#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/28/2012856.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012856
loop_
_publ_author_name
'Zhou, Bei-Chuan'
'Yao, You-Wei'
'Wang, Ru-Ji'
_publ_section_title
;
 Heptairon bis(phosphate) tetrakis(hydrogenphosphate)
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i109
_journal_page_last               i110
_journal_paper_doi               10.1107/S0108270102009873
_journal_volume                  58
_journal_year                    2002
_chemical_formula_structural     'Fe7 (P O4)2 (H P O4)4'
_chemical_formula_sum            'Fe7 H4 O24 P6'
_chemical_formula_weight         964.80
_chemical_name_systematic
;
Heptairon tetrakis(hydrogenphosphate) bis(phosphate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                104.03(4)
_cell_angle_beta                 109.17(2)
_cell_angle_gamma                101.66(3)
_cell_formula_units_Z            1
_cell_length_a                   6.528(3)
_cell_length_b                   7.956(4)
_cell_length_c                   9.501(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.4
_cell_measurement_theta_min      5.9
_cell_volume                     430.3(4)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Bruker, 1997)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       ω
_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  0.040
_diffrn_reflns_av_sigmaI/netI    0.052
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2420
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.431
_exptl_absorpt_correction_T_max  0.526
_exptl_absorpt_correction_T_min  0.282
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.22
_refine_diff_density_min         -0.94
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.053
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0010P)²+6.4359P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.100
_refine_ls_wR_factor_ref         0.106
_reflns_number_gt                1537
_reflns_number_total             1921
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            br1377.cif
_cod_data_source_block           I
_cod_original_cell_volume        430.3(3)
_cod_original_formula_sum        'H4 Fe7 O24 P6'
_cod_database_code               2012856
_cod_database_fobs_code          2012856
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Fe1 0.0000 0.0000 0.0000 0.0134(3) Uani d S 1 . . Fe
Fe2 0.38733(15) 0.45498(11) 0.11196(10) 0.0120(2) Uani d . 1 . . Fe
Fe3 -0.27718(15) 0.18673(11) -0.28076(11) 0.0138(2) Uani d . 1 . . Fe
Fe4 -0.04910(15) 0.28480(12) -0.51589(11) 0.0145(2) Uani d . 1 . . Fe
P1 0.2285(3) 0.1448(2) -0.22284(18) 0.0103(3) Uani d . 1 . . P
P2 0.0853(3) 0.5817(2) -0.17233(18) 0.0107(3) Uani d . 1 . . P
P3 -0.5879(3) 0.2307(2) -0.62669(19) 0.0125(3) Uani d . 1 . . P
O1 0.0196(7) 0.1730(6) -0.3368(5) 0.0134(9) Uani d . 1 . . O
O2 0.2267(7) 0.1886(5) -0.0558(5) 0.0129(8) Uani d . 1 . . O
O3 0.5509(7) 0.7509(6) 0.2279(5) 0.0128(8) Uani d . 1 . . O
O4 -0.2098(8) 0.0608(6) -0.7238(5) 0.0169(9) Uani d . 1 . . O
H4A -0.1630 0.0984 -0.7876 0.020 Uiso d R 1 . . H
O5 0.3000(7) 0.5378(6) -0.0860(5) 0.0136(9) Uani d . 1 . . O
O6 0.0557(8) 0.5458(6) -0.3451(5) 0.0153(9) Uani d . 1 . . O
O7 0.1098(8) -0.2181(6) -0.0941(6) 0.0196(10) Uani d . 1 . . O
O8 0.1257(7) 0.5392(6) 0.1668(5) 0.0143(9) Uani d . 1 . . O
O9 -0.3767(8) 0.2100(6) -0.5082(5) 0.0173(9) Uani d . 1 . . O
O10 0.4774(8) 0.3805(6) 0.3099(6) 0.0233(10) Uani d . 1 . . O
O11 0.2701(8) 0.2904(7) -0.5300(6) 0.0234(10) Uani d . 1 . . O
H11A 0.3285 0.2570 -0.4515 0.028 Uiso d R 1 . . H
O12 -0.2687(7) -0.0514(6) -0.2394(5) 0.0151(9) Uani d . 1 . . O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O7 Fe1 O7 2 . 180.0 no
O7 Fe1 O2 . . 91.31(17) no
O7 Fe1 O2 . 2 88.69(17) no
O2 Fe1 O2 . 2 180.0 no
O7 Fe1 O12 . . 91.16(18) no
O2 Fe1 O12 . . 87.35(16) no
O7 Fe1 O12 . 2 88.84(18) no
O2 Fe1 O12 . 2 92.65(16) no
O12 Fe1 O12 . 2 180.0 no
O10 Fe2 O5 . . 178.53(18) no
O10 Fe2 O2 . . 97.14(19) no
O5 Fe2 O2 . . 84.33(17) no
O10 Fe2 O8 . . 89.75(19) no
O5 Fe2 O8 . . 89.95(17) no
O2 Fe2 O8 . . 105.93(17) no
O10 Fe2 O5 . 2_665 94.42(19) no
O5 Fe2 O5 . 2_665 85.42(17) no
O2 Fe2 O5 . 2_665 91.33(17) no
O8 Fe2 O5 . 2_665 161.61(17) no
O10 Fe2 O3 . . 98.10(18) no
O5 Fe2 O3 . . 80.43(17) no
O2 Fe2 O3 . . 164.22(17) no
O8 Fe2 O3 . . 78.23(16) no
O5 Fe2 O3 2_665 . 83.45(16) no
O12 Fe3 O8 . 2_565 139.30(18) no
O12 Fe3 O9 . . 123.63(18) no
O8 Fe3 O9 2_565 . 94.01(18) no
O12 Fe3 O3 . 2_565 105.10(18) no
O8 Fe3 O3 2_565 2_565 81.74(17) no
O9 Fe3 O3 . 2_565 98.00(17) no
O12 Fe3 O1 . . 85.19(17) no
O8 Fe3 O1 2_565 . 89.19(17) no
O9 Fe3 O1 . . 77.31(17) no
O3 Fe3 O1 2_565 . 169.52(16) no
O1 Fe4 O4 . . 104.60(18) no
O1 Fe4 O6 . 2_564 166.02(17) no
O4 Fe4 O6 . 2_564 88.49(18) no
O1 Fe4 O6 . . 89.64(17) no
O4 Fe4 O6 . . 163.75(18) no
O6 Fe4 O6 2_564 . 78.15(19) no
O1 Fe4 O11 . . 92.02(19) no
O4 Fe4 O11 . . 89.63(19) no
O6 Fe4 O11 2_564 . 83.04(19) no
O6 Fe4 O11 . . 97.80(18) no
O1 Fe4 O9 . . 79.42(17) no
O4 Fe4 O9 . . 81.65(18) no
O6 Fe4 O9 2_564 . 107.82(18) no
O6 Fe4 O9 . . 93.55(18) no
O11 Fe4 O9 . . 165.75(19) no
O3 P1 O1 2_665 . 111.2(2) no
O3 P1 O2 2_665 . 114.2(2) no
O1 P1 O2 . . 110.2(2) no
O3 P1 O4 2_665 2_554 106.9(2) no
O1 P1 O4 . 2_554 108.8(2) no
O2 P1 O4 . 2_554 105.3(2) no
O5 P2 O6 . . 108.0(2) no
O5 P2 O7 . 1_565 109.9(3) no
O6 P2 O7 . 1_565 110.2(3) no
O5 P2 O8 . 2_565 110.8(2) no
O6 P2 O8 . 2_565 109.3(2) no
O7 P2 O8 1_565 2_565 108.6(3) no
O10 P3 O12 1_454 2_454 111.2(3) no
O10 P3 O9 1_454 . 111.2(3) no
O12 P3 O9 2_454 . 111.6(3) no
O10 P3 O11 1_454 1_455 107.4(3) no
O12 P3 O11 2_454 1_455 109.5(3) no
O9 P3 O11 . 1_455 105.7(3) no
P1 O1 Fe4 . . 137.1(3) no
P1 O1 Fe3 . . 121.6(2) no
Fe4 O1 Fe3 . . 98.34(18) no
P1 O2 Fe2 . . 121.2(2) no
P1 O2 Fe1 . . 121.3(2) no
Fe2 O2 Fe1 . . 116.2(2) no
P1 O3 Fe3 2_665 2_565 137.2(3) no
P1 O3 Fe2 2_665 . 123.8(2) no
Fe3 O3 Fe2 2_565 . 97.46(17) no
P1 O4 Fe4 2_554 . 137.5(3) no
P2 O5 Fe2 . . 130.4(3) no
P2 O5 Fe2 . 2_665 135.0(3) no
Fe2 O5 Fe2 . 2_665 94.58(17) no
P2 O6 Fe4 . 2_564 132.5(3) no
P2 O6 Fe4 . . 124.9(2) no
Fe4 O6 Fe4 2_564 . 101.85(19) no
P2 O7 Fe1 1_545 . 155.3(3) no
P2 O8 Fe3 2_565 2_565 127.3(3) no
P2 O8 Fe2 2_565 . 127.1(3) no
Fe3 O8 Fe2 2_565 . 102.52(18) no
P3 O9 Fe3 . . 136.6(3) no
P3 O9 Fe4 . . 122.3(3) no
Fe3 O9 Fe4 . . 98.88(18) no
P3 O10 Fe2 1_656 . 142.7(3) no
P3 O11 Fe4 1_655 . 150.2(3) no
P3 O12 Fe3 2_454 . 119.0(3) no
P3 O12 Fe1 2_454 . 129.7(3) no
Fe3 O12 Fe1 . . 110.78(19) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 O7 . 2.121(5) yes
Fe1 O2 . 2.174(4) yes
Fe1 O12 . 2.248(4) yes
Fe2 O10 . 2.047(5) yes
Fe2 O5 . 2.085(4) yes
Fe2 O2 . 2.121(4) yes
Fe2 O8 . 2.125(4) yes
Fe2 O5 2_665 2.126(5) yes
Fe2 O3 . 2.202(4) yes
Fe3 O12 . 2.033(4) yes
Fe3 O8 2_565 2.046(4) yes
Fe3 O9 . 2.108(5) yes
Fe3 O3 2_565 2.126(4) yes
Fe3 O1 . 2.187(4) yes
Fe4 O1 . 2.069(4) yes
Fe4 O4 . 2.087(5) yes
Fe4 O6 2_564 2.100(4) yes
Fe4 O6 . 2.115(5) yes
Fe4 O11 . 2.124(5) yes
Fe4 O9 . 2.132(5) yes
P1 O3 2_665 1.532(4) no
P1 O1 . 1.534(4) no
P1 O2 . 1.545(4) no
P1 O4 2_554 1.557(4) no
P2 O5 . 1.530(4) no
P2 O6 . 1.535(5) no
P2 O7 1_565 1.536(5) no
P2 O8 2_565 1.537(4) no
P3 O10 1_454 1.509(5) no
P3 O12 2_454 1.526(4) no
P3 O9 . 1.536(5) no
P3 O11 1_455 1.567(5) no
O3 P1 2_665 1.532(4) no
O3 Fe3 2_565 2.126(4) no
O4 P1 2_554 1.557(4) no
O5 Fe2 2_665 2.126(5) no
O6 Fe4 2_564 2.100(4) no
O7 P2 1_545 1.536(5) no
O8 P2 2_565 1.537(4) no
O8 Fe3 2_565 2.046(4) no
O10 P3 1_656 1.509(5) no
O11 P3 1_655 1.567(5) no
O12 P3 2_454 1.526(4) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O4 H4A O7 2_554 0.85 1.71 2.539(7) 163.5
O11 H11A O3 2_665 0.85 2.03 2.850(7) 161.6
