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

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Xiaoyang Liu'
_publ_contact_author_email       LIUXY@JLU.EDU.CN

_publ_section_title              
;
Helical Chain Observed under Transmission
Electron Microscope: Synthesis and Structure Refinement
of Lutetium Disilicate

;
loop_
_publ_author_name
'Xiaoyang Liu.'
'Shouhua Feng.'
'Michael E. Fleet'
'Zhenmin Jin.'
'Chao Wang.'
;
Ruren Xu
;

# Attachment 'sad.cif'

data_sad
_database_code_depnum_ccdc_archive 'CCDC 293623'
#TrackingRef 'sad.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          'not measured'
_chemical_formula_moiety         'Lu2 O7 Si2'
_chemical_formula_sum            'Lu2 O7 Si2'
_chemical_formula_weight         518.12

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
Lu Lu -0.4720 5.8584 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4(3)2(1)2

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

_cell_length_a                   6.5621(9)
_cell_length_b                   6.5621(9)
_cell_length_c                   11.954(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     514.74(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    759
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      30.01

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    6.686
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             904
_exptl_absorpt_coefficient_mu    38.581
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_T_max  0.483
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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 9.00cm
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_decay_%        none
_diffrn_reflns_number            8760
_diffrn_reflns_av_R_equivalents  0.1128
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.54
_diffrn_reflns_theta_max         30.01
_reflns_number_total             759
_reflns_number_gt                651
_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    SHELXP-97
_computing_publication_material  SHELXTL

_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^)+(0.0427P)^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     SHELXL
_refine_ls_extinction_coef       0.0118(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(5)
_refine_ls_number_reflns         759
_refine_ls_number_parameters     52
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0379
_refine_ls_wR_factor_ref         0.0815
_refine_ls_wR_factor_gt          0.0750
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.061
_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
Lu Lu 0.64807(8) 0.12376(7) 0.13407(4) 0.0100(2) Uani 1 1 d . . .
Si Si 0.6529(5) 0.5980(5) 0.1283(3) 0.0097(6) Uani 1 1 d . . .
O1 O 0.8371(12) 0.4466(12) 0.1777(7) 0.0103(17) Uani 1 1 d . . .
O2 O 0.4728(13) 0.4304(12) 0.1241(8) 0.0125(19) Uani 1 1 d . . .
O3 O 0.6379(13) 0.8030(13) 0.2014(7) 0.0116(17) Uani 1 1 d . . .
O4 O 0.6849(12) 0.6849(12) 0.0000 0.010(2) Uani 1 2 d SU . .

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
Lu 0.0094(3) 0.0108(3) 0.0099(3) -0.00004(19) -0.0003(2) 0.0002(2)
Si 0.0094(16) 0.0098(15) 0.0098(14) 0.0025(13) 0.0007(14) 0.0025(12)
O1 0.006(4) 0.013(4) 0.012(4) 0.001(3) -0.001(3) 0.004(4)
O2 0.013(4) 0.015(5) 0.009(4) 0.004(4) -0.002(3) -0.007(4)
O3 0.015(4) 0.010(4) 0.010(4) 0.002(3) 0.000(4) 0.001(4)
O4 0.013(3) 0.013(3) 0.005(4) 0.001(2) -0.001(2) -0.006(3)

_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
Lu O2 2.163(8) 6 ?
Lu O3 2.210(8) 3_644 ?
Lu O1 2.219(8) 6_455 ?
Lu O3 2.254(8) 1_545 ?
Lu O2 2.321(8) . ?
Lu O1 2.349(8) 8_665 ?
Lu O1 2.510(8) . ?
Lu Si 3.113(3) . ?
Lu Lu 3.4839(6) 3_544 ?
Lu Lu 3.4839(6) 4 ?
Lu Lu 3.4879(11) 8_665 ?
Lu Lu 3.6820(7) 6 ?
Si O3 1.607(9) . ?
Si O2 1.615(9) . ?
Si O4 1.650(5) . ?
Si O1 1.672(9) . ?
O1 Lu 2.219(8) 6 ?
O1 Lu 2.349(8) 8_665 ?
O2 Lu 2.163(8) 6_455 ?
O3 Lu 2.210(8) 4_565 ?
O3 Lu 2.254(8) 1_565 ?
O4 Si 1.650(5) 7 ?

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
O2 Lu O3 79.6(3) 6 3_644 ?
O2 Lu O1 149.0(3) 6 6_455 ?
O3 Lu O1 79.3(3) 3_644 6_455 ?
O2 Lu O3 83.8(3) 6 1_545 ?
O3 Lu O3 113.3(3) 3_644 1_545 ?
O1 Lu O3 84.1(3) 6_455 1_545 ?
O2 Lu O2 128.9(3) 6 . ?
O3 Lu O2 89.1(3) 3_644 . ?
O1 Lu O2 73.0(3) 6_455 . ?
O3 Lu O2 144.4(3) 1_545 . ?
O2 Lu O1 108.8(3) 6 8_665 ?
O3 Lu O1 168.8(3) 3_644 8_665 ?
O1 Lu O1 95.6(2) 6_455 8_665 ?
O3 Lu O1 75.7(3) 1_545 8_665 ?
O2 Lu O1 79.8(3) . 8_665 ?
O2 Lu O1 70.2(3) 6 . ?
O3 Lu O1 95.6(3) 3_644 . ?
O1 Lu O1 134.4(2) 6_455 . ?
O3 Lu O1 136.8(3) 1_545 . ?
O2 Lu O1 61.6(3) . . ?
O1 Lu O1 80.8(3) 8_665 . ?
O2 Lu Si 98.8(2) 6 . ?
O3 Lu Si 86.3(2) 3_644 . ?
O1 Lu Si 102.1(2) 6_455 . ?
O3 Lu Si 160.3(2) 1_545 . ?
O2 Lu Si 30.4(2) . . ?
O1 Lu Si 85.1(2) 8_665 . ?
O1 Lu Si 32.4(2) . . ?
O2 Lu Lu 118.3(2) 6 3_544 ?
O3 Lu Lu 39.2(2) 3_644 3_544 ?
O1 Lu Lu 41.7(2) 6_455 3_544 ?
O3 Lu Lu 109.5(2) 1_545 3_544 ?
O2 Lu Lu 70.3(2) . 3_544 ?
O1 Lu Lu 133.0(2) 8_665 3_544 ?
O1 Lu Lu 113.11(19) . 3_544 ?
Si Lu Lu 86.59(6) . 3_544 ?
O2 Lu Lu 90.0(2) 6 4 ?
O3 Lu Lu 151.2(2) 3_644 4 ?
O1 Lu Lu 97.9(2) 6_455 4 ?
O3 Lu Lu 38.2(2) 1_545 4 ?
O2 Lu Lu 117.7(2) . 4 ?
O1 Lu Lu 38.9(2) 8_665 4 ?
O1 Lu Lu 106.06(19) . 4 ?
Si Lu Lu 122.09(6) . 4 ?
Lu Lu Lu 137.372(15) 3_544 4 ?
O2 Lu Lu 71.5(2) 6 8_665 ?
O3 Lu Lu 134.8(2) 3_644 8_665 ?
O1 Lu Lu 138.5(2) 6_455 8_665 ?
O3 Lu Lu 97.5(2) 1_545 8_665 ?
O2 Lu Lu 83.2(2) . 8_665 ?
O1 Lu Lu 46.0(2) 8_665 8_665 ?
O1 Lu Lu 42.30(19) . 8_665 ?
Si Lu Lu 65.42(6) . 8_665 ?
Lu Lu Lu 151.853(15) 3_544 8_665 ?
Lu Lu Lu 63.758(16) 4 8_665 ?
O2 Lu Lu 36.2(2) 6 6 ?
O3 Lu Lu 78.1(2) 3_644 6 ?
O1 Lu Lu 153.3(2) 6_455 6 ?
O3 Lu Lu 117.9(2) 1_545 6 ?
O2 Lu Lu 92.8(2) . 6 ?
O1 Lu Lu 104.1(2) 8_665 6 ?
O1 Lu Lu 36.10(19) . 6 ?
Si Lu Lu 62.60(6) . 6 ?
Lu Lu Lu 112.65(2) 3_544 6 ?
Lu Lu Lu 108.77(2) 4 6 ?
Lu Lu Lu 58.069(17) 8_665 6 ?
O3 Si O2 122.8(5) . . ?
O3 Si O4 102.9(4) . . ?
O2 Si O4 107.4(5) . . ?
O3 Si O1 110.5(4) . . ?
O2 Si O1 97.8(4) . . ?
O4 Si O1 116.2(4) . . ?
O3 Si Lu 145.5(3) . . ?
O2 Si Lu 46.6(3) . . ?
O4 Si Lu 111.5(3) . . ?
O1 Si Lu 53.5(3) . . ?
Si O1 Lu 132.1(5) . 6 ?
Si O1 Lu 125.1(5) . 8_665 ?
Lu O1 Lu 99.4(3) 6 8_665 ?
Si O1 Lu 94.1(4) . . ?
Lu O1 Lu 102.1(3) 6 . ?
Lu O1 Lu 91.7(3) 8_665 . ?
Si O2 Lu 146.6(5) . 6_455 ?
Si O2 Lu 103.1(4) . . ?
Lu O2 Lu 110.4(3) 6_455 . ?
Si O3 Lu 131.4(5) . 4_565 ?
Si O3 Lu 125.9(4) . 1_565 ?
Lu O3 Lu 102.6(3) 4_565 1_565 ?
Si O4 Si 140.9(8) 7 . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        30.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         3.388
_refine_diff_density_min         -2.452
_refine_diff_density_rms         0.593
#=========================================================END