data_global 
_audit_creation_date        09-05-13
_audit_creation_method CRYSTALS_ver_12.85

_oxford_structure_analysis_title  'Sideronatrite, Na2Fe(SO4)2(OH)3H2O:  crystal structure of the orthorhombic polytype and OD character'
_chemical_name_systematic         Sideronatrite
_chemical_melting_point           ?

#looking for refcif 
 
 
# Check this file using the IUCr facility at: 
# http://checkcif.iucr.org/ 
 
# The content below is held in the file 'script/refcif.dat'. This is a text 
# file which you may edit to reflect local conditions. 
# Items which need looking at are represented by a '?'. 
# Items for which there are choices are prefixed with 'choose from'. 
 
_publ_contact_letter 
; 
 Please consider this CIF submission for 
 publication as a Regular Paper in American 
 Mineralogist. 
; 
_publ_contact_author_name         'Fernando Scordari' 
_publ_contact_author_address 
; 
 Dipartimento Geomineralogico, 
 Universita' di Bari, 
 via Orabona, N.4 I-70125, Bari (Italy). 
; 
 
_publ_contact_author_phone        '+39 80 5442587' 
_publ_contact_author_fax          '+39 80 5442591' 
_publ_contact_author_email        'f.scordari@geomin.uniba.it' 
_publ_requested_journal           'American Mineralogist' 
_publ_requested_category          EO # choose from: FI FM FO CI CM CO AD 
_publ_requested_coeditor_name     '-' 
 
_publ_section_title 
# Title of paper - generally just the systematic or trivial name 
; ? 
; 
 
# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary. 
loop_ 
 _publ_author_name 
 _publ_author_address 
 _publ_author_footnote 
 'Scordari, Fernando' # Author 1 
; 
 ? # Address for author 1 
; Dipartimento Geomineralogico, 
 Universita' degli Studi di Bari, 
 via Orabona, 4 I-70125 Bari, Italy.
; 
 ? # Footnote for author 1 
; 
 'Ventruti, Gennaro' # Author 2 
; 
 ? # Address 2 
; Dipartimento Geomineralogico, 
 Universita' degli Studi di Bari, 
 via Orabona, 4 I-70125 Bari, Italy.
; 
 ? # Footnote 2 
; 
 
  
; 

 
 
; 
 
_cell_length_a                    7.265(2)
_cell_length_b                    20.522(6)
_cell_length_c                    7.120(2)
_cell_angle_alpha                 90
_cell_angle_beta                  90
_cell_angle_gamma                 90
_cell_volume                      1061.5(5)
 
_symmetry_cell_setting            'Orthorhombic' 
_symmetry_space_group_name_H-M    'P 21 21 21 ' 
_symmetry_space_group_name_Hall   ? 
loop_
 _symmetry_equiv_pos_as_xyz
 'x,y,z'
 'x+1/2,-y+1/2,-z'
 '-x,y+1/2,-z+1/2'
 '-x+1/2,-y,z+1/2'

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source  
 Fe      0.3463   0.8444  11.7695   4.7611   7.3573   0.3072   3.5222  15.3535
   2.3045  76.8805   1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 S       0.1246   0.1234   6.9053   1.4679   5.2034  22.2151   1.4379   0.2536
   1.5863  56.1720   0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 Na      0.0362   0.0249   4.7626   3.2850   3.1736   8.8422   1.2674   0.3136
   1.1128 129.4240   0.6760 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 O       0.0106   0.0060   3.0485  13.2771   2.2868   5.7011   1.5463   0.3239
   0.8670  32.9089   0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
 
 
_cell_formula_units_Z                    4

# Given Formula = Fe0.50 Na1 O6 S1 
# Dc =      1.12 Fooo =    704.00 Mu =      9.75 M =    178.98
# Found Formula = Fe1 Na2 O12 S2 
# Dc =      2.24 FOOO =    704.00 Mu =     19.50 M =    357.95

_chemical_formula_sum             'Fe1 Na2 O12 S2'
_chemical_formula_moiety          'Fe1 Na2 O12 S2'
_chemical_compound_source                Sierra Gorda (Chile)
_chemical_formula_weight            357.95
 
 
_cell_measurement_reflns_used            10602
_cell_measurement_theta_min              4.473
_cell_measurement_theta_max              36.330
_cell_measurement_temperature          293
 
_exptl_crystal_description        'minute needles elongated [001]' 
_exptl_crystal_colour             'lemon-yellow' 
_exptl_crystal_size_min           0.020 
_exptl_crystal_size_mid           0.060 
_exptl_crystal_size_max           0.160 
 
_exptl_crystal_density_diffrn     2.240 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     'not measured' 
# Non-dispersive F(000): 
_exptl_crystal_F_000              704 
_exptl_absorpt_coefficient_mu     1.950 
 
# Sheldrick geometric approximatio 1.00 1.00 
_exptl_absorpt_correction_type    sadabs 
_exptl_absorpt_correction_T_min   0.6053 
_exptl_absorpt_correction_T_max   0.7479 
_diffrn_measurement_device        'Bruker Axs X8 ApexII' 
_diffrn_measurement_device_type   'Serial' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_radiation_type            'Mo K\a'
_diffrn_radiation_wavelength           0.71070
_diffrn_measurement_method        ω/2θ 
 
# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection        'USER DEFINED DATA COLLECTION' 
_computing_cell_refinement        'USER DEFINED CELL REFINEMENT' 
_computing_data_reduction         'USER DEFINED DATA REDUCTION' 
_computing_structure_solution     'USER DEFINED STRUCTURE SOLUTION' 
_computing_structure_refinement   'CRYSTALS (Betteridge et al., 2003)' 
_computing_publication_material   'CRYSTALS (Betteridge et al., 2003)' 
_computing_molecular_graphics     'CAMERON (Watkin et al., 1996)' 
 
_diffrn_standards_interval_time   . 
_diffrn_standards_interval_count  . 
_diffrn_standards_number          0 
_diffrn_standards_decay_%         ? 
 
_diffrn_ambient_temperature        293
_diffrn_reflns_number            10602 
_reflns_number_total              2888 
_diffrn_reflns_av_R_equivalents   0.072 
# Number of reflections with Friedels Law is 2888 
# Number of reflections without Friedels Law is 0 
# Theoretical number of reflections is about 2576 
 
 
_diffrn_reflns_theta_min          4.473 
_diffrn_reflns_theta_max          36.330 
_diffrn_measured_fraction_theta_max 0.985 
 
_diffrn_reflns_theta_full         36.330 
_diffrn_measured_fraction_theta_full 0.985 
 
 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        12 
_diffrn_reflns_limit_k_min        -34 
_diffrn_reflns_limit_k_max        32 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        3 
_reflns_limit_h_min               0 
_reflns_limit_h_max               12 
_reflns_limit_k_min               0 
_reflns_limit_k_max               34 
_reflns_limit_l_min               0 
_reflns_limit_l_max               11 
 
_oxford_diffrn_Wilson_B_factor    0.00 
_oxford_diffrn_Wilson_scale       0.00 
 
_atom_sites_solution_primary      direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens    geom
 
_refine_diff_density_min          -0.961 
_refine_diff_density_max          0.848 
 
 
# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 
 
 
# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref     I>3.0\s(I)
_refine_ls_number_reflns           798 
_refine_ls_number_restraints      15 
_refine_ls_number_parameters      58 
_oxford_refine_ls_R_factor_ref    0.0736 
_refine_ls_wR_factor_ref          0.0802 
_refine_ls_goodness_of_fit_ref    1.3560 
_refine_ls_shift/su_max           0.001674 
 
 
# The values computed from all data 
_oxford_reflns_number_all         2856 
_refine_ls_R_factor_all           0.2027 
_refine_ls_wR_factor_all          0.3151 
 
# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression      I>2.0σ(I)
_reflns_number_gt                 1027 
_refine_ls_R_factor_gt            0.0867 
_refine_ls_wR_factor_gt           0.0959 
 
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration  'unk' 
 
 
_refine_ls_structure_factor_coef  F 
_refine_ls_matrix_type            full
_refine_ls_hydrogen_treatment     none           # none, undef, noref, refall,
                                                 # refxyz, refU, constr or mixed
 
# WARNING. The IUCr will not accept Unit Weights 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
;
 Method= Quasi-Unit weights 
 W = 1.0 or 1./2F 
;
# Insert your own references if required - in alphabetical order 
_publ_section_references 
; 
User-defined structure solution reference 
 
User-defined data collection reference 
 
User defined data reduction 
 
User defined cell refinement 
 
Betteridge, P.W., Carruthers, J.R., Cooper, R.I., 
Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 
 
Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical 
Crystallography Laboratory, Oxford, UK. 
; 

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atomsattached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
Fe1 Fe 0.2500 0.0000 0.1250 0.0100 1.0000 Uani . . . . . . . 
S2 S 0.2251(5) 0.1317(2) 0.8781(3) 0.0139 1.0000 Uani . . . . . . . 
S3 S 0.8763(4) 0.0056(2) 0.3781(3) 0.0119 1.0000 Uani . . . . . . . 
Na4 Na 0.8294(6) 0.1224(2) 0.120(3) 0.0267(10) 1.0000 Uiso . . . . . . . 
Na5 Na 0.8294(6) 0.1224(2) 0.627(3) 0.0267(10) 1.0000 Uiso . . . . . . . 
O6 O 0.0291(19) 0.1452(7) 0.8781(3) 0.024(3) 1.0000 Uiso . . . . . . . 
O7 O 0.3299(18) 0.1927(6) 0.8781(3) 0.025(3) 1.0000 Uiso . . . . . . . 
O8 O 0.2795(11) 0.0944(4) 0.0463(9) 0.0195(17) 1.0000 Uiso . . . . . . . 
O9 O 0.2795(11) 0.0944(4) 0.7053(9) 0.0195(17) 1.0000 Uiso . . . . . . . 
O10 O 0.9901(10) 0.0185(4) 0.5497(9) 0.0164(15) 1.0000 Uiso . . . . . . . 
O11 O 0.9901(10) 0.0185(4) 0.2019(9) 0.0164(15) 1.0000 Uiso . . . . . . . 
O12 O 0.7222(18) 0.0511(6) 0.3781(3) 0.017(3) 1.0000 Uiso . . . . . . . 
O13 O 0.687(2) 0.0625(7) 0.8781(3) 0.023(3) 1.0000 Uiso . . . . . . . 
O14 O 0.3430(15) 0.0241(5) 0.3781(3) 0.015(2) 1.0000 Uiso . . . . . . . 
O15 O 0.5984(16) 0.1984(5) 0.5835(17) 0.047(3) 1.0000 Uiso . . . . . . . 
O16 O 0.032(2) 0.1661(8) 0.3781(3) 0.035(4) 1.0000 Uiso . . . . . . . 
O17 O 0.5984(16) 0.1984(5) 0.1676(17) 0.047(3) 1.0000 Uiso . . . . . . . 
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
Fe1 0.0086(6) 0.0163(7) 0.0050(6) 0.0014(18) 0.0024(14) 0.0009(8) 
S2 0.0070(10) 0.0252(15) 0.0096(10) 0.003(3) -0.006(3) 0.0001(10) 
S3 0.0072(10) 0.0204(15) 0.0083(10) 0.000(3) -0.001(3) -0.0001(10)

_refine_ls_extinction_method 
    'None'
_oxford_refine_ls_scale 0.671(5) 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_site_symmetry_1
 _geom_bond_atom_site_label_2
 _geom_bond_site_symmetry_2
 _geom_bond_distance
 _geom_bond_publ_flag
Fe1 . O9 4_554 2.032(7)    yes
Fe1 . O11 1_455 2.002(7)    yes
Fe1 . O10 4_654 1.999(7)    yes
Fe1 . O14 4_554 1.947(5)    yes
Fe1 . O8 . 2.029(7)    yes
Fe1 . O14 . 1.987(5)    yes
S2 . O8 1_556 1.475(7)    yes
S2 . O6 . 1.451(14)    yes
S2 . O7 . 1.467(14)    yes
S2 . O9 . 1.501(7)    yes
S3 . O13 4_654 1.471(15)    yes
S3 . O10 . 1.499(7)    yes
S3 . O11 . 1.526(7)    yes
S3 . O12 . 1.456(14)    yes
Na4 . O6 1_654 2.303(17)    yes
Na4 . O13 1_554 2.359(17)    yes
Na4 . O16 1_655 2.515(18)    yes
Na4 . O11 . 2.499(10)    yes
Na4 . O12 . 2.472(16)    yes
Na4 . O17 . 2.316(13)    yes
Na5 . O6 1_655 2.349(17)    yes
Na5 . O16 1_655 2.471(17)    yes
Na5 . O10 . 2.493(10)    yes
Na5 . O12 . 2.427(16)    yes
Na5 . O13 . 2.404(17)    yes
Na5 . O15 . 2.313(13)    yes
loop_
 _geom_angle_atom_site_label_1
 _geom_angle_site_symmetry_1
 _geom_angle_atom_site_label_2
 _geom_angle_site_symmetry_2
 _geom_angle_atom_site_label_3
 _geom_angle_site_symmetry_3
 _geom_angle
 _geom_angle_publ_flag
O9 4_554 Fe1 . O11 1_455 90.2(3)    yes
O9 4_554 Fe1 . O10 4_654 89.7(3)    yes
O11 1_455 Fe1 . O10 4_654 179.7(3)    yes
O9 4_554 Fe1 . O14 4_554 88.6(4)    yes
O11 1_455 Fe1 . O14 4_554 88.2(4)    yes
O10 4_654 Fe1 . O14 4_554 92.1(4)    yes
O9 4_554 Fe1 . O8 . 179.7(3)    yes
O11 1_455 Fe1 . O8 . 89.7(3)    yes
O10 4_654 Fe1 . O8 . 90.4(3)    yes
O14 4_554 Fe1 . O8 . 91.7(4)    yes
O9 4_554 Fe1 . O14 . 91.1(4)    yes
O11 1_455 Fe1 . O14 . 91.5(4)    yes
O10 4_654 Fe1 . O14 . 88.2(4)    yes
O14 4_554 Fe1 . O14 . 179.46(5)    yes
O8 . Fe1 . O14 . 88.7(4)    yes
O8 1_556 S2 . O6 . 111.3(4)    yes
O8 1_556 S2 . O7 . 107.7(4)    yes
O6 . S2 . O7 . 110.2(8)    yes
O8 1_556 S2 . O9 . 109.3(6)    yes
O6 . S2 . O9 . 110.9(4)    yes
O7 . S2 . O9 . 107.3(4)    yes
O13 4_654 S3 . O10 . 109.8(4)    yes
O13 4_654 S3 . O11 . 109.4(4)    yes
O10 . S3 . O11 . 109.9(5)    yes
O13 4_654 S3 . O12 . 111.6(8)    yes
O10 . S3 . O12 . 108.2(4)    yes
O11 . S3 . O12 . 107.8(4)    yes
O6 1_654 Na4 . O13 1_554 80.5(7)    yes
O6 1_654 Na4 . O16 1_655 96.1(4)    yes
O13 1_554 Na4 . O16 1_655 167.4(5)    yes
O6 1_654 Na4 . O11 . 93.1(5)    yes
O13 1_554 Na4 . O11 . 86.0(4)    yes
O16 1_655 Na4 . O11 . 82.1(5)    yes
O6 1_654 Na4 . O12 . 151.1(5)    yes
O13 1_554 Na4 . O12 . 95.5(3)    yes
O16 1_655 Na4 . O12 . 81.6(6)    yes
O11 . Na4 . O12 . 58.0(4)    yes
O6 1_654 Na4 . O17 . 115.3(7)    yes
O13 1_554 Na4 . O17 . 98.0(6)    yes
O16 1_655 Na4 . O17 . 94.4(7)    yes
O11 . Na4 . O17 . 151.6(8)    yes
O12 . Na4 . O17 . 93.6(6)    yes
O6 1_655 Na5 . O16 1_655 96.1(4)    yes
O6 1_655 Na5 . O10 . 92.9(5)    yes
O16 1_655 Na5 . O10 . 82.7(5)    yes
O6 1_655 Na5 . O12 . 151.0(5)    yes
O16 1_655 Na5 . O12 . 83.4(6)    yes
O10 . Na5 . O12 . 58.2(4)    yes
O6 1_655 Na5 . O13 . 78.6(7)    yes
O16 1_655 Na5 . O13 . 167.2(6)    yes
O10 . Na5 . O13 . 85.9(4)    yes
O12 . Na5 . O13 . 95.5(3)    yes
O6 1_655 Na5 . O15 . 114.5(6)    yes
O16 1_655 Na5 . O15 . 95.2(6)    yes
O10 . Na5 . O15 . 152.6(7)    yes
O12 . Na5 . O15 . 94.4(6)    yes
O13 . Na5 . O15 . 97.6(6)    yes


 
