# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2015

 
data_shelx
 
_audit_creation_method            'SHELXL-2014/7'
_shelx_SHELXL_version_number      '2014/7'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'F4 Mo1 Na2 O2' 
_chemical_formula_weight          249.92

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Na'  'Na'   0.0362   0.0249
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mo'  'Mo'  -1.6832   0.6857
 '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'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            14
_space_group_name_H-M_alt         'P 21/c'
_space_group_name_Hall            '-P 2ybc'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, y+1/2, -z+1/2'
 '-x, -y, -z'
 'x, -y-1/2, z-1/2'
 
_cell_length_a                    5.4800(11)
_cell_length_b                    5.701(7)
_cell_length_c                    16.319(3)
_cell_angle_alpha                 90
_cell_angle_beta                  91.316(8)
_cell_angle_gamma                 90
_cell_volume                      509.7(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     173(2)
_cell_measurement_reflns_used     1234
_cell_measurement_theta_min       3.6
_cell_measurement_theta_max       27.5
 
_exptl_crystal_description        'block'
_exptl_crystal_colour             'blue'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     'not measured'
_exptl_crystal_density_diffrn     3.257          
_exptl_crystal_F_000              464
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.2
_exptl_absorpt_coefficient_mu     2.749
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type          'Multi-scan'
_exptl_absorpt_correction_T_max         1.000
_exptl_absorpt_correction_T_min         0.855
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       173(2)
_diffrn_radiation_wavelength      0.71075
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'Sealed tube'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             4853
_diffrn_reflns_av_unetI/netI      0.0160
_diffrn_reflns_av_R_equivalents   0.0215
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        7
_diffrn_reflns_limit_k_min        -7
_diffrn_reflns_limit_k_max        7
_diffrn_reflns_limit_l_min        -21
_diffrn_reflns_limit_l_max        20
_diffrn_reflns_theta_min          3.719
_diffrn_reflns_theta_max          27.489
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.960
_diffrn_measured_fraction_theta_full  0.950
_diffrn_reflns_Laue_measured_fraction_max    0.960
_diffrn_reflns_Laue_measured_fraction_full   0.950
_diffrn_reflns_point_group_measured_fraction_max   0.960
_diffrn_reflns_point_group_measured_fraction_full  0.950
_reflns_number_total              1126
_reflns_number_gt                 1074
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b32 (Rigaku, 2014)
;
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0187P)²+0.3537P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    .
_refine_ls_hydrogen_treatment     undef
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          1126
_refine_ls_number_parameters      82
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0153
_refine_ls_R_factor_gt            0.0140
_refine_ls_wR_factor_ref          0.0381
_refine_ls_wR_factor_gt           0.0377
_refine_ls_goodness_of_fit_ref    1.142
_refine_ls_restrained_S_all       1.142
_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_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Mo1 Mo 0.22902(3) 0.72555(3) 0.11635(2) 0.00863(7) Uani 1 1 d . . . . .
Na1 Na 0.26089(13) 0.28075(13) 0.24859(5) 0.01435(17) Uani 1 1 d . . . . .
Na2 Na -0.26818(13) 0.23041(13) 0.12111(4) 0.01202(16) Uani 1 1 d . . . . .
O1 O 0.3391(3) 0.7404(2) 0.02102(9) 0.0180(3) Uani 1 1 d . . . . .
O2 O -0.0415(2) 0.8801(2) 0.10794(9) 0.0164(3) Uani 1 1 d . . . . .
F1 F 0.14304(19) 0.6764(2) 0.24126(6) 0.0131(2) Uani 1 1 d . . . . .
F2 F 0.52032(18) 0.53959(18) 0.16327(6) 0.0128(2) Uani 1 1 d . . . . .
F3 F 0.41859(19) 0.98879(19) 0.16161(6) 0.0133(2) Uani 1 1 d . . . . .
F4 F 0.0896(2) 0.41774(19) 0.10928(7) 0.0165(2) Uani 1 1 d . . . . .
 
 
_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
Mo1 O1 1.6837(15) . ?
Mo1 O2 1.7273(14) . ?
Mo1 F4 1.916(2) . ?
Mo1 F3 1.9599(18) . ?
Mo1 F2 2.0499(12) . ?
Mo1 F1 2.1212(11) . ?
Mo1 Na1 3.332(3) . ?
Mo1 Na1 3.5265(9) 2 ?
Mo1 Na1 3.5338(9) 2_655 ?
Na1 F1 2.3017(14) 2_545 ?
Na1 F2 2.3059(16) 2_645 ?
Na1 F1 2.349(3) . ?
Na1 F3 2.3639(19) 1_545 ?
Na1 F2 2.4956(17) . ?
Na1 F3 2.5537(15) 2_645 ?
Na1 F4 2.5615(15) . ?
Na1 O2 2.7160(17) 2_545 ?
Na1 Na2 3.330(3) 2 ?
Na1 Na2 3.3640(11) 1_655 ?
Na1 Mo1 3.5265(9) 2_545 ?
Na2 F2 2.227(2) 1_455 ?
Na2 F4 2.2447(15) . ?
Na2 F3 2.3092(16) 1_445 ?
Na2 O1 2.3486(17) 3_565 ?
Na2 F1 2.3534(13) 2_545 ?
Na2 O2 2.364(3) 1_545 ?
Na2 Na1 3.330(3) 2_545 ?
Na2 Na1 3.3640(11) 1_455 ?
Na2 Na1 3.790(3) 2 ?
O1 Na2 2.3487(17) 3_565 ?
O2 Na2 2.364(3) 1_565 ?
O2 Na1 2.7160(16) 2 ?
F1 Na1 2.3016(14) 2 ?
F1 Na2 2.3534(13) 2 ?
F2 Na2 2.227(2) 1_655 ?
F2 Na1 2.3059(16) 2_655 ?
F3 Na2 2.3092(16) 1_665 ?
F3 Na1 2.3639(19) 1_565 ?
F3 Na1 2.5537(15) 2_655 ?
 
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
O1 Mo1 O2 103.05(7) . . ?
O1 Mo1 F4 98.12(6) . . ?
O2 Mo1 F4 97.00(8) . . ?
O1 Mo1 F3 96.40(6) . . ?
O2 Mo1 F3 94.93(8) . . ?
F4 Mo1 F3 158.59(5) . . ?
O1 Mo1 F2 94.52(6) . . ?
O2 Mo1 F2 162.37(6) . . ?
F4 Mo1 F2 81.66(7) . . ?
F3 Mo1 F2 81.59(8) . . ?
O1 Mo1 F1 170.70(6) . . ?
O2 Mo1 F1 86.24(6) . . ?
F4 Mo1 F1 80.79(5) . . ?
F3 Mo1 F1 82.33(5) . . ?
F2 Mo1 F1 76.18(4) . . ?
O1 Mo1 Na1 128.49(6) . . ?
O2 Mo1 Na1 118.15(6) . . ?
F4 Mo1 Na1 49.98(6) . . ?
F3 Mo1 Na1 108.62(7) . . ?
F2 Mo1 Na1 48.37(4) . . ?
F1 Mo1 Na1 44.49(4) . . ?
O1 Mo1 Na1 150.12(5) . 2 ?
O2 Mo1 Na1 48.68(5) . 2 ?
F4 Mo1 Na1 79.11(4) . 2 ?
F3 Mo1 Na1 95.78(4) . 2 ?
F2 Mo1 Na1 114.22(3) . 2 ?
F1 Mo1 Na1 38.93(3) . 2 ?
Na1 Mo1 Na1 72.09(3) . 2 ?
O1 Mo1 Na1 106.07(6) . 2_655 ?
O2 Mo1 Na1 132.02(5) . 2_655 ?
F4 Mo1 Na1 115.32(4) . 2_655 ?
F3 Mo1 Na1 44.93(4) . 2_655 ?
F2 Mo1 Na1 38.28(5) . 2_655 ?
F1 Mo1 Na1 66.57(3) . 2_655 ?
Na1 Mo1 Na1 68.58(3) . 2_655 ?
Na1 Mo1 Na1 101.82(2) 2 2_655 ?
F1 Na1 F2 106.75(6) 2_545 2_645 ?
F1 Na1 F1 89.31(5) 2_545 . ?
F2 Na1 F1 137.97(6) 2_645 . ?
F1 Na1 F3 103.11(6) 2_545 1_545 ?
F2 Na1 F3 76.28(6) 2_645 1_545 ?
F1 Na1 F3 138.55(6) . 1_545 ?
F1 Na1 F2 138.94(5) 2_545 . ?
F2 Na1 F2 113.94(5) 2_645 . ?
F1 Na1 F2 64.10(6) . . ?
F3 Na1 F2 81.98(8) 1_545 . ?
F1 Na1 F3 136.77(5) 2_545 2_645 ?
F2 Na1 F3 65.04(7) 2_645 2_645 ?
F1 Na1 F3 76.57(6) . 2_645 ?
F3 Na1 F3 114.55(5) 1_545 2_645 ?
F2 Na1 F3 69.66(5) . 2_645 ?
F1 Na1 F4 79.00(5) 2_545 . ?
F2 Na1 F4 155.52(5) 2_645 . ?
F1 Na1 F4 64.36(4) . . ?
F3 Na1 F4 79.24(6) 1_545 . ?
F2 Na1 F4 61.74(4) . . ?
F3 Na1 F4 126.94(6) 2_645 . ?
F1 Na1 O2 63.03(4) 2_545 2_545 ?
F2 Na1 O2 79.67(5) 2_645 2_545 ?
F1 Na1 O2 73.56(4) . 2_545 ?
F3 Na1 O2 147.09(5) 1_545 2_545 ?
F2 Na1 O2 128.81(7) . 2_545 ?
F3 Na1 O2 73.78(4) 2_645 2_545 ?
F4 Na1 O2 122.76(5) . 2_545 ?
F1 Na1 Na2 98.65(4) 2_545 2 ?
F2 Na1 Na2 93.56(7) 2_645 2 ?
F1 Na1 Na2 44.96(5) . 2 ?
F3 Na1 Na2 157.84(4) 1_545 2 ?
F2 Na1 Na2 84.40(7) . 2 ?
F3 Na1 Na2 43.78(3) 2_645 2 ?
F4 Na1 Na2 109.32(6) . 2 ?
O2 Na1 Na2 44.61(3) 2_545 2 ?
F1 Na1 Mo1 101.95(4) 2_545 . ?
F2 Na1 Mo1 151.23(4) 2_645 . ?
F1 Na1 Mo1 39.26(4) . . ?
F3 Na1 Mo1 99.29(7) 1_545 . ?
F2 Na1 Mo1 37.88(3) . . ?
F3 Na1 Mo1 92.48(6) 2_645 . ?
F4 Na1 Mo1 34.96(3) . . ?
O2 Na1 Mo1 112.46(6) 2_545 . ?
Na2 Na1 Mo1 80.06(7) 2 . ?
F1 Na1 Na2 140.82(4) 2_545 1_655 ?
F2 Na1 Na2 86.54(4) 2_645 1_655 ?
F1 Na1 Na2 105.33(4) . 1_655 ?
F3 Na1 Na2 43.31(4) 1_545 1_655 ?
F2 Na1 Na2 41.45(5) . 1_655 ?
F3 Na1 Na2 82.37(4) 2_645 1_655 ?
F4 Na1 Na2 75.40(4) . 1_655 ?
O2 Na1 Na2 155.77(4) 2_545 1_655 ?
Na2 Na1 Na2 117.54(3) 2 1_655 ?
Mo1 Na1 Na2 72.18(3) . 1_655 ?
F1 Na1 Mo1 35.39(3) 2_545 2_545 ?
F2 Na1 Mo1 87.10(4) 2_645 2_545 ?
F1 Na1 Mo1 84.56(4) . 2_545 ?
F3 Na1 Mo1 127.34(5) 1_545 2_545 ?
F2 Na1 Mo1 148.55(5) . 2_545 ?
F3 Na1 Mo1 101.90(4) 2_645 2_545 ?
F4 Na1 Mo1 108.25(4) . 2_545 ?
O2 Na1 Mo1 28.53(3) 2_545 2_545 ?
Na2 Na1 Mo1 70.60(3) 2 2_545 ?
Mo1 Na1 Mo1 116.32(2) . 2_545 ?
Na2 Na1 Mo1 169.98(3) 1_655 2_545 ?
F2 Na2 F4 96.42(8) 1_455 . ?
F2 Na2 F3 89.32(8) 1_455 1_445 ?
F4 Na2 F3 164.75(5) . 1_445 ?
F2 Na2 O1 100.00(6) 1_455 3_565 ?
F4 Na2 O1 90.37(5) . 3_565 ?
F3 Na2 O1 102.57(5) 1_445 3_565 ?
F2 Na2 F1 87.19(5) 1_455 2_545 ?
F4 Na2 F1 84.74(5) . 2_545 ?
F3 Na2 F1 81.44(4) 1_445 2_545 ?
O1 Na2 F1 171.74(5) 3_565 2_545 ?
F2 Na2 O2 167.11(6) 1_455 1_545 ?
F4 Na2 O2 86.12(8) . 1_545 ?
F3 Na2 O2 85.28(8) 1_445 1_545 ?
O1 Na2 O2 92.60(5) 3_565 1_545 ?
F1 Na2 O2 80.45(5) 2_545 1_545 ?
F2 Na2 Na1 114.24(7) 1_455 2_545 ?
F4 Na2 Na1 115.05(5) . 2_545 ?
F3 Na2 Na1 49.93(4) 1_445 2_545 ?
O1 Na2 Na1 133.18(5) 3_565 2_545 ?
F1 Na2 Na1 44.85(4) 2_545 2_545 ?
O2 Na2 Na1 53.78(6) 1_545 2_545 ?
F2 Na2 Na1 47.89(4) 1_455 1_455 ?
F4 Na2 Na1 134.15(5) . 1_455 ?
F3 Na2 Na1 44.61(5) 1_445 1_455 ?
O1 Na2 Na1 119.52(5) 3_565 1_455 ?
F1 Na2 Na1 68.40(4) 2_545 1_455 ?
O2 Na2 Na1 122.71(5) 1_545 1_455 ?
Na1 Na2 Na1 70.67(3) 2_545 1_455 ?
F2 Na2 Na1 100.33(4) 1_455 . ?
F4 Na2 Na1 46.13(4) . . ?
F3 Na2 Na1 118.96(4) 1_445 . ?
O1 Na2 Na1 133.55(5) 3_565 . ?
F1 Na2 Na1 39.93(3) 2_545 . ?
O2 Na2 Na1 72.37(5) 1_545 . ?
Na1 Na2 Na1 71.92(3) 2_545 . ?
Na1 Na2 Na1 105.02(3) 1_455 . ?
F2 Na2 Na1 33.94(4) 1_455 2 ?
F4 Na2 Na1 69.91(5) . 2 ?
F3 Na2 Na1 109.36(6) 1_445 2 ?
O1 Na2 Na1 119.66(6) 3_565 2 ?
F1 Na2 Na1 64.76(5) 2_545 2 ?
O2 Na2 Na1 138.72(6) 1_545 2 ?
Na1 Na2 Na1 106.21(7) 2_545 2 ?
Na1 Na2 Na1 65.21(2) 1_455 2 ?
Na1 Na2 Na1 66.75(2) . 2 ?
Mo1 O1 Na2 149.48(9) . 3_565 ?
Mo1 O2 Na2 151.09(8) . 1_565 ?
Mo1 O2 Na1 102.78(6) . 2 ?
Na2 O2 Na1 81.60(6) 1_565 2 ?
Mo1 F1 Na1 105.68(5) . 2 ?
Mo1 F1 Na1 96.24(5) . . ?
Na1 F1 Na1 120.55(5) 2 . ?
Mo1 F1 Na2 146.46(6) . 2 ?
Na1 F1 Na2 99.04(5) 2 2 ?
Na1 F1 Na2 90.19(5) . 2 ?
Mo1 F2 Na2 134.44(6) . 1_655 ?
Mo1 F2 Na1 108.30(8) . 2_655 ?
Na2 F2 Na1 113.44(7) 1_655 2_655 ?
Mo1 F2 Na1 93.75(6) . . ?
Na2 F2 Na1 90.66(8) 1_655 . ?
Na1 F2 Na1 107.41(6) 2_655 . ?
Mo1 F3 Na2 137.73(6) . 1_665 ?
Mo1 F3 Na1 124.57(7) . 1_565 ?
Na2 F3 Na1 92.08(8) 1_665 1_565 ?
Mo1 F3 Na1 102.25(8) . 2_655 ?
Na2 F3 Na1 86.29(6) 1_665 2_655 ?
Na1 F3 Na1 103.80(6) 1_565 2_655 ?
Mo1 F4 Na2 141.10(6) . . ?
Mo1 F4 Na1 95.06(6) . . ?
Na2 F4 Na1 94.68(5) . . ?
 
_refine_diff_density_max    0.390
_refine_diff_density_min   -0.526
_refine_diff_density_rms    0.075



