# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

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#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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data_wz2013070201_0m

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'B2 F Li0.8 Mg2.1 O5'
_chemical_formula_weight         177.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   3.0881(4)
_cell_length_b                   13.602(2)
_cell_length_c                   9.6563(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.744(9)
_cell_angle_gamma                90.00
_cell_volume                     405.43(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1115
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      27.42

_exptl_crystal_description       needlelike
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.157
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             346
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.9269
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   face-indexed

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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            3484
_diffrn_reflns_av_R_equivalents  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.59
_diffrn_reflns_theta_max         27.52
_reflns_number_total             908
_reflns_number_gt                712
_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 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^)+(0.0645P)^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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         908
_refine_ls_number_parameters     107
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0507
_refine_ls_R_factor_gt           0.0366
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0935
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_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
Mg1 Mg 0.9918(2) 0.32464(7) 1.10099(8) 0.0103(3) Uani 1 1 d . . .
Mg2 Mg 0.9645(3) 0.35260(6) 0.73653(8) 0.0098(3) Uani 1 1 d . . .
Li1 Li 0.5000 0.5000 1.0000 0.0143(14) Uani 0.586(17) 2 d SP . 1
Mg3 Mg 0.5000 0.5000 1.0000 0.0143(14) Uani 0.207(8) 2 d SP . 2
Li2 Li 0.182(3) -0.0122(7) 1.0097(10) 0.025(2) Uani 0.50 1 d P . .
B1 B 0.4290(9) 0.1950(2) 0.9071(3) 0.0069(6) Uani 1 1 d . . .
B2 B 0.6091(8) 0.4581(2) 1.2838(3) 0.0080(6) Uani 1 1 d . . .
F1 F 0.9897(4) 0.40476(11) 0.93035(14) 0.0124(4) Uani 1 1 d . . .
O1 O 0.4816(5) 0.25058(13) 0.79029(16) 0.0082(4) Uani 1 1 d . . .
O2 O 1.4802(5) 0.22919(12) 1.03974(17) 0.0083(4) Uani 1 1 d . . .
O4 O 0.5079(5) 0.41403(12) 1.16351(16) 0.0083(4) Uani 1 1 d . . .
O3 O 1.4617(5) 0.44584(13) 0.68343(16) 0.0088(4) Uani 1 1 d . . .
O5 O 0.3111(6) 0.09538(13) 0.89472(16) 0.0110(4) 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
Mg1 0.0110(5) 0.0092(5) 0.0105(5) 0.0004(4) 0.0000(4) 0.0001(3)
Mg2 0.0115(5) 0.0076(5) 0.0103(5) 0.0004(3) 0.0003(3) -0.0002(3)
Li1 0.020(2) 0.011(2) 0.012(2) 0.0032(16) 0.0013(16) 0.0000(16)
Mg3 0.020(2) 0.011(2) 0.012(2) 0.0032(16) 0.0013(16) 0.0000(16)
Li2 0.032(5) 0.014(5) 0.028(6) 0.010(4) -0.002(5) 0.002(5)
B1 0.0071(13) 0.0035(15) 0.0103(13) -0.0016(10) 0.0028(11) -0.0005(10)
B2 0.0074(14) 0.0083(15) 0.0086(13) 0.0017(11) 0.0032(11) -0.0006(11)
F1 0.0167(8) 0.0108(9) 0.0099(8) 0.0010(6) 0.0007(6) -0.0002(6)
O1 0.0116(9) 0.0072(9) 0.0059(8) 0.0004(7) 0.0004(7) -0.0012(7)
O2 0.0094(9) 0.0081(10) 0.0075(8) -0.0003(7) 0.0002(7) 0.0004(7)
O4 0.0095(9) 0.0065(10) 0.0088(8) 0.0003(7) -0.0001(7) 0.0003(7)
O3 0.0110(9) 0.0068(10) 0.0087(9) -0.0005(7) 0.0007(7) 0.0007(7)
O5 0.0177(10) 0.0075(10) 0.0077(9) 0.0005(7) -0.0021(7) -0.0038(7)

_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
Mg1 F1 1.9754(16) . ?
Mg1 O4 2.0325(19) . ?
Mg1 O4 2.0795(19) 1_655 ?
Mg1 O2 2.0891(18) . ?
Mg1 O1 2.0958(18) 4_666 ?
Mg1 O2 2.1154(18) 1_455 ?
Mg2 F1 2.0008(16) . ?
Mg2 O3 2.0577(18) 1_455 ?
Mg2 O3 2.0681(18) . ?
Mg2 O1 2.1134(18) . ?
Mg2 O1 2.1665(18) 1_655 ?
Mg2 O2 2.2038(18) 4_565 ?
Li1 O4 1.9643(16) . ?
Li1 O4 1.9643(16) 3_667 ?
Li1 F1 2.1165(15) . ?
Li1 F1 2.1165(15) 3_667 ?
Li1 F1 2.1329(14) 1_455 ?
Li1 F1 2.1329(14) 3_767 ?
Li2 O5 1.888(10) . ?
Li2 O3 1.988(10) 2_646 ?
Li2 O3 2.039(11) 4_466 ?
Li2 O5 2.120(9) 3_657 ?
Li2 O5 2.129(10) 3_557 ?
B1 O2 1.367(3) 1_455 ?
B1 O1 1.371(3) . ?
B1 O5 1.408(3) . ?
B2 O4 1.336(3) . ?
B2 O3 1.364(3) 3_767 ?
B2 O5 1.423(3) 4_666 ?
F1 Mg3 2.1329(14) 1_655 ?
F1 Li1 2.1329(14) 1_655 ?
O1 Mg1 2.0958(18) 4_565 ?
O1 Mg2 2.1665(18) 1_455 ?
O2 B1 1.367(3) 1_655 ?
O2 Mg1 2.1154(18) 1_655 ?
O2 Mg2 2.2038(18) 4_666 ?
O4 Mg1 2.0795(18) 1_455 ?
O3 B2 1.364(3) 3_767 ?
O3 Li2 1.988(10) 2_656 ?
O3 Li2 2.039(11) 4_765 ?
O3 Mg2 2.0577(18) 1_655 ?
O5 B2 1.423(3) 4_565 ?
O5 Li2 2.120(9) 3_657 ?
O5 Li2 2.129(10) 3_557 ?

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 Mg1 O4 86.21(7) . . ?
F1 Mg1 O4 84.41(7) . 1_655 ?
O4 Mg1 O4 97.35(8) . 1_655 ?
F1 Mg1 O2 95.21(7) . . ?
O4 Mg1 O2 178.26(8) . . ?
O4 Mg1 O2 83.81(7) 1_655 . ?
F1 Mg1 O1 175.61(8) . 4_666 ?
O4 Mg1 O1 90.13(7) . 4_666 ?
O4 Mg1 O1 93.67(7) 1_655 4_666 ?
O2 Mg1 O1 88.50(7) . 4_666 ?
F1 Mg1 O2 97.00(7) . 1_455 ?
O4 Mg1 O2 84.29(7) . 1_455 ?
O4 Mg1 O2 177.92(8) 1_655 1_455 ?
O2 Mg1 O2 94.53(8) . 1_455 ?
O1 Mg1 O2 85.02(7) 4_666 1_455 ?
F1 Mg2 O3 91.26(7) . 1_455 ?
F1 Mg2 O3 90.37(7) . . ?
O3 Mg2 O3 96.92(8) 1_455 . ?
F1 Mg2 O1 90.61(7) . . ?
O3 Mg2 O1 86.17(7) 1_455 . ?
O3 Mg2 O1 176.74(8) . . ?
F1 Mg2 O1 89.75(6) . 1_655 ?
O3 Mg2 O1 178.21(7) 1_455 1_655 ?
O3 Mg2 O1 84.55(7) . 1_655 ?
O1 Mg2 O1 92.35(7) . 1_655 ?
F1 Mg2 O2 169.85(7) . 4_565 ?
O3 Mg2 O2 97.61(7) 1_455 4_565 ?
O3 Mg2 O2 93.43(7) . 4_565 ?
O1 Mg2 O2 85.10(7) . 4_565 ?
O1 Mg2 O2 81.25(7) 1_655 4_565 ?
O4 Li1 O4 180.000(1) . 3_667 ?
O4 Li1 F1 84.23(6) . . ?
O4 Li1 F1 95.77(6) 3_667 . ?
O4 Li1 F1 95.77(6) . 3_667 ?
O4 Li1 F1 84.23(6) 3_667 3_667 ?
F1 Li1 F1 180.000(1) . 3_667 ?
O4 Li1 F1 83.27(6) . 1_455 ?
O4 Li1 F1 96.73(6) 3_667 1_455 ?
F1 Li1 F1 93.22(6) . 1_455 ?
F1 Li1 F1 86.78(6) 3_667 1_455 ?
O4 Li1 F1 96.73(6) . 3_767 ?
O4 Li1 F1 83.27(6) 3_667 3_767 ?
F1 Li1 F1 86.78(6) . 3_767 ?
F1 Li1 F1 93.22(6) 3_667 3_767 ?
F1 Li1 F1 180.00(6) 1_455 3_767 ?
O5 Li2 O3 73.5(4) . 2_646 ?
O5 Li2 O3 102.8(5) . 4_466 ?
O3 Li2 O3 146.0(5) 2_646 4_466 ?
O5 Li2 O5 120.2(5) . 3_657 ?
O3 Li2 O5 113.3(5) 2_646 3_657 ?
O3 Li2 O5 98.0(4) 4_466 3_657 ?
O5 Li2 O5 146.5(5) . 3_557 ?
O3 Li2 O5 96.5(4) 2_646 3_557 ?
O3 Li2 O5 67.6(3) 4_466 3_557 ?
O5 Li2 O5 93.2(4) 3_657 3_557 ?
O2 B1 O1 124.8(2) 1_455 . ?
O2 B1 O5 115.4(2) 1_455 . ?
O1 B1 O5 119.8(2) . . ?
O4 B2 O3 126.6(2) . 3_767 ?
O4 B2 O5 120.7(2) . 4_666 ?
O3 B2 O5 112.6(2) 3_767 4_666 ?
Mg1 F1 Mg2 125.71(8) . . ?
Mg1 F1 Li1 93.26(6) . . ?
Mg2 F1 Li1 120.43(7) . . ?
Mg1 F1 Mg3 95.07(6) . 1_655 ?
Mg2 F1 Mg3 121.17(7) . 1_655 ?
Li1 F1 Mg3 93.22(6) . 1_655 ?
Mg1 F1 Li1 95.07(6) . 1_655 ?
Mg2 F1 Li1 121.17(7) . 1_655 ?
Li1 F1 Li1 93.22(6) . 1_655 ?
Mg3 F1 Li1 0.0 1_655 1_655 ?
B1 O1 Mg1 116.98(16) . 4_565 ?
B1 O1 Mg2 131.75(15) . . ?
Mg1 O1 Mg2 94.40(7) 4_565 . ?
B1 O1 Mg2 116.43(15) . 1_455 ?
Mg1 O1 Mg2 97.72(7) 4_565 1_455 ?
Mg2 O1 Mg2 92.35(7) . 1_455 ?
B1 O2 Mg1 114.36(15) 1_655 . ?
B1 O2 Mg1 122.32(15) 1_655 1_655 ?
Mg1 O2 Mg1 94.53(8) . 1_655 ?
B1 O2 Mg2 129.15(16) 1_655 4_666 ?
Mg1 O2 Mg2 91.98(7) . 4_666 ?
Mg1 O2 Mg2 96.00(7) 1_655 4_666 ?
B2 O4 Li1 115.39(16) . . ?
B2 O4 Mg1 111.84(14) . . ?
Li1 O4 Mg1 96.24(7) . . ?
B2 O4 Mg1 132.20(16) . 1_455 ?
Li1 O4 Mg1 97.13(7) . 1_455 ?
Mg1 O4 Mg1 97.35(8) . 1_455 ?
B2 O3 Li2 84.8(3) 3_767 2_656 ?
B2 O3 Li2 80.0(3) 3_767 4_765 ?
Li2 O3 Li2 34.0(5) 2_656 4_765 ?
B2 O3 Mg2 131.14(15) 3_767 1_655 ?
Li2 O3 Mg2 123.8(3) 2_656 1_655 ?
Li2 O3 Mg2 102.1(3) 4_765 1_655 ?
B2 O3 Mg2 113.87(14) 3_767 . ?
Li2 O3 Mg2 105.2(3) 2_656 . ?
Li2 O3 Mg2 138.1(3) 4_765 . ?
Mg2 O3 Mg2 96.92(8) 1_655 . ?
B1 O5 B2 131.5(2) . 4_565 ?
B1 O5 Li2 139.1(4) . . ?
B2 O5 Li2 87.2(3) 4_565 . ?
B1 O5 Li2 106.9(3) . 3_657 ?
B2 O5 Li2 110.9(3) 4_565 3_657 ?
Li2 O5 Li2 59.8(5) . 3_657 ?
B1 O5 Li2 131.4(3) . 3_557 ?
B2 O5 Li2 75.6(3) 4_565 3_557 ?
Li2 O5 Li2 33.5(5) . 3_557 ?
Li2 O5 Li2 93.2(4) 3_657 3_557 ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.102
_database_code_depnum_ccdc_archive 'CCDC 956687'