# Electronic Supplementary Material (ESI) for Chemical Science
# This journal is © The Royal Society of Chemistry 2011


data_global

_journal_coden_Cambridge         1475

loop_
_publ_author_name
'Kim, Sun Woo'
'Kim, Sang-Hwan'
'Halasyamani, P.'
'Green, Mark'
'Bhatti, Kanwal'
'Leighton, Chris'
'Das, Hena'
'Fennie, Craig'

_publ_contact_author_name        'Halasyamani, P.'
_publ_contact_author_email       psh@uh.edu

_publ_section_title              
;
RbFe2+Fe3+F6: Synthesis, Structure, and Characterization of
a New Charge-Ordered Magnetically Frustrated
Pyrochlore-Related Mixed-Metal Fluoride
;

data_rbfe2
_database_code_depnum_ccdc_archive 'CCDC 847959'
#TrackingRef '- RBFE2F6_New_cif.txt'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'F6 Fe2 Rb'
_chemical_formula_weight         311.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 '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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   7.0177(6)
_cell_length_b                   7.4499(6)
_cell_length_c                   10.1765(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     532.04(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3204
_cell_measurement_theta_min      3.39
_cell_measurement_theta_max      29.02

_exptl_crystal_description       rod-shape
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    3.885
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_absorpt_coefficient_mu    14.577
_exptl_absorpt_correction_type   Psi-Scan
_exptl_absorpt_correction_T_min  0.3235
_exptl_absorpt_correction_T_max  0.7592
_exptl_absorpt_process_details   'north et al., 1968'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Siemens area detector diffractometer'
_diffrn_measurement_method       omega_scans
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?

_diffrn_reflns_number            3204
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.39
_diffrn_reflns_theta_max         29.02
_reflns_number_total             727
_reflns_number_gt                662
_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 F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         727
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0214
_refine_ls_wR_factor_ref         0.0497
_refine_ls_wR_factor_gt          0.0485
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_restrained_S_all      1.089
_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
Rb1 Rb 0.99196(5) 0.2500 0.37795(4) 0.03192(13) Uani 1 2 d S . .
Fe1 Fe 0.79666(6) 0.2500 0.73150(4) 0.01307(13) Uani 1 2 d S . .
Fe2 Fe 0.5000 0.0000 0.5000 0.01134(13) Uani 1 2 d S . .
F1 F 0.73640(19) 0.06326(18) 0.58122(13) 0.0190(3) Uani 1 1 d . . .
F2 F 0.3737(2) 0.01037(17) 0.66606(14) 0.0217(3) Uani 1 1 d . . .
F3 F 0.4359(3) 0.2500 0.46502(19) 0.0197(4) Uani 1 2 d S . .
F4 F 0.5642(3) 0.2500 0.8384(2) 0.0229(4) Uani 1 2 d S . .

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
Rb1 0.0318(2) 0.0376(3) 0.0263(2) 0.000 0.00459(14) 0.000
Fe1 0.0131(2) 0.0133(2) 0.0129(2) 0.000 -0.00019(16) 0.000
Fe2 0.0142(2) 0.0088(2) 0.0111(2) -0.00100(15) -0.00084(15) 0.00008(15)
F1 0.0191(7) 0.0165(7) 0.0215(7) -0.0040(5) -0.0058(5) -0.0021(5)
F2 0.0288(8) 0.0203(7) 0.0159(7) -0.0018(5) 0.0050(5) 0.0035(6)
F3 0.0235(10) 0.0088(9) 0.0269(11) 0.000 -0.0035(8) 0.000
F4 0.0146(9) 0.0346(12) 0.0196(10) 0.000 0.0010(8) 0.000

_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
Rb1 F4 2.931(2) 6_657 ?
Rb1 F1 3.0419(14) 3_756 ?
Rb1 F1 3.0419(14) 5_756 ?
Rb1 F2 3.0498(15) 2_654 ?
Rb1 F2 3.0498(15) 8_765 ?
Rb1 F1 3.0709(14) . ?
Rb1 F1 3.0709(14) 7_565 ?
Rb1 F3 3.239(2) 1_655 ?
Rb1 F2 3.2477(14) 5_656 ?
Rb1 F2 3.2477(14) 3_656 ?
Fe1 F4 1.961(2) . ?
Fe1 F4 2.0076(19) 6_657 ?
Fe1 F1 2.1102(13) . ?
Fe1 F1 2.1102(13) 7_565 ?
Fe1 F2 2.1368(13) 4_556 ?
Fe1 F2 2.1368(13) 6_657 ?
Fe2 F2 1.9098(14) 5_656 ?
Fe2 F2 1.9098(14) . ?
Fe2 F1 1.9125(13) . ?
Fe2 F1 1.9125(13) 5_656 ?
Fe2 F3 1.9488(6) 5_656 ?
Fe2 F3 1.9488(6) . ?

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
F4 Rb1 F1 75.94(3) 6_657 3_756 ?
F4 Rb1 F1 75.94(3) 6_657 5_756 ?
F1 Rb1 F1 100.21(5) 3_756 5_756 ?
F4 Rb1 F2 130.01(3) 6_657 2_654 ?
F1 Rb1 F2 113.00(4) 3_756 2_654 ?
F1 Rb1 F2 54.19(4) 5_756 2_654 ?
F4 Rb1 F2 130.01(3) 6_657 8_765 ?
F1 Rb1 F2 54.19(4) 3_756 8_765 ?
F1 Rb1 F2 113.00(4) 5_756 8_765 ?
F2 Rb1 F2 78.99(5) 2_654 8_765 ?
F4 Rb1 F1 55.78(4) 6_657 . ?
F1 Rb1 F1 128.43(3) 3_756 . ?
F1 Rb1 F1 85.78(4) 5_756 . ?
F2 Rb1 F1 111.63(3) 2_654 . ?
F2 Rb1 F1 160.90(4) 8_765 . ?
F4 Rb1 F1 55.78(4) 6_657 7_565 ?
F1 Rb1 F1 85.78(4) 3_756 7_565 ?
F1 Rb1 F1 128.43(3) 5_756 7_565 ?
F2 Rb1 F1 160.90(4) 2_654 7_565 ?
F2 Rb1 F1 111.63(3) 8_765 7_565 ?
F1 Rb1 F1 53.87(5) . 7_565 ?
F4 Rb1 F3 64.17(5) 6_657 1_655 ?
F1 Rb1 F3 50.20(3) 3_756 1_655 ?
F1 Rb1 F3 50.20(3) 5_756 1_655 ?
F2 Rb1 F3 84.03(4) 2_654 1_655 ?
F2 Rb1 F3 84.03(4) 8_765 1_655 ?
F1 Rb1 F3 112.18(4) . 1_655 ?
F1 Rb1 F3 112.18(4) 7_565 1_655 ?
F4 Rb1 F2 105.81(4) 6_657 5_656 ?
F1 Rb1 F2 166.46(4) 3_756 5_656 ?
F1 Rb1 F2 93.20(3) 5_756 5_656 ?
F2 Rb1 F2 76.52(3) 2_654 5_656 ?
F2 Rb1 F2 121.78(3) 8_765 5_656 ?
F1 Rb1 F2 50.28(3) . 5_656 ?
F1 Rb1 F2 84.38(4) 7_565 5_656 ?
F3 Rb1 F2 142.91(2) 1_655 5_656 ?
F4 Rb1 F2 105.81(4) 6_657 3_656 ?
F1 Rb1 F2 93.20(3) 3_756 3_656 ?
F1 Rb1 F2 166.46(4) 5_756 3_656 ?
F2 Rb1 F2 121.78(3) 2_654 3_656 ?
F2 Rb1 F2 76.52(3) 8_765 3_656 ?
F1 Rb1 F2 84.38(4) . 3_656 ?
F1 Rb1 F2 50.28(3) 7_565 3_656 ?
F3 Rb1 F2 142.91(2) 1_655 3_656 ?
F2 Rb1 F2 73.35(5) 5_656 3_656 ?
F4 Rb1 F3 176.47(5) 6_657 6_656 ?
F1 Rb1 F3 101.88(3) 3_756 6_656 ?
F1 Rb1 F3 101.88(3) 5_756 6_656 ?
F2 Rb1 F3 48.09(3) 2_654 6_656 ?
F2 Rb1 F3 48.09(3) 8_765 6_656 ?
F1 Rb1 F3 127.15(4) . 6_656 ?
F1 Rb1 F3 127.15(4) 7_565 6_656 ?
F3 Rb1 F3 112.30(5) 1_655 6_656 ?
F2 Rb1 F3 76.97(4) 5_656 6_656 ?
F2 Rb1 F3 76.97(4) 3_656 6_656 ?
F4 Rb1 Fe1 30.81(4) 6_657 . ?
F1 Rb1 Fe1 95.48(3) 3_756 . ?
F1 Rb1 Fe1 95.48(3) 5_756 . ?
F2 Rb1 Fe1 140.42(3) 2_654 . ?
F2 Rb1 Fe1 140.42(3) 8_765 . ?
F1 Rb1 Fe1 33.14(2) . . ?
F1 Rb1 Fe1 33.14(2) 7_565 . ?
F3 Rb1 Fe1 94.98(4) 1_655 . ?
F2 Rb1 Fe1 81.23(3) 5_656 . ?
F2 Rb1 Fe1 81.23(3) 3_656 . ?
F3 Rb1 Fe1 152.72(3) 6_656 . ?
F4 Fe1 F4 167.05(6) . 6_657 ?
F4 Fe1 F1 103.60(6) . . ?
F4 Fe1 F1 86.03(6) 6_657 . ?
F4 Fe1 F1 103.60(6) . 7_565 ?
F4 Fe1 F1 86.03(6) 6_657 7_565 ?
F1 Fe1 F1 82.48(8) . 7_565 ?
F4 Fe1 F2 86.55(5) . 4_556 ?
F4 Fe1 F2 86.34(5) 6_657 4_556 ?
F1 Fe1 F2 162.75(6) . 4_556 ?
F1 Fe1 F2 81.58(5) 7_565 4_556 ?
F4 Fe1 F2 86.55(5) . 6_657 ?
F4 Fe1 F2 86.34(5) 6_657 6_657 ?
F1 Fe1 F2 81.58(5) . 6_657 ?
F1 Fe1 F2 162.75(6) 7_565 6_657 ?
F2 Fe1 F2 113.33(8) 4_556 6_657 ?
F4 Fe1 Rb1 144.54(6) . . ?
F4 Fe1 Rb1 48.41(6) 6_657 . ?
F1 Fe1 Rb1 52.70(4) . . ?
F1 Fe1 Rb1 52.70(4) 7_565 . ?
F2 Fe1 Rb1 111.46(4) 4_556 . ?
F2 Fe1 Rb1 111.46(4) 6_657 . ?
F4 Fe1 Rb1 116.428(8) . 5_766 ?
F4 Fe1 Rb1 64.649(11) 6_657 5_766 ?
F1 Fe1 Rb1 117.88(4) . 5_766 ?
F1 Fe1 Rb1 44.55(4) 7_565 5_766 ?
F2 Fe1 Rb1 44.97(4) 4_556 5_766 ?
F2 Fe1 Rb1 142.03(4) 6_657 5_766 ?
Rb1 Fe1 Rb1 67.850(8) . 5_766 ?
F4 Fe1 Rb1 116.428(8) . 5_756 ?
F4 Fe1 Rb1 64.649(11) 6_657 5_756 ?
F1 Fe1 Rb1 44.55(4) . 5_756 ?
F1 Fe1 Rb1 117.88(4) 7_565 5_756 ?
F2 Fe1 Rb1 142.03(4) 4_556 5_756 ?
F2 Fe1 Rb1 44.97(4) 6_657 5_756 ?
Rb1 Fe1 Rb1 67.850(8) . 5_756 ?
Rb1 Fe1 Rb1 127.054(14) 5_766 5_756 ?
F2 Fe2 F2 180.0 5_656 . ?
F2 Fe2 F1 89.41(6) 5_656 . ?
F2 Fe2 F1 90.59(6) . . ?
F2 Fe2 F1 90.59(6) 5_656 5_656 ?
F2 Fe2 F1 89.41(6) . 5_656 ?
F1 Fe2 F1 180.00(4) . 5_656 ?
F2 Fe2 F3 90.91(7) 5_656 5_656 ?
F2 Fe2 F3 89.09(7) . 5_656 ?
F1 Fe2 F3 87.50(7) . 5_656 ?
F1 Fe2 F3 92.50(7) 5_656 5_656 ?
F2 Fe2 F3 89.09(7) 5_656 . ?
F2 Fe2 F3 90.91(7) . . ?
F1 Fe2 F3 92.50(7) . . ?
F1 Fe2 F3 87.50(7) 5_656 . ?
F3 Fe2 F3 180.0 5_656 . ?
F2 Fe2 Rb1 50.34(4) 5_656 . ?
F2 Fe2 Rb1 129.66(4) . . ?
F1 Fe2 Rb1 44.85(4) . . ?
F1 Fe2 Rb1 135.15(4) 5_656 . ?
F3 Fe2 Rb1 107.10(6) 5_656 . ?
F3 Fe2 Rb1 72.90(6) . . ?
F2 Fe2 Rb1 129.66(4) 5_656 5_656 ?
F2 Fe2 Rb1 50.34(4) . 5_656 ?
F1 Fe2 Rb1 135.15(4) . 5_656 ?
F1 Fe2 Rb1 44.85(4) 5_656 5_656 ?
F3 Fe2 Rb1 72.90(6) 5_656 5_656 ?
F3 Fe2 Rb1 107.10(6) . 5_656 ?
Rb1 Fe2 Rb1 180.0 . 5_656 ?
F2 Fe2 Rb1 81.38(4) 5_656 5_756 ?
F2 Fe2 Rb1 98.62(4) . 5_756 ?
F1 Fe2 Rb1 41.14(4) . 5_756 ?
F1 Fe2 Rb1 138.86(4) 5_656 5_756 ?
F3 Fe2 Rb1 47.77(5) 5_656 5_756 ?
F3 Fe2 Rb1 132.23(6) . 5_756 ?
Rb1 Fe2 Rb1 65.085(7) . 5_756 ?
Rb1 Fe2 Rb1 114.915(7) 5_656 5_756 ?
F2 Fe2 Rb1 98.62(4) 5_656 1_455 ?
F2 Fe2 Rb1 81.38(4) . 1_455 ?
F1 Fe2 Rb1 138.86(4) . 1_455 ?
F1 Fe2 Rb1 41.14(4) 5_656 1_455 ?
F3 Fe2 Rb1 132.23(5) 5_656 1_455 ?
F3 Fe2 Rb1 47.77(6) . 1_455 ?
Rb1 Fe2 Rb1 114.915(7) . 1_455 ?
Rb1 Fe2 Rb1 65.085(7) 5_656 1_455 ?
Rb1 Fe2 Rb1 180.000(10) 5_756 1_455 ?
Fe2 F1 Fe1 130.51(7) . . ?
Fe2 F1 Rb1 114.43(6) . 5_756 ?
Fe1 F1 Rb1 106.33(5) . 5_756 ?
Fe2 F1 Rb1 109.10(6) . . ?
Fe1 F1 Rb1 94.16(5) . . ?
Rb1 F1 Rb1 94.22(4) 5_756 . ?
Fe2 F2 Fe1 125.65(7) . 6_557 ?
Fe2 F2 Rb1 117.16(6) . 2_655 ?
Fe1 F2 Rb1 105.34(5) 6_557 2_655 ?
Fe2 F2 Rb1 102.74(5) . 5_656 ?
Fe1 F2 Rb1 111.49(5) 6_557 5_656 ?
Rb1 F2 Rb1 87.82(3) 2_655 5_656 ?
Fe2 F3 Fe2 145.76(11) 3_656 . ?
Fe2 F3 Rb1 105.78(6) 3_656 1_455 ?
Fe2 F3 Rb1 105.78(6) . 1_455 ?
Fe2 F3 Rb1 98.96(6) 3_656 6_556 ?
Fe2 F3 Rb1 98.96(6) . 6_556 ?
Rb1 F3 Rb1 80.56(4) 1_455 6_556 ?
Fe1 F4 Fe1 125.57(10) . 6_557 ?
Fe1 F4 Rb1 133.65(9) . 6_557 ?
Fe1 F4 Rb1 100.78(7) 6_557 6_557 ?

_diffrn_measured_fraction_theta_max 0.957
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.764
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.257