#------------------------------------------------------------------------------
#$Date: 2018-01-23 11:47:50 +0200 (Tue, 23 Jan 2018) $
#$Revision: 205491 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/23/33/2233314.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_2233314
loop_
_publ_author_name
'Yang, Hexiong'
'Downs, Robert T.'
'Yang, Yongbo W.'
'Allen, Warren H.'
_publ_section_title
;
 Pyrosmalite-(Fe), Fe₈Si₆O₁₅(OH,Cl)₁₀
;
_journal_coden_ASTM              ACSEBH
_journal_coeditor_code           WM2570
_journal_issue                   1
_journal_name_full
;
 Acta Crystallographica, Section E: Structure Reports Online
;
_journal_page_first              i7
_journal_page_last               i8
_journal_paper_doi               10.1107/S1600536811052822
_journal_volume                  68
_journal_year                    2012
_chemical_compound_source        'Burguillos del Cerro, Badajos, Spain'
_chemical_formula_iupac          'Fe8 Si6 O15 (O H0.814 Cl0.186)10, 0.45H2 O'
_chemical_formula_moiety         'Cl1.855 Fe8 H7.58 O23.135 Si6, 0.45(H2 O)'
_chemical_formula_sum            'Cl1.855 Fe8 H8.48 O23.585 Si6'
_chemical_formula_weight         1067.35
_chemical_name_common            Pyrosmalite-(Fe)
_chemical_name_mineral           Pyrosmalite-(Fe)
_chemical_name_systematic
;
octairon(II) hexasilicate deca(chloride/hydroxide) 0.45-hydrate
;
_space_group_crystal_system      trigonal
_space_group_IT_number           164
_space_group_name_Hall           '-P 3 2"'
_space_group_name_H-M_alt        'P -3 m 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   13.3165(2)
_cell_length_b                   13.3165(2)
_cell_length_c                   7.0845(2)
_cell_measurement_reflns_used    2724
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.55
_cell_measurement_theta_min      2.875
_cell_volume                     1087.98(4)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'XtalDraw (Downs & Hall-Wallace, 2003)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0170
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13410
_diffrn_reflns_theta_full        32.55
_diffrn_reflns_theta_max         32.55
_diffrn_reflns_theta_min         1.77
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.848
_exptl_absorpt_correction_T_max  0.6529
_exptl_absorpt_correction_T_min  0.6221
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2005)'
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    3.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1039
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.557
_refine_ls_extinction_coef       0.00082(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0232
_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)+(0.0328P)²+0.4308P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                1141
_reflns_number_total             1476
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm2570.cif
_cod_data_source_block           I
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2018-01-23
;
_cod_database_code               2233314
_cod_database_fobs_code          2233314
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-y, x-y, z'
3 '-x+y, -x, z'
4 'y, x, -z'
5 'x-y, -y, -z'
6 '-x, -x+y, -z'
7 '-x, -y, -z'
8 'y, -x+y, -z'
9 'x-y, x, -z'
10 '-y, -x, z'
11 '-x+y, y, z'
12 'x, x-y, z'
loop_
_atom_site_type_symbol
_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_attached_hydrogens
Fe Fe1 0.0000 0.0000 0.0000 0.01547(19) Uani d S 1 0
Fe Fe2 0.25510(3) 0.0000 0.0000 0.01193(10) Uani d S 1 0
Fe Fe3 0.5000 0.0000 0.0000 0.01004(12) Uani d S 1 0
Fe Fe4 0.50261(3) 0.251306(15) 0.01962(5) 0.00953(10) Uani d S 1 0
Si Si1 0.43696(4) 0.10405(4) 0.62679(6) 0.00674(11) Uani d . 1 0
O O1 0.34125(13) 0.0000 0.5000 0.0126(3) Uani d S 1 0
O O2 0.56373(8) 0.12746(15) 0.5610(2) 0.0113(3) Uani d S 1 0
O O3 0.43070(15) 0.21535(8) 0.5580(2) 0.0122(3) Uani d S 1 0
O O4 0.41964(10) 0.08283(10) 0.84971(18) 0.0100(3) Uani d . 1 0
Cl Cl1 0.16942(9) 0.08471(4) 0.7741(2) 0.0189(4) Uani d SP 0.619(5) 0
O OH1 0.1647(4) 0.0824(2) 0.8785(9) 0.0133(11) Uani d SP 0.381(5) 1
O OH2 0.33476(14) 0.16738(7) 0.1306(2) 0.0129(4) Uani d S 1 0
O OH3 0.58147(7) 0.16295(14) 0.1443(2) 0.0106(3) Uani d S 1 0
O OH4 0.3333 0.6667 0.1263(4) 0.0111(6) Uani d S 1 0
O OW1 0.1055(17) 0.1055(17) 0.5000 0.069(8) Uiso d SP 0.147(8) 2
H H1 0.334(3) 0.1671(14) 0.255(5) 0.030 Uiso d S 1 0
H H2 0.5810(14) 0.162(3) 0.264(6) 0.030 Uiso d S 1 0
H H3 0.3333 0.6667 0.271(8) 0.030 Uiso d S 1 0
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Si Si 0.0817 0.0704 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
OH1 Fe1 OH1 9_556 3_554 180.0(4)
OH1 Fe1 OH1 9_556 8_556 104.15(19)
OH1 Fe1 OH1 3_554 8_556 75.85(19)
OH1 Fe1 OH1 9_556 1_554 75.85(19)
OH1 Fe1 OH1 3_554 1_554 104.15(19)
OH1 Fe1 OH1 8_556 1_554 75.85(19)
OH1 Fe1 OH1 9_556 2_554 75.85(19)
OH1 Fe1 OH1 3_554 2_554 104.15(19)
OH1 Fe1 OH1 8_556 2_554 180.00(18)
OH1 Fe1 OH1 1_554 2_554 104.15(19)
OH1 Fe1 OH1 9_556 7_556 104.15(19)
OH1 Fe1 OH1 3_554 7_556 75.85(19)
OH1 Fe1 OH1 8_556 7_556 104.15(19)
OH1 Fe1 OH1 1_554 7_556 180.0(4)
OH1 Fe1 OH1 2_554 7_556 75.85(19)
OH1 Fe1 Cl1 9_556 3_554 165.06(15)
OH1 Fe1 Cl1 3_554 3_554 14.94(15)
OH1 Fe1 Cl1 8_556 3_554 84.79(13)
OH1 Fe1 Cl1 1_554 3_554 95.21(13)
OH1 Fe1 Cl1 2_554 3_554 95.21(13)
OH1 Fe1 Cl1 7_556 3_554 84.79(13)
OH1 Fe1 Cl1 9_556 9_556 14.94(15)
OH1 Fe1 Cl1 3_554 9_556 165.06(15)
OH1 Fe1 Cl1 8_556 9_556 95.21(13)
OH1 Fe1 Cl1 1_554 9_556 84.79(13)
OH1 Fe1 Cl1 2_554 9_556 84.79(13)
OH1 Fe1 Cl1 7_556 9_556 95.21(13)
Cl1 Fe1 Cl1 3_554 9_556 180.00(7)
OH1 Fe1 Cl1 9_556 7_556 95.21(13)
OH1 Fe1 Cl1 3_554 7_556 84.79(13)
OH1 Fe1 Cl1 8_556 7_556 95.21(13)
OH1 Fe1 Cl1 1_554 7_556 165.06(15)
OH1 Fe1 Cl1 2_554 7_556 84.79(13)
OH1 Fe1 Cl1 7_556 7_556 14.94(15)
Cl1 Fe1 Cl1 3_554 7_556 95.87(4)
Cl1 Fe1 Cl1 9_556 7_556 84.13(4)
OH1 Fe1 Cl1 9_556 8_556 95.21(13)
OH1 Fe1 Cl1 3_554 8_556 84.79(13)
OH1 Fe1 Cl1 8_556 8_556 14.94(15)
OH1 Fe1 Cl1 1_554 8_556 84.79(13)
OH1 Fe1 Cl1 2_554 8_556 165.06(15)
OH1 Fe1 Cl1 7_556 8_556 95.21(13)
Cl1 Fe1 Cl1 3_554 8_556 95.87(4)
Cl1 Fe1 Cl1 9_556 8_556 84.13(4)
Cl1 Fe1 Cl1 7_556 8_556 84.13(4)
OH1 Fe1 Cl1 9_556 1_554 84.79(13)
OH1 Fe1 Cl1 3_554 1_554 95.21(13)
OH1 Fe1 Cl1 8_556 1_554 84.79(13)
OH1 Fe1 Cl1 1_554 1_554 14.94(15)
OH1 Fe1 Cl1 2_554 1_554 95.21(13)
OH1 Fe1 Cl1 7_556 1_554 165.06(15)
Cl1 Fe1 Cl1 3_554 1_554 84.13(4)
Cl1 Fe1 Cl1 9_556 1_554 95.87(4)
Cl1 Fe1 Cl1 7_556 1_554 180.00(7)
Cl1 Fe1 Cl1 8_556 1_554 95.87(4)
OH1 Fe1 Cl1 9_556 2_554 84.79(13)
OH1 Fe1 Cl1 3_554 2_554 95.21(13)
OH1 Fe1 Cl1 8_556 2_554 165.06(15)
OH1 Fe1 Cl1 1_554 2_554 95.21(13)
OH1 Fe1 Cl1 2_554 2_554 14.94(15)
OH1 Fe1 Cl1 7_556 2_554 84.79(13)
Cl1 Fe1 Cl1 3_554 2_554 84.13(4)
Cl1 Fe1 Cl1 9_556 2_554 95.87(4)
Cl1 Fe1 Cl1 7_556 2_554 95.87(4)
Cl1 Fe1 Cl1 8_556 2_554 180.00(4)
Cl1 Fe1 Cl1 1_554 2_554 84.13(4)
OH2 Fe2 OH2 . 8 177.13(8)
OH2 Fe2 OH1 . 1_554 75.92(12)
OH2 Fe2 OH1 8 1_554 101.70(12)
OH2 Fe2 OH1 . 8_556 101.70(12)
OH2 Fe2 OH1 8 8_556 75.92(12)
OH1 Fe2 OH1 1_554 8_556 72.4(3)
OH2 Fe2 O4 . 1_554 80.48(6)
OH2 Fe2 O4 8 1_554 101.72(5)
OH1 Fe2 O4 1_554 1_554 102.83(15)
OH1 Fe2 O4 8_556 1_554 173.86(16)
OH2 Fe2 O4 . 5_556 101.72(5)
OH2 Fe2 O4 8 5_556 80.48(6)
OH1 Fe2 O4 1_554 5_556 173.86(16)
OH1 Fe2 O4 8_556 5_556 102.83(15)
O4 Fe2 O4 1_554 5_556 82.21(6)
OH2 Fe2 Cl1 . 1_554 84.75(4)
OH2 Fe2 Cl1 8 1_554 93.31(5)
OH1 Fe2 Cl1 1_554 1_554 15.84(15)
OH1 Fe2 Cl1 8_556 1_554 82.88(16)
O4 Fe2 Cl1 1_554 1_554 91.65(4)
O4 Fe2 Cl1 5_556 1_554 170.13(4)
OH2 Fe2 Cl1 . 8_556 93.31(5)
OH2 Fe2 Cl1 8 8_556 84.75(4)
OH1 Fe2 Cl1 1_554 8_556 82.88(16)
OH1 Fe2 Cl1 8_556 8_556 15.84(15)
O4 Fe2 Cl1 1_554 8_556 170.13(4)
O4 Fe2 Cl1 5_556 8_556 91.65(4)
Cl1 Fe2 Cl1 1_554 8_556 95.43(6)
OH3 Fe3 OH3 7_655 . 180.00(8)
OH3 Fe3 O4 7_655 1_554 98.78(4)
OH3 Fe3 O4 . 1_554 81.22(4)
OH3 Fe3 O4 7_655 7_656 81.22(4)
OH3 Fe3 O4 . 7_656 98.78(4)
O4 Fe3 O4 1_554 7_656 180.00(7)
OH3 Fe3 O4 7_655 5_556 81.22(4)
OH3 Fe3 O4 . 5_556 98.78(4)
O4 Fe3 O4 1_554 5_556 82.83(6)
O4 Fe3 O4 7_656 5_556 97.17(6)
OH3 Fe3 O4 7_655 11_654 98.78(4)
OH3 Fe3 O4 . 11_654 81.22(4)
O4 Fe3 O4 1_554 11_654 97.17(6)
O4 Fe3 O4 7_656 11_654 82.83(6)
O4 Fe3 O4 5_556 11_654 180.00(7)
OH2 Fe4 OH3 . 3_665 103.91(5)
OH2 Fe4 OH3 . . 103.91(5)
OH3 Fe4 OH3 3_665 . 106.62(9)
OH2 Fe4 OH4 . 7_665 173.45(7)
OH3 Fe4 OH4 3_665 7_665 79.84(5)
OH3 Fe4 OH4 . 7_665 79.84(5)
OH2 Fe4 O4 . 1_554 79.07(5)
OH3 Fe4 O4 3_665 1_554 172.72(5)
OH3 Fe4 O4 . 1_554 78.78(5)
OH4 Fe4 O4 7_665 1_554 96.59(5)
OH2 Fe4 O4 . 12_554 79.07(5)
OH3 Fe4 O4 3_665 12_554 78.78(5)
OH3 Fe4 O4 . 12_554 172.72(5)
OH4 Fe4 O4 7_665 12_554 96.59(5)
O4 Fe4 O4 1_554 12_554 95.44(6)
O4 Si1 O3 . . 113.19(7)
O4 Si1 O1 . . 114.64(5)
O3 Si1 O1 . . 104.01(7)
O4 Si1 O2 . . 111.17(7)
O3 Si1 O2 . . 105.38(9)
O1 Si1 O2 . . 107.77(8)
Si1 O1 Si1 . 5_556 137.58(12)
Si1 O2 Si1 . 11_655 141.27(11)
Si1 O3 Si1 12 . 144.19(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Fe1 OH1 9_556 2.085(5)
Fe1 OH1 3_554 2.085(5)
Fe1 OH1 8_556 2.085(5)
Fe1 OH1 1_554 2.085(5)
Fe1 OH1 2_554 2.085(5)
Fe1 OH1 7_556 2.085(5)
Fe1 Cl1 3_554 2.5255(12)
Fe1 Cl1 9_556 2.5255(12)
Fe1 Cl1 7_556 2.5255(12)
Fe1 Cl1 8_556 2.5255(12)
Fe1 Cl1 1_554 2.5255(12)
Fe1 Cl1 2_554 2.5255(12)
Fe2 OH2 . 2.1413(11)
Fe2 OH2 8 2.1413(11)
Fe2 OH1 1_554 2.171(3)
Fe2 OH1 8_556 2.171(3)
Fe2 O4 1_554 2.1759(12)
Fe2 O4 5_556 2.1759(11)
Fe2 Cl1 1_554 2.5342(10)
Fe2 Cl1 8_556 2.5342(10)
Fe3 OH3 7_655 2.1394(16)
Fe3 OH3 . 2.1394(16)
Fe3 O4 1_554 2.1624(11)
Fe3 O4 7_656 2.1624(11)
Fe3 O4 5_556 2.1624(11)
Fe3 O4 11_654 2.1624(11)
Fe4 OH2 . 2.0893(17)
Fe4 OH3 3_665 2.1222(10)
Fe4 OH3 . 2.1222(10)
Fe4 OH4 7_665 2.1560(13)
Fe4 O4 1_554 2.2856(12)
Fe4 O4 12_554 2.2856(12)
Si1 O4 . 1.6006(13)
Si1 O3 . 1.6014(6)
Si1 O1 . 1.6078(8)
Si1 O2 . 1.6242(7)
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
OH2 H1 O3 . 0.88(4) 2.42(4) 3.224(2) 152(3)
OH3 H2 O2 . 0.85(4) 2.14(4) 2.980(2) 170(3)
OH4 H3 O2 7_666 1.03(5) 2.66(2) 3.247(2) 116.6(12)
OH4 H3 O2 8_566 1.03(5) 2.66(2) 3.247(2) 116.6(12)
OH4 H3 O2 9_556 1.03(5) 2.66(2) 3.247(2) 116.6(12)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 AMCSD 0018558
