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

data_global

_journal_coden_Cambridge         182
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Hevia, Eva'
'Clegg, W'
'Klett, Jan'
'Garcia-Alvarez, Pablo'
'Russo, Luca'
'Baillie, Sharon'

_publ_contact_author_name        'Hevia, Eva'
_publ_contact_author_email       eva.hevia@strath.ac.uk

_publ_section_title              
;
Synthesis and Characterization
of an Infinite Sheet of Metal-Alkyl Bonds:
Unfolding the Elusive Structure
of an Unsolvated Alkali-Metal Trisalkylmagnesiate
;

# Attachment '- cif.cif'

data_rem550_compound1
_database_code_depnum_ccdc_archive 'CCDC 783163'
#TrackingRef '- cif.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H33 Mg Na Si3'
_chemical_formula_sum            'C12 H33 Mg Na Si3'
_chemical_formula_weight         308.95

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.0486 0.0363 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'

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

_cell_length_a                   16.8522(4)
_cell_length_b                   12.7158(4)
_cell_length_c                   19.3676(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4150.3(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    4553
_cell_measurement_theta_min      2.8942
_cell_measurement_theta_max      28.6307

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1360
_exptl_absorpt_coefficient_mu    0.264
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_monochromator  none
_diffrn_measurement_device_type  
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 10.3968
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18574
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.1065
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.90
_diffrn_reflns_theta_max         28.69
_reflns_number_total             4610
_reflns_number_gt                2442
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan 5 2010,16:28:46)
;
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'

_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^)+(0.0304P)^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         4610
_refine_ls_number_parameters     163
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0919
_refine_ls_R_factor_gt           0.0361
_refine_ls_wR_factor_ref         0.0707
_refine_ls_wR_factor_gt          0.0642
_refine_ls_goodness_of_fit_ref   0.780
_refine_ls_restrained_S_all      0.780
_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
Mg Mg 0.13901(4) 0.77480(5) 0.22276(3) 0.02557(16) Uani 1 1 d . . .
Na Na -0.11276(4) 0.62437(6) 0.21705(5) 0.0431(2) Uani 1 1 d . . .
C1 C 0.11977(11) 0.94154(14) 0.21229(10) 0.0279(5) Uani 1 1 d . . .
H1A H 0.0750 0.9616 0.2426 0.033 Uiso 1 1 calc R . .
H1B H 0.1676 0.9785 0.2295 0.033 Uiso 1 1 calc R . .
C2 C 0.17567(14) 0.93953(19) 0.06427(12) 0.0513(6) Uani 1 1 d . . .
H2A H 0.2282 0.9629 0.0797 0.077 Uiso 1 1 calc R . .
H2B H 0.1653 0.9671 0.0179 0.077 Uiso 1 1 calc R . .
H2C H 0.1741 0.8625 0.0632 0.077 Uiso 1 1 calc R . .
C3 C -0.00129(13) 0.93908(19) 0.09862(12) 0.0523(7) Uani 1 1 d . . .
H3A H 0.0016 0.8630 0.0911 0.078 Uiso 1 1 calc R . .
H3B H -0.0177 0.9738 0.0558 0.078 Uiso 1 1 calc R . .
H3C H -0.0400 0.9542 0.1351 0.078 Uiso 1 1 calc R . .
C4 C 0.09744(13) 1.13634(16) 0.11403(12) 0.0452(6) Uani 1 1 d . . .
H4A H 0.0550 1.1666 0.1423 0.068 Uiso 1 1 calc R . .
H4B H 0.0881 1.1535 0.0654 0.068 Uiso 1 1 calc R . .
H4C H 0.1486 1.1654 0.1286 0.068 Uiso 1 1 calc R . .
C5 C 0.04088(10) 0.67019(15) 0.20156(10) 0.0279(5) Uani 1 1 d . . .
H5A H 0.0211 0.6407 0.2456 0.034 Uiso 1 1 calc R . .
H5B H -0.0029 0.7109 0.1804 0.034 Uiso 1 1 calc R . .
C6 C 0.13054(13) 0.61430(18) 0.07185(12) 0.0466(6) Uani 1 1 d . . .
H6A H 0.1015 0.6699 0.0476 0.070 Uiso 1 1 calc R . .
H6B H 0.1430 0.5574 0.0395 0.070 Uiso 1 1 calc R . .
H6C H 0.1799 0.6431 0.0907 0.070 Uiso 1 1 calc R . .
C7 C 0.12488(12) 0.46073(16) 0.19349(11) 0.0434(6) Uani 1 1 d . . .
H7A H 0.1720 0.4933 0.2141 0.065 Uiso 1 1 calc R . .
H7B H 0.1413 0.4040 0.1624 0.065 Uiso 1 1 calc R . .
H7C H 0.0911 0.4319 0.2301 0.065 Uiso 1 1 calc R . .
C8 C -0.01460(12) 0.48833(18) 0.09954(10) 0.0388(5) Uani 1 1 d . . .
H8A H -0.0505 0.4589 0.1344 0.058 Uiso 1 1 calc R . .
H8B H 0.0077 0.4313 0.0716 0.058 Uiso 1 1 calc R . .
H8C H -0.0441 0.5366 0.0696 0.058 Uiso 1 1 calc R . .
C9 C 0.24875(10) 0.72211(14) 0.26969(10) 0.0261(4) Uani 1 1 d . . .
H9A H 0.2555 0.6454 0.2631 0.031 Uiso 1 1 calc R . .
H9B H 0.2947 0.7587 0.2487 0.031 Uiso 1 1 calc R . .
C10 C 0.14166(12) 0.71004(17) 0.39321(11) 0.0384(5) Uani 1 1 d . . .
H10A H 0.1001 0.7484 0.3683 0.058 Uiso 1 1 calc R . .
H10B H 0.1372 0.7244 0.4428 0.058 Uiso 1 1 calc R . .
H10C H 0.1355 0.6344 0.3850 0.058 Uiso 1 1 calc R . .
C11 C 0.25119(12) 0.89878(14) 0.37472(11) 0.0358(5) Uani 1 1 d . . .
H11A H 0.3038 0.9217 0.3594 0.054 Uiso 1 1 calc R . .
H11B H 0.2446 0.9154 0.4238 0.054 Uiso 1 1 calc R . .
H11C H 0.2104 0.9353 0.3478 0.054 Uiso 1 1 calc R . .
C12 C 0.31658(12) 0.69282(16) 0.42095(11) 0.0402(6) Uani 1 1 d . . .
H12A H 0.3138 0.6161 0.4172 0.060 Uiso 1 1 calc R . .
H12B H 0.3054 0.7139 0.4686 0.060 Uiso 1 1 calc R . .
H12C H 0.3698 0.7167 0.4079 0.060 Uiso 1 1 calc R . .
Si1 Si 0.09850(3) 0.98928(5) 0.12519(3) 0.03136(15) Uani 1 1 d . . .
Si2 Si 0.06816(3) 0.56182(4) 0.14372(3) 0.02742(14) Uani 1 1 d . . .
Si3 Si 0.24132(3) 0.75380(4) 0.36167(3) 0.02564(13) Uani 1 1 d . . .

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
Mg 0.0228(3) 0.0254(3) 0.0284(4) -0.0032(3) -0.0015(3) -0.0001(3)
Na 0.0222(4) 0.0369(5) 0.0703(6) 0.0169(5) 0.0040(4) 0.0021(4)
C1 0.0226(10) 0.0265(11) 0.0345(12) -0.0079(10) -0.0018(9) -0.0011(9)
C2 0.0566(15) 0.0533(15) 0.0440(15) -0.0083(12) 0.0097(12) -0.0107(13)
C3 0.0444(14) 0.0624(17) 0.0501(17) 0.0181(14) -0.0170(12) -0.0126(13)
C4 0.0510(14) 0.0437(14) 0.0408(14) 0.0122(11) -0.0035(12) 0.0000(12)
C5 0.0203(10) 0.0302(11) 0.0332(12) 0.0040(9) -0.0017(9) -0.0030(9)
C6 0.0406(13) 0.0482(14) 0.0509(16) 0.0020(12) 0.0110(12) -0.0050(12)
C7 0.0436(13) 0.0335(13) 0.0530(16) 0.0023(11) -0.0099(11) 0.0048(11)
C8 0.0354(12) 0.0459(14) 0.0350(13) -0.0094(11) 0.0008(10) -0.0056(11)
C9 0.0190(10) 0.0220(10) 0.0374(12) -0.0025(9) 0.0022(9) 0.0011(9)
C10 0.0327(11) 0.0458(13) 0.0368(13) -0.0020(11) 0.0042(11) -0.0021(10)
C11 0.0416(12) 0.0283(11) 0.0376(14) -0.0052(9) -0.0020(11) 0.0026(10)
C12 0.0359(12) 0.0425(14) 0.0421(14) -0.0002(11) -0.0067(11) 0.0030(11)
Si1 0.0285(3) 0.0339(3) 0.0316(3) 0.0018(3) -0.0028(3) -0.0052(3)
Si2 0.0233(3) 0.0278(3) 0.0311(3) 0.0020(3) -0.0011(3) -0.0014(2)
Si3 0.0220(3) 0.0241(3) 0.0308(3) -0.0019(3) -0.0014(3) 0.0007(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
Mg C1 2.154(2) . ?
Mg C5 2.1617(19) . ?
Mg C9 2.1668(18) . ?
Na C1 2.700(2) 3_545 ?
Na C5 2.6708(19) . ?
Na C9 2.6566(19) 6_556 ?
Na C12 3.053(2) 6_556 ?
C1 Na 2.700(2) 3 ?
C1 H1A 0.990 . ?
C1 H1B 0.990 . ?
C1 Si1 1.828(2) . ?
C2 H2A 0.980 . ?
C2 H2B 0.980 . ?
C2 H2C 0.980 . ?
C2 Si1 1.866(2) . ?
C3 H3A 0.980 . ?
C3 H3B 0.980 . ?
C3 H3C 0.980 . ?
C3 Si1 1.871(2) . ?
C4 H4A 0.980 . ?
C4 H4B 0.980 . ?
C4 H4C 0.980 . ?
C4 Si1 1.882(2) . ?
C5 H5A 0.990 . ?
C5 H5B 0.990 . ?
C5 Si2 1.834(2) . ?
C6 H6A 0.980 . ?
C6 H6B 0.980 . ?
C6 H6C 0.980 . ?
C6 Si2 1.868(2) . ?
C7 H7A 0.980 . ?
C7 H7B 0.980 . ?
C7 H7C 0.980 . ?
C7 Si2 1.870(2) . ?
C8 H8A 0.980 . ?
C8 H8B 0.980 . ?
C8 H8C 0.980 . ?
C8 Si2 1.8842(19) . ?
C9 Na 2.6567(19) 6_656 ?
C9 H9A 0.990 . ?
C9 H9B 0.990 . ?
C9 Si3 1.8307(19) . ?
C10 H10A 0.980 . ?
C10 H10B 0.980 . ?
C10 H10C 0.980 . ?
C10 Si3 1.872(2) . ?
C11 H11A 0.980 . ?
C11 H11B 0.980 . ?
C11 H11C 0.980 . ?
C11 Si3 1.8682(19) . ?
C12 H12A 0.980 . ?
C12 H12B 0.980 . ?
C12 H12C 0.980 . ?
C12 Si3 1.878(2) . ?

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
C1 Mg C5 118.20(7) . . ?
C1 Mg C9 118.18(7) . . ?
C5 Mg C9 122.84(8) . . ?
C1 Na C5 106.69(6) 3_545 . ?
C1 Na C9 108.38(6) 3_545 6_556 ?
C1 Na C12 132.23(7) 3_545 6_556 ?
C5 Na C9 139.51(7) . 6_556 ?
C5 Na C12 102.57(6) . 6_556 ?
C9 Na C12 66.95(6) 6_556 6_556 ?
Mg C1 Na 143.73(9) . 3 ?
Mg C1 H1A 108.2 . . ?
Mg C1 H1B 108.2 . . ?
Mg C1 Si1 116.30(10) . . ?
Na C1 H1A 56.2 3 . ?
Na C1 H1B 57.1 3 . ?
Na C1 Si1 99.97(8) 3 . ?
H1A C1 H1B 107.4 . . ?
H1A C1 Si1 108.2 . . ?
H1B C1 Si1 108.2 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2A C2 Si1 109.5 . . ?
H2B C2 H2C 109.5 . . ?
H2B C2 Si1 109.5 . . ?
H2C C2 Si1 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3A C3 Si1 109.5 . . ?
H3B C3 H3C 109.5 . . ?
H3B C3 Si1 109.5 . . ?
H3C C3 Si1 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4A C4 Si1 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H4B C4 Si1 109.5 . . ?
H4C C4 Si1 109.5 . . ?
Mg C5 Na 148.71(9) . . ?
Mg C5 H5A 109.0 . . ?
Mg C5 H5B 109.0 . . ?
Mg C5 Si2 112.74(9) . . ?
Na C5 H5A 59.7 . . ?
Na C5 H5B 55.9 . . ?
Na C5 Si2 98.49(8) . . ?
H5A C5 H5B 107.8 . . ?
H5A C5 Si2 109.0 . . ?
H5B C5 Si2 109.0 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6A C6 Si2 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H6B C6 Si2 109.5 . . ?
H6C C6 Si2 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7A C7 Si2 109.5 . . ?
H7B C7 H7C 109.5 . . ?
H7B C7 Si2 109.5 . . ?
H7C C7 Si2 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8A C8 Si2 109.5 . . ?
H8B C8 H8C 109.5 . . ?
H8B C8 Si2 109.5 . . ?
H8C C8 Si2 109.5 . . ?
Mg C9 Na 159.23(9) . 6_656 ?
Mg C9 H9A 110.5 . . ?
Mg C9 H9B 110.5 . . ?
Mg C9 Si3 106.37(8) . . ?
Na C9 H9A 56.6 6_656 . ?
Na C9 H9B 64.7 6_656 . ?
Na C9 Si3 93.95(7) 6_656 . ?
H9A C9 H9B 108.6 . . ?
H9A C9 Si3 110.5 . . ?
H9B C9 Si3 110.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10A C10 Si3 109.5 . . ?
H10B C10 H10C 109.5 . . ?
H10B C10 Si3 109.5 . . ?
H10C C10 Si3 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11A C11 Si3 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H11B C11 Si3 109.5 . . ?
H11C C11 Si3 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12A C12 Si3 109.5 . . ?
H12B C12 H12C 109.5 . . ?
H12B C12 Si3 109.5 . . ?
H12C C12 Si3 109.5 . . ?
C1 Si1 C2 109.52(10) . . ?
C1 Si1 C3 108.47(9) . . ?
C1 Si1 C4 115.95(9) . . ?
C2 Si1 C3 109.68(11) . . ?
C2 Si1 C4 105.71(11) . . ?
C3 Si1 C4 107.39(11) . . ?
C5 Si2 C6 109.14(10) . . ?
C5 Si2 C7 109.25(10) . . ?
C5 Si2 C8 117.67(9) . . ?
C6 Si2 C7 110.01(10) . . ?
C6 Si2 C8 104.80(10) . . ?
C7 Si2 C8 105.76(10) . . ?
C9 Si3 C10 108.26(9) . . ?
C9 Si3 C11 110.05(9) . . ?
C9 Si3 C12 117.24(9) . . ?
C10 Si3 C11 109.21(9) . . ?
C10 Si3 C12 106.48(10) . . ?
C11 Si3 C12 105.34(10) . . ?

_diffrn_measured_fraction_theta_max 0.859
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.279
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.047

#===END

data_jksha11_compound3
_database_code_depnum_ccdc_archive 'CCDC 783164'
#TrackingRef '- cif.cif'

_audit_creation_method           shelxl-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C4 H11 Na Si'
_chemical_formula_sum            'C4 H11 Na Si'
_chemical_formula_weight         110.21

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'
na na 0.0362 0.0249 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'C 2/c'

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

_cell_length_a                   21.481(2)
_cell_length_b                   12.4281(7)
_cell_length_c                   12.7071(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 123.555(14)
_cell_angle_gamma                90.00
_cell_volume                     2827.1(4)
_cell_formula_units_z            16
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    2673
_cell_measurement_theta_min      3.17
_cell_measurement_theta_max      28.91

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_f_000             960
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_t_min  0.897
_exptl_absorpt_correction_t_max  1.000
_exptl_absorpt_process_details   CrysAlisPro

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7086
_diffrn_reflns_av_r_equivalents  0.0285
_diffrn_reflns_av_sigmai/neti    0.0613
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.18
_diffrn_reflns_theta_max         28.97
_reflns_number_total             3258
_reflns_number_gt                2273
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       CrysAlisPro
_computing_cell_refinement       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_structure_solution    SHELXS97
_computing_structure_refinement  SHELXL97
_computing_molecular_graphics    ?
_computing_publication_material  SHELXL97

_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^)+(0.0334P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3258
_refine_ls_number_parameters     131
_refine_ls_number_restraints     0
_refine_ls_r_factor_all          0.0540
_refine_ls_r_factor_gt           0.0332
_refine_ls_wr_factor_ref         0.0728
_refine_ls_wr_factor_gt          0.0704
_refine_ls_goodness_of_fit_ref   0.928
_refine_ls_restrained_s_all      0.928
_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
si2 si 0.00653(3) 0.78245(4) 0.46717(4) 0.01635(12) uani 1 1 d . . .
si1 si -0.20710(3) 0.54468(4) 0.50701(5) 0.02347(13) uani 1 1 d . . .
na2 na -0.01084(4) 0.57886(5) 0.62156(5) 0.02054(16) uani 1 1 d . . .
na1 na -0.08123(3) 0.37317(5) 0.68018(5) 0.01982(16) uani 1 1 d . . .
c2 c 0.00722(11) 0.64103(14) 0.42923(15) 0.0172(4) uani 1 1 d . . .
c1 c -0.11874(10) 0.57171(15) 0.65697(16) 0.0195(4) uani 1 1 d . . .
c23 c -0.01011(10) 0.81543(14) 0.59451(15) 0.0245(4) uani 1 1 d . . .
h23a h -0.0577 0.7840 0.5727 0.037 uiso 1 1 calc r . .
h23b h -0.0119 0.8937 0.6018 0.037 uiso 1 1 calc r . .
h23c h 0.0306 0.7858 0.6752 0.037 uiso 1 1 calc r . .
c22 c -0.07080(10) 0.85297(16) 0.32293(16) 0.0326(5) uani 1 1 d . . .
h22a h -0.0595 0.8545 0.2581 0.049 uiso 1 1 calc r . .
h22b h -0.0754 0.9268 0.3449 0.049 uiso 1 1 calc r . .
h22c h -0.1179 0.8145 0.2905 0.049 uiso 1 1 calc r . .
c21 c 0.09838(10) 0.84639(15) 0.52176(16) 0.0293(4) uani 1 1 d . . .
h21a h 0.1089 0.8384 0.4563 0.044 uiso 1 1 calc r . .
h21b h 0.1379 0.8113 0.5996 0.044 uiso 1 1 calc r . .
h21c h 0.0965 0.9230 0.5380 0.044 uiso 1 1 calc r . .
c13 c -0.29431(10) 0.60217(16) 0.4844(2) 0.0405(5) uani 1 1 d . . .
h13a h -0.2917 0.6809 0.4853 0.061 uiso 1 1 calc r . .
h13b h -0.2991 0.5777 0.5529 0.061 uiso 1 1 calc r . .
h13c h -0.3377 0.5780 0.4033 0.061 uiso 1 1 calc r . .
c12 c -0.22584(10) 0.39472(16) 0.48577(19) 0.0407(5) uani 1 1 d . . .
h12a h -0.2214 0.3650 0.5611 0.061 uiso 1 1 calc r . .
h12b h -0.1894 0.3598 0.4734 0.061 uiso 1 1 calc r . .
h12c h -0.2764 0.3818 0.4118 0.061 uiso 1 1 calc r . .
c11 c -0.20305(11) 0.59132(18) 0.37010(17) 0.0414(5) uani 1 1 d . . .
h11a h -0.2510 0.5768 0.2909 0.062 uiso 1 1 calc r . .
h11b h -0.1632 0.5527 0.3703 0.062 uiso 1 1 calc r . .
h11c h -0.1928 0.6688 0.3778 0.062 uiso 1 1 calc r . .
h2b h 0.0486(10) 0.6043(14) 0.4952(15) 0.025(5) uiso 1 1 d . . .
h1b h -0.1272(10) 0.5575(15) 0.7214(16) 0.035(5) uiso 1 1 d . . .
h2a h -0.0359(10) 0.6063(15) 0.4052(15) 0.029(5) uiso 1 1 d . . .
h1a h -0.1134(11) 0.6428(18) 0.6625(18) 0.046(6) uiso 1 1 d . . .

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
si2 0.0205(3) 0.0153(2) 0.0145(2) -0.00019(19) 0.01049(19) 0.0008(2)
si1 0.0147(3) 0.0200(3) 0.0292(3) -0.0013(2) 0.0080(2) 0.0012(2)
na2 0.0250(4) 0.0220(4) 0.0182(3) 0.0008(3) 0.0142(3) 0.0001(3)
na1 0.0186(4) 0.0197(4) 0.0198(3) 0.0001(3) 0.0098(3) 0.0001(3)
c2 0.0181(10) 0.0174(9) 0.0161(8) -0.0018(7) 0.0094(8) -0.0009(8)
c1 0.0217(9) 0.0172(9) 0.0222(9) -0.0004(8) 0.0137(8) -0.0015(8)
c23 0.0337(11) 0.0205(9) 0.0254(9) 0.0005(8) 0.0202(8) 0.0036(8)
c22 0.0393(12) 0.0291(11) 0.0241(9) 0.0043(8) 0.0142(9) 0.0089(10)
c21 0.0348(11) 0.0261(11) 0.0309(10) -0.0085(8) 0.0206(9) -0.0082(9)
c13 0.0256(11) 0.0284(11) 0.0639(14) 0.0027(11) 0.0224(11) 0.0038(10)
c12 0.0169(10) 0.0277(11) 0.0511(12) -0.0096(10) 0.0021(9) -0.0022(9)
c11 0.0303(12) 0.0569(15) 0.0246(10) 0.0032(10) 0.0074(9) 0.0036(11)

_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
si2 c2 1.8248(18) . ?
si2 c21 1.8688(18) . ?
si2 c22 1.8765(18) . ?
si2 c23 1.8851(16) . ?
si1 c1 1.8299(19) . ?
si1 c13 1.8730(19) . ?
si1 c11 1.8808(19) . ?
si1 c12 1.894(2) . ?
na2 c1 2.5953(19) . ?
na2 c1 2.649(2) 2_556 ?
na2 c2 2.7872(17) . ?
na2 c2 2.8189(18) 5_566 ?
na2 h2b 2.564(16) . ?
na2 h2a 2.515(16) . ?
na2 h1a 2.65(2) . ?
na1 c2 2.6335(18) 5_566 ?
na1 c2 2.6476(19) 6_566 ?
na1 h1b 2.658(18) . ?
c2 na1 2.6335(18) 5_566 ?
c2 na1 2.6476(19) 6_565 ?
c2 na2 2.8189(18) 5_566 ?
c2 h2b 0.937(17) . ?
c2 h2a 0.909(18) . ?
c1 na2 2.6488(19) 2_556 ?
c1 h1b 0.947(18) . ?
c1 h1a 0.89(2) . ?
c23 h23a 0.980 . ?
c23 h23b 0.980 . ?
c23 h23c 0.980 . ?
c22 h22a 0.980 . ?
c22 h22b 0.980 . ?
c22 h22c 0.980 . ?
c21 h21a 0.980 . ?
c21 h21b 0.980 . ?
c21 h21c 0.980 . ?
c13 h13a 0.980 . ?
c13 h13b 0.980 . ?
c13 h13c 0.980 . ?
c12 h12a 0.980 . ?
c12 h12b 0.980 . ?
c12 h12c 0.980 . ?
c11 h11a 0.980 . ?
c11 h11b 0.980 . ?
c11 h11c 0.980 . ?

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
c2 si2 c21 110.27(9) . . ?
c2 si2 c22 108.90(8) . . ?
c21 si2 c22 110.30(9) . . ?
c2 si2 c23 117.99(8) . . ?
c21 si2 c23 104.55(8) . . ?
c22 si2 c23 104.56(8) . . ?
c1 si1 c13 117.60(9) . . ?
c1 si1 c11 110.79(9) . . ?
c13 si1 c11 107.13(9) . . ?
c1 si1 c12 110.21(9) . . ?
c13 si1 c12 103.75(9) . . ?
c11 si1 c12 106.64(10) . . ?
c1 na2 c1 109.23(5) . 2_556 ?
c1 na2 c2 137.05(6) . . ?
c1 na2 c2 111.54(6) 2_556 . ?
c1 na2 c2 98.44(6) . 5_566 ?
c1 na2 c2 93.73(6) 2_556 5_566 ?
c2 na2 c2 91.90(5) . 5_566 ?
c1 na2 h2b 156.1(4) . . ?
c1 na2 h2b 94.3(4) 2_556 . ?
c2 na2 h2b 19.6(4) . . ?
c2 na2 h2b 83.7(4) 5_566 . ?
c1 na2 h2a 121.5(4) . . ?
c1 na2 h2a 129.1(4) 2_556 . ?
c2 na2 h2a 18.8(4) . . ?
c2 na2 h2a 84.1(4) 5_566 . ?
h2b na2 h2a 34.8(5) . . ?
c1 na2 h1a 19.5(5) . . ?
c1 na2 h1a 107.5(4) 2_556 . ?
c2 na2 h1a 128.5(4) . . ?
c2 na2 h1a 117.8(5) 5_566 . ?
h2b na2 h1a 147.3(6) . . ?
h2a na2 h1a 118.4(6) . . ?
c2 na1 c2 112.51(5) 5_566 6_566 ?
c2 na1 h1b 124.0(4) 5_566 . ?
c2 na1 h1b 85.5(4) 6_566 . ?
si2 c2 na1 107.42(8) . 5_566 ?
si2 c2 na1 105.95(8) . 6_565 ?
na1 c2 na1 66.94(4) 5_566 6_565 ?
si2 c2 na2 90.57(6) . . ?
na1 c2 na2 149.49(8) 5_566 . ?
na1 c2 na2 132.37(8) 6_565 . ?
si2 c2 na2 178.28(9) . 5_566 ?
na1 c2 na2 73.33(5) 5_566 5_566 ?
na1 c2 na2 75.77(5) 6_565 5_566 ?
na2 c2 na2 88.10(5) . 5_566 ?
si2 c2 h2b 112.0(11) . . ?
na1 c2 h2b 83.6(10) 5_566 . ?
na1 c2 h2b 137.4(10) 6_565 . ?
na2 c2 h2b 66.6(10) . . ?
na2 c2 h2b 66.4(10) 5_566 . ?
si2 c2 h2a 113.0(12) . . ?
na1 c2 h2a 126.3(11) 5_566 . ?
na1 c2 h2a 69.0(10) 6_565 . ?
na2 c2 h2a 63.4(10) . . ?
na2 c2 h2a 67.3(11) 5_566 . ?
h2b c2 h2a 110.8(15) . . ?
si1 c1 na2 109.72(8) . . ?
si1 c1 na2 171.33(10) . 2_556 ?
na2 c1 na2 70.63(5) . 2_556 ?
si1 c1 h1b 106.4(11) . . ?
na2 c1 h1b 140.5(11) . . ?
na2 c1 h1b 71.3(11) 2_556 . ?
si1 c1 h1a 106.2(13) . . ?
na2 c1 h1a 83.7(13) . . ?
na2 c1 h1a 82.5(13) 2_556 . ?
h1b c1 h1a 101.3(16) . . ?
si2 c23 h23a 109.5 . . ?
si2 c23 h23b 109.5 . . ?
h23a c23 h23b 109.5 . . ?
si2 c23 h23c 109.5 . . ?
h23a c23 h23c 109.5 . . ?
h23b c23 h23c 109.5 . . ?
si2 c22 h22a 109.5 . . ?
si2 c22 h22b 109.5 . . ?
h22a c22 h22b 109.5 . . ?
si2 c22 h22c 109.5 . . ?
h22a c22 h22c 109.5 . . ?
h22b c22 h22c 109.5 . . ?
si2 c21 h21a 109.5 . . ?
si2 c21 h21b 109.5 . . ?
h21a c21 h21b 109.5 . . ?
si2 c21 h21c 109.5 . . ?
h21a c21 h21c 109.5 . . ?
h21b c21 h21c 109.5 . . ?
si1 c13 h13a 109.5 . . ?
si1 c13 h13b 109.5 . . ?
h13a c13 h13b 109.5 . . ?
si1 c13 h13c 109.5 . . ?
h13a c13 h13c 109.5 . . ?
h13b c13 h13c 109.5 . . ?
si1 c12 h12a 109.5 . . ?
si1 c12 h12b 109.5 . . ?
h12a c12 h12b 109.5 . . ?
si1 c12 h12c 109.5 . . ?
h12a c12 h12c 109.5 . . ?
h12b c12 h12c 109.5 . . ?
si1 c11 h11a 109.5 . . ?
si1 c11 h11b 109.5 . . ?
h11a c11 h11b 109.5 . . ?
si1 c11 h11c 109.5 . . ?
h11a c11 h11c 109.5 . . ?
h11b c11 h11c 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.867
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.052

#===END