# Supplementary Material (ESI) for Chemical Science
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               'Chemical Science'

_journal_coden_Cambridge         1475

loop_
_publ_author_name
'Long, Jeffrey'

_publ_contact_author_name        'Long, Jeffrey'
_publ_contact_author_email       jrlong@berkeley.edu

_publ_section_title              
;
Hydrogen Storage and Carbon Dioxide Capture in an Iron-Based
Sodalite-Type Metal-Organic Framework (Fe-BTT) Discovered via
High-Throughput Methods
;

# Attachment 'FeBTT.cif'

data_shelxl
_database_code_depnum_ccdc_archive 'CCDC 766493'
#TrackingRef 'FeBTT.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            FeBTT
_chemical_melting_point          '>500 K'
_chemical_formula_moiety         'C24 H8 Cl Fe4 N32 O4'
_chemical_formula_sum            'C24 H8 Cl Fe4 N32 O4'
_chemical_formula_weight         1067.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'P m -3 m'
_symmetry_space_group_name_Hall  '-P 4 2 3'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y, x, -z'
'-y, -x, -z'
'y, -x, z'
'-y, x, z'
'x, z, -y'
'-x, z, y'
'-x, -z, -y'
'x, -z, y'
'z, y, -x'
'z, -y, x'
'-z, y, x'
'-z, -y, -x'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y, -x, z'
'y, x, z'
'-y, x, -z'
'y, -x, -z'
'-x, -z, y'
'x, -z, -y'
'x, z, y'
'-x, z, -y'
'-z, -y, x'
'-z, y, -x'
'z, -y, -x'
'z, y, x'

_cell_length_a                   18.8235(11)
_cell_length_b                   18.8235(11)
_cell_length_c                   18.8235(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6669.6(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9008
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      65.41

_exptl_crystal_description       block-shaped
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    0.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1587
_exptl_absorpt_coefficient_mu    5.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_T_max  0.593
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'microfocus rotating anode'
_diffrn_radiation_monochromator  'HELIOS multilayer mirrors'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_reflns_number            22659
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0130
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         65.41
_reflns_number_total             1205
_reflns_number_gt                1116
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2 v. 2009.1'
_computing_cell_refinement       'Bruker APEX2 v. 2009.1'
_computing_data_reduction        'Bruker APEX2 v. 2009.1'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  CIFTAB

_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.
;

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 1043 287 ' '
2 -0.023 0.442 0.455 3350 1071 ' '
_platon_squeeze_details          
;
;

_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^)+(0.0677P)^2^+0.9465P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1207
_refine_ls_number_parameters     47
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0990
_refine_ls_wR_factor_gt          0.0971
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_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 0.85929(3) 0.0000 0.5000 0.0212(2) Uani 1 4 d S . .
Cl2 Cl 1.0000 0.0000 0.5000 0.0226(4) Uani 1 16 d S . .
N2 N 0.86917(8) -0.08129(8) 0.42169(8) 0.0295(4) Uani 1 1 d . . .
O1 O 0.75020(17) 0.0000 0.5000 0.0621(9) Uani 1 4 d S . .
N1 N 0.82542(8) -0.09125(8) 0.36667(8) 0.0366(4) Uani 1 1 d . . .
C1 C 0.85044(15) -0.24031(12) 0.24031(12) 0.0482(8) Uani 1 2 d S . .
H1 H 0.8919 -0.2607 0.2607 0.058 Uiso 1 2 calc SR . .
C3 C 0.85119(11) -0.14881(11) 0.33428(16) 0.0397(7) Uani 1 2 d S . .
C2 C 0.81997(12) -0.18003(12) 0.27058(16) 0.0448(8) 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
Fe1 0.0275(3) 0.0187(3) 0.0175(3) 0.000 0.000 0.000
Cl2 0.0222(5) 0.0222(5) 0.0234(8) 0.000 0.000 0.000
N2 0.0308(8) 0.0302(8) 0.0274(8) -0.0056(7) -0.0076(6) 0.0042(6)
O1 0.0376(17) 0.062(2) 0.087(2) 0.000 0.000 0.000
N1 0.0385(9) 0.0357(9) 0.0354(9) -0.0175(7) -0.0186(7) 0.0138(7)
C1 0.0473(18) 0.0486(12) 0.0486(12) -0.0230(15) -0.0294(12) 0.0294(12)
C3 0.0395(10) 0.0395(10) 0.0402(16) -0.0179(10) -0.0179(10) 0.0154(13)
C2 0.0468(11) 0.0468(11) 0.0408(17) -0.0236(11) -0.0236(11) 0.0227(14)

_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 O1 2.053(3) . ?
Fe1 N2 2.1328(15) . ?
Fe1 N2 2.1329(15) 4_556 ?
Fe1 N2 2.1329(15) 27 ?
Fe1 N2 2.1329(15) 26_556 ?
Fe1 Cl2 2.6487(5) . ?
Cl2 Fe1 2.6487(5) 37_665 ?
Cl2 Fe1 2.6487(5) 13_646 ?
Cl2 Fe1 2.6487(5) 25_756 ?
N2 N2 1.319(3) 38_645 ?
N2 N1 1.336(2) . ?
N1 C3 1.334(2) . ?
C1 C2 1.3932(17) 11_656 ?
C1 C2 1.3933(17) . ?
C3 N1 1.334(2) 38_645 ?
C3 C2 1.459(4) . ?
C2 C1 1.3932(17) 8_645 ?

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
O1 Fe1 N2 95.00(4) . . ?
O1 Fe1 N2 95.00(4) . 4_556 ?
N2 Fe1 N2 169.99(8) . 4_556 ?
O1 Fe1 N2 95.00(4) . 27 ?
N2 Fe1 N2 91.69(8) . 27 ?
N2 Fe1 N2 87.44(8) 4_556 27 ?
O1 Fe1 N2 95.00(4) . 26_556 ?
N2 Fe1 N2 87.44(8) . 26_556 ?
N2 Fe1 N2 91.69(8) 4_556 26_556 ?
N2 Fe1 N2 169.99(8) 27 26_556 ?
O1 Fe1 Cl2 180.0 . . ?
N2 Fe1 Cl2 85.00(4) . . ?
N2 Fe1 Cl2 85.00(4) 4_556 . ?
N2 Fe1 Cl2 85.00(4) 27 . ?
N2 Fe1 Cl2 85.00(4) 26_556 . ?
Fe1 Cl2 Fe1 180.0 37_665 13_646 ?
Fe1 Cl2 Fe1 90.0 37_665 25_756 ?
Fe1 Cl2 Fe1 90.0 13_646 25_756 ?
Fe1 Cl2 Fe1 90.0 37_665 . ?
Fe1 Cl2 Fe1 90.0 13_646 . ?
Fe1 Cl2 Fe1 180.0 25_756 . ?
N2 N2 N1 109.66(9) 38_645 . ?
N2 N2 Fe1 124.68(4) 38_645 . ?
N1 N2 Fe1 125.63(11) . . ?
C3 N1 N2 104.13(15) . . ?
C2 C1 C2 119.8(3) 11_656 . ?
N1 C3 N1 112.4(2) 38_645 . ?
N1 C3 C2 123.79(11) 38_645 . ?
N1 C3 C2 123.79(11) . . ?
C1 C2 C1 120.2(3) 8_645 . ?
C1 C2 C3 119.89(13) 8_645 . ?
C1 C2 C3 119.89(13) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        65.41
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.050