data_kornelite
_publ_requested_journal          Am.Miner.
_publ_contact_author_name        'Juraj Majzlan'
_publ_contact_author_address     
'Institute of Mineralogy and Geochemistry, Freiburg'
_publ_contact_author_email       Juraj.Majzlan@minpet.uni-freiburg.de
loop_
_publ_author_name
_publ_author_address
'Ackermann, Sonia' 'Institute of Mineralogy and Geochemistry, Freiburg'
'Lazic, Biljana' 'Institute of Geology, Bern'
'Armbruster, Thomas' 'Institute of Geology, Bern'
'Doyle, Stephen'
'Forschungszentrum Karlsruhe, Institute for Synchrotron Radiation'
'Grevel, Klaus-Dieter' 'Institute of Mineralogy and Geochemistry, Freiburg'
'Majzlan, Juraj'
;Institute of Mineralogy and Geochemistry, Freiburg
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'Fe2 H12 O18 S3, O1.76'
_chemical_formula_sum            'Fe2 H12 O19.76 S3'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            violet

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         536.20

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   14.3125(3)
_cell_length_b                   20.1235(5)
_cell_length_c                   5.43100(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 96.8133(14)
_cell_angle_gamma                90.00
_cell_volume                     1553.18(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2540
_cell_measurement_theta_min      1.75
_cell_measurement_theta_max      24.37
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.005
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.293
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1080
_exptl_absorpt_coefficient_mu    2.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_process_details   SADAPS

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Apex II SMART (Bruker)'
_diffrn_measurement_method       'phi, omega'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21599
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         1.75
_diffrn_reflns_theta_max         24.37
_reflns_number_total             2540
_reflns_number_gt                1887
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0415P)²+1.4870P] 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         2540
_refine_ls_number_parameters     261
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.0977
_refine_ls_wR_factor_gt          0.0896
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.83024(5) 0.10292(3) 0.29736(12) 0.0177(2) Uani 1 1 d . . .
Fe2 Fe 0.83302(5) 0.38536(3) 0.77282(12) 0.0170(2) Uani 1 1 d . . .
S1 S 0.64829(9) 0.03559(6) 0.4920(2) 0.0168(3) Uani 1 1 d . . .
S2 S 0.89887(9) 0.24297(6) 0.5567(2) 0.0180(3) Uani 1 1 d . . .
S3 S 0.84574(9) -0.04884(6) 0.0716(2) 0.0169(3) Uani 1 1 d . . .
O1 O 0.5879(2) 0.05702(17) 0.6719(6) 0.0274(9) Uani 1 1 d . . .
O2 O 0.7297(2) 0.08181(17) 0.5036(6) 0.0258(9) Uani 1 1 d . . .
O3 O 0.6894(3) -0.03050(17) 0.5565(6) 0.0299(9) Uani 1 1 d . . .
O4 O 0.6000(2) 0.03345(18) 0.2411(6) 0.0285(9) Uani 1 1 d . . .
O5 O 0.9554(2) 0.26888(17) 0.3733(6) 0.0289(9) Uani 1 1 d . . .
O6 O 0.8358(2) 0.29533(16) 0.6342(6) 0.0255(9) Uani 1 1 d . . .
O7 O 0.9580(2) 0.21632(18) -0.2315(6) 0.0327(9) Uani 1 1 d . . .
O8 O 0.8330(2) 0.19135(17) 0.4446(6) 0.0287(9) Uani 1 1 d . . .
O9 O 0.9048(2) -0.04728(17) -0.1283(6) 0.0278(9) Uani 1 1 d . . .
O10 O 0.8954(2) -0.07560(17) 0.3002(6) 0.0250(9) Uani 1 1 d . . .
O11 O 0.8099(2) 0.01883(16) 0.1094(6) 0.0275(9) Uani 1 1 d . . .
O12 O 0.7622(2) -0.09166(17) 0.0074(6) 0.0263(9) Uani 1 1 d . . .
OW1 O 0.9422(3) 0.36298(19) 1.0248(7) 0.0302(10) Uani 1 1 d D . .
OW2 O 0.5729(3) -0.07599(18) -0.0664(6) 0.0224(8) Uani 1 1 d D . .
OW3 O 0.7619(3) -0.15293(19) 0.5259(8) 0.0378(11) Uani 1 1 d D . .
OW4 O 0.7457(3) 0.1413(2) 0.0150(8) 0.0458(12) Uani 1 1 d D . .
OW5 O 0.9206(3) 0.06040(18) 0.5604(6) 0.0253(9) Uani 1 1 d D . .
OW6 O 0.9437(3) 0.1251(2) 0.1302(7) 0.0320(11) Uani 1 1 d . . .
OW8A O 0.8638(9) -0.2473(6) 0.837(3) 0.064(3) Uiso 0.402(11) 1 d P . .
OW8B O 0.8565(5) -0.2589(4) 0.6628(16) 0.064(3) Uiso 0.658(13) 1 d P . .
OW7A O 0.8529(8) -0.2552(5) 1.203(3) 0.064(3) Uiso 0.465(17) 1 d P . .
OW7B O 0.8614(16) -0.2523(11) 1.072(6) 0.064(3) Uiso 0.237(16) 1 d P . .
H1A H 0.941(4) 0.334(2) 1.132(9) 0.050 Uiso 1 1 d D . .
H1B H 0.981(4) 0.393(3) 1.067(10) 0.050 Uiso 1 1 d D . .
H2A H 0.515(3) -0.065(3) -0.137(10) 0.050 Uiso 1 1 d D . .
H2B H 0.593(4) -0.044(2) 0.025(9) 0.050 Uiso 1 1 d D . .
H3A H 0.795(4) -0.126(3) 0.485(11) 0.050 Uiso 1 1 d D . .
H3B H 0.792(4) -0.187(2) 0.546(11) 0.050 Uiso 1 1 d D . .
H4A H 0.717(4) 0.114(3) -0.067(10) 0.050 Uiso 1 1 d D . .
H4B H 0.708(4) 0.174(3) 0.036(11) 0.050 Uiso 1 1 d D . .
H5A H 0.908(4) 0.027(2) 0.647(9) 0.050 Uiso 1 1 d D . .
H5B H 0.980(2) 0.068(3) 0.606(10) 0.050 Uiso 1 1 d D . .
H6A H 0.939(5) 0.149(3) 0.042(12) 0.050 Uiso 1 1 d . . .
H6B H 0.988(4) 0.102(3) 0.126(11) 0.050 Uiso 1 1 d . . .


_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 O8 1.949(3) . ?
Fe1 O2 1.972(3) . ?
Fe1 O11 1.980(3) . ?
Fe1 OW4 1.992(4) . ?
Fe1 OW5 2.002(3) . ?
Fe1 OW6 2.003(4) . ?
Fe2 O6 1.964(3) . ?
Fe2 O12 1.973(3) 2_655 ?
Fe2 O3 1.975(3) 2_656 ?
Fe2 OW3 1.996(4) 2_656 ?
Fe2 OW1 2.003(4) . ?
Fe2 OW2 2.009(3) 2_655 ?
S1 O1 1.445(3) . ?
S1 O4 1.453(3) . ?
S1 O3 1.479(3) . ?
S1 O2 1.486(3) . ?
S2 O7 1.448(3) 1_556 ?
S2 O5 1.452(3) . ?
S2 O6 1.481(3) . ?
S2 O8 1.484(3) . ?
S3 O9 1.453(3) . ?
S3 O10 1.459(3) . ?
S3 O11 1.478(3) . ?
S3 O12 1.482(3) . ?
O3 Fe2 1.975(3) 2_646 ?
O7 S2 1.448(3) 1_554 ?
O12 Fe2 1.973(3) 2_645 ?
OW1 H1A 0.83(4) . ?
OW1 H1B 0.84(4) . ?
OW2 Fe2 2.009(3) 2_645 ?
OW2 H2A 0.90(4) . ?
OW2 H2B 0.85(4) . ?
OW3 Fe2 1.996(4) 2_646 ?
OW3 H3A 0.77(4) . ?
OW3 H3B 0.81(4) . ?
OW4 H4A 0.79(4) . ?
OW4 H4B 0.87(4) . ?
OW5 H5A 0.86(3) . ?
OW5 H5B 0.86(3) . ?
OW6 H6A 0.68(6) . ?
OW6 H6B 0.79(6) . ?
OW8A OW8B 0.969(13) . ?
OW8A OW7B 1.29(3) . ?
OW7A OW7B 0.74(3) . ?

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
O8 Fe1 O2 86.81(14) . . ?
O8 Fe1 O11 170.50(14) . . ?
O2 Fe1 O11 92.08(14) . . ?
O8 Fe1 OW4 86.73(16) . . ?
O2 Fe1 OW4 95.92(18) . . ?
O11 Fe1 OW4 84.00(15) . . ?
O8 Fe1 OW5 96.76(15) . . ?
O2 Fe1 OW5 87.48(15) . . ?
O11 Fe1 OW5 92.61(14) . . ?
OW4 Fe1 OW5 175.27(18) . . ?
O8 Fe1 OW6 90.25(16) . . ?
O2 Fe1 OW6 172.39(16) . . ?
O11 Fe1 OW6 91.96(17) . . ?
OW4 Fe1 OW6 90.91(19) . . ?
OW5 Fe1 OW6 85.90(16) . . ?
O6 Fe2 O12 87.93(14) . 2_655 ?
O6 Fe2 O3 169.29(14) . 2_656 ?
O12 Fe2 O3 91.45(15) 2_655 2_656 ?
O6 Fe2 OW3 84.24(15) . 2_656 ?
O12 Fe2 OW3 93.47(18) 2_655 2_656 ?
O3 Fe2 OW3 85.12(15) 2_656 2_656 ?
O6 Fe2 OW1 90.29(15) . . ?
O12 Fe2 OW1 172.35(15) 2_655 . ?
O3 Fe2 OW1 91.67(16) 2_656 . ?
OW3 Fe2 OW1 93.75(18) 2_656 . ?
O6 Fe2 OW2 95.63(14) . 2_655 ?
O12 Fe2 OW2 85.77(14) 2_655 2_655 ?
O3 Fe2 OW2 94.99(14) 2_656 2_655 ?
OW3 Fe2 OW2 179.23(17) 2_656 2_655 ?
OW1 Fe2 OW2 87.01(15) . 2_655 ?
O1 S1 O4 112.8(2) . . ?
O1 S1 O3 111.2(2) . . ?
O4 S1 O3 109.1(2) . . ?
O1 S1 O2 108.3(2) . . ?
O4 S1 O2 110.0(2) . . ?
O3 S1 O2 105.4(2) . . ?
O7 S2 O5 110.9(2) 1_556 . ?
O7 S2 O6 110.9(2) 1_556 . ?
O5 S2 O6 110.3(2) . . ?
O7 S2 O8 110.5(2) 1_556 . ?
O5 S2 O8 110.4(2) . . ?
O6 S2 O8 103.6(2) . . ?
O9 S3 O10 112.1(2) . . ?
O9 S3 O11 109.0(2) . . ?
O10 S3 O11 111.3(2) . . ?
O9 S3 O12 111.2(2) . . ?
O10 S3 O12 106.5(2) . . ?
O11 S3 O12 106.5(2) . . ?
S1 O2 Fe1 137.0(2) . . ?
S1 O3 Fe2 143.1(2) . 2_646 ?
S2 O6 Fe2 143.7(2) . . ?
S2 O8 Fe1 142.0(2) . . ?
S3 O11 Fe1 145.8(2) . . ?
S3 O12 Fe2 141.4(2) . 2_645 ?
Fe2 OW1 H1A 124(4) . . ?
Fe2 OW1 H1B 117(4) . . ?
H1A OW1 H1B 113(6) . . ?
Fe2 OW2 H2A 120(4) 2_645 . ?
Fe2 OW2 H2B 115(4) 2_645 . ?
H2A OW2 H2B 107(5) . . ?
Fe2 OW3 H3A 112(5) 2_646 . ?
Fe2 OW3 H3B 130(4) 2_646 . ?
H3A OW3 H3B 107(6) . . ?
Fe1 OW4 H4A 113(5) . . ?
Fe1 OW4 H4B 122(4) . . ?
H4A OW4 H4B 109(6) . . ?
Fe1 OW5 H5A 125(4) . . ?
Fe1 OW5 H5B 131(4) . . ?
H5A OW5 H5B 104(5) . . ?
Fe1 OW6 H6A 117(6) . . ?
Fe1 OW6 H6B 126(5) . . ?
H6A OW6 H6B 115(7) . . ?
OW8B OW8A OW7B 160.0(17) . . ?
OW7A OW7B OW8A 172(3) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.37
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.118

