# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2008

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Mir Wais Hosseini'
_publ_contact_author_email       HOSSEINI@CHIMIE.U-STRASBG.FR

_publ_section_title              
;
Molecular tectonics: modulation of size and shape of
cuboid 3-D coordination networks
;
loop_
_publ_author_name
'Mir Wais Hosseini'
'Abdelaziz Jouaiti'
'Nathalie Kyritsakas'
'Mei-Jin Lin.'

# Attachment 'New 1-ZnSiF6.cif'

data_e1267a
_database_code_depnum_ccdc_archive 'CCDC 693608'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C20 H16 F6 N4 Si Zn), 36(H2 O)'
_chemical_formula_sum            'C80 H136 F24 N16 O36 Si4 Zn4'
_chemical_formula_weight         2727.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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           Tetragonal
_symmetry_space_group_name_H-M   I4/mcm
_symmetry_space_group_name_Hall  '-I 4 2c'

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

_cell_length_a                   16.0491(8)
_cell_length_b                   16.0491(8)
_cell_length_c                   15.3683(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3958.5(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    643
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      24.83

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9188
_exptl_absorpt_correction_T_max  0.9582
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6674
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         27.49
_reflns_number_total             1229
_reflns_number_gt                881
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1974P)²+31.3990P] where P=(Fo²+2Fc²)/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         1229
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0886
_refine_ls_wR_factor_ref         0.3060
_refine_ls_wR_factor_gt          0.2779
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_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
Zn1 Zn 0.0000 1.0000 0.2500 0.0101(5) Uani 1 8 d S . .
Si2 Si 0.0000 1.0000 0.0000 0.0151(8) Uani 1 8 d S . .
F1 F 0.0000 1.0000 0.1119(4) 0.0242(14) Uani 1 4 d S A .
F2 F -0.0220(6) 1.1015(4) 0.0000 0.040 Uani 0.684(10) 2 d SP A 1
F3 F 0.0305(14) 1.0971(9) 0.0000 0.040 Uani 0.316(10) 2 d SP A 2
N1 N 0.0939(2) 0.9061(2) 0.2500 0.0195(13) Uani 1 2 d S . .
C1 C 0.0987(5) 0.8499(4) 0.3130(5) 0.0506(19) Uani 1 1 d . . .
H1 H 0.0591 0.8522 0.3589 0.061 Uiso 1 1 calc R . .
C2 C 0.1585(5) 0.7883(5) 0.3147(5) 0.055(2) Uani 1 1 d . . .
H2 H 0.1592 0.7493 0.3611 0.066 Uiso 1 1 calc R . .
C3 C 0.2170(3) 0.7830(3) 0.2500 0.0285(17) Uani 1 2 d S . .
O1 O 0.2485(17) 0.7956(13) 0.5000 0.093(6) Uani 0.50 2 d SP . .
O2 O 0.3498(10) 0.8498(10) 0.0000 0.063(6) Uani 0.50 4 d SP . .
O3 O 0.2895(7) 0.0585(8) 0.0943(9) 0.075(3) Uani 0.50 1 d P . .
O4 O 0.264(2) 0.978(3) 0.0000 0.073(9) Uani 0.25 2 d SP . .
O5 O 0.411(5) 0.0000 0.2500 0.15(3) Uani 0.25 2 d SP . .

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
Zn1 0.0084(6) 0.0084(6) 0.0135(8) 0.000 0.000 0.000
Si2 0.0167(11) 0.0167(11) 0.0119(17) 0.000 0.000 0.000
F1 0.030(2) 0.030(2) 0.013(3) 0.000 0.000 0.000
F2 0.072 0.022 0.025 0.000 0.000 0.024
F3 0.072 0.022 0.025 0.000 0.000 0.024
N1 0.0130(17) 0.0130(17) 0.033(3) 0.0009(16) 0.0009(16) 0.007(2)
C1 0.052(4) 0.048(4) 0.052(4) 0.025(3) 0.023(3) 0.034(3)
C2 0.056(4) 0.052(4) 0.058(4) 0.029(3) 0.027(3) 0.038(4)
C3 0.021(2) 0.021(2) 0.044(5) 0.003(2) 0.003(2) 0.009(3)
O1 0.144(17) 0.091(13) 0.043(9) 0.000 0.000 0.048(12)
O2 0.076(9) 0.076(9) 0.036(11) 0.000 0.000 -0.006(12)
O3 0.067(8) 0.071(8) 0.087(8) 0.012(7) -0.011(6) -0.018(6)
O4 0.05(2) 0.10(2) 0.06(2) 0.000 0.000 -0.004(19)
O5 0.21(7) 0.18(6) 0.05(2) -0.05(3) 0.000 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
Zn1 F1 2.122(6) . ?
Zn1 F1 2.122(6) 5 ?
Zn1 N1 2.132(6) . ?
Zn1 N1 2.132(6) 3_665 ?
Zn1 N1 2.132(6) 4_465 ?
Zn1 N1 2.132(6) 2_575 ?
Si2 F3 1.633(16) 17_575 ?
Si2 F3 1.633(16) . ?
Si2 F3 1.633(16) 19_465 ?
Si2 F3 1.633(16) 3_665 ?
Si2 F2 1.666(7) 19_465 ?
Si2 F2 1.666(7) 17_575 ?
Si2 F2 1.666(7) . ?
Si2 F2 1.666(7) 3_665 ?
Si2 F1 1.720(6) 17_575 ?
Si2 F1 1.720(6) . ?
N1 C1 1.324(7) 8_665 ?
N1 C1 1.324(7) . ?
C1 C2 1.378(8) . ?
C1 H1 0.9500 . ?
C2 C3 1.370(7) . ?
C2 H2 0.9500 . ?
C3 C2 1.370(7) 8_665 ?
C3 C3 1.497(15) 25_565 ?

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
F1 Zn1 F1 179.999(1) . 5 ?
F1 Zn1 N1 90.0 . . ?
F1 Zn1 N1 90.0 5 . ?
F1 Zn1 N1 90.000(1) . 3_665 ?
F1 Zn1 N1 90.001(1) 5 3_665 ?
N1 Zn1 N1 90.0 . 3_665 ?
F1 Zn1 N1 90.000(1) . 4_465 ?
F1 Zn1 N1 89.999(1) 5 4_465 ?
N1 Zn1 N1 90.0 . 4_465 ?
N1 Zn1 N1 180.0 3_665 4_465 ?
F1 Zn1 N1 90.0 . 2_575 ?
F1 Zn1 N1 90.0 5 2_575 ?
N1 Zn1 N1 180.00(15) . 2_575 ?
N1 Zn1 N1 90.000(1) 3_665 2_575 ?
N1 Zn1 N1 90.0 4_465 2_575 ?
F3 Si2 F3 179.997(3) 17_575 . ?
F3 Si2 F3 90.002(2) 17_575 19_465 ?
F3 Si2 F3 90.001(2) . 19_465 ?
F3 Si2 F3 89.997(2) 17_575 3_665 ?
F3 Si2 F3 90.000(2) . 3_665 ?
F3 Si2 F3 179.999(2) 19_465 3_665 ?
F3 Si2 F2 119.7(7) 17_575 19_465 ?
F3 Si2 F2 60.3(7) . 19_465 ?
F3 Si2 F2 150.3(7) 3_665 19_465 ?
F2 Si2 F2 90.002(2) 19_465 17_575 ?
F3 Si2 F2 150.3(7) 17_575 . ?
F3 Si2 F2 119.7(7) 19_465 . ?
F3 Si2 F2 60.3(7) 3_665 . ?
F2 Si2 F2 90.001(1) 19_465 . ?
F2 Si2 F2 179.997(2) 17_575 . ?
F3 Si2 F2 60.3(7) 17_575 3_665 ?
F3 Si2 F2 119.7(7) . 3_665 ?
F3 Si2 F2 150.3(7) 19_465 3_665 ?
F2 Si2 F2 180.0 19_465 3_665 ?
F2 Si2 F2 89.999(1) 17_575 3_665 ?
F2 Si2 F2 89.998(1) . 3_665 ?
F3 Si2 F1 90.0 17_575 17_575 ?
F3 Si2 F1 90.0 . 17_575 ?
F3 Si2 F1 90.001(1) 19_465 17_575 ?
F3 Si2 F1 89.999(1) 3_665 17_575 ?
F2 Si2 F1 90.001(1) 19_465 17_575 ?
F2 Si2 F1 90.0 17_575 17_575 ?
F2 Si2 F1 90.0 . 17_575 ?
F2 Si2 F1 89.999(1) 3_665 17_575 ?
F3 Si2 F1 90.0 17_575 . ?
F3 Si2 F1 90.0 . . ?
F3 Si2 F1 90.000(1) 19_465 . ?
F3 Si2 F1 90.000(1) 3_665 . ?
F2 Si2 F1 90.000(1) 19_465 . ?
F2 Si2 F1 90.0 17_575 . ?
F2 Si2 F1 90.0 . . ?
F2 Si2 F1 90.000(1) 3_665 . ?
F1 Si2 F1 179.999(1) 17_575 . ?
Si2 F1 Zn1 180.0 . . ?
C1 N1 C1 117.1(7) 8_665 . ?
C1 N1 Zn1 121.4(3) 8_665 . ?
C1 N1 Zn1 121.4(3) . . ?
N1 C1 C2 122.8(6) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C3 C2 C1 120.6(6) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C2 C3 C2 116.1(7) . 8_665 ?
C2 C3 C3 122.0(4) . 25_565 ?
C2 C3 C3 122.0(4) 8_665 25_565 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.251

# Attachment 'New 2-ZnSiF6.cif'

data_e1268a
_database_code_depnum_ccdc_archive 'CCDC 693609'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C24 H16 F6 N4 Si Zn, 0.242(C4 H4 Cl12), C2 H2 Cl6'
_chemical_formula_sum            'C26.97 H18.97 Cl8.90 F6 N4 Si Zn'
_chemical_formula_weight         922.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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           Tetragonal
_symmetry_space_group_name_H-M   I4/mcm
_symmetry_space_group_name_Hall  '-I 4 2c'

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

_cell_length_a                   19.5940(3)
_cell_length_b                   19.5940(3)
_cell_length_c                   15.0666(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5784.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2277
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      23.83

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1832.6
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8999
_exptl_absorpt_correction_T_max  0.9398
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            22910
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         27.59
_reflns_number_total             1813
_reflns_number_gt                1421
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.1741P)²+35.8575P] where P=(Fo²+2Fc²)/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         1813
_refine_ls_number_parameters     81
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1601
_refine_ls_R_factor_gt           0.1088
_refine_ls_wR_factor_ref         0.3287
_refine_ls_wR_factor_gt          0.2958
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_restrained_S_all      1.138
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.035

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
Zn1 Zn 1.0000 1.0000 0.7500 0.0292(6) Uani 1 8 d S . .
Si1 Si 1.0000 1.0000 1.0000 0.0360(10) Uani 1 8 d S . .
F1 F 1.0000 1.0000 0.8873(4) 0.051(2) Uani 1 4 d S . .
F2 F 1.0831(3) 0.9816(3) 1.0000 0.0504(15) Uani 1 2 d S . .
N1 N 0.9233(3) 0.9233(3) 0.7500 0.0428(17) Uani 1 2 d S . .
C1 C 0.9212(4) 0.8762(3) 0.6858(4) 0.0446(16) Uani 1 1 d . . .
H1 H 0.9545 0.8776 0.6400 0.054 Uiso 1 1 calc R . .
C2 C 0.8721(4) 0.8255(4) 0.6839(5) 0.0557(19) Uani 1 1 d . . .
H2 H 0.8720 0.7925 0.6377 0.067 Uiso 1 1 calc R . .
C3 C 0.8233(4) 0.8233(4) 0.7500 0.058(3) Uani 1 2 d S . .
C4 C 0.7709(4) 0.7709(4) 0.7500 0.069(3) Uani 1 2 d S . .
C5 C 0.9139(18) 0.2250(13) 0.5000 0.080(8) Uani 0.50 2 d SP . .
H5 H 0.9169 0.1741 0.5000 0.096 Uiso 0.50 2 calc SPR . .
Cl1 Cl 0.9579(5) 0.2509(5) 0.4065(7) 0.133(3) Uani 0.50 1 d P . .
Cl2 Cl 0.8360(7) 0.2414(7) 0.5000 0.142(5) Uani 0.50 2 d SP . .
C6 C 0.868(3) 0.595(6) 0.555(5) 0.210 Uani 0.121(3) 1 d PD . .
H6 H 0.8407 0.5518 0.5579 0.252 Uiso 0.121(3) 1 calc PR . .
Cl3 Cl 0.9491(15) 0.5822(15) 0.512(8) 0.210 Uani 0.121(3) 1 d PD . .
Cl5 Cl 0.8194(18) 0.6626(17) 0.510(12) 0.210 Uani 0.121(3) 1 d PD . .
Cl4 Cl 0.880(4) 0.630(4) 0.660(4) 0.210 Uani 0.121(3) 1 d PD . .

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
Zn1 0.0353(7) 0.0353(7) 0.0171(8) 0.000 0.000 0.000
Si1 0.0469(16) 0.0469(16) 0.0144(18) 0.000 0.000 0.000
F1 0.069(3) 0.069(3) 0.014(3) 0.000 0.000 0.000
F2 0.043(3) 0.075(4) 0.033(3) 0.000 0.000 0.010(3)
N1 0.047(3) 0.047(3) 0.034(4) -0.004(3) 0.004(3) -0.004(3)
C1 0.060(4) 0.040(3) 0.033(3) -0.005(3) 0.011(3) -0.009(3)
C2 0.072(5) 0.050(4) 0.045(4) -0.010(3) 0.002(4) -0.016(4)
C3 0.058(4) 0.058(4) 0.059(6) 0.011(4) -0.011(4) -0.021(5)
C4 0.067(4) 0.067(4) 0.073(8) 0.007(5) -0.007(5) -0.019(5)
C5 0.12(2) 0.038(12) 0.085(19) 0.000 0.000 0.010(13)
Cl1 0.134(7) 0.114(5) 0.152(7) -0.020(5) 0.028(6) -0.002(5)
Cl2 0.162(11) 0.171(11) 0.094(7) 0.000 0.000 0.077(9)
C6 0.133 0.133 0.363 0.000 0.026 0.025
Cl3 0.133 0.133 0.363 0.000 0.026 0.025
Cl5 0.133 0.133 0.363 0.000 0.026 0.025
Cl4 0.133 0.133 0.363 0.000 0.026 0.025

_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
Zn1 F1 2.069(7) . ?
Zn1 F1 2.069(7) 5_756 ?
Zn1 N1 2.124(8) . ?
Zn1 N1 2.124(8) 3_755 ?
Zn1 N1 2.124(8) 2_775 ?
Zn1 N1 2.124(8) 4_575 ?
Si1 F2 1.668(6) 17_777 ?
Si1 F2 1.668(6) 19_577 ?
Si1 F2 1.668(6) . ?
Si1 F2 1.668(6) 3_755 ?
Si1 F1 1.698(7) 17_777 ?
Si1 F1 1.698(7) . ?
N1 C1 1.339(7) . ?
N1 C1 1.339(7) 7_556 ?
C1 C2 1.383(10) . ?
C1 H1 0.9500 . ?
C2 C3 1.382(10) . ?
C2 H2 0.9500 . ?
C3 C2 1.382(10) 7_556 ?
C3 C4 1.452(15) . ?
C4 C4 1.16(2) 25_666 ?
C5 Cl2 1.56(4) . ?
C5 Cl1 1.73(2) . ?
C5 Cl1 1.73(2) 18_556 ?
C5 H5 1.0000 . ?
C6 Cl4 1.74(2) . ?
C6 Cl3 1.74(2) . ?
C6 Cl5 1.76(3) . ?
C6 H6 1.0000 . ?

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
F1 Zn1 F1 179.998(1) . 5_756 ?
N1 Zn1 N1 179.999(1) . 2_775 ?
N1 Zn1 N1 90.000(1) 3_755 2_775 ?
F1 Zn1 N1 90.000(1) . 4_575 ?
F1 Zn1 N1 89.999(1) 5_756 4_575 ?
N1 Zn1 N1 90.001(1) . 4_575 ?
N1 Zn1 N1 179.997(1) 3_755 4_575 ?
N1 Zn1 N1 89.997(1) 2_775 4_575 ?
F2 Si1 F2 90.003(2) 17_777 19_577 ?
F2 Si1 F2 179.999(1) 17_777 . ?
F2 Si1 F2 89.998(1) 19_577 . ?
F2 Si1 F2 89.996(1) 17_777 3_755 ?
F2 Si1 F2 180.00(8) 19_577 3_755 ?
F2 Si1 F2 90.003(2) . 3_755 ?
Si1 F1 Zn1 180.0 . . ?
C1 N1 C1 118.6(8) . 7_556 ?
C1 N1 Zn1 120.7(4) . . ?
C1 N1 Zn1 120.7(4) 7_556 . ?
N1 C1 C2 122.2(7) . . ?
N1 C1 H1 118.9 . . ?
C2 C1 H1 118.9 . . ?
C3 C2 C1 119.3(7) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C2 118.5(10) . 7_556 ?
C2 C3 C4 120.8(5) . . ?
C2 C3 C4 120.7(5) 7_556 . ?
C4 C4 C3 179.964(3) 25_666 . ?
Cl2 C5 Cl1 115.3(11) . . ?
Cl2 C5 Cl1 115.3(11) . 18_556 ?
Cl1 C5 Cl1 109(2) . 18_556 ?
Cl2 C5 H5 105.3 . . ?
Cl1 C5 H5 105.3 . . ?
Cl1 C5 H5 105.3 18_556 . ?
Cl4 C6 Cl3 105(6) . . ?
Cl4 C6 Cl5 98(9) . . ?
Cl3 C6 Cl5 117(3) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.401
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.260

# Attachment 'New 3-ZnSiF6.cif'

data_e1215a
_database_code_depnum_ccdc_archive 'CCDC 693610'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H24 F6 N4 Si Zn'
_chemical_formula_sum            'C32 H24 F6 N4 Si Zn'
_chemical_formula_weight         672.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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           Tetragonal
_symmetry_space_group_name_H-M   I4/mcm
_symmetry_space_group_name_Hall  '-I 4 2 c'

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

_cell_length_a                   22.0593(13)
_cell_length_b                   22.0593(13)
_cell_length_c                   15.0937(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7344.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    730
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      22.17

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    0.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1368
_exptl_absorpt_coefficient_mu    0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9777
_exptl_absorpt_correction_T_max  0.9850
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;

Owing to large disorder of the solvent present in the cavities
of this structure, the SQUEEZE command has been applied

;

_diffrn_ambient_temperature      173(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10236
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0684
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.31
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2262
_reflns_number_gt                1274
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0963P)²+0.0000P] where P=(Fo²+2Fc²)/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         2262
_refine_ls_number_parameters     56
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0704
_refine_ls_wR_factor_ref         0.1927
_refine_ls_wR_factor_gt          0.1860
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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
Zn1 Zn 0.0000 0.0000 0.2500 0.0172(3) Uani 1 8 d S . .
Si1 Si 0.0000 0.0000 0.0000 0.0207(5) Uani 1 8 d S . .
F1 F 0.01785(16) -0.07277(13) 0.0000 0.0469(9) Uani 1 2 d S . .
F2 F 0.0000 0.0000 0.1134(2) 0.0349(9) Uani 1 4 d S . .
N1 N 0.06787(10) 0.06787(10) 0.2500 0.0230(7) Uani 1 2 d S . .
C1 C 0.06911(16) 0.11100(15) 0.1883(2) 0.0295(8) Uani 1 1 d . . .
H1 H 0.0388 0.1103 0.1436 0.035 Uiso 1 1 calc R . .
C2 C 0.11251(17) 0.15727(16) 0.1854(3) 0.0378(9) Uani 1 1 d . . .
H2 H 0.1113 0.1876 0.1408 0.045 Uiso 1 1 calc R . .
C3 C 0.15731(14) 0.15731(14) 0.2500 0.0361(11) Uani 1 2 d S . .
C4 C 0.20514(14) 0.20514(14) 0.2500 0.0460(13) Uani 1 2 d S . .
C5 C 0.1909(2) 0.2632(2) 0.2295(4) 0.090(2) Uani 1 1 d . . .
H5 H 0.1503 0.2735 0.2151 0.108 Uiso 1 1 calc R . .

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
Zn1 0.0162(3) 0.0162(3) 0.0194(4) 0.000 0.000 0.000
Si1 0.0220(7) 0.0220(7) 0.0181(10) 0.000 0.000 0.000
F1 0.078(3) 0.0244(16) 0.0383(16) 0.000 0.000 0.0143(14)
F2 0.0413(13) 0.0413(13) 0.0220(17) 0.000 0.000 0.000
N1 0.0219(10) 0.0219(10) 0.0250(15) -0.0013(14) 0.0013(14) -0.0048(12)
C1 0.0289(18) 0.0223(17) 0.0372(17) 0.0033(15) -0.0042(16) -0.0051(13)
C2 0.038(2) 0.029(2) 0.047(2) 0.0106(18) -0.0002(18) -0.0082(16)
C3 0.0273(14) 0.0273(14) 0.054(3) 0.001(2) -0.001(2) -0.0119(17)
C4 0.0342(17) 0.0342(17) 0.070(4) 0.002(3) -0.002(3) -0.016(2)
C5 0.036(2) 0.052(3) 0.181(7) 0.045(4) -0.027(3) -0.018(2)

_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
Zn1 F2 2.062(3) 5 ?
Zn1 F2 2.062(3) . ?
Zn1 N1 2.117(3) . ?
Zn1 N1 2.117(3) 2 ?
Zn1 N1 2.117(3) 4 ?
Zn1 N1 2.117(3) 3 ?
Si1 F1 1.653(3) . ?
Si1 F1 1.653(3) 19 ?
Si1 F1 1.653(3) 3 ?
Si1 F1 1.653(3) 17 ?
Si1 F2 1.712(3) . ?
Si1 F2 1.712(3) 17 ?
N1 C1 1.332(4) . ?
N1 C1 1.332(4) 7 ?
C1 C2 1.400(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 C2 1.388(4) 7 ?
C3 C4 1.492(6) . ?
C4 C5 1.355(5) 7 ?
C4 C5 1.355(5) . ?
C5 C5 1.432(8) 31 ?
C5 H5 0.9500 . ?

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
F2 Zn1 F2 180.0 5 . ?
F2 Zn1 N1 90.0 5 . ?
F2 Zn1 N1 90.0 . . ?
F2 Zn1 N1 90.0 5 2 ?
F2 Zn1 N1 90.0 . 2 ?
N1 Zn1 N1 180.0 . 2 ?
F2 Zn1 N1 90.0 5 4 ?
F2 Zn1 N1 90.0 . 4 ?
N1 Zn1 N1 90.0 . 4 ?
N1 Zn1 N1 90.0 2 4 ?
F2 Zn1 N1 90.0 5 3 ?
F2 Zn1 N1 90.0 . 3 ?
N1 Zn1 N1 90.0 . 3 ?
N1 Zn1 N1 90.0 2 3 ?
N1 Zn1 N1 180.0 4 3 ?
F1 Si1 F1 90.0 . 19 ?
F1 Si1 F1 90.0 . 3 ?
F1 Si1 F1 180.0 19 3 ?
F1 Si1 F1 180.0 . 17 ?
F1 Si1 F1 90.0 19 17 ?
F1 Si1 F1 90.0 3 17 ?
F1 Si1 F2 90.0 . . ?
F1 Si1 F2 90.0 19 . ?
F1 Si1 F2 90.0 3 . ?
F1 Si1 F2 90.0 17 . ?
F1 Si1 F2 90.0 . 17 ?
F1 Si1 F2 90.0 19 17 ?
F1 Si1 F2 90.0 3 17 ?
F1 Si1 F2 90.0 17 17 ?
F2 Si1 F2 180.0 . 17 ?
Si1 F2 Zn1 180.0 . . ?
C1 N1 C1 117.4(4) . 7 ?
C1 N1 Zn1 121.30(19) . . ?
C1 N1 Zn1 121.31(19) 7 . ?
N1 C1 C2 123.8(3) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C3 C2 C1 117.8(3) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C2 119.5(4) 7 . ?
C2 C3 C4 120.3(2) 7 . ?
C2 C3 C4 120.3(2) . . ?
C5 C4 C5 119.4(5) 7 . ?
C5 C4 C3 120.3(2) 7 . ?
C5 C4 C3 120.3(2) . . ?
C4 C5 C5 120.3(2) . 31 ?
C4 C5 H5 119.8 . . ?
C5 C5 H5 119.8 31 . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.137


