# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
#TrackingRef 'clo.cif'

#==============================================================================

loop_
_audit_conform_dict_name
_audit_conform_dict_version
_audit_conform_dict_location
cif_core.dic.ftp://ftp.iucr.org/pub/cif_core.dic
cif_pd.dic.ftp://ftp.iucr.org/pub/cif_pd.dic .

# 1. SUBMISSION DETAILS

_publ_contact_author_name        'J. H. Lin'
_publ_contact_author_address     
;
College of Chemistry and Molecular Engineering, Peaking University,
Beijing, 100871, China
;
_publ_contact_author_email       jhlin@pku.edu.cn
_publ_contact_author_fax         '86 10 6275 1708'
_publ_contact_author_phone       '86 10 6275 1715'
_publ_contact_letter             
; ?
;
_publ_requested_coeditor_name    ?
_publ_requested_category         ? # Acta Cryst. C: one of FI/FM/FO/AD
# Acta Cryst. E: one of EI/EM/EO/AD
#==============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
A Silicogermanate with a CLO Type of Zeolite Framework
;
_publ_section_title_footnote     
; ?
;

# 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
'Su, J.'
;
College of Chemistry and Molecular Engineering,Peaking University,
Beijing 100871, China
Inorganic and Structural Chemistry and Berzelii Center EXSELENT on
Porous Materials, Department of Materials and Environmental Chemistry,
Stockholm University, SE-106 91 Stockholm, Sweden
;
'Wang, Y. X.'
;
College of Chemistry and Molecular Engineering,Peaking University,
Beijing 100871, China
;
'Lin, J. H.'
;
College of Chemistry and Molecular Engineering,Peaking University,
Beijing 100871, China
;
'Liang, J.'
;
College of Chemistry and Molecular Engineering,Peaking University,
Beijing 100871, China
;
'Sun, J. L.'
;
Inorganic and Structural Chemistry and Berzelii Center EXSELENT on
Porous Materials, Department of Materials and Environmental Chemistry,
Stockholm University, SE-106 91 Stockholm, Sweden
;
'Zou, X. D.'
;
Inorganic and Structural Chemistry and Berzelii Center EXSELENT on
Porous Materials, Department of Materials and Environmental Chemistry,
Stockholm University, SE-106 91 Stockholm, Sweden
;

data_PKU-12
_database_code_depnum_ccdc_archive 'CCDC 903298'
#TrackingRef 'clo.cif'

loop_
_audit_conform_dict_name
_audit_conform_dict_version
_audit_conform_dict_location
cif_core.dic . ftp://ftp.iucr.org/pub/cif_core.dic
cif_pd.dic . ftp://ftp.iucr.org/pub/cif_pd.dic

# 5. CHEMICAL DATA

_chemical_name_systematic        
; ?
;
_chemical_name_common            'silicogermanate analogue of cloverite'
_chemical_formula_moiety         ?
_chemical_formula_structural     ?
_chemical_formula_analytical     
(Si0.45Ge0.55)192O372(OH)24F24(C9H22N)24(H2O)96
_chemical_formula_sum            'C10 F1 Ge4.39 O19.60 Si3.61'
_chemical_formula_weight         872.78
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_length_neutron # include if applicable
? ? ? ? ? ?

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_space_group_crystal_system      Cubic
_space_group_name_H-M_alt        'P m -3 m'
_space_group_name_Hall           '-P 4 2 3'

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
1 'x, y, z'
2 '-x, -y, -z'
3 '-x, -y, z'
4 '-x, -z, -y'
5 '-x, -z, y'
6 '-x, z, -y'
7 '-x, z, y'
8 '-x, y, -z'
9 '-x, y, z'
10 '-y, -x, -z'
11 '-y, -x, z'
12 '-y, -z, -x'
13 '-y, -z, x'
14 '-y, z, -x'
15 '-y, z, x'
16 '-y, x, -z'
17 '-y, x, z'
18 '-z, -x, -y'
19 '-z, -x, y'
20 '-z, -y, -x'
21 '-z, -y, x'
22 '-z, y, -x'
23 '-z, y, x'
24 '-z, x, -y'
25 '-z, x, y'
26 'z, -x, -y'
27 'z, -x, y'
28 'z, -y, -x'
29 'z, -y, x'
30 'z, y, -x'
31 'z, y, x'
32 'z, x, -y'
33 'z, x, y'
34 'y, -x, -z'
35 'y, -x, z'
36 'y, -z, -x'
37 'y, -z, x'
38 'y, z, -x'
39 'y, z, x'
40 'y, x, -z'
41 'y, x, z'
42 'x, -y, -z'
43 'x, -y, z'
44 'x, -z, -y'
45 'x, -z, y'
46 'x, z, -y'
47 'x, z, y'
48 'x, y, -z'

_cell_length_a                   26.2373(2)
_cell_length_b                   26.2373(2)
_cell_length_c                   26.2373(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18061.7(4)
_cell_formula_units_Z            24
_cell_measurement_temperature    298
_exptl_crystal_density_diffrn    1.926

_cell_special_details            
; ?
;

# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;
_pd_spec_mount_mode              reflection # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   cylinder # options are 'cylinder'
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     cubic
_pd_char_colour                  white # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min. The pressure at which the sample was
# prepared is in kPa. The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ? # include if applicable
_exptl_absorpt_process_details   ? # include if applicable
_exptl_absorpt_correction_T_min  ? # include if applicable
_exptl_absorpt_correction_T_max  ? # include if applicable

#==============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;

_diffrn_ambient_temperature      298
_diffrn_source                   ?
_diffrn_source_target            'Cu Ka1'
_diffrn_source_type              Cu
_diffrn_radiation_type           ?
_diffrn_measurement_device_type  'PANalytical XPert Pro'
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             cont # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     1.540596
_diffrn_radiation_monochromator  'Ge 1 1 1'

# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.

_pd_meas_number_of_points        6778
_pd_meas_2theta_range_min        2
_pd_meas_2theta_range_max        90.9971
_pd_meas_2theta_range_inc        0.0131

# The following three items are used for time-of-flight measurements only.

_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?

#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     'PearsonVII Peak Type'
_pd_proc_ls_background_function  'Chebychev polynomial'
_pd_proc_ls_pref_orient_corr     
; ?
;

_pd_proc_ls_prof_R_factor        0.0467
_pd_proc_ls_prof_wR_factor       0.0619
_pd_proc_ls_prof_wR_expected     0.0321
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         ?
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_matrix_type           ?
_refine_ls_weighting_scheme      
? # options are 'sigma' (based on measured su's)
# or 'calc' (calculated weights)
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     114
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.925

_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        ?
_pd_proc_2theta_range_max        ?
_pd_proc_2theta_range_inc        ?
_pd_proc_wavelength              ?

# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting
# of one data block containing a single powder profile. The value of
# _pd_block_diffractogram_id is used to associate each refinement with
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.

_pd_block_diffractogram_id       ?

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'Topas 3.0'
_computing_molecular_graphics    ?
_computing_publication_material  ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ge1 Ge 48 0.18550(21) 0.73020(23) 0.44077(23) 0.616(20) 0.830(91)
Si1 Si 48 0.18550(21) 0.73020(23) 0.44077(23) 0.384(20) 0.830(91)
Ge2 Ge 48 0.26972(25) 0.64802(23) 0.56142(25) 0.532(19) 0.830(91)
Si2 Si 48 0.26972(25) 0.64802(23) 0.56142(25) 0.468(19) 0.830(91)
Ge3 Ge 48 0.08385(26) 0.70701(23) 0.62326(26) 0.457(19) 0.830(91)
Si3 Si 48 0.08385(26) 0.70701(23) 0.62326(26) 0.543(19) 0.830(91)
Ge4 Ge 24 0 0.64715(31) 0.43811(37) 0.572(23) 0.830(91)
Si4 Si 24 0 0.64715(31) 0.43811(37) 0.428(23) 0.830(91)
Ge5 Ge 24 0 0.68363(32) 0.76894(34) 0.610(21) 0.830(91)
Si5 Si 24 0 0.68363(32) 0.76894(34) 0.390(21) 0.830(91)
O1 O 24 0.1639(11) 0.7318(10) 0.5 1 1.07(25)
O2 O 24 0.22221(84) 0.77779(84) 0.4250(12) 1 1.07(25)
O3 O 48 0.21399(80) 0.67423(80) 0.42569(76) 1 1.07(25)
O4 O 48 0.13555(84) 0.73677(75) 0.40066(82) 1 1.07(25)
O5 O 24 0.31810(82) 0.68190(82) 0.5856(10) 1 1.07(25)
O6 O 24 0.2719(11) 0.59004(76) 0.59004(76) 1 1.07(25)
O7 O 24 0.2776(12) 0.6372(13) 0.5 1 1.07(25)
O8 O 24 0.1040(12) 0.66539(82) 0.66539(82) 1 1.07(25)
O9 O 48 0.05201(82) 0.75438(83) 0.65076(73) 1 1.07(25)
O10 O 48 0.05239(84) 0.68080(78) 0.57573(80) 1 1.07(25)
O11 O 12 0 0.5909(11) 0.4091(11) 1 1.07(25)
O12 O 12 0 0.6328(16) 0.5 1 1.07(25)
O13 O 12 0 0.7416(12) 0.7416(12) 1 1.07(25)
O14 O 24 0 0.6937(10) 0.8343(11) 1 1.07(25)
F1 F 12 0.73075(12) 0.73075(12) 0.5 0.918(36) 12.0(16)
F2 F 12 0.33473(12) 0.33473(12) 0 0.492(35) 12.0(16)
F3 F 8 0.4342(15) 0.4342(15) 0.4342(15) 0.885(75) 12.0(16)
C1 C 24 0.1845(16) 0.9567(15) 0.0433(15) 1 12.7(12)
C2 C 24 0.5657(18) 0.8844(30) 0.5657(18) 1 12.7(12)
C3 C 24 0.2241(22) 0.8662(31) 0.2241(22) 1 12.7(12)
C4 C 48 0.0469(36) 0.8745(29) 0.5555(40) 0.5 12.7(12)
C5 C 24 0.5 0.8715(27) 0.4178(30) 1 12.7(12)
C6 C 24 0.8672(14) 0.3598(24) 0.1328(14) 1 12.7(12)
C7 C 48 0.0831(33) 0.1054(32) 0.5121(47) 0.5 12.7(12)
C8 C 48 0.5400(27) 0.9827(49) 0.8331(25) 0.5 12.7(12)
C9 C 24 0.8492(18) 0.4784(17) 0.4784(17) 1 12.7(12)
C10 C 48 0.6544(26) 0.0360(33) 0.9354(25) 0.5 12.7(12)
O1w O 48 0.7473(22) 0.8227(23) 0.2070(27) 0.588(24) 25.0(27)
O2w O 24 0.5217(23) 0.5217(23) 0.6331(21) 0.705(32) 25.0(27)
O3w O 24 0.2978(20) 0.7453(23) 0.7453(23) 0.762(38) 25.0(27)
O4w O 24 0.5214(64) 0.5 0.2620(36) 0.459(31) 25.0(27)

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
_atom_site_aniso_type_symbol
? ? ? ? ? ? ? ?
_geom_special_details            ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O1 ? ? 1.655(11) ?
Ge1 O1 . . 1.655(11) .
Si1 O2 . . 1.631(10) .
Ge1 O2 . . 1.631(10) .
Si1 O3 . . 1.694(22) .
Ge1 O3 . . 1.694(22) .
Si1 O4 . . 1.690(22) .
Ge1 O4 . . 1.690(22) .
Si2 O3 . 48_556 1.651(22) .
Ge2 O3 . 48_556 1.651(22) .
Si2 O5 . . 1.675(14) .
Ge2 O5 . . 1.675(14) .
Si2 O6 . . 1.697(11) .
Ge2 O6 . . 1.697(11) .
Si2 O7 . . 1.6491(95) .
Ge2 O7 . . 1.6491(95) .
Si3 O4 . 48_556 1.686(23) .
Ge3 O4 . 48_556 1.686(23) .
Si3 O8 . . 1.642(13) .
Ge3 O8 . . 1.642(13) .
Si3 O9 . . 1.662(22) .
Ge3 O9 . . 1.662(22) .
Si3 O10 . . 1.646(22) .
Ge3 O10 . . 1.646(22) .
Si4 O10 . 8_556 1.674(23) .
Ge4 O10 . 8_556 1.674(23) .
Si4 O10 . 48_556 1.674(23) .
Ge4 O10 . 48_556 1.674(23) .
Si4 O11 . . 1.661(12) .
Ge4 O11 . . 1.661(12) .
Si4 O12 . . 1.667(13) .
Ge4 O12 . . 1.667(13) .
Si5 O9 . 7_555 1.659(21) .
Ge5 O9 . 7_555 1.659(21) .
Si5 O9 . 47_555 1.659(21) .
Ge5 O9 . 47_555 1.659(21) .
Si5 O13 . . 1.682(15) .
Ge5 O13 . . 1.682(15) .
Si5 O14 . . 1.735(30) .
Ge5 O14 . . 1.735(30) .
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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Si1 O2 ? ? ? 114.9(15) ?
O1 Ge1 O2 . . . 114.9(15) .
O1 Si1 O3 . . . 113.1(12) .
O1 Ge1 O3 . . . 113.1(12) .
O1 Si1 O4 . . . 108.4(12) .
O1 Ge1 O4 . . . 108.4(12) .
O2 Si1 O3 . . . 110.1(12) .
O2 Ge1 O3 . . . 110.1(12) .
O2 Si1 O4 . . . 102.8(13) .
O2 Ge1 O4 . . . 102.8(13) .
O3 Si1 O4 . . . 106.58(85) .
O3 Ge1 O4 . . . 106.58(85) .
O3 Si2 O5 48_556 . . 111.9(13) .
O3 Ge2 O5 48_556 . . 111.9(13) .
O3 Si2 O6 48_556 . . 108.25(87) .
O3 Ge2 O6 48_556 . . 108.25(87) .
O3 Si2 O7 48_556 . . 112.5(14) .
O3 Ge2 O7 48_556 . . 112.5(14) .
O5 Si2 O6 . . . 106.37(99) .
O5 Ge2 O6 . . . 106.37(99) .
O5 Si2 O7 . . . 111.5(15) .
O5 Ge2 O7 . . . 111.5(15) .
O6 Si2 O7 . . . 105.9(15) .
O6 Ge2 O7 . . . 105.9(15) .
O4 Si3 O8 48_556 . . 107.4(12) .
O4 Ge3 O8 48_556 . . 107.4(12) .
O4 Si3 O9 48_556 . . 102.68(99) .
O4 Ge3 O9 48_556 . . 102.68(99) .
O4 Si3 O10 48_556 . . 108.4(11) .
O4 Ge3 O10 48_556 . . 108.4(11) .
O8 Si3 O9 . . . 111.5(13) .
O8 Ge3 O9 . . . 111.5(13) .
O8 Si3 O10 . . . 113.2(13) .
O8 Ge3 O10 . . . 113.2(13) .
O9 Si3 O10 . . . 112.9(11) .
O9 Ge3 O10 . . . 112.9(11) .
O10 Si4 O10 48_556 . 8_556 110.4(15) .
O10 Ge4 O10 48_556 . 8_556 110.4(15) .
O10 Si4 O11 48_556 . . 111.69(72) .
O10 Ge4 O11 48_556 . . 111.69(72) .
O10 Si4 O12 48_556 . . 109.27(80) .
O10 Ge4 O12 48_556 . . 109.27(80) .
O10 Si4 O11 8_556 . . 111.69(72) .
O10 Ge4 O11 8_556 . . 111.69(72) .
O10 Si4 O12 8_556 . . 109.27(80) .
O10 Ge4 O12 8_556 . . 109.27(80) .
O11 Si4 O12 . . . 104.2(13) .
O11 Ge4 O12 . . . 104.2(13) .
O9 Si5 O9 7_555 . 47_555 110.7(15) .
O9 Ge5 O9 7_555 . 47_555 110.7(15) .
O9 Si5 O13 7_555 . . 111.8(10) .
O9 Ge5 O13 7_555 . . 111.8(10) .
O9 Si5 O14 7_555 . . 107.85(88) .
O9 Ge5 O14 7_555 . . 107.85(88) .
O9 Si5 O13 47_555 . . 111.8(10) .
O9 Ge5 O13 47_555 . . 111.8(10) .
O9 Si5 O14 47_555 . . 107.85(88) .
O9 Ge5 O14 47_555 . . 107.85(88) .
O13 Si5 O14 . . . 106.5(17) .
O13 Ge5 O14 . . . 106.5(17) .
Si1 O1 Si1 . . 48_556 139.8(19) .
Si1 O2 Si1 . . 11_665 147.16(42) .
Si1 O3 Si2 . . 48_556 134.7(10) .
Si1 O4 Si3 . . 48_556 143.9(13) .
Si2 O5 Si2 . . 11_665 131.3(16) .
Si2 O6 Si2 . . 47_555 142.35(43) .
Si2 O7 Si2 . . 48_556 155.48(44) .
Si3 O8 Si3 . . 47_555 142.40(48) .
Si3 O9 Si5 . . 47_555 144.21(37) .
Si3 O10 Si4 . . 48_556 142.81(24) .
Si4 O11 Si4 . . 4_566 144.52(65) .
Si4 O12 Si4 . . 8_556 153.97(57) .
Si5 O13 Si5 . . 7_555 140.48(60) .