16 N17 Fe1 O1B -166.9(5) . . . . ?
C18 N17 Fe1 O1A 25.2(4) . . . . ?
C16 N17 Fe1 O1A -165.5(4) . . . . ?
C18 N17 Fe1 N10 112.5(2) . . . . ?
C16 N17 Fe1 N10 -78.2(2) . . . . ?
C18 N17 Fe1 N4 -129.2(2) . . . . ?
C16 N17 Fe1 N4 40.2(3) . . . . ?
C18 N17 Fe1 N24 -58.3(2) . . . . ?
C16 N17 Fe1 N24 111.0(2) . . . . ?
C18 N17 Fe1 N1 -168.3(2) . . . . ?
C16 N17 Fe1 N1 1.1(2) . . . . ?
C11 N10 Fe1 O1B 50.5(5) . . . . ?
C9 N10 Fe1 O1B -131.7(5) . . . . ?
C11 N10 Fe1 N17 -55.5(2) . . . . ?
C9 N10 Fe1 N17 122.3(2) . . . . ?
C11 N10 Fe1 O1A 36.8(3) . . . . ?
C9 N10 Fe1 O1A -145.3(3) . . . . ?
C11 N10 Fe1 N4 158.1(2) . . . . ?
C9 N10 Fe1 N4 -24.0(2) . . . . ?
C11 N10 Fe1 N24 98.3(3) . . . . ?
C9 N10 Fe1 N24 -83.8(3) . . . . ?
C11 N10 Fe1 N1 -130.5(2) . . . . ?
C9 N10 Fe1 N1 47.3(2) . . . . ?
C22 N4 Fe1 O1B -33.2(4) . . . . ?
C5 N4 Fe1 O1B 87.7(4) . . . . ?
C3 N4 Fe1 O1B -151.8(4) . . . . ?
C22 N4 Fe1 N17 119.52(19) . . . . ?
C5 N4 Fe1 N17 -119.54(19) . . . . ?
C3 N4 Fe1 N17 0.9(2) . . . . ?
C22 N4 Fe1 O1A -30.0(5) . . . . ?
C5 N4 Fe1 O1A 90.9(5) . . . . ?
C3 N4 Fe1 O1A -148.6(4) . . . . ?
C22 N4 Fe1 N10 -120.15(17) . . . . ?
C5 N4 Fe1 N10 0.78(19) . . . . ?
C3 N4 Fe1 N10 121.27(17) . . . . ?
C22 N4 Fe1 N24 40.92(17) . . . . ?
C5 N4 Fe1 N24 161.9(2) . . . . ?
C3 N4 Fe1 N24 -77.66(17) . . . . ?
C22 N4 Fe1 N1 159.69(19) . . . . ?
C5 N4 Fe1 N1 -79.37(18) . . . . ?
C3 N4 Fe1 N1 41.11(16) . . . . ?
C25 N24 Fe1 O1B -88.3(5) . . . . ?
C23 N24 Fe1 O1B 85.9(5) . . . . ?
C25 N24 Fe1 N17 17.6(3) . . . . ?
C23 N24 Fe1 N17 -168.13(19) . . . . ?
C25 N24 Fe1 O1A -74.7(4) . . . . ?
C23 N24 Fe1 O1A 99.5(3) . . . . ?
C25 N24 Fe1 N10 -136.8(3) . . . . ?
C23 N24 Fe1 N10 37.5(3) . . . . ?
C25 N24 Fe1 N4 159.6(3) . . . . ?
C23 N24 Fe1 N4 -26.17(18) . . . . ?
C25 N24 Fe1 N1 96.2(3) . . . . ?
C23 N24 Fe1 N1 -89.5(2) . . . . ?
C15 N1 Fe1 O1B 94(2) . . . . ?
C2 N1 Fe1 O1B -150(2) . . . . ?
C7 N1 Fe1 O1B -34(2) . . . . ?
C15 N1 Fe1 N17 -16.30(18) . . . . ?
C2 N1 Fe1 N17 99.95(17) . . . . ?
C7 N1 Fe1 N17 -144.2(2) . . . . ?
C15 N1 Fe1 O1A 38.6(12) . . . . ?
C2 N1 Fe1 O1A 154.8(11) . . . . ?
C7 N1 Fe1 O1A -89.3(12) . . . . ?
C15 N1 Fe1 N10 88.89(19) . . . . ?
C2 N1 Fe1 N10 -154.87(17) . . . . ?
C7 N1 Fe1 N10 -39.06(19) . . . . ?
C15 N1 Fe1 N4 -171.9(2) . . . . ?
C2 N1 Fe1 N4 -55.62(16) . . . . ?
C7 N1 Fe1 N4 60.18(18) . . . . ?
C15 N1 Fe1 N24 -107.95(18) . . . . ?
C2 N1 Fe1 N24 8.30(18) . . . . ?
C7 N1 Fe1 N24 124.11(18) . . . . ?
O1B Fe1 O1A S1A -9.0(18) . . . . ?
N17 Fe1 O1A S1A 176.7(14) . . . . ?
N10 Fe1 O1A S1A 73.9(14) . . . . ?
N4 Fe1 O1A S1A -21.8(16) . . . . ?
N24 Fe1 O1A S1A -87.6(14) . . . . ?
N1 Fe1 O1A S1A 123.7(10) . . . . ?
Fe1 O1A S1A O2A 22.0(19) . . . . ?
Fe1 O1A S1A O3A -124.2(15) . . . . ?
Fe1 O1A S1A C29A 139.5(14) . . . . ?
O2A S1A C29A F3A -60.7(12) . . . . ?
O3A S1A C29A F3A 53.9(13) . . . . ?
O1A S1A C29A F3A 159.6(11) . . . . ?
O2A S1A C29A F1A -172.0(12) . . . . ?
O3A S1A C29A F1A -57.5(13) . . . . ?
O1A S1A C29A F1A 48.2(11) . . . . ?
O2A S1A C29A F2A 67.8(11) . . . . ?
O3A S1A C29A F2A -177.7(12) . . . . ?
O1A S1A C29A F2A -72.0(10) . . . . ?
O1B S1B C29B F3B -171.2(11) . . . . ?
O2B S1B C29B F3B -69.2(11) . . . . ?
O3B S1B C29B F3B 59.6(12) . . . . ?
O1B S1B C29B F1B 50.7(12) . . . . ?
O2B S1B C29B F1B 152.6(11) . . . . ?
O3B S1B C29B F1B -78.5(12) . . . . ?
O1B S1B C29B F2B -61.5(11) . . . . ?
O2B S1B C29B F2B 40.4(11) . . . . ?
O3B S1B C29B F2B 169.3(10) . . . . ?
F6 C30 S2 O5 -179.8(3) . . . . ?
F5 C30 S2 O5 -59.9(3) . . . . ?
F4 C30 S2 O5 58.7(3) . . . . ?
F6 C30 S2 O6 60.6(3) . . . . ?
F5 C30 S2 O6 -179.5(2) . . . . ?
F4 C30 S2 O6 -60.8(3) . . . . ?
F6 C30 S2 O4 -58.8(3) . . . . ?
F5 C30 S2 O4 61.1(3) . . . . ?
F4 C30 S2 O4 179.7(3) . . . . ?

# 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
####################################################################### 
# 
# 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_mer-2-otf
_database_code_depnum_ccdc_archive 'CCDC 1008835'
_audit_update_record             
;
2014-06-17 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;

_audit_creation_date             2014-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;(trifluoromethanesulfonato)[N¹,N³,2-trimethyl-2-(pyridin-2-yl)-
        N¹,N³-bis(pyridin-2-ylmethyl)propane-1,3-diamine]iron(II)
        trifluoromethanesulfonate--dichloromethane(1/1)
;
_chemical_formula_iupac          
'[Fe(C F3 S O3)(C23 H29 N5)](C F3 S O3).C H2 Cl2'
_chemical_formula_moiety         
'C24 H29 F3 Fe N5 O3 S 1+, C F3 O3 S 1-, C H2 Cl2'
_chemical_formula_sum            'C26 H31 Cl2 F6 Fe N5 O6 S2'
_chemical_formula_weight         814.43

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

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 21/c'
_space_group_IT_number           14
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   13.4336(2)
_cell_length_b                   20.5689(2)
_cell_length_c                   13.4353(2)
_cell_angle_alpha                90
_cell_angle_beta                 115.080(2)
_cell_angle_gamma                90
_cell_volume                     3362.35(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    20146
_cell_measurement_theta_min      3.621
_cell_measurement_theta_max      73.648

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

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.283
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1664
_exptl_crystal_recrystallization_method 
'precipitation: dichloromethane, diethyl ether, vapour diffusion, r.t., 5 d'

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

_exptl_absorpt_coefficient_mu    6.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.32926
_exptl_absorpt_correction_T_max  1.00000

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

_diffrn_source                   'micro-focus sealed tube'
_diffrn_source_type              'Agilent Nova'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Atlas'
_diffrn_detector_area_resol_mean 10.5435
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova (Single Source)'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.02
_diffrn_reflns_number            30155
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.63
_diffrn_reflns_theta_max         70
_diffrn_reflns_theta_full        70
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             6379
_reflns_number_gt                6111
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

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

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

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

_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.
 The trifluoromethanesulfonato ligand exhibits rotational disorder about the
 O40-S43 axis and was modelled in two discrete positions. Occupancies refined
 to 0.52(3)/0.48(3).
;
_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)+(0.0487P)²+2.6248P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6379
_refine_ls_number_parameters     491
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0339
_refine_ls_wR_factor_ref         0.0899
_refine_ls_wR_factor_gt          0.0885
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.061

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_restr_special_details           
;
 The two positions of the trifluoromethanesulfonato ligand were treated using
 equal-1,2- and equal-1,3-distance restraints generated by SHELXL-97 SAME
 (for the whole ligand) with standard weights.
;
loop_
_restr_U_rigid_atom_site_label_1
_restr_U_rigid_site_symmetry_1
_restr_U_rigid_atom_site_label_2
_restr_U_rigid_site_symmetry_2
_restr_U_rigid_target_weight_param
_restr_U_rigid_U_parallel
_restr_U_rigid_diff
_restr_U_rigid_details
S43 . O41B . 0.01 0 0.0003 'SHELXL DELU'
S43 . O42A . 0.01 0 0.0011 'SHELXL DELU'
S43 . O41A . 0.01 0 0.001 'SHELXL DELU'
S43 . O42B . 0.01 0 0.0012 'SHELXL DELU'
S43 . C44A . 0.01 0 0.0083 'SHELXL DELU'
S43 . F45A . 0.01 0 0.0075 'SHELXL DELU'
S43 . F47A . 0.01 0 0.0025 'SHELXL DELU'
S43 . F46A . 0.01 0 0.0057 'SHELXL DELU'
S43 . C44B . 0.01 0 0.0043 'SHELXL DELU'
S43 . F47B . 0.01 0 0.001 'SHELXL DELU'
S43 . F45B . 0.01 0 0.0046 'SHELXL DELU'
S43 . F46B . 0.01 0 0.0046 'SHELXL DELU'
O41A . O42A . 0.01 0 0.0003 'SHELXL DELU'
O41A . C44A . 0.01 0 0.0001 'SHELXL DELU'
O42A . C44A . 0.01 0 0.0094 'SHELXL DELU'
C44A . F45A . 0.01 0 0.0019 'SHELXL DELU'
C44A . F47A . 0.01 0 0.0041 'SHELXL DELU'
C44A . F46A . 0.01 0 0.0018 'SHELXL DELU'
F45A . F47A . 0.01 0 0.0026 'SHELXL DELU'
F45A . F46A . 0.01 0 0.0095 'SHELXL DELU'
F46A . F47A . 0.01 0 0.0069 'SHELXL DELU'
O41B . O42B . 0.01 0 0.0034 'SHELXL DELU'
O41B . C44B . 0.01 0 0.0066 'SHELXL DELU'
O42B . C44B . 0.01 0 0.0009 'SHELXL DELU'
C44B . F47B . 0.01 0 0.0023 'SHELXL DELU'
C44B . F45B . 0.01 0 0.001 'SHELXL DELU'
C44B . F46B . 0.01 0 0.0078 'SHELXL DELU'
F45B . F47B . 0.01 0 0.0022 'SHELXL DELU'
F45B . F46B . 0.01 0 0.0027 'SHELXL DELU'
F46B . F47B . 0.01 0 0.0017 'SHELXL DELU'

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
O41A 0.01
O42A 0.01
C44A 0.01
F45A 0.01
F46A 0.01
F47A 0.01
O41B 0.01
O42B 0.01
C44B 0.01
F45B 0.01
F46B 0.01
F47B 0.01

loop_
_restr_parameter_class_class_id
_restr_parameter_class_parameter_type
_restr_parameter_class_target
_restr_parameter_class_target_weight_param
_restr_parameter_class_details
1 occupancy 1 0 'total s.o.f. of 1'
2 occupancy 1 0 'total s.o.f. of 1'
3 occupancy 1 0 'total s.o.f. of 1'
4 occupancy 1 0 'total s.o.f. of 1'
5 occupancy 1 0 'total s.o.f. of 1'
6 occupancy 1 0 'total s.o.f. of 1'

loop_
_restr_parameter_id
_restr_parameter_class_id
_restr_parameter_atom_site_label
_restr_parameter_atom_coefficient
1 1 O41A 1
2 1 O41B 1
3 2 O42A 1
4 2 O42B 1
5 3 C44A 1
6 3 C44B 1
7 4 F45A 1
8 4 F45B 1
9 5 F46A 1
10 5 F46B 1
11 6 F47A 1
12 6 F47B 1

#----------------------------------------------------------------------------#
#                   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 0.0181 0.0091 '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 -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.44421(17) 0.63152(10) 0.59352(17) 0.0238(4) Uani 1 1 d . . .
H11 H 0.4557 0.5888 0.5735 0.029 Uiso 1 1 calc R . .
C12 C 0.49811(19) 0.68252(11) 0.57087(18) 0.0296(5) Uani 1 1 d . . .
H12 H 0.5459 0.6753 0.5363 0.036 Uiso 1 1 calc R . .
C13 C 0.48043(19) 0.74440(11) 0.59998(18) 0.0300(5) Uani 1 1 d . . .
H13 H 0.5169 0.7806 0.5864 0.036 Uiso 1 1 calc R . .
C14 C 0.40948(18) 0.75339(10) 0.64902(17) 0.0250(4) Uani 1 1 d . . .
H14 H 0.396 0.7959 0.6681 0.03 Uiso 1 1 calc R . .
C15 C 0.35785(16) 0.70001(9) 0.67041(15) 0.0183(4) Uani 1 1 d . . .
C16 C 0.28208(16) 0.70523(9) 0.72870(16) 0.0184(4) Uani 1 1 d . . .
C17 C 0.27414(18) 0.77594(9) 0.76252(18) 0.0262(4) Uani 1 1 d . . .
H17A H 0.3472 0.7911 0.8137 0.039 Uiso 1 1 calc R . .
H17B H 0.224 0.778 0.7983 0.039 Uiso 1 1 calc R . .
H17C H 0.2462 0.8037 0.6971 0.039 Uiso 1 1 calc R . .
C21 C 0.20080(17) 0.42030(10) 0.70063(18) 0.0233(4) Uani 1 1 d . . .
H21 H 0.1959 0.4101 0.6297 0.028 Uiso 1 1 calc R . .
C22 C 0.18166(18) 0.37150(10) 0.7609(2) 0.0284(5) Uani 1 1 d . . .
H22 H 0.163 0.3288 0.7319 0.034 Uiso 1 1 calc R . .
C23 C 0.19041(19) 0.38649(11) 0.8648(2) 0.0309(5) Uani 1 1 d . . .
H23 H 0.1783 0.354 0.9086 0.037 Uiso 1 1 calc R . .
C24 C 0.21707(19) 0.44938(11) 0.90408(19) 0.0282(5) Uani 1 1 d . . .
H24 H 0.2236 0.4605 0.9752 0.034 Uiso 1 1 calc R . .
C25 C 0.23401(17) 0.49581(10) 0.83826(16) 0.0210(4) Uani 1 1 d . . .
C26 C 0.25849(18) 0.56598(10) 0.87342(17) 0.0227(4) Uani 1 1 d . . .
H26A H 0.1891 0.5911 0.845 0.027 Uiso 1 1 calc R . .
H26B H 0.2919 0.5686 0.9547 0.027 Uiso 1 1 calc R . .
C28 C 0.33277(17) 0.66736(9) 0.83865(15) 0.0194(4) Uani 1 1 d . . .
H28A H 0.4093 0.6826 0.8802 0.023 Uiso 1 1 calc R . .
H28B H 0.2915 0.6791 0.8821 0.023 Uiso 1 1 calc R . .
C29 C 0.44771(17) 0.57044(10) 0.89915(17) 0.0238(4) Uani 1 1 d . . .
H29A H 0.4731 0.5869 0.9744 0.036 Uiso 1 1 calc R . .
H29B H 0.4972 0.5856 0.8675 0.036 Uiso 1 1 calc R . .
H29C H 0.4473 0.5228 0.9001 0.036 Uiso 1 1 calc R . .
C31 C 0.22593(16) 0.47187(9) 0.44869(16) 0.0206(4) Uani 1 1 d . . .
H31 H 0.2753 0.4402 0.4952 0.025 Uiso 1 1 calc R . .
C32 C 0.17075(18) 0.45851(10) 0.33785(17) 0.0251(4) Uani 1 1 d . . .
H32 H 0.1805 0.4181 0.3089 0.03 Uiso 1 1 calc R . .
C33 C 0.10094(18) 0.50528(12) 0.26988(17) 0.0290(5) Uani 1 1 d . . .
H33 H 0.0624 0.4976 0.1932 0.035 Uiso 1 1 calc R . .
C34 C 0.08788(18) 0.56326(11) 0.31474(17) 0.0253(4) Uani 1 1 d . . .
H34 H 0.0412 0.5962 0.269 0.03 Uiso 1 1 calc R . .
C35 C 0.14349(16) 0.57310(9) 0.42713(16) 0.0185(4) Uani 1 1 d . . .
C36 C 0.13220(16) 0.63493(9) 0.48112(15) 0.0194(4) Uani 1 1 d . . .
H36A H 0.1889 0.6664 0.4832 0.023 Uiso 1 1 calc R . .
H36B H 0.0591 0.6544 0.4374 0.023 Uiso 1 1 calc R . .
C38 C 0.16183(16) 0.68505(9) 0.65613(16) 0.0186(4) Uani 1 1 d . . .
H38A H 0.1223 0.6824 0.7037 0.022 Uiso 1 1 calc R . .
H38B H 0.1269 0.7201 0.6021 0.022 Uiso 1 1 calc R . .
C39 C 0.04201(16) 0.59192(10) 0.58741(17) 0.0223(4) Uani 1 1 d . . .
H39A H -0.0194 0.6221 0.552 0.034 Uiso 1 1 calc R . .
H39B H 0.0494 0.5816 0.6614 0.034 Uiso 1 1 calc R . .
H39C H 0.028 0.5519 0.544 0.034 Uiso 1 1 calc R . .
Fe1 Fe 0.28822(2) 0.556717(13) 0.66505(2) 0.01386(9) Uani 1 1 d . . .
N10 N 0.37613(13) 0.63936(8) 0.64263(13) 0.0181(3) Uani 1 1 d . . .
N20 N 0.22613(13) 0.48165(8) 0.73762(13) 0.0192(3) Uani 1 1 d . . .
N27 N 0.33467(13) 0.59472(7) 0.83153(12) 0.0165(3) Uani 1 1 d . . .
N30 N 0.21261(13) 0.52800(8) 0.49375(13) 0.0178(3) Uani 1 1 d . . .
N37 N 0.14478(13) 0.62235(7) 0.59474(13) 0.0166(3) Uani 1 1 d . . .
O40 O 0.41902(12) 0.49293(7) 0.68425(12) 0.0247(3) Uani 1 1 d D A .
S43 S 0.48746(4) 0.43524(2) 0.72396(4) 0.02127(12) Uani 1 1 d DU . .
O41A O 0.459(2) 0.3845(9) 0.6432(17) 0.032(3) Uani 0.52(3) 1 d PDU A 1
O42A O 0.4997(13) 0.4161(8) 0.8314(8) 0.036(2) Uani 0.52(3) 1 d PDU A 1
C44A C 0.6200(7) 0.4646(5) 0.7409(13) 0.035(2) Uani 0.52(3) 1 d PDU A 1
F45A F 0.6478(12) 0.5184(6) 0.7990(13) 0.059(3) Uani 0.52(3) 1 d PDU A 1
F46A F 0.6140(11) 0.4760(7) 0.6417(13) 0.074(3) Uani 0.52(3) 1 d PDU A 1
F47A F 0.6975(6) 0.4213(4) 0.7896(15) 0.066(3) Uani 0.52(3) 1 d PDU A 1
O41B O 0.454(2) 0.3811(9) 0.6509(19) 0.030(3) Uani 0.48(3) 1 d PDU A 2
O42B O 0.5280(12) 0.4214(9) 0.8393(8) 0.035(2) Uani 0.48(3) 1 d PDU A 2
C44B C 0.6108(8) 0.4665(5) 0.7124(11) 0.025(2) Uani 0.48(3) 1 d PDU A 2
F45B F 0.6502(13) 0.5183(6) 0.7760(12) 0.0425(19) Uani 0.48(3) 1 d PDU A 2
F46B F 0.5894(10) 0.4854(4) 0.6108(9) 0.042(2) Uani 0.48(3) 1 d PDU A 2
F47B F 0.6892(9) 0.4220(4) 0.7412(16) 0.055(3) Uani 0.48(3) 1 d PDU A 2
C54 C 0.9928(2) 0.37399(12) 1.0185(2) 0.0354(5) Uani 1 1 d . . .
O50 O 0.85972(13) 0.29610(8) 1.04985(14) 0.0327(4) Uani 1 1 d . . .
O51 O 1.05015(14) 0.26361(8) 1.11347(16) 0.0403(4) Uani 1 1 d . . .
O52 O 0.99946(15) 0.35006(9) 1.20703(14) 0.0402(4) Uani 1 1 d . . .
S53 S 0.97348(4) 0.31380(2) 1.10779(4) 0.02150(11) Uani 1 1 d . . .
F55 F 0.92679(17) 0.42511(8) 1.00364(18) 0.0660(5) Uani 1 1 d . . .
F56 F 0.97312(16) 0.34933(10) 0.92051(13) 0.0602(5) Uani 1 1 d . . .
F57 F 1.09557(14) 0.39698(8) 1.06168(14) 0.0511(4) Uani 1 1 d . . .
Cl60 Cl 0.20998(7) 0.21072(4) 0.96067(9) 0.0660(2) Uani 1 1 d . . .
C61 C 0.2819(2) 0.23797(13) 1.0966(3) 0.0480(7) Uani 1 1 d . . .
H61A H 0.2288 0.2497 1.127 0.058 Uiso 1 1 calc R . .
H61B H 0.3289 0.2024 1.1421 0.058 Uiso 1 1 calc R . .
Cl62 Cl 0.36411(7) 0.30567(4) 1.10367(8) 0.0770(3) Uani 1 1 d . . .


#----------------------------------------------------------------------------#
#                   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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.345(3) . ?
C11 C12 1.380(3) . ?
C12 C13 1.381(3) . ?
C13 C14 1.382(3) . ?
C14 C15 1.392(3) . ?
C15 N10 1.354(2) . ?
C15 C16 1.529(3) . ?
C16 C17 1.541(2) . ?
C16 C38 1.548(3) . ?
C16 C28 1.549(3) . ?
C21 N20 1.346(3) . ?
C21 C22 1.380(3) . ?
C22 C23 1.385(3) . ?
C23 C24 1.386(3) . ?
C24 C25 1.384(3) . ?
C25 N20 1.343(3) . ?
C25 C26 1.511(3) . ?
C26 N27 1.484(2) . ?
C28 N27 1.498(2) . ?
C29 N27 1.487(3) . ?
C31 N30 1.350(2) . ?
C31 C32 1.381(3) . ?
C32 C33 1.383(3) . ?
C33 C34 1.380(3) . ?
C34 C35 1.387(3) . ?
C35 N30 1.349(3) . ?
C35 C36 1.503(3) . ?
C36 N37 1.486(2) . ?
C38 N37 1.495(2) . ?
C39 N37 1.481(2) . ?
Fe1 O40 2.1194(14) . ?
Fe1 N10 2.1626(16) . ?
Fe1 N30 2.1669(16) . ?
Fe1 N20 2.1725(16) . ?
Fe1 N27 2.1954(15) . ?
Fe1 N37 2.2101(16) . ?
O40 S43 1.4567(14) . ?
S43 O41B 1.426(9) . ?
S43 O42A 1.437(8) . ?
S43 O41A 1.436(9) . ?
S43 O42B 1.437(9) . ?
S43 C44A 1.801(9) . ?
S43 C44B 1.844(8) . ?
C44A F45A 1.314(10) . ?
C44A F47A 1.314(9) . ?
C44A F46A 1.322(9) . ?
C44B F47B 1.323(9) . ?
C44B F45B 1.328(10) . ?
C44B F46B 1.329(10) . ?
C54 F56 1.329(3) . ?
C54 F57 1.337(3) . ?
C54 F55 1.335(3) . ?
C54 S53 1.817(2) . ?
O50 S53 1.4371(16) . ?
O51 S53 1.4372(17) . ?
O52 S53 1.4359(16) . ?
Cl60 C61 1.757(4) . ?
C61 Cl62 1.755(3) . ?

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
N10 C11 C12 123.1(2) . . ?
C11 C12 C13 118.0(2) . . ?
C14 C13 C12 119.63(19) . . ?
C13 C14 C15 119.8(2) . . ?
N10 C15 C14 120.35(19) . . ?
N10 C15 C16 116.35(16) . . ?
C14 C15 C16 123.27(18) . . ?
C15 C16 C17 111.20(16) . . ?
C15 C16 C38 113.71(15) . . ?
C17 C16 C38 104.75(15) . . ?
C15 C16 C28 109.53(15) . . ?
C17 C16 C28 104.53(15) . . ?
C38 C16 C28 112.66(16) . . ?
N20 C21 C22 123.1(2) . . ?
C21 C22 C23 118.1(2) . . ?
C22 C23 C24 119.3(2) . . ?
C25 C24 C23 119.1(2) . . ?
N20 C25 C24 121.97(19) . . ?
N20 C25 C26 115.85(17) . . ?
C24 C25 C26 122.15(19) . . ?
N27 C26 C25 110.83(16) . . ?
N27 C28 C16 116.94(15) . . ?
N30 C31 C32 122.76(19) . . ?
C31 C32 C33 118.51(19) . . ?
C34 C33 C32 119.26(19) . . ?
C33 C34 C35 119.5(2) . . ?
N30 C35 C34 121.59(18) . . ?
N30 C35 C36 116.33(17) . . ?
C34 C35 C36 122.07(18) . . ?
N37 C36 C35 110.96(15) . . ?
N37 C38 C16 116.97(15) . . ?
O40 Fe1 N10 91.72(6) . . ?
O40 Fe1 N30 87.23(6) . . ?
N10 Fe1 N30 95.98(6) . . ?
O40 Fe1 N20 87.80(6) . . ?
N10 Fe1 N20 163.21(6) . . ?
N30 Fe1 N20 100.76(6) . . ?
O40 Fe1 N27 103.50(6) . . ?
N10 Fe1 N27 85.75(6) . . ?
N30 Fe1 N27 169.10(6) . . ?
N20 Fe1 N27 78.07(6) . . ?
O40 Fe1 N37 163.31(6) . . ?
N10 Fe1 N37 83.62(6) . . ?
N30 Fe1 N37 77.37(6) . . ?
N20 Fe1 N37 101.24(6) . . ?
N27 Fe1 N37 92.16(6) . . ?
C11 N10 C15 119.08(17) . . ?
C11 N10 Fe1 119.94(13) . . ?
C15 N10 Fe1 120.81(13) . . ?
C25 N20 C21 118.35(17) . . ?
C25 N20 Fe1 114.60(13) . . ?
C21 N20 Fe1 125.85(14) . . ?
C26 N27 C29 108.93(15) . . ?
C26 N27 C28 109.87(15) . . ?
C29 N27 C28 109.67(15) . . ?
C26 N27 Fe1 107.50(12) . . ?
C29 N27 Fe1 106.17(11) . . ?
C28 N27 Fe1 114.52(11) . . ?
C35 N30 C31 118.38(17) . . ?
C35 N30 Fe1 113.47(12) . . ?
C31 N30 Fe1 128.15(13) . . ?
C39 N37 C36 107.97(15) . . ?
C39 N37 C38 108.77(15) . . ?
C36 N37 C38 109.93(14) . . ?
C39 N37 Fe1 112.93(11) . . ?
C36 N37 Fe1 104.14(11) . . ?
C38 N37 Fe1 112.90(11) . . ?
S43 O40 Fe1 155.63(10) . . ?
O42A S43 O41A 116.1(11) . . ?
O41B S43 O42B 116.9(12) . . ?
O41B S43 O40 114.8(11) . . ?
O42A S43 O40 112.1(6) . . ?
O41A S43 O40 113.1(10) . . ?
O42B S43 O40 116.7(7) . . ?
O42A S43 C44A 106.2(5) . . ?
O41A S43 C44A 105.7(10) . . ?
O40 S43 C44A 102.1(4) . . ?
O41B S43 C44B 104.2(11) . . ?
O42B S43 C44B 102.5(6) . . ?
O40 S43 C44B 97.8(3) . . ?
F45A C44A F47A 108.0(10) . . ?
F45A C44A F46A 109.3(10) . . ?
F47A C44A F46A 108.6(9) . . ?
F45A C44A S43 112.0(9) . . ?
F47A C44A S43 111.6(8) . . ?
F46A C44A S43 107.3(7) . . ?
F47B C44B F45B 108.5(11) . . ?
F47B C44B F46B 107.5(8) . . ?
F45B C44B F46B 106.2(9) . . ?
F47B C44B S43 111.5(7) . . ?
F45B C44B S43 110.7(8) . . ?
F46B C44B S43 112.2(7) . . ?
F56 C54 F57 107.5(2) . . ?
F56 C54 F55 108.2(2) . . ?
F57 C54 F55 106.5(2) . . ?
F56 C54 S53 111.70(17) . . ?
F57 C54 S53 111.41(18) . . ?
F55 C54 S53 111.33(18) . . ?
O52 S53 O50 114.75(10) . . ?
O52 S53 O51 115.92(12) . . ?
O50 S53 O51 114.87(10) . . ?
O52 S53 C54 102.26(11) . . ?
O50 S53 C54 103.40(11) . . ?
O51 S53 C54 102.98(12) . . ?
Cl62 C61 Cl60 111.43(17) . . ?

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
N10 C11 C12 C13 -0.3(3) . . . . ?
C11 C12 C13 C14 -0.7(3) . . . . ?
C12 C13 C14 C15 1.1(3) . . . . ?
C13 C14 C15 N10 -0.5(3) . . . . ?
C13 C14 C15 C16 177.32(19) . . . . ?
N10 C15 C16 C17 176.26(16) . . . . ?
C14 C15 C16 C17 -1.7(3) . . . . ?
N10 C15 C16 C38 -65.8(2) . . . . ?
C14 C15 C16 C38 116.3(2) . . . . ?
N10 C15 C16 C28 61.2(2) . . . . ?
C14 C15 C16 C28 -116.7(2) . . . . ?
N20 C21 C22 C23 -0.8(3) . . . . ?
C21 C22 C23 C24 0.4(3) . . . . ?
C22 C23 C24 C25 0.2(3) . . . . ?
C23 C24 C25 N20 -0.5(3) . . . . ?
C23 C24 C25 C26 177.3(2) . . . . ?
N20 C25 C26 N27 -36.3(2) . . . . ?
C24 C25 C26 N27 145.8(2) . . . . ?
C15 C16 C28 N27 -70.0(2) . . . . ?
C17 C16 C28 N27 170.76(17) . . . . ?
C38 C16 C28 N27 57.6(2) . . . . ?
N30 C31 C32 C33 1.6(3) . . . . ?
C31 C32 C33 C34 -0.6(3) . . . . ?
C32 C33 C34 C35 -1.0(3) . . . . ?
C33 C34 C35 N30 1.8(3) . . . . ?
C33 C34 C35 C36 -179.58(19) . . . . ?
N30 C35 C36 N37 -32.4(2) . . . . ?
C34 C35 C36 N37 148.92(19) . . . . ?
C15 C16 C38 N37 48.0(2) . . . . ?
C17 C16 C38 N37 169.61(16) . . . . ?
C28 C16 C38 N37 -77.4(2) . . . . ?
C12 C11 N10 C15 0.8(3) . . . . ?
C12 C11 N10 Fe1 176.22(17) . . . . ?
C14 C15 N10 C11 -0.4(3) . . . . ?
C16 C15 N10 C11 -178.41(17) . . . . ?
C14 C15 N10 Fe1 -175.78(14) . . . . ?
C16 C15 N10 Fe1 6.2(2) . . . . ?
O40 Fe1 N10 C11 32.50(15) . . . . ?
N30 Fe1 N10 C11 -54.90(15) . . . . ?
N20 Fe1 N10 C11 120.6(2) . . . . ?
N27 Fe1 N10 C11 135.91(15) . . . . ?
N37 Fe1 N10 C11 -131.43(15) . . . . ?
O40 Fe1 N10 C15 -152.19(15) . . . . ?
N30 Fe1 N10 C15 120.42(14) . . . . ?
N20 Fe1 N10 C15 -64.1(3) . . . . ?
N27 Fe1 N10 C15 -48.77(14) . . . . ?
N37 Fe1 N10 C15 43.89(14) . . . . ?
C24 C25 N20 C21 0.1(3) . . . . ?
C26 C25 N20 C21 -177.82(18) . . . . ?
C24 C25 N20 Fe1 -168.16(17) . . . . ?
C26 C25 N20 Fe1 13.9(2) . . . . ?
C22 C21 N20 C25 0.6(3) . . . . ?
C22 C21 N20 Fe1 167.37(16) . . . . ?
O40 Fe1 N20 C25 110.65(14) . . . . ?
N10 Fe1 N20 C25 22.0(3) . . . . ?
N30 Fe1 N20 C25 -162.59(14) . . . . ?
N27 Fe1 N20 C25 6.35(14) . . . . ?
N37 Fe1 N20 C25 -83.50(14) . . . . ?
O40 Fe1 N20 C21 -56.58(17) . . . . ?
N10 Fe1 N20 C21 -145.2(2) . . . . ?
N30 Fe1 N20 C21 30.19(17) . . . . ?
N27 Fe1 N20 C21 -160.87(17) . . . . ?
N37 Fe1 N20 C21 109.28(16) . . . . ?
C25 C26 N27 C29 -76.0(2) . . . . ?
C25 C26 N27 C28 163.90(16) . . . . ?
C25 C26 N27 Fe1 38.69(18) . . . . ?
C16 C28 N27 C26 -111.92(19) . . . . ?
C16 C28 N27 C29 128.38(18) . . . . ?
C16 C28 N27 Fe1 9.2(2) . . . . ?
O40 Fe1 N27 C26 -109.31(12) . . . . ?
N10 Fe1 N27 C26 159.94(12) . . . . ?
N30 Fe1 N27 C26 60.4(4) . . . . ?
N20 Fe1 N27 C26 -24.53(12) . . . . ?
N37 Fe1 N27 C26 76.50(12) . . . . ?
O40 Fe1 N27 C29 7.16(13) . . . . ?
N10 Fe1 N27 C29 -83.60(12) . . . . ?
N30 Fe1 N27 C29 176.8(3) . . . . ?
N20 Fe1 N27 C29 91.93(12) . . . . ?
N37 Fe1 N27 C29 -167.03(12) . . . . ?
O40 Fe1 N27 C28 128.32(13) . . . . ?
N10 Fe1 N27 C28 37.57(13) . . . . ?
N30 Fe1 N27 C28 -62.0(4) . . . . ?
N20 Fe1 N27 C28 -146.91(14) . . . . ?
N37 Fe1 N27 C28 -45.87(13) . . . . ?
C34 C35 N30 C31 -0.8(3) . . . . ?
C36 C35 N30 C31 -179.53(16) . . . . ?
C34 C35 N30 Fe1 179.79(15) . . . . ?
C36 C35 N30 Fe1 1.1(2) . . . . ?
C32 C31 N30 C35 -0.9(3) . . . . ?
C32 C31 N30 Fe1 178.39(14) . . . . ?
O40 Fe1 N30 C35 -154.63(14) . . . . ?
N10 Fe1 N30 C35 -63.18(14) . . . . ?
N20 Fe1 N30 C35 118.14(13) . . . . ?
N27 Fe1 N30 C35 35.4(4) . . . . ?
N37 Fe1 N30 C35 18.89(13) . . . . ?
O40 Fe1 N30 C31 26.08(16) . . . . ?
N10 Fe1 N30 C31 117.52(16) . . . . ?
N20 Fe1 N30 C31 -61.15(17) . . . . ?
N27 Fe1 N30 C31 -143.9(3) . . . . ?
N37 Fe1 N30 C31 -160.41(17) . . . . ?
C35 C36 N37 C39 -75.78(19) . . . . ?
C35 C36 N37 C38 165.71(15) . . . . ?
C35 C36 N37 Fe1 44.49(17) . . . . ?
C16 C38 N37 C39 146.52(17) . . . . ?
C16 C38 N37 C36 -95.46(19) . . . . ?
C16 C38 N37 Fe1 20.3(2) . . . . ?
O40 Fe1 N37 C39 106.4(2) . . . . ?
N10 Fe1 N37 C39 -179.08(13) . . . . ?
N30 Fe1 N37 C39 83.31(13) . . . . ?
N20 Fe1 N37 C39 -15.34(13) . . . . ?
N27 Fe1 N37 C39 -93.60(13) . . . . ?
O40 Fe1 N37 C36 -10.4(3) . . . . ?
N10 Fe1 N37 C36 64.04(11) . . . . ?
N30 Fe1 N37 C36 -33.57(11) . . . . ?
N20 Fe1 N37 C36 -132.22(11) . . . . ?
N27 Fe1 N37 C36 149.52(11) . . . . ?
O40 Fe1 N37 C38 -129.7(2) . . . . ?
N10 Fe1 N37 C38 -55.17(12) . . . . ?
N30 Fe1 N37 C38 -152.78(13) . . . . ?
N20 Fe1 N37 C38 108.57(12) . . . . ?
N27 Fe1 N37 C38 30.31(13) . . . . ?
N10 Fe1 O40 S43 152.8(2) . . . . ?
N30 Fe1 O40 S43 -111.3(2) . . . . ?
N20 Fe1 O40 S43 -10.4(2) . . . . ?
N27 Fe1 O40 S43 66.7(3) . . . . ?
N37 Fe1 O40 S43 -133.9(2) . . . . ?
Fe1 O40 S43 O41B 92.5(13) . . . . ?
Fe1 O40 S43 O42A -34.4(8) . . . . ?
Fe1 O40 S43 O41A 99.2(12) . . . . ?
Fe1 O40 S43 O42B -49.7(8) . . . . ?
Fe1 O40 S43 C44A -147.7(6) . . . . ?
Fe1 O40 S43 C44B -157.9(5) . . . . ?
O42A S43 C44A F45A -66.6(11) . . . . ?
O41A S43 C44A F45A 169.4(14) . . . . ?
O40 S43 C44A F45A 51.0(10) . . . . ?
O42A S43 C44A F47A 54.6(10) . . . . ?
O41A S43 C44A F47A -69.4(13) . . . . ?
O40 S43 C44A F47A 172.2(7) . . . . ?
O42A S43 C44A F46A 173.5(10) . . . . ?
O41A S43 C44A F46A 49.5(14) . . . . ?
O40 S43 C44A F46A -68.9(10) . . . . ?
O41B S43 C44B F47B -60.0(14) . . . . ?
O42B S43 C44B F47B 62.3(11) . . . . ?
O40 S43 C44B F47B -178.1(8) . . . . ?
O41B S43 C44B F45B 179.1(15) . . . . ?
O42B S43 C44B F45B -58.6(13) . . . . ?
O40 S43 C44B F45B 61.0(10) . . . . ?
O41B S43 C44B F46B 60.6(13) . . . . ?
O42B S43 C44B F46B -177.1(10) . . . . ?
O40 S43 C44B F46B -57.4(7) . . . . ?
F56 C54 S53 O52 179.53(19) . . . . ?
F57 C54 S53 O52 59.3(2) . . . . ?
F55 C54 S53 O52 -59.4(2) . . . . ?
F56 C54 S53 O50 -61.0(2) . . . . ?
F57 C54 S53 O50 178.83(17) . . . . ?
F55 C54 S53 O50 60.0(2) . . . . ?
F56 C54 S53 O51 58.9(2) . . . . ?
F57 C54 S53 O51 -61.3(2) . . . . ?
F55 C54 S53 O51 179.95(18) . . . . ?

# 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
####################################################################### 
# 
# 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_mer-2-cl
_database_code_depnum_ccdc_archive 'CCDC 1008836'
_audit_update_record             
;
2014-06-17 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;

_audit_creation_date             2014-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;chlorido[N¹,N³,2-trimethyl-2-(pyridin-2-yl)-N¹,N³-bis(pyridin-
2-ylmethyl)propane-1,3-diamine]iron(II) hexafluorophosphate--diethyl ether(4/1)
;
_chemical_formula_iupac          '[Fe (C23 H29 N5) Cl](P F6).0.25C2 H5 O H'
_chemical_formula_moiety         'C23 H29 Cl Fe N5 1+, F6 P 1-, 0.25(C4 H10 O)'
_chemical_formula_sum            'C24 H31.50 Cl F6 Fe N5 O0.25 P'
_chemical_formula_weight         630.31

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

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_IT_number           2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.2754(4)
_cell_length_b                   12.0926(5)
_cell_length_c                   13.8127(6)
_cell_angle_alpha                99.414(3)
_cell_angle_beta                 90.005(4)
_cell_angle_gamma                90.983(3)
_cell_volume                     1363.43(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    5607
_cell_measurement_theta_min      3.4402
_cell_measurement_theta_max      32.4688

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

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.721
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.156
_exptl_crystal_density_diffrn    1.54
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             649
_exptl_crystal_recrystallization_method 
'precipitation: acetonitrile, diethyl ether, vapour diffusion, r.t., 2 d'

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

_exptl_absorpt_coefficient_mu    0.776
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.85009
_exptl_absorpt_correction_T_max  1.00000

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

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_number            10611
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.45
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_reflns_number_total             5338
_reflns_number_gt                4817
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

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

_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

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

_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.
 A strongly disordered diethyl-ether moiety occupies a center of inversion.
 As it could not be modelled discretely, it was treated with SQUEEZE/PLATON.
;
_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)+(0.0431P)²+1.3447P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         5338
_refine_ls_number_parameters     337
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0814
_refine_ls_wR_factor_gt          0.079
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      0.925
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.057
_platon_squeeze_details          
;
 The unit cell contains half a diethyl-ether molecule that has been treated as
 a diffuse contribution to the overall scattering without specific atom
 positions by SQUEEZE/PLATON.
;
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.022 0.5 0 127 17 '0.5(C4 H10 O)'

#----------------------------------------------------------------------------#
#                   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 0.0033 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Fe Fe 0.3463 0.8444 '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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.5703(2) 0.48166(17) 0.24654(16) 0.0249(4) Uani 1 1 d . . .
H11 H 0.666 0.439 0.2435 0.03 Uiso 1 1 calc R . .
C12 C 0.5788(3) 0.58663(19) 0.21989(19) 0.0354(5) Uani 1 1 d . . .
H12 H 0.6779 0.6156 0.1989 0.042 Uiso 1 1 calc R . .
C13 C 0.4401(3) 0.64835(18) 0.22450(19) 0.0361(5) Uani 1 1 d . . .
H13 H 0.442 0.7211 0.2069 0.043 Uiso 1 1 calc R . .
C14 C 0.2979(3) 0.60350(17) 0.25504(17) 0.0289(5) Uani 1 1 d . . .
H14 H 0.2014 0.6454 0.2588 0.035 Uiso 1 1 calc R . .
C15 C 0.2965(2) 0.49641(15) 0.28031(14) 0.0191(4) Uani 1 1 d . . .
C16 C 0.1439(2) 0.44046(15) 0.31298(14) 0.0193(4) Uani 1 1 d . . .
C17 C 0.0009(2) 0.52113(17) 0.32216(16) 0.0262(4) Uani 1 1 d . . .
H17A H 0.0274 0.5879 0.3703 0.039 Uiso 1 1 calc R . .
H17B H -0.0953 0.4836 0.3437 0.039 Uiso 1 1 calc R . .
H17C H -0.0205 0.5433 0.2583 0.039 Uiso 1 1 calc R . .
C21 C 0.4690(2) 0.01272(16) 0.33256(15) 0.0233(4) Uani 1 1 d . . .
H21 H 0.5536 0.0102 0.2858 0.028 Uiso 1 1 calc R . .
C22 C 0.4396(3) -0.08064(17) 0.37643(16) 0.0275(4) Uani 1 1 d . . .
H22 H 0.5023 -0.1461 0.3595 0.033 Uiso 1 1 calc R . .
C23 C 0.3178(3) -0.07719(17) 0.44519(16) 0.0287(5) Uani 1 1 d . . .
H23 H 0.2945 -0.1405 0.4758 0.034 Uiso 1 1 calc R . .
C24 C 0.2299(2) 0.02028(17) 0.46879(16) 0.0255(4) Uani 1 1 d . . .
H24 H 0.1474 0.0255 0.517 0.031 Uiso 1 1 calc R . .
C25 C 0.2648(2) 0.10994(16) 0.42076(14) 0.0203(4) Uani 1 1 d . . .
C26 C 0.1687(2) 0.21635(16) 0.43906(15) 0.0221(4) Uani 1 1 d . . .
H26A H 0.0776 0.2103 0.392 0.026 Uiso 1 1 calc R . .
H26B H 0.1232 0.2262 0.5062 0.026 Uiso 1 1 calc R . .
C28 C 0.1678(2) 0.41317(16) 0.41766(14) 0.0219(4) Uani 1 1 d . . .
H28A H 0.2148 0.4806 0.4591 0.026 Uiso 1 1 calc R . .
H28B H 0.0599 0.3994 0.4447 0.026 Uiso 1 1 calc R . .
C29 C 0.3712(2) 0.34400(17) 0.51869(15) 0.0252(4) Uani 1 1 d . . .
H29A H 0.3003 0.3635 0.5755 0.038 Uiso 1 1 calc R . .
H29B H 0.443 0.4078 0.5129 0.038 Uiso 1 1 calc R . .
H29C H 0.436 0.2792 0.5273 0.038 Uiso 1 1 calc R . .
C31 C 0.6702(2) 0.14290(17) 0.13457(15) 0.0239(4) Uani 1 1 d . . .
H31 H 0.7383 0.1304 0.187 0.029 Uiso 1 1 calc R . .
C32 C 0.7182(3) 0.10430(18) 0.03944(16) 0.0293(5) Uani 1 1 d . . .
H32 H 0.8175 0.0663 0.0269 0.035 Uiso 1 1 calc R . .
C33 C 0.6196(3) 0.12192(19) -0.03744(16) 0.0306(5) Uani 1 1 d . . .
H33 H 0.651 0.0975 -0.1035 0.037 Uiso 1 1 calc R . .
C34 C 0.4742(3) 0.17585(17) -0.01626(15) 0.0256(4) Uani 1 1 d . . .
H34 H 0.4029 0.187 -0.0676 0.031 Uiso 1 1 calc R . .
C35 C 0.4346(2) 0.21322(15) 0.08093(14) 0.0195(4) Uani 1 1 d . . .
C36 C 0.2822(2) 0.27745(16) 0.10774(14) 0.0202(4) Uani 1 1 d . . .
H36A H 0.306 0.3588 0.1134 0.024 Uiso 1 1 calc R . .
H36B H 0.201 0.2567 0.055 0.024 Uiso 1 1 calc R . .
C39 C 0.1389(2) 0.13994(16) 0.18107(16) 0.0248(4) Uani 1 1 d . . .
H39A H 0.0542 0.1387 0.1313 0.037 Uiso 1 1 calc R . .
H39B H 0.0915 0.1211 0.2414 0.037 Uiso 1 1 calc R . .
H39C H 0.2212 0.085 0.1567 0.037 Uiso 1 1 calc R . .
C83 C 0.0889(2) 0.33735(16) 0.23737(14) 0.0200(4) Uani 1 1 d . . .
H83A H 0.0005 0.2982 0.2671 0.024 Uiso 1 1 calc R . .
H83B H 0.0432 0.3649 0.1797 0.024 Uiso 1 1 calc R . .
N10 N 0.43342(18) 0.43667(13) 0.27656(12) 0.0184(3) Uani 1 1 d . . .
N20 N 0.38282(19) 0.10672(13) 0.35334(12) 0.0198(3) Uani 1 1 d . . .
N27 N 0.27153(19) 0.31591(13) 0.42824(12) 0.0193(3) Uani 1 1 d . . .
N30 N 0.53047(19) 0.19764(13) 0.15630(12) 0.0194(3) Uani 1 1 d . . .
N37 N 0.21475(18) 0.25368(12) 0.20184(11) 0.0174(3) Uani 1 1 d . . .
Cl1 Cl 0.70463(5) 0.28244(4) 0.37516(4) 0.02398(12) Uani 1 1 d . . .
Fe1 Fe 0.44057(3) 0.26400(2) 0.303910(19) 0.01541(8) Uani 1 1 d . . .
F2 F 0.9205(2) 0.90591(13) 0.12554(11) 0.0483(4) Uani 1 1 d . . .
F3 F 1.11949(17) 0.86041(16) 0.22101(13) 0.0554(4) Uani 1 1 d . . .
F4 F 0.73535(16) 0.83998(13) 0.22366(12) 0.0472(4) Uani 1 1 d . . .
F5 F 0.9359(2) 0.79447(14) 0.31927(11) 0.0528(4) Uani 1 1 d . . .
F6 F 0.91829(19) 0.97120(11) 0.28881(11) 0.0454(4) Uani 1 1 d . . .
F7 F 0.9345(2) 0.72886(12) 0.15731(12) 0.0525(4) Uani 1 1 d . . .
P1 P 0.92822(6) 0.85044(4) 0.22256(4) 0.02224(12) Uani 1 1 d . . .


#----------------------------------------------------------------------------#
#                   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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.343(2) . ?
C11 C12 1.379(3) . ?
C12 C13 1.376(3) . ?
C13 C14 1.382(3) . ?
C14 C15 1.395(3) . ?
C15 N10 1.351(2) . ?
C15 C16 1.525(3) . ?
C16 C17 1.539(2) . ?
C16 C28 1.548(3) . ?
C16 C83 1.551(3) . ?
C21 N20 1.343(2) . ?
C21 C22 1.384(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.389(3) . ?
C24 C25 1.387(3) . ?
C25 N20 1.346(3) . ?
C25 C26 1.510(3) . ?
C26 N27 1.490(2) . ?
C28 N27 1.494(2) . ?
C29 N27 1.486(3) . ?
C31 N30 1.351(2) . ?
C31 C32 1.381(3) . ?
C32 C33 1.386(3) . ?
C33 C34 1.387(3) . ?
C34 C35 1.386(3) . ?
C35 N30 1.348(2) . ?
C35 C36 1.506(3) . ?
C36 N37 1.483(2) . ?
C39 N37 1.486(2) . ?
C83 N37 1.491(2) . ?
N10 Fe1 2.1837(15) . ?
N20 Fe1 2.1692(15) . ?
N27 Fe1 2.2312(16) . ?
N30 Fe1 2.2000(16) . ?
N37 Fe1 2.3301(15) . ?
Cl1 Fe1 2.3884(5) . ?
F2 P1 1.5954(14) . ?
F3 P1 1.5857(15) . ?
F4 P1 1.5992(14) . ?
F5 P1 1.5948(14) . ?
F6 P1 1.5949(14) . ?
F7 P1 1.5955(15) . ?

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
N10 C11 C12 123.29(19) . . ?
C13 C12 C11 118.3(2) . . ?
C12 C13 C14 119.34(19) . . ?
C13 C14 C15 119.8(2) . . ?
N10 C15 C14 120.63(18) . . ?
N10 C15 C16 116.54(16) . . ?
C14 C15 C16 122.83(17) . . ?
C15 C16 C17 111.01(15) . . ?
C15 C16 C28 109.93(15) . . ?
C17 C16 C28 104.75(15) . . ?
C15 C16 C83 112.11(15) . . ?
C17 C16 C83 105.45(15) . . ?
C28 C16 C83 113.26(15) . . ?
N20 C21 C22 122.73(19) . . ?
C23 C22 C21 118.94(19) . . ?
C22 C23 C24 118.92(18) . . ?
C25 C24 C23 118.9(2) . . ?
N20 C25 C24 122.39(18) . . ?
N20 C25 C26 115.85(16) . . ?
C24 C25 C26 121.73(18) . . ?
N27 C26 C25 111.22(15) . . ?
N27 C28 C16 117.39(15) . . ?
N30 C31 C32 122.82(18) . . ?
C31 C32 C33 119.00(19) . . ?
C32 C33 C34 118.85(19) . . ?
C35 C34 C33 118.96(19) . . ?
N30 C35 C34 122.69(18) . . ?
N30 C35 C36 116.20(17) . . ?
C34 C35 C36 121.09(17) . . ?
N37 C36 C35 111.41(15) . . ?
N37 C83 C16 116.78(15) . . ?
C11 N10 C15 118.70(16) . . ?
C11 N10 Fe1 117.65(13) . . ?
C15 N10 Fe1 123.41(12) . . ?
C21 N20 C25 118.14(16) . . ?
C21 N20 Fe1 125.13(13) . . ?
C25 N20 Fe1 116.05(12) . . ?
C29 N27 C26 107.46(15) . . ?
C29 N27 C28 109.32(15) . . ?
C26 N27 C28 110.12(14) . . ?
C29 N27 Fe1 107.21(12) . . ?
C26 N27 Fe1 107.41(11) . . ?
C28 N27 Fe1 115.03(11) . . ?
C35 N30 C31 117.66(17) . . ?
C35 N30 Fe1 115.86(12) . . ?
C31 N30 Fe1 126.48(13) . . ?
C36 N37 C39 106.75(15) . . ?
C36 N37 C83 109.58(14) . . ?
C39 N37 C83 109.37(14) . . ?
C36 N37 Fe1 103.44(10) . . ?
C39 N37 Fe1 113.48(11) . . ?
C83 N37 Fe1 113.79(11) . . ?
N20 Fe1 N10 163.27(6) . . ?
N20 Fe1 N30 99.03(6) . . ?
N10 Fe1 N30 93.94(6) . . ?
N20 Fe1 N27 77.22(6) . . ?
N10 Fe1 N27 87.09(6) . . ?
N30 Fe1 N27 160.92(6) . . ?
N20 Fe1 N37 93.61(6) . . ?
N10 Fe1 N37 79.54(5) . . ?
N30 Fe1 N37 74.92(6) . . ?
N27 Fe1 N37 86.56(6) . . ?
N20 Fe1 Cl1 94.90(4) . . ?
N10 Fe1 Cl1 94.79(4) . . ?
N30 Fe1 Cl1 93.59(4) . . ?
N27 Fe1 Cl1 105.33(4) . . ?
N37 Fe1 Cl1 166.66(4) . . ?
F3 P1 F5 90.47(9) . . ?
F3 P1 F2 89.57(9) . . ?
F5 P1 F2 179.75(9) . . ?
F3 P1 F6 90.59(9) . . ?
F5 P1 F6 89.81(9) . . ?
F2 P1 F6 90.43(8) . . ?
F3 P1 F7 90.53(9) . . ?
F5 P1 F7 89.59(9) . . ?
F2 P1 F7 90.16(9) . . ?
F6 P1 F7 178.74(9) . . ?
F3 P1 F4 179.73(11) . . ?
F5 P1 F4 89.64(9) . . ?
F2 P1 F4 90.32(9) . . ?
F6 P1 F4 89.65(8) . . ?
F7 P1 F4 89.23(9) . . ?

# 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
####################################################################### 
# 
# 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_mer-nil2
_database_code_depnum_ccdc_archive 'CCDC 1008837'
_audit_update_record             
;
2014-06-17 deposited with the CCDC.
2015-10-08 downloaded from the CCDC.
;

_audit_creation_date             2014-06-17
_audit_creation_method           'WinGX routine CIF_UPDATE'

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

_chemical_name_systematic        
;
aqua[N¹,N³,2-trimethyl-2-(pyridin-2-yl)-N¹,N³-bis(pyridin-
        2-ylmethyl)propane-1,3-diamine]nickel(II) perchlorate
;
_chemical_formula_iupac          '[Ni (C23 H29 N5) (H2 O)] (Cl O4)2'
_chemical_formula_moiety         'C23 H31 N5 Ni O 2+, 2(Cl O4 1-)'
_chemical_formula_sum            'C23 H31 Cl2 N5 Ni O9'
_chemical_formula_weight         651.14
_chemical_absolute_configuration ad

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

_space_group_crystal_system      orthorhombic
_space_group_name_H-M_alt        'P n a 21'
_space_group_IT_number           33
loop_
_space_group_symop_operation_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'

_cell_length_a                   16.5101(6)
_cell_length_b                   13.5280(4)
_cell_length_c                   12.2737(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2741.31(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.00(10)
_cell_measurement_reflns_used    4380
_cell_measurement_theta_min      3.685
_cell_measurement_theta_max      32.132

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

_exptl_crystal_description       needle
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_size_max          0.438
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.066
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_meas      ?
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method 
'precipitation: wet methanol, diethyl ether, vapour diffusion, r.t., 4 d'

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

_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.81018
_exptl_absorpt_correction_T_max  1.00000

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

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Agilent Enhance'
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Agilent Sapphire3'
_diffrn_detector_area_resol_mean 16.3031
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'glass capillary'
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_number            11982
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.65
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_full        26
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_reflns_Friedel_coverage         0.75
_reflns_number_total             4759
_reflns_number_gt                4548
_reflns_threshold_expression     I>2σ(I)

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

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
        (compiled Dec  3 2012,18:21:49)
;
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'

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

_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap

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

_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.
 H atoms on aqua ligand were locate on a difference map and refined semi-freely.
 The perchlorate moiety centered at Cl2 exhibits rotational disorder along
 the O6-Cl2 axis and was refined in two discrete positions with final a s.o.f.
 of 0.716(9)/0.284(9) and an average Cl-O distance of 1.427(7) Å.
;
_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)+(0.0393P)²+0.3523P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    heteroxyz
_refine_ls_extinction_method     none
_refine_ls_number_reflns         4759
_refine_ls_number_parameters     399
_refine_ls_number_restraints     59
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0754
_refine_ls_wR_factor_gt          0.0742
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(12)
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.053

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_restr_special_details           
;
 Equal-distance classes 1 and 2 were refined using a single free variable
 (d₂ = 1.633 * d₁) to make the O atoms fit a regular tetrahedron around Cl2.
;
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
_restr_distance_details
O1 H1A 0.84 0.02 0.01(2) 'SHELXL DFIX'
O1 H1B 0.84 0.02 0.01(2) 'SHELXL DFIX'
H1A H1B 1.33 0.04 0.01(3) 'SHELXL DANG'

loop_
_restr_equal_distance_class_class_id
_restr_equal_distance_class_target_weight_param
_restr_equal_distance_class_average
_restr_equal_distance_class_esd
_restr_equal_distance_class_diff_max
_restr_equal_distance_class_details
1 0.02 1.427 0.007 0.158 'refined bonding Cl-O distance'
2 0.04 2.33 0.01 0.072 'refined non-bonding O-O distance'

loop_
_restr_equal_distance_atom_site_label_1
_restr_equal_distance_atom_site_label_2
_restr_equal_distance_class_id
_restr_equal_distance_details
Cl2 O6 1 .
Cl2 O7A 1 .
Cl2 O8A 1 .
Cl2 O9A 1 .
Cl2 O7B 1 .
Cl2 O8B 1 .
Cl2 O9B 1 .
O6 O7A 2 .
O6 O8A 2 .
O6 O9A 2 .
O7A O8A 2 .
O7A O9A 2 .
O8A O9A 2 .
O6 O7B 2 .
O6 O8B 2 .
O6 O9B 2 .
O7B O8B 2 .
O7B O9B 2 .
O8B O9B 2 .

loop_
_restr_U_iso_atom_site_label
_restr_U_iso_weight_param
O7A 0.01
O8A 0.01
O9A 0.01
O7B 0.01
O8B 0.01
O9B 0.01

loop_
_restr_parameter_class_class_id
_restr_parameter_class_parameter_type
_restr_parameter_class_target
_restr_parameter_class_target_weight_param
_restr_parameter_class_details
1 occupancy 1 0 'total s.o.f. of 1'
2 occupancy 1 0 'total s.o.f. of 1'
3 occupancy 1 0 'total s.o.f. of 1'

loop_
_restr_parameter_id
_restr_parameter_class_id
_restr_parameter_atom_site_label
_restr_parameter_atom_coefficient
1 1 O7A 1
2 1 O7B 1
3 2 O8A 1
4 2 O8B 1
5 3 O9A 1
6 3 O9B 1


#----------------------------------------------------------------------------#
#                   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 0.0033 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'
Cl Cl 0.1484 0.1585 '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'

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
C11 C 0.3573(2) 0.5839(2) 0.5135(3) 0.0243(7) Uani 1 1 d . . .
H11 H 0.397 0.5341 0.5248 0.029 Uiso 1 1 calc R . .
C12 C 0.3825(2) 0.6819(2) 0.5070(3) 0.0281(8) Uani 1 1 d . . .
H12 H 0.438 0.6992 0.5147 0.034 Uiso 1 1 calc R . .
C13 C 0.3242(2) 0.7533(2) 0.4888(3) 0.0311(8) Uani 1 1 d . . .
H13 H 0.339 0.8211 0.4853 0.037 Uiso 1 1 calc R . .
C14 C 0.2444(2) 0.7258(2) 0.4758(3) 0.0270(8) Uani 1 1 d . . .
H14 H 0.2043 0.7744 0.461 0.032 Uiso 1 1 calc R . .
C15 C 0.22267(19) 0.6264(2) 0.4844(3) 0.0194(6) Uani 1 1 d . . .
C16 C 0.13516(19) 0.5895(2) 0.4776(3) 0.0191(7) Uani 1 1 d . . .
C17 C 0.0778(2) 0.6690(2) 0.4335(3) 0.0249(7) Uani 1 1 d . . .
H17A H 0.0818 0.7284 0.4789 0.037 Uiso 1 1 calc R . .
H17B H 0.0221 0.6442 0.4351 0.037 Uiso 1 1 calc R . .
H17C H 0.0928 0.6852 0.3584 0.037 Uiso 1 1 calc R . .
C21 C 0.2119(2) 0.2179(2) 0.6786(3) 0.0219(7) Uani 1 1 d . . .
H21 H 0.261 0.2297 0.7169 0.026 Uiso 1 1 calc R . .
C22 C 0.1672(2) 0.1349(2) 0.7046(3) 0.0263(7) Uani 1 1 d . . .
H22 H 0.1846 0.0914 0.7608 0.032 Uiso 1 1 calc R . .
C23 C 0.0970(2) 0.1164(2) 0.6478(3) 0.0283(8) Uani 1 1 d . . .
H23 H 0.0653 0.0596 0.6638 0.034 Uiso 1 1 calc R . .
C24 C 0.07297(18) 0.1815(2) 0.5668(3) 0.0264(7) Uani 1 1 d . . .
H24 H 0.0251 0.1695 0.5259 0.032 Uiso 1 1 calc R . .
C25 C 0.11977(19) 0.26417(19) 0.5464(3) 0.0208(7) Uani 1 1 d . . .
C26 C 0.09243(18) 0.3424(2) 0.4685(3) 0.0196(7) Uani 1 1 d . . .
H26A H 0.0519 0.3851 0.5047 0.023 Uiso 1 1 calc R . .
H26B H 0.066 0.3107 0.4051 0.023 Uiso 1 1 calc R . .
C28 C 0.1301(2) 0.5035(2) 0.3944(3) 0.0197(6) Uani 1 1 d . . .
H28A H 0.0726 0.4953 0.3733 0.024 Uiso 1 1 calc R . .
H28B H 0.1601 0.5235 0.3281 0.024 Uiso 1 1 calc R . .
C29 C 0.1987(2) 0.3546(2) 0.3344(3) 0.0229(7) Uani 1 1 d . . .
H29A H 0.2155 0.2877 0.3552 0.034 Uiso 1 1 calc R . .
H29B H 0.2461 0.3923 0.31 0.034 Uiso 1 1 calc R . .
H29C H 0.1591 0.3508 0.2751 0.034 Uiso 1 1 calc R . .
C31 C 0.37970(18) 0.3853(2) 0.7274(3) 0.0210(7) Uani 1 1 d . . .
H31 H 0.4002 0.3376 0.6777 0.025 Uiso 1 1 calc R . .
C32 C 0.4211(2) 0.4022(2) 0.8231(3) 0.0245(8) Uani 1 1 d . . .
H32 H 0.4699 0.3678 0.8383 0.029 Uiso 1 1 calc R . .
C33 C 0.3905(2) 0.4698(2) 0.8963(3) 0.0279(8) Uani 1 1 d . . .
H33 H 0.417 0.4812 0.9639 0.033 Uiso 1 1 calc R . .
C34 C 0.3205(2) 0.5207(2) 0.8699(3) 0.0240(7) Uani 1 1 d . . .
H34 H 0.2984 0.5679 0.919 0.029 Uiso 1 1 calc R . .
C35 C 0.28307(19) 0.5023(2) 0.7712(3) 0.0192(6) Uani 1 1 d . . .
C36 C 0.21071(19) 0.5620(2) 0.7327(3) 0.0198(7) Uani 1 1 d . . .
H36A H 0.1794 0.5855 0.7964 0.024 Uiso 1 1 calc R . .
H36B H 0.2297 0.6206 0.6916 0.024 Uiso 1 1 calc R . .
C38 C 0.10413(19) 0.5651(2) 0.5930(2) 0.0180(7) Uani 1 1 d . . .
H38A H 0.0958 0.628 0.6326 0.022 Uiso 1 1 calc R . .
H38B H 0.0506 0.5327 0.5861 0.022 Uiso 1 1 calc R . .
C39 C 0.10641(19) 0.4403(2) 0.7357(3) 0.0230(7) Uani 1 1 d . . .
H39A H 0.0728 0.4843 0.7801 0.035 Uiso 1 1 calc R . .
H39B H 0.1413 0.4007 0.7833 0.035 Uiso 1 1 calc R . .
H39C H 0.0715 0.3964 0.6929 0.035 Uiso 1 1 calc R . .
N10 N 0.27941(15) 0.55655(18) 0.5046(2) 0.0179(5) Uani 1 1 d . . .
N20 N 0.18917(15) 0.28244(17) 0.6015(2) 0.0182(5) Uani 1 1 d . . .
N27 N 0.16149(16) 0.40470(16) 0.4296(2) 0.0180(5) Uani 1 1 d . . .
N30 N 0.31118(15) 0.43423(16) 0.7020(2) 0.0174(5) Uani 1 1 d . . .
N37 N 0.15734(15) 0.50010(17) 0.6612(2) 0.0175(5) Uani 1 1 d . . .
O1 O 0.34160(14) 0.34580(15) 0.49175(19) 0.0218(5) Uani 1 1 d D . .
H1A H 0.341(2) 0.2844(13) 0.487(3) 0.026 Uiso 1 1 d D . .
H1B H 0.363(2) 0.365(2) 0.434(2) 0.026 Uiso 1 1 d D . .
Ni1 Ni 0.241351(19) 0.41776(2) 0.56223(4) 0.01477(9) Uani 1 1 d . . .
O2 O 0.91876(17) 0.3729(2) 0.6365(2) 0.0453(7) Uani 1 1 d . . .
O3 O 0.92368(15) 0.48770(18) 0.4921(2) 0.0364(6) Uani 1 1 d . . .
O4 O 0.81484(17) 0.49020(19) 0.6141(2) 0.0433(7) Uani 1 1 d . . .
O5 O 0.82747(15) 0.35922(15) 0.4908(2) 0.0303(6) Uani 1 1 d . . .
Cl1 Cl 0.87137(4) 0.42826(5) 0.55936(8) 0.02260(15) Uani 1 1 d . . .
Cl2 Cl 0.04940(6) 0.84384(6) 0.74174(8) 0.0357(2) Uani 1 1 d D . .
O6 O 0.0776(2) 0.92208(16) 0.8130(2) 0.0408(7) Uani 1 1 d D A .
O7A O 0.0799(4) 0.7535(3) 0.7820(4) 0.067(2) Uani 0.716(8) 1 d PDU A 1
O8A O 0.0615(4) 0.8633(4) 0.6343(4) 0.0514(16) Uani 0.716(8) 1 d PDU A 1
O9A O -0.0403(3) 0.8348(5) 0.7601(4) 0.0647(17) Uani 0.716(8) 1 d PDU A 1
O7B O 0.1285(7) 0.7972(11) 0.7015(14) 0.084(5) Uani 0.284(8) 1 d PDU A 2
O8B O 0.0193(10) 0.8971(9) 0.6452(12) 0.060(4) Uani 0.284(8) 1 d PDU A 2
O9B O 0.0034(11) 0.7739(11) 0.7722(13) 0.086(5) Uani 0.284(8) 1 d PDU A 2


#----------------------------------------------------------------------------#
#                   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_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C11 N10 1.343(4) . ?
C11 C12 1.392(4) . ?
C12 C13 1.383(5) . ?
C13 C14 1.378(5) . ?
C14 C15 1.396(4) . ?
C15 N10 1.353(4) . ?
C15 C16 1.531(4) . ?
C16 C17 1.531(4) . ?
C16 C38 1.542(5) . ?
C16 C28 1.551(4) . ?
C21 N20 1.341(4) . ?
C21 C22 1.381(4) . ?
C22 C23 1.376(5) . ?
C23 C24 1.386(5) . ?
C24 C25 1.382(4) . ?
C25 N20 1.354(4) . ?
C25 C26 1.495(4) . ?
C26 N27 1.496(4) . ?
C28 N27 1.498(4) . ?
C29 N27 1.484(4) . ?
C31 N30 1.347(4) . ?
C31 C32 1.378(5) . ?
C32 C33 1.378(5) . ?
C33 C34 1.384(5) . ?
C34 C35 1.383(4) . ?
C35 N30 1.336(4) . ?
C35 C36 1.518(4) . ?
C36 N37 1.499(4) . ?
C38 N37 1.498(4) . ?
C39 N37 1.482(4) . ?
N10 Ni1 2.103(2) . ?
N20 Ni1 2.080(2) . ?
N27 Ni1 2.102(3) . ?
N30 Ni1 2.079(3) . ?
N37 Ni1 2.154(3) . ?
O1 Ni1 2.106(2) . ?
O2 Cl1 1.438(3) . ?
O3 Cl1 1.440(3) . ?
O4 Cl1 1.423(3) . ?
O5 Cl1 1.451(2) . ?
Cl2 O9B 1.269(10) . ?
Cl2 O8A 1.359(5) . ?
Cl2 O7A 1.412(4) . ?
Cl2 O6 1.450(3) . ?
Cl2 O8B 1.473(11) . ?
Cl2 O9A 1.502(5) . ?
Cl2 O7B 1.531(11) . ?

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
N10 C11 C12 123.0(3) . . ?
C13 C12 C11 117.8(3) . . ?
C14 C13 C12 119.8(3) . . ?
C13 C14 C15 119.8(3) . . ?
N10 C15 C14 120.6(3) . . ?
N10 C15 C16 115.9(2) . . ?
C14 C15 C16 123.5(3) . . ?
C15 C16 C17 112.0(3) . . ?
C15 C16 C38 109.5(3) . . ?
C17 C16 C38 105.6(3) . . ?
C15 C16 C28 109.4(3) . . ?
C17 C16 C28 105.1(3) . . ?
C38 C16 C28 115.2(2) . . ?
N20 C21 C22 122.9(3) . . ?
C23 C22 C21 118.7(3) . . ?
C22 C23 C24 119.3(3) . . ?
C25 C24 C23 119.0(3) . . ?
N20 C25 C24 122.0(3) . . ?
N20 C25 C26 116.5(2) . . ?
C24 C25 C26 121.3(3) . . ?
C25 C26 N27 111.9(2) . . ?
N27 C28 C16 117.4(3) . . ?
N30 C31 C32 122.1(3) . . ?
C31 C32 C33 119.0(3) . . ?
C32 C33 C34 118.9(3) . . ?
C33 C34 C35 119.3(3) . . ?
N30 C35 C34 121.7(3) . . ?
N30 C35 C36 116.3(3) . . ?
C34 C35 C36 121.9(3) . . ?
N37 C36 C35 110.3(2) . . ?
N37 C38 C16 116.4(2) . . ?
C11 N10 C15 119.0(3) . . ?
C11 N10 Ni1 120.3(2) . . ?
C15 N10 Ni1 118.6(2) . . ?
C21 N20 C25 118.1(3) . . ?
C21 N20 Ni1 128.4(2) . . ?
C25 N20 Ni1 113.3(2) . . ?
C29 N27 C26 108.0(2) . . ?
C29 N27 C28 108.9(2) . . ?
C26 N27 C28 109.3(2) . . ?
C29 N27 Ni1 112.9(2) . . ?
C26 N27 Ni1 106.17(18) . . ?
C28 N27 Ni1 111.47(17) . . ?
C35 N30 C31 118.9(3) . . ?
C35 N30 Ni1 113.9(2) . . ?
C31 N30 Ni1 127.1(2) . . ?
C39 N37 C36 106.1(3) . . ?
C39 N37 C38 109.4(2) . . ?
C36 N37 C38 110.1(2) . . ?
C39 N37 Ni1 115.53(17) . . ?
C36 N37 Ni1 103.91(17) . . ?
C38 N37 Ni1 111.47(18) . . ?
N30 Ni1 N20 97.62(10) . . ?
N30 Ni1 N10 90.94(10) . . ?
N20 Ni1 N10 171.03(10) . . ?
N30 Ni1 N27 174.75(10) . . ?
N20 Ni1 N27 81.13(10) . . ?
N10 Ni1 N27 90.11(10) . . ?
N30 Ni1 O1 87.29(10) . . ?
N20 Ni1 O1 90.80(9) . . ?
N10 Ni1 O1 92.27(9) . . ?
N27 Ni1 O1 97.82(10) . . ?
N30 Ni1 N37 80.58(10) . . ?
N20 Ni1 N37 93.30(9) . . ?
N10 Ni1 N37 85.44(9) . . ?
N27 Ni1 N37 94.38(10) . . ?
O1 Ni1 N37 167.60(10) . . ?
O4 Cl1 O2 110.65(19) . . ?
O4 Cl1 O3 109.59(16) . . ?
O2 Cl1 O3 109.97(16) . . ?
O4 Cl1 O5 108.99(15) . . ?
O2 Cl1 O5 108.56(15) . . ?
O3 Cl1 O5 109.05(17) . . ?
O8A Cl2 O7A 117.1(4) . . ?
O9B Cl2 O6 123.9(8) . . ?
O8A Cl2 O6 113.3(2) . . ?
O7A Cl2 O6 107.8(2) . . ?
O9B Cl2 O8B 113.6(10) . . ?
O6 Cl2 O8B 103.7(5) . . ?
O7A Cl2 O9A 103.2(4) . . ?
O6 Cl2 O9A 106.6(3) . . ?
O9B Cl2 O7B 107.3(10) . . ?
O6 Cl2 O7B 102.8(4) . . ?
O8B Cl2 O7B 103.3(10) . . ?

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
N10 C11 C12 C13 -1.0(5) . . . . ?
C11 C12 C13 C14 -1.2(5) . . . . ?
C12 C13 C14 C15 2.0(6) . . . . ?
C13 C14 C15 N10 -0.5(5) . . . . ?
C13 C14 C15 C16 176.4(3) . . . . ?
N10 C15 C16 C17 -169.1(3) . . . . ?
C14 C15 C16 C17 13.8(5) . . . . ?
N10 C15 C16 C38 74.1(3) . . . . ?
C14 C15 C16 C38 -103.0(4) . . . . ?
N10 C15 C16 C28 -53.1(4) . . . . ?
C14 C15 C16 C28 129.8(3) . . . . ?
N20 C21 C22 C23 1.3(5) . . . . ?
C21 C22 C23 C24 -0.4(5) . . . . ?
C22 C23 C24 C25 -0.9(5) . . . . ?
C23 C24 C25 N20 1.3(5) . . . . ?
C23 C24 C25 C26 -173.4(3) . . . . ?
N20 C25 C26 N27 24.7(4) . . . . ?
C24 C25 C26 N27 -160.2(3) . . . . ?
C15 C16 C28 N27 75.8(3) . . . . ?
C17 C16 C28 N27 -163.8(3) . . . . ?
C38 C16 C28 N27 -48.0(4) . . . . ?
N30 C31 C32 C33 1.4(5) . . . . ?
C31 C32 C33 C34 -2.0(5) . . . . ?
C32 C33 C34 C35 0.3(5) . . . . ?
C33 C34 C35 N30 2.2(5) . . . . ?
C33 C34 C35 C36 -174.3(3) . . . . ?
N30 C35 C36 N37 32.8(4) . . . . ?
C34 C35 C36 N37 -150.5(3) . . . . ?
C15 C16 C38 N37 -50.2(3) . . . . ?
C17 C16 C38 N37 -170.9(2) . . . . ?
C28 C16 C38 N37 73.5(3) . . . . ?
C12 C11 N10 C15 2.4(5) . . . . ?
C12 C11 N10 Ni1 -161.0(3) . . . . ?
C14 C15 N10 C11 -1.6(5) . . . . ?
C16 C15 N10 C11 -178.8(3) . . . . ?
C14 C15 N10 Ni1 162.1(3) . . . . ?
C16 C15 N10 Ni1 -15.1(3) . . . . ?
C22 C21 N20 C25 -0.9(5) . . . . ?
C22 C21 N20 Ni1 173.0(2) . . . . ?
C24 C25 N20 C21 -0.5(5) . . . . ?
C26 C25 N20 C21 174.5(3) . . . . ?
C24 C25 N20 Ni1 -175.2(3) . . . . ?
C26 C25 N20 Ni1 -0.2(3) . . . . ?
C25 C26 N27 C29 86.1(3) . . . . ?
C25 C26 N27 C28 -155.5(3) . . . . ?
C25 C26 N27 Ni1 -35.2(3) . . . . ?
C16 C28 N27 C29 -145.2(3) . . . . ?
C16 C28 N27 C26 97.0(3) . . . . ?
C16 C28 N27 Ni1 -20.1(3) . . . . ?
C34 C35 N30 C31 -2.8(4) . . . . ?
C36 C35 N30 C31 173.9(3) . . . . ?
C34 C35 N30 Ni1 177.9(2) . . . . ?
C36 C35 N30 Ni1 -5.4(3) . . . . ?
C32 C31 N30 C35 0.9(4) . . . . ?
C32 C31 N30 Ni1 -179.8(2) . . . . ?
C35 C36 N37 C39 81.5(3) . . . . ?
C35 C36 N37 C38 -160.2(2) . . . . ?
C35 C36 N37 Ni1 -40.7(3) . . . . ?
C16 C38 N37 C39 -149.0(3) . . . . ?
C16 C38 N37 C36 94.7(3) . . . . ?
C16 C38 N37 Ni1 -20.0(3) . . . . ?
C35 N30 Ni1 N20 -106.8(2) . . . . ?
C31 N30 Ni1 N20 74.0(3) . . . . ?
C35 N30 Ni1 N10 70.5(2) . . . . ?
C31 N30 Ni1 N10 -108.7(2) . . . . ?
C35 N30 Ni1 O1 162.8(2) . . . . ?
C31 N30 Ni1 O1 -16.5(2) . . . . ?
C35 N30 Ni1 N37 -14.7(2) . . . . ?
C31 N30 Ni1 N37 166.1(3) . . . . ?
C21 N20 Ni1 N30 -15.2(3) . . . . ?
C25 N20 Ni1 N30 158.9(2) . . . . ?
C21 N20 Ni1 N27 169.9(3) . . . . ?
C25 N20 Ni1 N27 -16.0(2) . . . . ?
C21 N20 Ni1 O1 72.1(3) . . . . ?
C25 N20 Ni1 O1 -113.7(2) . . . . ?
C21 N20 Ni1 N37 -96.2(3) . . . . ?
C25 N20 Ni1 N37 78.0(2) . . . . ?
C11 N10 Ni1 N30 42.5(3) . . . . ?
C15 N10 Ni1 N30 -121.0(2) . . . . ?
C11 N10 Ni1 N27 -142.7(3) . . . . ?
C15 N10 Ni1 N27 53.9(2) . . . . ?
C11 N10 Ni1 O1 -44.8(3) . . . . ?
C15 N10 Ni1 O1 151.7(2) . . . . ?
C11 N10 Ni1 N37 123.0(3) . . . . ?
C15 N10 Ni1 N37 -40.5(2) . . . . ?
C29 N27 Ni1 N20 -90.8(2) . . . . ?
C26 N27 Ni1 N20 27.37(17) . . . . ?
C28 N27 Ni1 N20 146.3(2) . . . . ?
C29 N27 Ni1 N10 91.14(19) . . . . ?
C26 N27 Ni1 N10 -150.73(18) . . . . ?
C28 N27 Ni1 N10 -31.8(2) . . . . ?
C29 N27 Ni1 O1 -1.17(19) . . . . ?
C26 N27 Ni1 O1 116.96(18) . . . . ?
C28 N27 Ni1 O1 -124.1(2) . . . . ?
C29 N27 Ni1 N37 176.57(19) . . . . ?
C26 N27 Ni1 N37 -65.29(18) . . . . ?
C28 N27 Ni1 N37 53.7(2) . . . . ?
C39 N37 Ni1 N30 -85.8(2) . . . . ?
C36 N37 Ni1 N30 30.01(17) . . . . ?
C38 N37 Ni1 N30 148.54(19) . . . . ?
C39 N37 Ni1 N20 11.4(2) . . . . ?
C36 N37 Ni1 N20 127.20(19) . . . . ?
C38 N37 Ni1 N20 -114.27(19) . . . . ?
C39 N37 Ni1 N10 -177.5(2) . . . . ?
C36 N37 Ni1 N10 -61.70(18) . . . . ?
C38 N37 Ni1 N10 56.83(19) . . . . ?
C39 N37 Ni1 N27 92.7(2) . . . . ?
C36 N37 Ni1 N27 -151.45(18) . . . . ?
C38 N37 Ni1 N27 -32.93(19) . . . . ?
C39 N37 Ni1 O1 -97.7(4) . . . . ?
C36 N37 Ni1 O1 18.1(5) . . . . ?
C38 N37 Ni1 O1 136.6(4) . . . . ?

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 H1A O5 0.832(18) 1.957(18) 2.783(3) 172(3) 3_455
O1 H1B O6 0.832(19) 1.942(19) 2.767(4) 171(4) 4_544

# The following lines are used to test the character set of files sent by
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# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
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# END of CIF
