# Supplementary Material (ESI) for Journal of Materials Chemistry
# This journal is (C) The Royal Society of Chemistry 2007


data_global
_journal_coden_Cambridge         1145
_journal_name_full               'J. Mater. Chem.'

_publ_contact_author_name        'Dr Philip Lightfoot'
_publ_contact_author_address     
;
School of Chemistry
University of St Andrews
St Andrews
Fife
KY16 9ST
UNITED KINGDOM
;

loop_
_publ_author_name
'Philip Lightfoot'
'Adrian A. Finch'
'Anil C. A. Jayasundera'
'P. D. Townsend'

_publ_contact_author_email       PL@ST-ANDREWS.AC.UK

_publ_section_title              
;
Hydrothermal synthesis and luminescent properties of a new family of
organically-templated lanthanide fluorides
;

data_yb
_database_code_depnum_ccdc_archive 'CCDC 648817'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'F7 Yb2, C1 H5 N'
_chemical_formula_sum            'C H5 F7 N Yb2'
_chemical_formula_weight         510.14

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'
H H 0.0000 0.0000 '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'
Yb Yb -0.3850 5.5486 '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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'F d d d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   7.9565(11)
_cell_length_b                   13.906(2)
_cell_length_c                   22.415(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2480.1(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    113
_cell_measurement_reflns_used    1990
_cell_measurement_theta_min      2.9295
_cell_measurement_theta_max      28.3389

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.0300
_exptl_crystal_size_mid          0.0300
_exptl_crystal_size_min          0.0300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    5.465
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3536
_exptl_absorpt_coefficient_mu    30.059
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_max  0.406
_exptl_absorpt_correction_T_min  0.392
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      113
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_detector       CCD
_diffrn_measurement_device       
;
Mercury70 (2x2 bin mode)
;
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measurement_method       dtprofit.ref

_diffrn_reflns_number            4125
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         28.54
_reflns_number_total             706
_reflns_number_gt                584
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_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^)+(0.0286P)^2^+0.0000P] 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         706
_refine_ls_number_parameters     51
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0194
_refine_ls_wR_factor_ref         0.0458
_refine_ls_wR_factor_gt          0.0435
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_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
Yb1 Yb 0.1250 0.44296(2) 0.1250 0.00291(11) Uani 1 2 d S . .
Yb2 Yb 0.1250 0.6250 -0.000282(13) 0.00393(11) Uani 1 2 d S . .
F1 F 0.3750 0.3750 0.12729(17) 0.0065(9) Uani 1 2 d S . .
F2 F 0.2607(4) 0.54193(19) 0.06674(11) 0.0089(6) Uani 1 1 d . . .
F3 F 0.1322(3) 0.3490(2) 0.20562(13) 0.0073(6) Uani 1 1 d . . .
F4 F 0.3038(4) 0.5132(2) 0.19874(12) 0.0084(6) Uani 1 1 d . . .
N1 N 0.1289(15) 0.6387(9) 0.5418(3) 0.0094(19) Uiso 0.50 1 d P . .
H1A H 0.1289 0.6904 0.5184 0.014 Uiso 0.50 1 calc PR . .
H1B H 0.0386 0.6031 0.5340 0.014 Uiso 0.50 1 calc PR . .
H1C H 0.2212 0.6043 0.5350 0.014 Uiso 0.50 1 calc PR . .
C1 C 0.1256(14) 0.6692(9) 0.6049(5) 0.020(3) Uiso 0.50 1 d P . .
H1D H 0.0258 0.7073 0.6125 0.024 Uiso 0.50 1 calc PR . .
H1E H 0.2233 0.7086 0.6136 0.024 Uiso 0.50 1 calc PR . .

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
Yb1 0.00310(17) 0.00391(19) 0.00171(17) 0.000 -0.00024(10) 0.000
Yb2 0.00456(18) 0.00413(19) 0.00311(17) 0.000 0.000 -0.00081(11)
F1 0.007(2) 0.001(2) 0.012(2) 0.000 0.000 0.0020(15)
F2 0.0089(15) 0.0082(15) 0.0094(15) 0.0057(12) 0.0008(10) -0.0016(11)
F3 0.0059(14) 0.0117(17) 0.0045(14) 0.0014(13) -0.0008(10) -0.0014(11)
F4 0.0106(14) 0.0072(15) 0.0072(14) -0.0004(12) 0.0005(11) 0.0006(12)

_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
Yb1 F2 2.183(3) . ?
Yb1 F2 2.183(3) 4 ?
Yb1 F1 2.2028(3) 15_455 ?
Yb1 F1 2.2028(3) . ?
Yb1 F3 2.231(3) 4 ?
Yb1 F3 2.231(3) . ?
Yb1 F4 2.389(3) . ?
Yb1 F4 2.389(3) 4 ?
Yb1 Yb2 3.5588(5) 17_565 ?
Yb1 Yb2 3.5588(5) 27 ?
Yb1 Yb2 3.7808(5) . ?
Yb1 Yb2 3.7808(6) 3_565 ?
Yb2 F2 2.181(3) . ?
Yb2 F2 2.181(3) 2_565 ?
Yb2 F3 2.200(2) 20_565 ?
Yb2 F3 2.200(2) 31 ?
Yb2 F4 2.307(3) 20_565 ?
Yb2 F4 2.307(3) 31 ?
Yb2 F4 2.403(3) 3_565 ?
Yb2 F4 2.403(3) 4 ?
Yb2 F1 2.744(4) 31 ?
Yb2 Yb1 3.5588(5) 17_565 ?
Yb2 Yb1 3.5588(5) 30 ?
F1 Yb1 2.2028(3) 14 ?
F1 Yb2 2.744(4) 27 ?
F3 Yb2 2.200(2) 27 ?
F4 Yb2 2.307(3) 27 ?
F4 Yb2 2.403(3) 3_565 ?
N1 C1 1.477(13) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
C1 C1 1.52(2) 3_566 ?
C1 H1D 0.9700 . ?
C1 H1E 0.9700 . ?

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 Yb1 F2 101.82(15) . 4 ?
F2 Yb1 F1 134.68(11) . 15_455 ?
F2 Yb1 F1 80.67(10) 4 15_455 ?
F2 Yb1 F1 80.67(10) . . ?
F2 Yb1 F1 134.68(11) 4 . ?
F1 Yb1 F1 129.188(17) 15_455 . ?
F2 Yb1 F3 84.12(10) . 4 ?
F2 Yb1 F3 147.27(10) 4 4 ?
F1 Yb1 F3 72.93(11) 15_455 4 ?
F1 Yb1 F3 77.93(10) . 4 ?
F2 Yb1 F3 147.27(10) . . ?
F2 Yb1 F3 84.12(10) 4 . ?
F1 Yb1 F3 77.93(10) 15_455 . ?
F1 Yb1 F3 72.93(11) . . ?
F3 Yb1 F3 108.27(15) 4 . ?
F2 Yb1 F4 82.05(10) . . ?
F2 Yb1 F4 67.84(11) 4 . ?
F1 Yb1 F4 136.81(12) 15_455 . ?
F1 Yb1 F4 67.77(10) . . ?
F3 Yb1 F4 144.60(9) 4 . ?
F3 Yb1 F4 70.36(10) . . ?
F2 Yb1 F4 67.84(11) . 4 ?
F2 Yb1 F4 82.05(10) 4 4 ?
F1 Yb1 F4 67.77(10) 15_455 4 ?
F1 Yb1 F4 136.81(12) . 4 ?
F3 Yb1 F4 70.36(10) 4 4 ?
F3 Yb1 F4 144.60(9) . 4 ?
F4 Yb1 F4 131.74(13) . 4 ?
F2 Yb1 Yb2 88.50(7) . 17_565 ?
F2 Yb1 Yb2 111.16(7) 4 17_565 ?
F1 Yb1 Yb2 50.44(10) 15_455 17_565 ?
F1 Yb1 Yb2 114.15(9) . 17_565 ?
F3 Yb1 Yb2 36.26(6) 4 17_565 ?
F3 Yb1 Yb2 119.68(7) . 17_565 ?
F4 Yb1 Yb2 169.96(7) . 17_565 ?
F4 Yb1 Yb2 39.86(7) 4 17_565 ?
F2 Yb1 Yb2 111.16(7) . 27 ?
F2 Yb1 Yb2 88.50(7) 4 27 ?
F1 Yb1 Yb2 114.15(9) 15_455 27 ?
F1 Yb1 Yb2 50.44(10) . 27 ?
F3 Yb1 Yb2 119.68(7) 4 27 ?
F3 Yb1 Yb2 36.26(6) . 27 ?
F4 Yb1 Yb2 39.86(7) . 27 ?
F4 Yb1 Yb2 169.96(7) 4 27 ?
Yb2 Yb1 Yb2 149.200(11) 17_565 27 ?
F2 Yb1 Yb2 29.94(7) . . ?
F2 Yb1 Yb2 91.27(7) 4 . ?
F1 Yb1 Yb2 105.66(8) 15_455 . ?
F1 Yb1 Yb2 107.73(8) . . ?
F3 Yb1 Yb2 77.92(8) 4 . ?
F3 Yb1 Yb2 173.67(8) . . ?
F4 Yb1 Yb2 103.89(7) . . ?
F4 Yb1 Yb2 38.05(7) 4 . ?
Yb2 Yb1 Yb2 66.067(10) 17_565 . ?
Yb2 Yb1 Yb2 139.577(7) 27 . ?
F2 Yb1 Yb2 91.27(7) . 3_565 ?
F2 Yb1 Yb2 29.94(7) 4 3_565 ?
F1 Yb1 Yb2 107.73(8) 15_455 3_565 ?
F1 Yb1 Yb2 105.66(8) . 3_565 ?
F3 Yb1 Yb2 173.67(8) 4 3_565 ?
F3 Yb1 Yb2 77.92(8) . 3_565 ?
F4 Yb1 Yb2 38.05(7) . 3_565 ?
F4 Yb1 Yb2 103.89(7) 4 3_565 ?
Yb2 Yb1 Yb2 139.577(7) 17_565 3_565 ?
Yb2 Yb1 Yb2 66.067(10) 27 3_565 ?
Yb2 Yb1 Yb2 95.934(16) . 3_565 ?
F2 Yb2 F2 92.92(15) . 2_565 ?
F2 Yb2 F3 146.23(10) . 20_565 ?
F2 Yb2 F3 77.75(11) 2_565 20_565 ?
F2 Yb2 F3 77.75(11) . 31 ?
F2 Yb2 F3 146.23(10) 2_565 31 ?
F3 Yb2 F3 126.60(15) 20_565 31 ?
F2 Yb2 F4 91.23(10) . 20_565 ?
F2 Yb2 F4 131.38(10) 2_565 20_565 ?
F3 Yb2 F4 72.47(11) 20_565 20_565 ?
F3 Yb2 F4 81.71(11) 31 20_565 ?
F2 Yb2 F4 131.38(10) . 31 ?
F2 Yb2 F4 91.23(10) 2_565 31 ?
F3 Yb2 F4 81.71(11) 20_565 31 ?
F3 Yb2 F4 72.47(11) 31 31 ?
F4 Yb2 F4 120.60(13) 20_565 31 ?
F2 Yb2 F4 73.65(10) . 3_565 ?
F2 Yb2 F4 67.61(10) 2_565 3_565 ?
F3 Yb2 F4 129.00(10) 20_565 3_565 ?
F3 Yb2 F4 78.63(10) 31 3_565 ?
F4 Yb2 F4 157.31(14) 20_565 3_565 ?
F4 Yb2 F4 63.50(11) 31 3_565 ?
F2 Yb2 F4 67.61(10) . 4 ?
F2 Yb2 F4 73.65(10) 2_565 4 ?
F3 Yb2 F4 78.63(10) 20_565 4 ?
F3 Yb2 F4 129.00(10) 31 4 ?
F4 Yb2 F4 63.50(11) 20_565 4 ?
F4 Yb2 F4 157.31(14) 31 4 ?
F4 Yb2 F4 122.53(13) 3_565 4 ?
F2 Yb2 F1 133.54(7) . 31 ?
F2 Yb2 F1 133.54(7) 2_565 31 ?
F3 Yb2 F1 63.30(7) 20_565 31 ?
F3 Yb2 F1 63.30(7) 31 31 ?
F4 Yb2 F1 60.30(6) 20_565 31 ?
F4 Yb2 F1 60.30(6) 31 31 ?
F4 Yb2 F1 118.74(7) 3_565 31 ?
F4 Yb2 F1 118.74(7) 4 31 ?
F2 Yb2 Yb1 132.62(7) . 17_565 ?
F2 Yb2 Yb1 113.90(7) 2_565 17_565 ?
F3 Yb2 Yb1 36.87(8) 20_565 17_565 ?
F3 Yb2 Yb1 95.40(7) 31 17_565 ?
F4 Yb2 Yb1 41.61(7) 20_565 17_565 ?
F4 Yb2 Yb1 88.24(7) 31 17_565 ?
F4 Yb2 Yb1 151.68(7) 3_565 17_565 ?
F4 Yb2 Yb1 82.82(7) 4 17_565 ?
F1 Yb2 Yb1 38.229(7) 31 17_565 ?
F2 Yb2 Yb1 113.90(7) . 30 ?
F2 Yb2 Yb1 132.62(7) 2_565 30 ?
F3 Yb2 Yb1 95.40(7) 20_565 30 ?
F3 Yb2 Yb1 36.87(8) 31 30 ?
F4 Yb2 Yb1 88.24(7) 20_565 30 ?
F4 Yb2 Yb1 41.61(7) 31 30 ?
F4 Yb2 Yb1 82.82(7) 3_565 30 ?
F4 Yb2 Yb1 151.68(7) 4 30 ?
F1 Yb2 Yb1 38.229(7) 31 30 ?
Yb1 Yb2 Yb1 76.458(13) 17_565 30 ?
F2 Yb2 Yb1 29.97(7) . . ?
F2 Yb2 Yb1 80.97(7) 2_565 . ?
F3 Yb2 Yb1 116.36(7) 20_565 . ?
F3 Yb2 Yb1 102.92(8) 31 . ?
F4 Yb2 Yb1 79.05(7) 20_565 . ?
F4 Yb2 Yb1 157.80(7) 31 . ?
F4 Yb2 Yb1 94.36(7) 3_565 . ?
F4 Yb2 Yb1 37.79(7) 4 . ?
F1 Yb2 Yb1 137.967(8) 31 . ?
Yb1 Yb2 Yb1 113.933(10) 17_565 . ?
Yb1 Yb2 Yb1 139.577(7) 30 . ?
Yb1 F1 Yb1 177.3(2) 14 . ?
Yb1 F1 Yb2 91.33(10) 14 27 ?
Yb1 F1 Yb2 91.33(10) . 27 ?
Yb2 F2 Yb1 120.09(13) . . ?
Yb2 F3 Yb1 106.87(11) 27 . ?
Yb2 F4 Yb1 98.53(10) 27 . ?
Yb2 F4 Yb2 116.50(11) 27 3_565 ?
Yb1 F4 Yb2 104.16(11) . 3_565 ?
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
N1 C1 C1 109.5(12) . 3_566 ?
N1 C1 H1D 109.8 . . ?
C1 C1 H1D 109.8 3_566 . ?
N1 C1 H1E 109.8 . . ?
C1 C1 H1E 109.8 3_566 . ?
H1D C1 H1E 108.2 . . ?

_diffrn_measured_fraction_theta_max 0.887
_diffrn_reflns_theta_full        28.54
_diffrn_measured_fraction_theta_full 0.887
_refine_diff_density_max         1.411
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.327