#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/20/7032087.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7032087
loop_
_publ_author_name
'Schönfeld, F'
'Wirthensohn, R.'
'Schmitt, H.-C.'
'Constantinidis, P.'
'Fischer, I.'
'Müller-Buschbaum, K'
_publ_section_title
;
 Tuning of the dimensional linkage from the complex to the framework by
 thermal conversion in the system Fe/Cl/piperazine.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15398
_journal_page_last               15406
_journal_paper_doi               10.1039/c4dt01987c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C8 H22 Cl3 Fe N4, C4 N2, 2(Cl)'
_chemical_formula_sum            'C12 H22 Cl5 Fe N6'
_chemical_formula_weight         483.46
_chemical_name_systematic
;
Piperazinium-di-chlorido-di-piperazinium-iron(II)-tri-chloride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.93(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6314(13)
_cell_length_b                   9.7352(19)
_cell_length_c                   16.909(3)
_cell_measurement_reflns_used    9860
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.80
_cell_volume                     1083.6(4)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13778
_diffrn_reflns_theta_full        28.41
_diffrn_reflns_theta_max         28.41
_diffrn_reflns_theta_min         3.09
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6394
_exptl_absorpt_correction_type   empirical
_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_crystal_colour            red
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.222
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2829
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.045
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0314P)²+8.3034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                2371
_reflns_number_total             2829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01987c2.cif
_cod_data_source_block           c:\cryst\fb_pip~1\test
_cod_depositor_comments
'Adding full bibliography for 7032085--7032087.cif.'
_cod_original_formula_sum        'C12 H22 Cl5 Fe1 N6'
_cod_database_code               7032087
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'
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
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_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'
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
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 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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
