 
data_a
 
_audit_creation_method            'SHELXL-2016/6'
_shelx_SHELXL_version_number      '2016/6'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'F H6 N Na O4 P' 
_chemical_formula_weight          157.02

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'N'  'N'   0.0061   0.0033
 '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'
 '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'
 'Na'  'Na'   0.0362   0.0249
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.1023   0.0942
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       monoclinic
_space_group_IT_number            7
_space_group_name_H-M_alt         'P n'
_space_group_name_Hall            'P -2yac'
 
_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+1/2, -y, z+1/2'
 
_cell_length_a                    4.9431(4)
_cell_length_b                    9.0200(7)
_cell_length_c                    6.0536(5)
_cell_angle_alpha                 90
_cell_angle_beta                  90.797(3)
_cell_angle_gamma                 90
_cell_volume                      269.88(4)
_cell_formula_units_Z             2
_cell_measurement_temperature     273(2)
_cell_measurement_reflns_used     2593
_cell_measurement_theta_min       4.00
_cell_measurement_theta_max       27.49
 
_exptl_crystal_description        'plate'
_exptl_crystal_colour             'colorless'
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.932          
_exptl_crystal_F_000              160
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max           ?
_exptl_crystal_size_mid           ?
_exptl_crystal_size_min           ?
_exptl_absorpt_coefficient_mu     0.542
_shelx_estimated_absorpt_T_min    ?
_shelx_estimated_absorpt_T_max    ?
_exptl_absorpt_correction_type    ?
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?
_exptl_absorpt_special_details    ?
_diffrn_ambient_temperature       273(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_source                    ?
_diffrn_measurement_device_type   'BRUKER D8 QUEST PHOTON II'
_diffrn_measurement_method        ?
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             4027
_diffrn_reflns_av_unetI/netI      0.0242
_diffrn_reflns_av_R_equivalents   0.0234
_diffrn_reflns_limit_h_min        -6
_diffrn_reflns_limit_h_max        6
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -7
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          4.054
_diffrn_reflns_theta_max          27.481
_diffrn_reflns_theta_full         25.242
_diffrn_measured_fraction_theta_max   0.992
_diffrn_measured_fraction_theta_full  0.990
_diffrn_reflns_Laue_measured_fraction_max    0.992
_diffrn_reflns_Laue_measured_fraction_full   0.990
_diffrn_reflns_point_group_measured_fraction_max   0.986
_diffrn_reflns_point_group_measured_fraction_full  0.990
_reflns_number_total              1228
_reflns_number_gt                 1207
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.971
_reflns_Friedel_fraction_max      0.981
_reflns_Friedel_fraction_full     0.990
 
_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        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     ?
_computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)'
_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)+(0.0298P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    difmap
_refine_ls_hydrogen_treatment     refall
_refine_ls_extinction_method      'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_extinction_coef        0.17(3)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_abs_structure_details
;
 Flack x determined using 578 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack    0.03(4)
_chemical_absolute_configuration  ?
_refine_ls_number_reflns          1228
_refine_ls_number_parameters      98
_refine_ls_number_restraints      2
_refine_ls_R_factor_all           0.0229
_refine_ls_R_factor_gt            0.0222
_refine_ls_wR_factor_ref          0.0574
_refine_ls_wR_factor_gt           0.0571
_refine_ls_goodness_of_fit_ref    1.294
_refine_ls_restrained_S_all       1.293
_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_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
P1 P 0.20926(10) 0.28129(7) 0.32885(9) 0.0144(2) Uani 1 1 d . . . . .
Na1 Na 0.5967(2) 0.54127(14) 0.32147(19) 0.0220(3) Uani 1 1 d . . . . .
N1 N 0.2034(7) 0.0466(3) -0.1717(6) 0.0261(5) Uani 1 1 d . . . . .
O2 O 0.3137(4) 0.3269(3) 0.1071(3) 0.0268(5) Uani 1 1 d . . . . .
O3 O 0.1998(5) 0.1157(2) 0.3657(4) 0.0260(5) Uani 1 1 d . . . . .
O11 O 0.2464(5) 0.7225(3) 0.3115(5) 0.0317(6) Uani 1 1 d . . . . .
F1 F -0.1030(3) 0.3266(2) 0.3216(3) 0.0290(4) Uani 1 1 d . . . . .
O1 O 0.3257(4) 0.3670(2) 0.5196(3) 0.0237(5) Uani 1 1 d . . . . .
H11 H 0.228(11) 0.117(7) -0.073(9) 0.061(16) Uiso 1 1 d . . . . .
H13 H 0.364(10) -0.014(4) -0.147(6) 0.038(12) Uiso 1 1 d . . . . .
H14 H 0.206(10) 0.080(5) -0.311(9) 0.040(11) Uiso 1 1 d . . . . .
H21 H 0.145(14) 0.701(6) 0.199(12) 0.068(17) Uiso 1 1 d . . . . .
H22 H 0.149(12) 0.704(5) 0.415(9) 0.043(14) Uiso 1 1 d . . . . .
H12 H 0.070(13) -0.009(5) -0.129(8) 0.056(16) Uiso 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
P1 O1 1.498(2) . ?
P1 O2 1.502(2) . ?
P1 O3 1.511(2) . ?
P1 F1 1.5966(17) . ?
P1 Na1 3.0284(14) . ?
P1 Na1 3.4366(13) 2_465 ?
Na1 O1 2.316(2) 2_564 ?
Na1 O2 2.346(2) 2_565 ?
Na1 O11 2.382(3) . ?
Na1 O1 2.397(2) . ?
Na1 F1 2.440(2) 1_655 ?
Na1 O2 2.708(3) . ?
Na1 Na1 3.9517(5) 2_565 ?
Na1 Na1 3.9517(5) 2_464 ?
Na1 Na1 4.0040(5) 2_465 ?
Na1 Na1 4.0041(5) 2_564 ?
 
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 P1 O2 114.48(13) . . ?
O1 P1 O3 114.15(12) . . ?
O2 P1 O3 114.45(13) . . ?
O1 P1 F1 104.47(11) . . ?
O2 P1 F1 104.44(12) . . ?
O3 P1 F1 103.01(11) . . ?
O1 P1 Na1 51.34(8) . . ?
O2 P1 Na1 63.24(10) . . ?
O3 P1 Na1 142.04(9) . . ?
F1 P1 Na1 114.38(8) . . ?
O1 P1 Na1 32.41(8) . 2_465 ?
O2 P1 Na1 135.22(10) . 2_465 ?
O3 P1 Na1 109.07(9) . 2_465 ?
F1 P1 Na1 74.73(7) . 2_465 ?
Na1 P1 Na1 76.24(2) . 2_465 ?
O1 Na1 O2 100.21(9) 2_564 2_565 ?
O1 Na1 O11 95.62(10) 2_564 . ?
O2 Na1 O11 89.73(11) 2_565 . ?
O1 Na1 O1 155.73(9) 2_564 . ?
O2 Na1 O1 102.51(9) 2_565 . ?
O11 Na1 O1 92.95(9) . . ?
O1 Na1 F1 88.84(8) 2_564 1_655 ?
O2 Na1 F1 97.49(9) 2_565 1_655 ?
O11 Na1 F1 170.73(9) . 1_655 ?
O1 Na1 F1 79.86(8) . 1_655 ?
O1 Na1 O2 97.58(8) 2_564 . ?
O2 Na1 O2 160.61(9) 2_565 . ?
O11 Na1 O2 96.17(9) . . ?
O1 Na1 O2 58.86(7) . . ?
F1 Na1 O2 75.14(7) 1_655 . ?
O1 Na1 P1 127.18(7) 2_564 . ?
O2 Na1 P1 131.64(7) 2_565 . ?
O11 Na1 P1 94.14(7) . . ?
O1 Na1 P1 29.21(5) . . ?
F1 Na1 P1 76.72(6) 1_655 . ?
O2 Na1 P1 29.69(5) . . ?
O1 Na1 P1 20.29(5) 2_564 2_564 ?
O2 Na1 P1 109.00(7) 2_565 2_564 ?
O11 Na1 P1 77.57(8) . 2_564 ?
O1 Na1 P1 146.90(6) . 2_564 ?
F1 Na1 P1 105.31(6) 1_655 2_564 ?
O2 Na1 P1 90.32(6) . 2_564 ?
P1 Na1 P1 118.91(4) . 2_564 ?
O1 Na1 Na1 111.37(6) 2_564 2_565 ?
O2 Na1 Na1 41.95(6) 2_565 2_565 ?
O11 Na1 Na1 126.55(9) . 2_565 ?
O1 Na1 Na1 80.87(6) . 2_565 ?
F1 Na1 Na1 58.41(6) 1_655 2_565 ?
O2 Na1 Na1 123.10(7) . 2_565 ?
P1 Na1 Na1 103.40(5) . 2_565 ?
P1 Na1 Na1 130.19(3) 2_564 2_565 ?
O1 Na1 Na1 76.71(6) 2_564 2_464 ?
O2 Na1 Na1 159.18(9) 2_565 2_464 ?
O11 Na1 Na1 70.32(9) . 2_464 ?
O1 Na1 Na1 84.94(6) . 2_464 ?
F1 Na1 Na1 102.99(7) 1_655 2_464 ?
O2 Na1 Na1 35.40(5) . 2_464 ?
P1 Na1 Na1 58.43(3) . 2_464 ?
P1 Na1 Na1 61.98(3) 2_564 2_464 ?
Na1 Na1 Na1 158.28(7) 2_565 2_464 ?
O1 Na1 Na1 167.58(7) 2_564 2_465 ?
O2 Na1 Na1 79.50(6) 2_565 2_465 ?
O11 Na1 Na1 71.97(8) . 2_465 ?
O1 Na1 Na1 31.22(5) . 2_465 ?
F1 Na1 Na1 103.54(7) 1_655 2_465 ?
O2 Na1 Na1 84.79(6) . 2_465 ?
P1 Na1 Na1 56.48(3) . 2_465 ?
P1 Na1 Na1 148.39(4) 2_564 2_465 ?
Na1 Na1 Na1 76.823(12) 2_565 2_465 ?
Na1 Na1 Na1 99.086(17) 2_464 2_465 ?
O1 Na1 Na1 32.46(5) 2_564 2_564 ?
O2 Na1 Na1 111.77(6) 2_565 2_564 ?
O11 Na1 Na1 124.38(9) . 2_564 ?
O1 Na1 Na1 127.69(8) . 2_564 ?
F1 Na1 Na1 58.05(6) 1_655 2_564 ?
O2 Na1 Na1 79.93(6) . 2_564 ?
P1 Na1 Na1 105.33(5) . 2_564 ?
P1 Na1 Na1 47.28(2) 2_564 2_564 ?
Na1 Na1 Na1 99.086(17) 2_565 2_564 ?
Na1 Na1 Na1 76.822(12) 2_464 2_564 ?
Na1 Na1 Na1 158.57(7) 2_465 2_564 ?
P1 O2 Na1 129.66(13) . 2_464 ?
P1 O2 Na1 87.07(10) . . ?
Na1 O2 Na1 102.65(9) 2_464 . ?
P1 F1 Na1 142.28(12) . 1_455 ?
P1 O1 Na1 127.30(11) . 2_465 ?
P1 O1 Na1 99.45(11) . . ?
Na1 O1 Na1 116.32(9) 2_465 . ?
 
_refine_diff_density_max    0.335
_refine_diff_density_min   -0.431
_refine_diff_density_rms    0.136



