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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_c2c
_audit_creation_date             2014-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_chemical_name_common            ?
_chemical_name_systematic        Di-chloro-mono-piperazine-iron(II)

_chemical_formula_moiety         '0.25(C16 H40 Cl8 Fe4 N8)'
_chemical_formula_sum            'C4 H10 Cl2 Fe N2'
_chemical_formula_weight         212.89
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   9.4288(6)
_cell_length_b                   12.9976(8)
_cell_length_c                   6.3958(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.616(2)
_cell_angle_gamma                90.00
_cell_volume                     783.50(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2966
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.67
_exptl_absorpt_coefficient_mu    2.521
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6966
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0571 before and 0.0346 after correction.
The Ratio of minimum to maximum transmission is 0.9338.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6158
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.67
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_number_gt                958
_reflns_number_total             1107
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        XPrep
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Microsoft Word (2010)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         1107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0176
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0090P)²+0.9932P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0352
_refine_ls_wR_factor_ref         0.0369
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.0000 0.427806(19) 0.2500 0.00594(7) Uani 1 d . . 2 S T P
Cl1 Cl -0.14604(3) 0.42932(2) 0.57133(4) 0.00781(7) Uani 1 d . . 1 . . .
N1 N 0.14752(11) 0.32878(8) 0.42762(16) 0.0076(2) Uani 1 d . . 1 . . .
H1 H 0.1526 0.3596 0.5588 0.009 Uiso 1 calc . . 1 R . .
C1 C 0.29732(13) 0.32878(10) 0.36202(19) 0.0098(2) Uani 1 d . . 1 . . .
H1A H 0.3284 0.4005 0.3390 0.012 Uiso 1 calc . . 1 R . .
H1B H 0.3041 0.2913 0.2279 0.012 Uiso 1 calc . . 1 R . .
C2 C 0.10470(13) 0.22155(10) 0.4745(2) 0.0101(2) Uani 1 d . . 1 . . .
H2A H 0.1054 0.1805 0.3442 0.012 Uiso 1 calc . . 1 R . .
H2B H 0.0066 0.2216 0.5257 0.012 Uiso 1 calc . . 1 R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.00631(12) 0.00605(12) 0.00539(12) 0.000 -0.00095(9) 0.000
Cl1 0.00865(14) 0.00814(14) 0.00664(14) -0.00025(10) 0.00042(10) -0.00069(10)
N1 0.0079(5) 0.0075(5) 0.0073(5) 0.0001(4) 0.0004(4) 0.0014(4)
C1 0.0074(6) 0.0110(6) 0.0109(6) 0.0032(5) 0.0015(5) 0.0016(5)
C2 0.0085(6) 0.0087(6) 0.0130(6) 0.0022(5) -0.0008(5) 0.0007(5)

_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 Cl1 2.5060(3) . ?
Fe1 Cl1 2.5616(3) 5_566 ?
Fe1 Cl1 2.5616(3) 6_565 ?
Fe1 Cl1 2.5060(3) 2 ?
Fe1 N1 2.1893(10) . ?
Fe1 N1 2.1893(10) 2 ?
Cl1 Fe1 2.5616(3) 5_566 ?
N1 C1 1.4847(15) . ?
N1 C2 1.4840(16) . ?
C1 C2 1.5231(17) 7_556 ?
C2 C1 1.5231(17) 7_556 ?

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
Cl1 Fe1 Cl1 93.397(11) 2 5_566 ?
Cl1 Fe1 Cl1 85.950(11) . 5_566 ?
Cl1 Fe1 Cl1 179.101(19) 2 . ?
Cl1 Fe1 Cl1 87.071(15) 5_566 6_565 ?
Cl1 Fe1 Cl1 93.398(11) . 6_565 ?
Cl1 Fe1 Cl1 85.950(11) 2 6_565 ?
N1 Fe1 Cl1 169.54(3) . 6_565 ?
N1 Fe1 Cl1 82.48(3) 2 6_565 ?
N1 Fe1 Cl1 86.26(3) . . ?
N1 Fe1 Cl1 86.26(3) 2 2 ?
N1 Fe1 Cl1 94.27(3) . 2 ?
N1 Fe1 Cl1 169.54(3) 2 5_566 ?
N1 Fe1 Cl1 82.48(3) . 5_566 ?
N1 Fe1 Cl1 94.27(3) 2 . ?
N1 Fe1 N1 107.98(6) . 2 ?
Fe1 Cl1 Fe1 94.050(11) . 5_566 ?
C1 N1 Fe1 116.67(7) . . ?
C2 N1 Fe1 118.98(7) . . ?
C2 N1 C1 108.88(10) . . ?
N1 C1 C2 111.68(10) . 7_556 ?
N1 C2 C1 112.27(10) . 7_556 ?

_database_code_depnum_ccdc_archive 'CCDC 1003591'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_p-1
_audit_creation_date             2014-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2899 for OlexSys, GUI svn.r4781)
;
_chemical_name_common            ?
_chemical_name_systematic        Piperazino-di-chloro-tri-piperazine-iron(II)

_chemical_formula_moiety         'C6 H15 Cl2 Fe N3, C2 H4 N'
_chemical_formula_sum            'C8 H20 Cl2 Fe N4'
_chemical_formula_weight         299.03
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

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

_cell_length_a                   7.1460(13)
_cell_length_b                   8.3668(16)
_cell_length_c                   11.438(2)
_cell_angle_alpha                108.112(6)
_cell_angle_beta                 98.174(6)
_cell_angle_gamma                101.691(6)
_cell_volume                     620.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4519
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.65
_exptl_absorpt_coefficient_mu    1.620
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6356
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0891 before and 0.0356 after correction.
The Ratio of minimum to maximum transmission is 0.8528.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.600
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             312
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_exptl_special_details           
;
 ? 
;
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8074
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.65
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_reflns_number_gt                2281
_reflns_number_total             2515
_reflns_threshold_expression     >2sigma(I)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        XPrep
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Microsoft Word (2010)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_refine_diff_density_max         1.278
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2515
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0274
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0264P)²+0.9093P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0691
_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. 
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
2.a Ternary CH refined with riding coordinates:
 N3(H3), N1(H1), N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C2(H2A,H2B), C7(H7A,H7B), C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B),
 C8(H8A,H8B), C6(H6A,H6B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_refinement_flags_posn
Fe1 Fe 0.18679(4) 0.16719(4) 0.32892(3) 0.00920(10) Uani 1 d . . .
Cl1 Cl 0.49724(7) 0.34054(7) 0.31521(5) 0.01473(13) Uani 1 d . . .
Cl2 Cl -0.10746(7) -0.05021(7) 0.31146(5) 0.01325(12) Uani 1 d . . .
N3 N 0.1297(3) 0.3912(2) 0.45206(16) 0.0109(4) Uani 1 d . . .
H3 H 0.2472 0.4666 0.4969 0.013 Uiso 1 calc . . R
N1 N 0.1008(3) 0.1128(2) 0.12930(16) 0.0109(4) Uani 1 d . . .
H1 H 0.1821 0.1960 0.1108 0.013 Uiso 1 calc . . R
N2 N 0.3350(2) 0.0585(2) 0.45021(16) 0.0106(4) Uani 1 d . . .
H2 H 0.2434 0.0095 0.4855 0.013 Uiso 1 calc . . R
N4 N 0.3556(3) 0.4024(3) 0.0481(2) 0.0302(5) Uani 1 d . . .
C4 C 0.4030(3) -0.0849(3) 0.3708(2) 0.0134(4) Uani 1 d . . .
H4A H 0.4942 -0.0381 0.3270 0.016 Uiso 1 calc . . R
H4B H 0.2917 -0.1686 0.3077 0.016 Uiso 1 calc . . R
C2 C -0.1023(3) 0.1069(3) 0.0756(2) 0.0130(4) Uani 1 d . . .
H2A H -0.1251 0.2206 0.1119 0.016 Uiso 1 calc . . R
H2B H -0.1926 0.0238 0.0979 0.016 Uiso 1 calc . . R
C7 C 0.5085(3) 0.3299(3) -0.0050(2) 0.0189(5) Uani 1 d . . .
H7A H 0.4536 0.2554 -0.0922 0.023 Uiso 1 calc . . R
H7B H 0.5490 0.2581 0.0407 0.023 Uiso 1 calc . . R
C3 C 0.4979(3) 0.1782(3) 0.5550(2) 0.0125(4) Uani 1 d . . .
H3A H 0.4481 0.2641 0.6115 0.015 Uiso 1 calc . . R
H3B H 0.5941 0.2396 0.5212 0.015 Uiso 1 calc . . R
C5 C 0.0133(3) 0.3599(3) 0.5432(2) 0.0146(4) Uani 1 d . . .
H5A H 0.0843 0.3131 0.5977 0.018 Uiso 1 calc . . R
H5B H -0.1092 0.2732 0.4976 0.018 Uiso 1 calc . . R
C1 C 0.1424(3) -0.0553(3) 0.06659(19) 0.0128(4) Uani 1 d . . .
H1A H 0.0625 -0.1455 0.0884 0.015 Uiso 1 calc . . R
H1B H 0.2787 -0.0473 0.0979 0.015 Uiso 1 calc . . R
C8 C 0.3135(4) 0.5331(4) -0.0004(3) 0.0338(7) Uani 1 d . . .
H8A H 0.2285 0.5903 0.0469 0.041 Uiso 1 calc . . R
H8B H 0.2420 0.4762 -0.0875 0.041 Uiso 1 calc . . R
C6 C 0.0307(3) 0.4768(3) 0.3765(2) 0.0130(4) Uani 1 d . . .
H6A H -0.0909 0.3955 0.3234 0.016 Uiso 1 calc . . R
H6B H 0.1131 0.5064 0.3218 0.016 Uiso 1 calc . . R

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.00959(16) 0.01058(16) 0.00784(15) 0.00354(12) 0.00120(11) 0.00350(12)
Cl1 0.0114(3) 0.0186(3) 0.0130(2) 0.0071(2) 0.00130(19) -0.0003(2)
Cl2 0.0116(3) 0.0156(3) 0.0125(2) 0.0067(2) 0.00207(19) 0.00092(19)
N3 0.0095(8) 0.0119(9) 0.0115(8) 0.0045(7) 0.0019(7) 0.0028(7)
N1 0.0098(9) 0.0114(9) 0.0104(8) 0.0038(7) 0.0008(7) 0.0015(7)
N2 0.0084(8) 0.0123(9) 0.0122(8) 0.0056(7) 0.0026(7) 0.0027(7)
N4 0.0224(11) 0.0273(12) 0.0562(15) 0.0278(12) 0.0188(11) 0.0117(9)
C4 0.0134(11) 0.0147(10) 0.0121(10) 0.0043(9) 0.0021(8) 0.0049(8)
C2 0.0129(11) 0.0158(11) 0.0116(10) 0.0050(9) 0.0029(8) 0.0059(8)
C7 0.0192(12) 0.0169(11) 0.0231(12) 0.0094(10) 0.0049(9) 0.0062(9)
C3 0.0123(10) 0.0113(10) 0.0130(10) 0.0033(8) 0.0014(8) 0.0034(8)
C5 0.0188(11) 0.0150(11) 0.0156(10) 0.0092(9) 0.0080(9) 0.0074(9)
C1 0.0131(10) 0.0146(10) 0.0108(10) 0.0044(9) 0.0008(8) 0.0050(8)
C8 0.0257(14) 0.0297(15) 0.0552(19) 0.0211(14) 0.0170(13) 0.0114(12)
C6 0.0153(11) 0.0143(10) 0.0124(10) 0.0065(9) 0.0051(8) 0.0060(9)

_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 Cl1 2.4467(7) . ?
Fe1 Cl2 2.4238(7) . ?
Fe1 N3 2.1197(18) . ?
Fe1 N1 2.1539(18) . ?
Fe1 N2 2.1515(18) . ?
N3 C5 1.475(3) . ?
N3 C6 1.475(3) . ?
N1 C2 1.478(3) . ?
N1 C1 1.478(3) . ?
N2 C4 1.478(3) . ?
N2 C3 1.476(3) . ?
N4 C7 1.469(3) . ?
N4 C8 1.434(3) . ?
C4 C3 1.515(3) 2_656 ?
C2 C1 1.514(3) 2 ?
C7 C8 1.509(4) 2_665 ?
C3 C4 1.515(3) 2_656 ?
C5 C6 1.512(3) 2_566 ?
C1 C2 1.514(3) 2 ?
C8 C7 1.509(4) 2_665 ?
C6 C5 1.512(3) 2_566 ?

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
Cl2 Fe1 Cl1 168.87(2) . . ?
N3 Fe1 Cl1 91.40(5) . . ?
N3 Fe1 Cl2 99.66(5) . . ?
N3 Fe1 N1 117.41(7) . . ?
N3 Fe1 N2 105.26(7) . . ?
N1 Fe1 Cl1 85.27(5) . . ?
N1 Fe1 Cl2 88.52(5) . . ?
N2 Fe1 Cl1 91.89(5) . . ?
N2 Fe1 Cl2 86.42(5) . . ?
N2 Fe1 N1 137.27(7) . . ?
C5 N3 Fe1 115.49(13) . . ?
C5 N3 C6 109.21(16) . . ?
C6 N3 Fe1 109.08(13) . . ?
C2 N1 Fe1 118.74(13) . . ?
C2 N1 C1 109.60(16) . . ?
C1 N1 Fe1 106.07(12) . . ?
C4 N2 Fe1 108.23(13) . . ?
C3 N2 Fe1 117.80(13) . . ?
C3 N2 C4 109.88(16) . . ?
C8 N4 C7 111.5(2) . . ?
N2 C4 C3 113.38(17) . 2_656 ?
N1 C2 C1 112.03(17) . 2 ?
N4 C7 C8 113.6(2) . 2_665 ?
N2 C3 C4 112.77(18) . 2_656 ?
N3 C5 C6 112.74(18) . 2_566 ?
N1 C1 C2 112.72(18) . 2 ?
N4 C8 C7 114.7(2) . 2_665 ?
N3 C6 C5 112.83(18) . 2_566 ?

_database_code_depnum_ccdc_archive 'CCDC 1003592'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_c:\cryst\fb_pip~1\test

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 'Piperazinium-di-chlorido-di-piperazinium-iron(II)-tri-chloride' 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H22 Cl3 Fe N4, C4 N2, 2(Cl)'
_chemical_formula_sum            'C12 H22 Cl5 Fe1 N6'
_chemical_formula_weight         483.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z'
3 '-x, -y, -z'
4 'x, -y-1/2, z'

_cell_length_a                   6.6314(13)
_cell_length_b                   9.7352(19)
_cell_length_c                   16.909(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.93(3)
_cell_angle_gamma                90.00
_cell_volume                     1083.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9860
_cell_measurement_theta_min      2.80
_cell_measurement_theta_max      28.37

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             494
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_process_details   
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0817 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.8514.
The λ/2 correction factor is 0.0015.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13778
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         28.41
_reflns_number_total             2829
_reflns_number_gt                2371
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker Apex II'
_computing_cell_refinement       'Bruker Apex II'
_computing_data_reduction        XPrep
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Microsoft Word (2010)'

_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)+(0.0314P)²+8.3034P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2829
_refine_ls_number_parameters     154
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1200
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_restrained_S_all      1.159
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.010

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 0.10876(16) 0.2500 0.28214(6) 0.0184(3) Uani 1 2 d S . .
Cl2 Cl 0.7610(3) 0.7500 0.42713(12) 0.0330(5) Uani 1 2 d S . .
Cl3 Cl 0.2986(3) 0.44501(19) 0.32932(10) 0.0466(5) Uani 1 1 d . . .
Cl4 Cl 0.2093(4) 0.7500 0.04141(15) 0.0484(6) Uani 1 2 d S . .
N2 N 0.2566(10) 0.2500 0.1703(4) 0.0226(14) Uani 1 2 d S . .
C6 C 0.2137(10) 0.3739(6) 0.1216(3) 0.0305(13) Uani 1 1 d . . .
H6A H 0.2585 0.4554 0.1541 0.037 Uiso 1 1 calc R . .
H6B H 0.0651 0.3815 0.1068 0.037 Uiso 1 1 calc R . .
C7 C 0.3167(11) 0.3752(8) 0.0465(4) 0.0426(16) Uani 1 1 d . . .
H7A H 0.2758 0.4582 0.0147 0.051 Uiso 1 1 calc R . .
H7B H 0.4660 0.3772 0.0604 0.051 Uiso 1 1 calc R . .
Cl1 Cl -0.2093(4) 0.2500 0.20494(14) 0.0541(15) Uani 1 2 d S . .
N1 N -0.0441(10) 0.2500 0.3921(4) 0.0258(14) Uani 1 2 d S . .
N4 N 0.2563(12) 0.2500 -0.0005(4) 0.0397(19) Uani 1 2 d S . .
H4A H 0.3176 0.2500 -0.0465 0.048 Uiso 1 2 calc SR . .
H4B H 0.1178 0.2500 -0.0146 0.048 Uiso 1 2 calc SR . .
N3 N -0.4078(11) 0.2500 0.4697(4) 0.042(2) Uani 1 2 d S . .
H3A H -0.4991 0.2500 0.4242 0.051 Uiso 1 2 calc SR . .
H3B H -0.4799 0.2500 0.5129 0.051 Uiso 1 2 calc SR . .
C4 C -0.1661(10) 0.3739(7) 0.3992(4) 0.0416(17) Uani 1 1 d . . .
H4C H -0.2647 0.3831 0.3507 0.050 Uiso 1 1 calc R . .
H4D H -0.0754 0.4550 0.4021 0.050 Uiso 1 1 calc R . .
C5 C -0.2809(11) 0.3737(10) 0.4715(5) 0.060(2) Uani 1 1 d . . .
H5A H -0.1837 0.3748 0.5208 0.072 Uiso 1 1 calc R . .
H5B H -0.3672 0.4567 0.4711 0.072 Uiso 1 1 calc R . .
N11A N -0.236(6) 0.615(3) 0.243(2) 0.139(12) Uani 0.50 1 d P . .
N11B N -0.254(3) 0.618(2) 0.1879(14) 0.083(8) Uani 0.50 1 d P . .
C2A C -0.081(4) 0.682(2) 0.2538(16) 0.074(7) Uani 0.50 1 d P . .
C2B C -0.057(2) 0.6732(19) 0.2168(7) 0.030(4) Uani 0.50 1 d P . .
C1A C -0.4311(17) 0.6767(12) 0.2113(8) 0.027(3) Uani 0.50 1 d P . .
C1B C -0.404(3) 0.685(2) 0.1609(13) 0.077(6) Uani 0.50 1 d P . .
H2 H 0.373(12) 0.2500 0.186(4) 0.02(2) Uiso 1 2 d S . .
H1 H 0.050(13) 0.2500 0.428(5) 0.02(2) Uiso 1 2 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe1 0.0168(5) 0.0190(5) 0.0202(5) 0.000 0.0056(4) 0.000
Cl2 0.0281(10) 0.0510(13) 0.0216(9) 0.000 0.0097(8) 0.000
Cl3 0.0519(10) 0.0482(10) 0.0445(9) -0.0196(8) 0.0261(8) -0.0294(8)
Cl4 0.0558(15) 0.0570(16) 0.0323(12) 0.000 0.0051(11) 0.000
N2 0.021(3) 0.025(3) 0.023(3) 0.000 0.007(3) 0.000
C6 0.044(3) 0.022(3) 0.027(3) -0.001(2) 0.013(3) -0.004(3)
C7 0.052(4) 0.045(4) 0.034(3) 0.008(3) 0.018(3) -0.010(3)
Cl1 0.0173(11) 0.117(5) 0.0226(11) 0.000 0.0049(9) 0.000
N1 0.017(3) 0.041(4) 0.019(3) 0.000 0.002(3) 0.000
N4 0.041(4) 0.061(5) 0.019(3) 0.000 0.013(3) 0.000
N3 0.019(3) 0.089(7) 0.020(3) 0.000 0.006(3) 0.000
C4 0.038(3) 0.037(4) 0.055(4) -0.012(3) 0.029(3) 0.001(3)
C5 0.046(4) 0.083(6) 0.056(5) -0.032(5) 0.032(4) 0.000(4)
N11A 0.18(3) 0.049(14) 0.20(3) 0.04(2) 0.05(3) 0.033(17)
N11B 0.045(9) 0.056(12) 0.14(2) -0.063(14) -0.007(12) -0.006(8)
C2A 0.060(14) 0.054(11) 0.095(17) -0.025(14) -0.041(14) 0.024(10)
C2B 0.028(6) 0.053(9) 0.010(5) 0.000(6) 0.004(5) 0.015(6)
C1A 0.024(5) 0.026(6) 0.033(6) -0.004(5) 0.018(5) -0.016(5)
C1B 0.049(10) 0.084(14) 0.092(15) -0.039(12) -0.015(10) 0.011(9)

_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 N1 2.222(6) . ?
Fe1 N2 2.233(6) . ?
Fe1 Cl1 2.343(3) . ?
Fe1 Cl3 2.3630(17) . ?
Fe1 Cl3 2.3630(17) 4_565 ?
N2 C6 1.469(7) 4_565 ?
N2 C6 1.469(7) . ?
C6 C7 1.513(8) . ?
C7 N4 1.484(8) . ?
N1 C4 1.465(7) 4_565 ?
N1 C4 1.465(7) . ?
N4 C7 1.484(8) 4_565 ?
N3 C5 1.468(9) . ?
N3 C5 1.468(9) 4_565 ?
C4 C5 1.516(8) . ?
N11A N11B 0.92(4) . ?
N11A C2A 1.21(4) . ?
N11A C2B 1.43(4) . ?
N11A C1A 1.47(3) . ?
N11A C1B 1.80(4) . ?
N11B C1B 1.23(3) . ?
N11B C1A 1.41(2) . ?
N11B C2B 1.44(3) . ?
N11B C2A 1.63(3) . ?
C2A C2B 0.67(3) . ?
C2A C2A 1.33(5) 4_575 ?
C2A C2B 1.56(2) 4_575 ?
C2B C2B 1.49(4) 4_575 ?
C2B C2A 1.56(2) 4_575 ?
C1A C1B 0.89(2) . ?
C1A C1A 1.43(2) 4_575 ?
C1A C1B 1.61(2) 4_575 ?
C1B C1B 1.27(4) 4_575 ?
C1B C1A 1.61(2) 4_575 ?

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 Fe1 N2 178.9(3) . . ?
N1 Fe1 Cl1 89.72(19) . . ?
N2 Fe1 Cl1 89.2(2) . . ?
N1 Fe1 Cl3 89.76(12) . . ?
N2 Fe1 Cl3 90.88(12) . . ?
Cl1 Fe1 Cl3 126.54(6) . . ?
N1 Fe1 Cl3 89.76(11) . 4_565 ?
N2 Fe1 Cl3 90.88(12) . 4_565 ?
Cl1 Fe1 Cl3 126.54(6) . 4_565 ?
Cl3 Fe1 Cl3 106.91(11) . 4_565 ?
C6 N2 C6 110.4(6) 4_565 . ?
C6 N2 Fe1 113.5(3) 4_565 . ?
C6 N2 Fe1 113.5(3) . . ?
N2 C6 C7 113.6(5) . . ?
N4 C7 C6 108.8(5) . . ?
C4 N1 C4 110.8(7) 4_565 . ?
C4 N1 Fe1 112.4(4) 4_565 . ?
C4 N1 Fe1 112.4(4) . . ?
C7 N4 C7 110.4(7) . 4_565 ?
C5 N3 C5 110.3(8) . 4_565 ?
N1 C4 C5 113.7(7) . . ?
N3 C5 C4 109.1(6) . . ?
N11B N11A C2A 99(4) . . ?
N11B N11A C2B 72(3) . . ?
C2A N11A C2B 27.8(15) . . ?
N11B N11A C1A 68(3) . . ?
C2A N11A C1A 122(2) . . ?
C2B N11A C1A 117(2) . . ?
N11B N11A C1B 39(2) . . ?
C2A N11A C1B 111(2) . . ?
C2B N11A C1B 94.3(19) . . ?
C1A N11A C1B 29.5(9) . . ?
N11A N11B C1B 113(3) . . ?
N11A N11B C1A 75(3) . . ?
C1B N11B C1A 38.9(12) . . ?
N11A N11B C2B 70(3) . . ?
C1B N11B C2B 126(2) . . ?
C1A N11B C2B 120.2(14) . . ?
N11A N11B C2A 47(3) . . ?
C1B N11B C2A 121.3(18) . . ?
C1A N11B C2A 101.1(15) . . ?
C2B N11B C2A 24.3(10) . . ?
C2B C2A N11A 95(4) . . ?
C2B C2A C2A 97(3) . 4_575 ?
N11A C2A C2A 122.5(17) . 4_575 ?
C2B C2A C2B 72(4) . 4_575 ?
N11A C2A C2B 123(2) . 4_575 ?
C2A C2A C2B 25.2(10) 4_575 4_575 ?
C2B C2A N11B 63(3) . . ?
N11A C2A N11B 34.0(19) . . ?
C2A C2A N11B 112.7(12) 4_575 . ?
C2B C2A N11B 99.9(18) 4_575 . ?
C2A C2B N11A 58(3) . . ?
C2A C2B N11B 93(3) . . ?
N11A C2B N11B 37.3(15) . . ?
C2A C2B C2B 83(3) . 4_575 ?
N11A C2B C2B 113.4(13) . 4_575 ?
N11B C2B C2B 112.0(12) . 4_575 ?
C2A C2B C2A 58(3) . 4_575 ?
N11A C2B C2A 96.1(16) . 4_575 ?
N11B C2B C2A 110.0(17) . 4_575 ?
C2B C2B C2A 25.2(10) 4_575 4_575 ?
C1B C1A N11B 60.0(17) . . ?
C1B C1A C1A 84.9(17) . 4_575 ?
N11B C1A C1A 114.2(10) . 4_575 ?
C1B C1A N11A 97(2) . . ?
N11B C1A N11A 37.3(14) . . ?
C1A C1A N11A 114.2(13) 4_575 . ?
C1B C1A C1B 51(2) . 4_575 ?
N11B C1A C1B 92.6(14) . 4_575 ?
C1A C1A C1B 33.5(8) 4_575 4_575 ?
N11A C1A C1B 112.6(15) . 4_575 ?
C1A C1B N11B 81(2) . . ?
C1A C1B C1B 95.1(17) . 4_575 ?
N11B C1B C1B 122.2(13) . 4_575 ?
C1A C1B C1A 61.7(16) . 4_575 ?
N11B C1B C1A 112.6(16) . 4_575 ?
C1B C1B C1A 33.5(8) 4_575 4_575 ?
C1A C1B N11A 54.0(18) . . ?
N11B C1B N11A 28.0(15) . . ?
C1B C1B N11A 112.2(12) 4_575 . ?
C1A C1B N11A 90.5(14) 4_575 . ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        28.41
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.111

_database_code_depnum_ccdc_archive 'CCDC 1003593'
