#------------------------------------------------------------------------------
#$Date: 2016-03-26 16:08:45 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180377 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/46/7204650.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_7204650
loop_
_publ_author_name
'Abu-Shandi, Khalid'
'Winkler, Heiner'
'Wu, Biao'
'Janiak, Christoph'
_publ_section_title
;
 Open-framework iron phosphates: Syntheses, structures, sorption
 studies and oxidation catalysisThis article is based (partly) on a
 presentation which will be made at the European Research Conference
 (EURESCO) on "Molecular Crystal Engineering - EuroConference on Design
 and Preparation of Molecular Materials" (Acquafredda di Maratea,
 Italy, 31 May - 5 June 2003) organised by the European Science
 Foundation and supported by the European Commission, Research DG,
 Human Potential Programme, High-Level Scientific Conferences, Contract
 HPCF-CT-2002-00270. This information is the sole responsibility of the
 author(s) and does not reflect the ESF or Community's opinion. The ESF
 and the Community are not responsible for any use that might be made
 of data appearing in this publication.
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              180
_journal_paper_doi               10.1039/b303498d
_journal_volume                  5
_journal_year                    2003
_chemical_formula_moiety         'Fe(H2O)6, C4H12N2, 2(HPO4)'
_chemical_formula_sum            'C4 H26 Fe N2 O14 P2'
_chemical_formula_weight         444.06
_chemical_name_common
Hexaaquairon(ii)-H2piperazinedium-bis(hydrogenphosphate)
_chemical_name_systematic
;
Hexaaquairon(II)-H2piperazinedium-bis(hydrogenphosphate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.574(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.317(4)
_cell_length_b                   9.643(5)
_cell_length_c                   12.877(7)
_cell_measurement_temperature    213(2)
_cell_volume                     783.6(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker AXS CCD'
_diffrn_measurement_method       'ω scan'
_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  0.0277
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4479
_diffrn_reflns_theta_full        28.63
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         2.64
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_T_max  0.8755
_exptl_absorpt_correction_T_min  0.7548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.882
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       isometric
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1808
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0330
_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)+(0.0471P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0819
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                1370
_reflns_number_total             1808
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303498d.txt
_cod_data_source_block           k8
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7204650
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Fe Fe 0.0000 0.0000 0.0000 0.01360(14) Uani 1 2 d S . .
O1 O -0.2953(3) 0.0942(2) -0.02336(15) 0.0245(4) Uani 1 1 d . . .
H11 H -0.364(6) 0.133(4) 0.025(3) 0.047(11) Uiso 1 1 d . . .
H12 H -0.367(5) 0.088(3) -0.079(3) 0.035(9) Uiso 1 1 d . . .
O2 O 0.0835(3) 0.1768(2) 0.08921(14) 0.0242(4) Uani 1 1 d . . .
H21 H 0.001(6) 0.203(4) 0.148(3) 0.054(11) Uiso 1 1 d . . .
H22 H 0.213(6) 0.192(4) 0.105(3) 0.054(11) Uiso 1 1 d . . .
O3 O 0.0973(3) 0.1017(2) -0.13332(15) 0.0288(5) Uani 1 1 d . . .
H31 H 0.010(6) 0.141(4) -0.177(3) 0.052(11) Uiso 1 1 d . . .
H32 H 0.213(7) 0.104(4) -0.161(3) 0.061(13) Uiso 1 1 d . . .
P P -0.41649(10) 0.24529(7) -0.26768(5) 0.01850(17) Uani 1 1 d . . .
O4 O -0.5079(3) 0.26682(19) -0.37780(13) 0.0241(4) Uani 1 1 d . . .
O5 O -0.5091(3) 0.11808(18) -0.21390(13) 0.0216(4) Uani 1 1 d . . .
O6 O -0.4874(4) 0.3736(2) -0.19799(14) 0.0325(5) Uani 1 1 d . . .
H6 H -0.497(7) 0.460(4) -0.230(3) 0.063(12) Uiso 1 1 d . . .
O7 O -0.1749(3) 0.2426(2) -0.26142(15) 0.0320(5) Uani 1 1 d . . .
N N -0.0918(5) 0.3850(3) -0.0548(2) 0.0373(6) Uani 1 1 d . . .
HN1 H -0.018(6) 0.308(4) -0.008(3) 0.056 Uiso 1 1 d . . .
HN2 H -0.186(6) 0.361(4) -0.124(3) 0.056 Uiso 1 1 d . . .
C1 C -0.2232(5) 0.4797(3) 0.0065(3) 0.0475(9) Uani 1 1 d . . .
H1A H -0.3426 0.4286 0.0339 0.057 Uiso 1 1 calc R . .
H1B H -0.2800 0.5545 -0.0380 0.057 Uiso 1 1 calc R . .
C2 C 0.0865(7) 0.4598(4) -0.0959(3) 0.0519(10) Uani 1 1 d . . .
H2A H 0.0342 0.5345 -0.1417 0.062 Uiso 1 1 calc R . .
H2B H 0.1715 0.3966 -0.1366 0.062 Uiso 1 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
Fe 0.0121(2) 0.0146(3) 0.0141(2) -0.00016(19) 0.00010(16) 0.00038(19)
O1 0.0187(9) 0.0346(11) 0.0201(9) -0.0028(8) -0.0009(8) 0.0049(8)
O2 0.0187(10) 0.0309(11) 0.0230(9) -0.0066(8) -0.0001(8) -0.0020(8)
O3 0.0200(10) 0.0417(13) 0.0250(10) 0.0120(9) 0.0027(8) 0.0047(9)
P 0.0166(3) 0.0199(3) 0.0188(3) 0.0038(2) -0.0012(2) -0.0007(2)
O4 0.0205(9) 0.0317(11) 0.0200(9) 0.0043(8) -0.0016(7) 0.0005(8)
O5 0.0224(9) 0.0196(9) 0.0229(9) 0.0029(7) 0.0015(7) -0.0010(7)
O6 0.0521(14) 0.0201(11) 0.0257(10) 0.0009(8) 0.0053(9) 0.0013(9)
O7 0.0162(10) 0.0441(12) 0.0354(11) 0.0183(9) -0.0022(8) -0.0029(8)
N 0.0489(16) 0.0276(14) 0.0341(14) -0.0008(11) -0.0118(12) -0.0072(12)
C1 0.0209(15) 0.0325(18) 0.090(3) 0.0103(18) 0.0096(16) 0.0004(13)
C2 0.082(3) 0.0316(18) 0.045(2) -0.0085(15) 0.037(2) -0.0104(18)
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'
O O 0.0106 0.0060 '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'
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
_geom_angle_publ_flag
O1 Fe O1 180.00(11) 3 . ?
O1 Fe O3 88.36(8) 3 3 ?
O1 Fe O3 91.64(8) . 3 ?
O1 Fe O3 91.64(8) 3 . ?
O1 Fe O3 88.36(8) . . ?
O3 Fe O3 180.00(16) 3 . ?
O1 Fe O2 94.23(8) 3 . ?
O1 Fe O2 85.77(8) . . ?
O3 Fe O2 90.43(9) 3 . ?
O3 Fe O2 89.57(9) . . ?
O1 Fe O2 85.77(8) 3 3 ?
O1 Fe O2 94.23(8) . 3 ?
O3 Fe O2 89.57(9) 3 3 ?
O3 Fe O2 90.43(9) . 3 ?
O2 Fe O2 180.00(8) . 3 ?
Fe O1 H11 124(2) . . ?
Fe O1 H12 123(2) . . ?
H11 O1 H12 112(3) . . ?
Fe O2 H21 120(2) . . ?
Fe O2 H22 119(2) . . ?
H21 O2 H22 108(3) . . ?
Fe O3 H31 123(2) . . ?
Fe O3 H32 132(3) . . ?
H31 O3 H32 104(3) . . ?
O4 P O7 112.86(11) . . ?
O4 P O5 113.13(10) . . ?
O7 P O5 111.29(11) . . ?
O4 P O6 108.21(11) . . ?
O7 P O6 106.70(12) . . ?
O5 P O6 104.00(11) . . ?
P O6 H6 118(3) . . ?
C2 N C1 110.4(2) . . ?
C2 N HN1 103(2) . . ?
C1 N HN1 111.9(19) . . ?
C2 N HN2 102.5(19) . . ?
C1 N HN2 105.7(19) . . ?
HN1 N HN2 123(3) . . ?
N C1 C2 109.0(3) . 3_565 ?
N C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 3_565 . ?
N C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 3_565 . ?
H1A C1 H1B 108.3 . . ?
N C2 C1 109.7(3) . 3_565 ?
N C2 H2A 109.7 . . ?
C1 C2 H2A 109.7 3_565 . ?
N C2 H2B 109.7 . . ?
C1 C2 H2B 109.7 3_565 . ?
H2A C2 H2B 108.2 . . ?
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
Fe O1 2.084(2) 3 ?
Fe O1 2.084(2) . ?
Fe O3 2.093(2) 3 ?
Fe O3 2.093(2) . ?
Fe O2 2.110(2) . ?
Fe O2 2.110(2) 3 ?
O1 H11 0.86(4) . ?
O1 H12 0.83(3) . ?
O2 H21 0.97(4) . ?
O2 H22 0.85(4) . ?
O3 H31 0.86(4) . ?
O3 H32 0.83(4) . ?
P O4 1.5210(19) . ?
P O7 1.525(2) . ?
P O5 1.5373(19) . ?
P O6 1.604(2) . ?
O6 H6 0.93(4) . ?
N C2 1.456(4) . ?
N C1 1.485(4) . ?
N HN1 1.05(4) . ?
N HN2 1.08(3) . ?
C1 C2 1.523(5) 3_565 ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C2 C1 1.523(5) 3_565 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
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 H11 O4 0.86(4) 1.85(4) 2.709(3) 174(3) 4_566
O1 H12 O5 0.83(3) 1.94(3) 2.757(3) 166(3) .
O2 H21 O7 0.97(4) 1.73(4) 2.692(3) 171(3) 4_566
O2 H22 O4 0.85(4) 1.81(4) 2.653(3) 173(3) 4_666
O3 H31 O7 0.86(4) 1.84(4) 2.697(3) 174(3) .
O3 H32 O5 0.83(4) 1.92(4) 2.741(3) 174(4) 1_655
O6 H6 O5 0.93(4) 1.69(4) 2.616(3) 175(4) 2_454
N HN1 O2 1.05(4) 1.88(4) 2.917(3) 172(3) .
N HN2 O6 1.08(3) 2.09(4) 3.040(4) 146(3) .
N HN2 O7 1.08(3) 2.11(3) 3.018(3) 141(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C2 N C1 C2 -59.4(4) . . . 3_565 ?
C1 N C2 C1 59.8(4) . . . 3_565 ?
