# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_0709_3_0ma
_database_code_depnum_ccdc_archive 'CCDC 1872035'
_audit_update_record             
;
2019-04-26 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;

_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 H8 N2 O8 S2 Sb2'
_chemical_formula_weight         547.70

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   9.5730(7)
_cell_length_b                   11.5948(7)
_cell_length_c                   5.1311(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     569.54(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    462
_cell_measurement_theta_min      5.521
_cell_measurement_theta_max      52.441

_exptl_crystal_description       block-like
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    3.194
_exptl_crystal_F_000             512
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    5.202
_shelx_estimated_absorpt_T_min   0.408
_shelx_estimated_absorpt_T_max   0.454
_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      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            3778
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         2.759
_diffrn_reflns_theta_max         26.336
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.931
_reflns_number_total             1087
_reflns_number_gt                987
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.685
_reflns_Friedel_fraction_max     0.860
_reflns_Friedel_fraction_full    0.849

_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-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)+(0.0270P)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     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 380 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1087
_refine_ls_number_parameters     98
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0223
_refine_ls_wR_factor_ref         0.0554
_refine_ls_wR_factor_gt          0.0537
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001

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
Sb1 Sb 0.16783(4) 0.58335(3) 0.17349(17) 0.02151(15) Uani 1 1 d . . . . .
S1 S 0.21412(18) 0.36668(15) 0.7173(4) 0.0238(4) Uani 1 1 d . . . . .
F1 F 0.3690(4) 0.5735(3) 0.1498(18) 0.0272(11) Uani 1 1 d . . . . .
O1 O 0.3067(6) 0.4448(5) 0.5810(13) 0.0276(12) Uani 1 1 d . . . . .
N1 N 0.5094(7) 0.3456(6) 1.193(2) 0.0262(13) Uani 1 1 d D . . . .
O2 O 0.0952(5) 0.3316(4) 0.5590(12) 0.0283(12) Uani 1 1 d . . . . .
F2 F 0.1719(4) 0.6512(4) -0.1692(9) 0.0264(10) Uani 1 1 d . . . . .
O3 O 0.2965(6) 0.2631(5) 0.8061(13) 0.0310(13) Uani 1 1 d . . . . .
O4 O 0.1608(6) 0.4194(5) 0.9655(14) 0.0291(14) Uani 1 1 d . . . . .
H1 H 0.578(7) 0.403(6) 1.15(3) 0.03(2) Uiso 1 1 d D . . . .
H2 H 0.462(10) 0.324(9) 1.07(2) 0.04(3) Uiso 1 1 d . . . . .
H3 H 0.544(10) 0.274(9) 1.24(3) 0.05(3) Uiso 1 1 d . . . . .
H4 H 0.461(11) 0.381(9) 1.30(3) 0.05(4) 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
Sb1 0.0224(2) 0.0211(2) 0.0211(2) 0.0006(3) 0.0005(3) 0.00000(14)
S1 0.0241(7) 0.0220(7) 0.0253(12) -0.0011(8) -0.0002(9) 0.0011(6)
F1 0.0233(17) 0.0307(19) 0.028(3) 0.005(2) 0.002(3) 0.0002(14)
O1 0.031(3) 0.028(3) 0.023(3) 0.000(2) 0.002(2) -0.001(2)
N1 0.027(3) 0.028(3) 0.024(4) 0.005(4) -0.003(4) -0.001(2)
O2 0.023(3) 0.030(3) 0.032(3) -0.005(2) -0.002(2) 0.002(2)
F2 0.032(2) 0.029(2) 0.018(3) 0.002(2) 0.0001(18) 0.0037(16)
O3 0.037(3) 0.025(3) 0.030(3) 0.000(3) -0.008(2) 0.004(2)
O4 0.038(3) 0.025(3) 0.025(3) -0.001(2) 0.005(2) 0.001(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
Sb1 F2 1.927(5) . ?
Sb1 F1 1.933(4) . ?
Sb1 O4 2.181(6) 1_554 ?
Sb1 O3 2.219(6) 4_554 ?
S1 O1 1.447(6) . ?
S1 O2 1.456(6) . ?
S1 O4 1.502(7) . ?
S1 O3 1.507(6) . ?
N1 H1 0.96(6) . ?
N1 H2 0.83(12) . ?
N1 H3 0.92(11) . ?
N1 H4 0.82(12) . ?
O3 Sb1 2.219(6) 4_545 ?
O4 Sb1 2.181(6) 1_556 ?

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
F2 Sb1 F1 87.0(3) . . ?
F2 Sb1 O4 84.8(2) . 1_554 ?
F1 Sb1 O4 87.0(2) . 1_554 ?
F2 Sb1 O3 83.9(2) . 4_554 ?
F1 Sb1 O3 85.5(2) . 4_554 ?
O4 Sb1 O3 166.8(2) 1_554 4_554 ?
O1 S1 O2 112.6(4) . . ?
O1 S1 O4 111.3(3) . . ?
O2 S1 O4 108.7(3) . . ?
O1 S1 O3 108.9(3) . . ?
O2 S1 O3 110.8(3) . . ?
O4 S1 O3 104.2(4) . . ?
H1 N1 H2 114(10) . . ?
H1 N1 H3 116(7) . . ?
H2 N1 H3 96(10) . . ?
H1 N1 H4 101(9) . . ?
H2 N1 H4 111(9) . . ?
H3 N1 H4 120(10) . . ?
S1 O3 Sb1 137.4(4) . 4_545 ?
S1 O4 Sb1 139.4(4) . 1_556 ?

_refine_diff_density_max         0.508
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.114

_shelx_res_file                  
;

    mo_0709_3_0ma.res created by SHELXL-2014/7


TITL mo_0709_3_0ma_d.res in Pna2(1)
REM Old TITL mo_0709_3_0ma_a.res in Pnma
REM SHELXT solution in Pna2(1)
REM R1 0.050, Rweak 0.003, Alpha 0.039, Orientation a'=-a, b'=c, c'=b
REM Flack x = 0.009 ( 0.038 ) from Parsons' quotients
REM Formula found by SHELXT: N3 O F3 S2 Sb
CELL 0.71073 9.573 11.5948 5.1311 90 90 90
ZERR 2 0.0007 0.0007 0.0004 0 0 0
LATT -1
SYMM -X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,+Z
SYMM 0.5-X,0.5+Y,0.5+Z
SFAC N H O F S Sb
UNIT 4 16 16 8 4 4

L.S. 10
PLAN  20
ACTA
SIZE 0.03 0.1 0.18
TEMP -123.15
BOND $H
LIST 6
fmap 2
REM <olex2.extras>
REM <HklSrc "%.\\mo_0709_3_0ma.hkl">
REM </olex2.extras>
size 0.21 0.19 0.18
dfix 0.87 0.05 N1 H1
WGHT    0.027000
FVAR       0.50802
SB1   6    0.167832    0.583348    0.173493    11.00000    0.02238    0.02111 =
         0.02105    0.00057    0.00049    0.00000
S1    5    0.214118    0.366677    0.717258    11.00000    0.02409    0.02204 =
         0.02532   -0.00106   -0.00018    0.00114
F1    4    0.369031    0.573479    0.149840    11.00000    0.02334    0.03071 =
         0.02757    0.00473    0.00230    0.00018
O1    3    0.306701    0.444801    0.581023    11.00000    0.03128    0.02818 =
         0.02326    0.00038    0.00150   -0.00103
N1    1    0.509359    0.345584    1.193460    11.00000    0.02705    0.02767 =
         0.02395    0.00483   -0.00342   -0.00091
O2    3    0.095154    0.331620    0.559042    11.00000    0.02321    0.03018 =
         0.03158   -0.00498   -0.00156    0.00241
F2    4    0.171870    0.651186   -0.169215    11.00000    0.03208    0.02875 =
         0.01844    0.00248    0.00011    0.00367
O3    3    0.296453    0.263139    0.806147    11.00000    0.03718    0.02535 =
         0.03042    0.00001   -0.00755    0.00432
O4    3    0.160836    0.419429    0.965499    11.00000    0.03781    0.02496 =
         0.02457   -0.00112    0.00484    0.00093
H1    2    0.577542    0.402615    1.150156    11.00000    0.03000
H2    2    0.462338    0.323578    1.066884    11.00000    0.03737
H3    2    0.544236    0.273923    1.236046    11.00000    0.04701
H4    2    0.460950    0.381480    1.298706    11.00000    0.04773
HKLF 4

REM  mo_0709_3_0ma_d.res in Pna2(1)
REM R1 =  0.0223 for     987 Fo > 4sig(Fo)  and  0.0261 for all    1087 data
REM     98 parameters refined using      2 restraints

END

WGHT      0.0235      0.0000

REM Highest difference peak  0.508,  deepest hole -0.531,  1-sigma level  0.114
Q1    1   0.0773  0.5901  0.0268  11.00000  0.05    0.51
Q2    1   0.0751  0.5807  0.3184  11.00000  0.05    0.46
Q3    1   0.2616  0.5816  0.3265  11.00000  0.05    0.42
Q4    1   0.0996  0.5359  0.1002  11.00000  0.05    0.37
Q5    1  -0.0137  0.4986  1.0747  11.00000  0.05    0.37
Q6    1   0.3732  0.4303  0.6681  11.00000  0.05    0.35
Q7    1   0.0330  0.3487  0.5705  11.00000  0.05    0.34
Q8    1   0.6670  0.2484  1.1720  11.00000  0.05    0.34
Q9    1   0.0346  0.4256  0.8610  11.00000  0.05    0.34
Q10   1   0.0499  0.6129 -0.3614  11.00000  0.05    0.33
Q11   1   0.0420  0.5926 -0.4215  11.00000  0.05    0.32
Q12   1   0.3868  0.3509  1.1949  11.00000  0.05    0.32
Q13   1   0.0405  0.4313  0.4702  11.00000  0.05    0.32
Q14   1   0.3311  0.5114  0.6477  11.00000  0.05    0.31
Q15   1   0.0069  0.5083  0.7756  11.00000  0.05    0.31
Q16   1   0.1190  0.2442  0.5702  11.00000  0.05    0.30
Q17   1   0.2601  0.5800  0.0108  11.00000  0.05    0.30
Q18   1   0.3573  0.4707  0.1553  11.00000  0.05    0.29
Q19   1   0.4988  0.1400  1.2852  11.00000  0.05    0.29
Q20   1   0.5261  0.4873  1.1777  11.00000  0.05    0.28
;
_shelx_res_checksum              57205
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_mo_0123_6_0ma
_database_code_depnum_ccdc_archive 'CCDC 1906990'
_audit_update_record             
;
2019-04-01 deposited with the CCDC.	2020-03-26 downloaded from the CCDC.
;

_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            'F H6 N O5 P Sb'
_chemical_formula_weight         271.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
P P 0.1023 0.0942 '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'
Sb Sb -0.5866 1.5461 '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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   6.5374(4)
_cell_length_b                   6.5425(5)
_cell_length_c                   8.3743(6)
_cell_angle_alpha                68.272(3)
_cell_angle_beta                 68.966(3)
_cell_angle_gamma                89.938(4)
_cell_volume                     306.95(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5865
_cell_measurement_theta_min      5.677
_cell_measurement_theta_max      56.629

_exptl_crystal_description       flakelike
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.941
_exptl_crystal_F_000             256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.735
_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      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9316
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.838
_diffrn_reflns_theta_max         28.350
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1541
_reflns_number_gt                1400
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_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)+(0.0753P)²+0.6096P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1541
_refine_ls_number_parameters     106
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0948
_refine_ls_wR_factor_gt          0.0910
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.003
_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
Sb1 Sb 0.27454(5) 0.77565(5) 0.44372(4) 0.01015(14) Uani 1 1 d . . . . .
P1 P 0.2497(2) 0.25022(19) 0.4996(2) 0.0100(2) Uani 1 1 d . . . . .
F1 F 0.3973(5) 0.9030(5) 0.1748(4) 0.0144(6) Uani 1 1 d . . . . .
O1 O 0.3710(6) 0.2490(6) 0.6277(5) 0.0133(7) Uani 1 1 d . . . . .
O2 O 0.3679(6) 0.1300(6) 0.3727(5) 0.0126(7) Uani 1 1 d . . . . .
O3 O 0.2485(6) 0.4912(5) 0.3742(5) 0.0121(7) Uani 1 1 d . . . . .
O4 O 0.0104(6) 0.1310(6) 0.6258(5) 0.0140(7) Uani 1 1 d . . . . .
N1 N 0.7195(8) 0.3486(9) 0.0131(7) 0.0182(9) Uani 1 1 d D . . . .
O5 O 0.1482(8) 0.2278(8) 0.9962(7) 0.0293(10) Uani 1 1 d D . . . .
H1 H 0.632(11) 0.263(11) 0.115(8) 0.03(2) Uiso 1 1 d D . . . .
H2 H 0.708(17) 0.326(17) -0.073(10) 0.05(3) Uiso 1 1 d D . . . .
H5 H 0.134(19) 0.123(15) 1.113(10) 0.07(3) Uiso 1 1 d D . . . .
H6 H 0.232(17) 0.244(19) 0.871(9) 0.08(4) Uiso 1 1 d D . . . .
H3 H 0.832(11) 0.277(14) 0.009(13) 0.04(2) Uiso 1 1 d D . . . .
H4 H 0.73(2) 0.486(10) -0.001(19) 0.10(5) Uiso 1 1 d 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
Sb1 0.0130(2) 0.00821(19) 0.0093(2) -0.00383(13) -0.00402(13) 0.00125(12)
P1 0.0120(6) 0.0077(5) 0.0113(6) -0.0046(4) -0.0049(4) 0.0013(4)
F1 0.0187(14) 0.0135(13) 0.0093(14) -0.0040(12) -0.0039(12) 0.0016(11)
O1 0.0147(17) 0.0142(16) 0.0126(17) -0.0055(14) -0.0069(14) 0.0025(13)
O2 0.0156(17) 0.0087(16) 0.0129(17) -0.0057(14) -0.0032(14) 0.0012(12)
O3 0.0201(17) 0.0074(15) 0.0110(17) -0.0042(13) -0.0080(14) 0.0038(13)
O4 0.0115(16) 0.0127(16) 0.0144(18) -0.0037(14) -0.0031(14) -0.0010(12)
N1 0.019(2) 0.023(2) 0.012(2) -0.0075(19) -0.0046(19) -0.0018(18)
O5 0.034(3) 0.026(2) 0.027(2) -0.009(2) -0.012(2) 0.0089(18)

_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
Sb1 F1 1.930(3) . ?
Sb1 O4 2.167(4) 2_566 ?
Sb1 O3 2.169(3) . ?
Sb1 O2 2.196(3) 1_565 ?
Sb1 O1 2.198(4) 2_666 ?
P1 O3 1.539(3) . ?
P1 O2 1.540(4) . ?
P1 O4 1.542(4) . ?
P1 O1 1.544(4) . ?
O1 Sb1 2.198(3) 2_666 ?
O2 Sb1 2.196(3) 1_545 ?
O4 Sb1 2.167(3) 2_566 ?

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 Sb1 O4 76.53(14) . 2_566 ?
F1 Sb1 O3 76.68(13) . . ?
O4 Sb1 O3 87.35(13) 2_566 . ?
F1 Sb1 O2 76.61(13) . 1_565 ?
O4 Sb1 O2 86.90(13) 2_566 1_565 ?
O3 Sb1 O2 153.29(14) . 1_565 ?
F1 Sb1 O1 76.66(13) . 2_666 ?
O4 Sb1 O1 153.19(15) 2_566 2_666 ?
O3 Sb1 O1 87.02(13) . 2_666 ?
O2 Sb1 O1 86.46(13) 1_565 2_666 ?
O3 P1 O2 108.0(2) . . ?
O3 P1 O4 110.3(2) . . ?
O2 P1 O4 110.4(2) . . ?
O3 P1 O1 110.1(2) . . ?
O2 P1 O1 110.6(2) . . ?
O4 P1 O1 107.5(2) . . ?
P1 O1 Sb1 123.2(2) . 2_666 ?
P1 O2 Sb1 123.3(2) . 1_545 ?
P1 O3 Sb1 124.1(2) . . ?
P1 O4 Sb1 123.6(2) . 2_566 ?

_refine_diff_density_max         3.215
_refine_diff_density_min         -1.805
_refine_diff_density_rms         0.258

_shelx_res_file                  
;

    mo_0123_6_0ma.res created by SHELXL-2014/7


TITL mo_0123_6_0ma_a.res in P-1
REM Old TITL mo_0123_6_0ma in P1
REM SHELXT solution in P-1: R1 0.047, Rweak 0.008, Alpha 0.034
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: P O6 Sb F
CELL 0.71073 6.5374 6.5425 8.3743 68.272 68.966 89.938
ZERR 2 0.0004 0.0005 0.0006 0.003 0.003 0.004
LATT 1
SFAC P O Sb F N H
UNIT 2 10 2 2 2 12

L.S. 10
PLAN  20
ACTA
TEMP -123.17
BOND
FMAP 2
list 4
REM <olex2.extras>
REM <HklSrc "%.\\mo_0123_6_0ma.hkl">
REM </olex2.extras>
DFIX 0.87 0.05 N1 H1
DFIX 0.87 0.05 N1 H2
DFIX 0.87 0.05 N1 H3
DFIX 0.87 0.05 N1 H4
DFIX 0.95 0.05 O5 H5
DFIX 0.95 0.05 O5 H6
WGHT    0.075346    0.609596
FVAR       0.87144
SB1   3    0.274536    0.775655    0.443717    11.00000    0.01296    0.00821 =
         0.00935   -0.00383   -0.00402    0.00125
P1    1    0.249688    0.250218    0.499612    11.00000    0.01200    0.00772 =
         0.01127   -0.00455   -0.00491    0.00135
F1    4    0.397273    0.902990    0.174758    11.00000    0.01868    0.01352 =
         0.00930   -0.00397   -0.00393    0.00161
O1    2    0.370957    0.248999    0.627709    11.00000    0.01471    0.01417 =
         0.01264   -0.00554   -0.00686    0.00249
O2    2    0.367859    0.130012    0.372748    11.00000    0.01557    0.00875 =
         0.01285   -0.00567   -0.00320    0.00120
O3    2    0.248476    0.491203    0.374205    11.00000    0.02008    0.00744 =
         0.01104   -0.00423   -0.00796    0.00385
O4    2    0.010411    0.130975    0.625832    11.00000    0.01149    0.01273 =
         0.01443   -0.00366   -0.00315   -0.00097
N1    5    0.719498    0.348598    0.013120    11.00000    0.01900    0.02251 =
         0.01238   -0.00753   -0.00456   -0.00180
O5    2    0.148181    0.227808    0.996247    11.00000    0.03435    0.02622 =
         0.02654   -0.00887   -0.01249    0.00894
H1    6    0.632143    0.263229    0.115402    11.00000    0.02723
H2    6    0.707651    0.325950   -0.072598    11.00000    0.05241
H5    6    0.133599    0.122886    1.112594    11.00000    0.07314
H6    6    0.231621    0.243940    0.870881    11.00000    0.07688
H3    6    0.832156    0.277423    0.008717    11.00000    0.03982
H4    6    0.732292    0.486167   -0.000963    11.00000    0.09806
HKLF 4

REM  mo_0123_6_0ma_a.res in P-1
REM R1 =  0.0344 for    1400 Fo > 4sig(Fo)  and  0.0396 for all    1541 data
REM    106 parameters refined using      6 restraints

END

WGHT      0.0655      0.5687

REM Highest difference peak  3.215,  deepest hole -1.805,  1-sigma level  0.258
Q1    1   0.4017  0.7620  0.4394  11.00000  0.05    3.22
Q2    1   0.1453  0.7468  0.4462  11.00000  0.05    2.02
Q3    1   0.3030  0.9108  0.4414  11.00000  0.05    1.58
Q4    1   0.2323  0.6541  0.4435  11.00000  0.05    1.30
Q5    1   0.1608  0.6663  0.6822  11.00000  0.05    0.92
Q6    1   0.0005  0.2453  1.0352  11.00000  0.05    0.86
Q7    1   0.2627  0.3468  0.9892  11.00000  0.05    0.76
Q8    1  -0.1124  0.1336  0.6438  11.00000  0.05    0.74
Q9    1   0.3317  0.7097  0.3088  11.00000  0.05    0.73
Q10   1   0.5087  0.9877  0.1787  11.00000  0.05    0.66
Q11   1   0.1209  0.2595  0.5196  11.00000  0.05    0.65
Q12   1   0.4382 -0.0143  0.3221  11.00000  0.05    0.64
Q13   1   0.1925  0.2028  0.6199  11.00000  0.05    0.62
Q14   1   0.7893  0.4050 -0.0213  11.00000  0.05    0.62
Q15   1   0.5120  0.0785  0.4393  11.00000  0.05    0.62
Q16   1   0.1142  0.6151  0.5648  11.00000  0.05    0.61
Q17   1   0.5311  0.8774  0.1652  11.00000  0.05    0.60
Q18   1   0.4956  0.0976  0.3723  11.00000  0.05    0.60
Q19   1   0.3607  0.2565  0.5121  11.00000  0.05    0.59
Q20   1   0.7090  0.3449 -0.0378  11.00000  0.05    0.58
;
_shelx_res_checksum              37425
