# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_MgTFA2_100k
_database_code_depnum_ccdc_archive 'CCDC 1443800'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H8 F6 Mg O8'
_chemical_formula_weight         322.41

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'
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'

_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                   8.0985(9)
_cell_length_b                   9.0458(11)
_cell_length_c                   9.3604(11)
_cell_angle_alpha                88.324(6)
_cell_angle_beta                 65.021(5)
_cell_angle_gamma                71.131(6)
_cell_volume                     583.55(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9923
_cell_measurement_theta_min      3.1871
_cell_measurement_theta_max      24.9688

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_F_000             324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.269
_shelx_estimated_absorpt_T_min   0.948
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   'TWINABS (Bruker, 2012)'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            34199
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.398
_diffrn_reflns_theta_max         25.251
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             34199
_reflns_number_gt                29303
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0299P)²+0.1114P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         34199
_refine_ls_number_parameters     197
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0775
_refine_ls_wR_factor_gt          0.0737
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.037
_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
Mg1 Mg 0.26844(11) 0.59719(9) 0.39021(9) 0.0120(2) Uani 1 1 d . . . . .
O1W O 0.3082(3) 0.7415(2) 0.2184(2) 0.0179(4) Uani 1 1 d D . . . .
H1 H 0.275(4) 0.835(3) 0.247(3) 0.027 Uiso 1 1 d D U . . .
H1' H 0.280(4) 0.726(3) 0.151(3) 0.027 Uiso 1 1 d D U . . .
O2W O -0.0307(2) 0.7107(2) 0.50527(19) 0.0140(4) Uani 1 1 d D . . . .
H2B H -0.083(3) 0.808(3) 0.512(3) 0.021 Uiso 1 1 d D U . . .
H2A H -0.084(4) 0.677(3) 0.589(3) 0.021 Uiso 1 1 d D U . . .
O2W' O 0.5641(2) 0.47703(19) 0.2891(2) 0.0140(4) Uani 1 1 d D . . . .
H2A' H 0.603(4) 0.392(3) 0.318(3) 0.021 Uiso 1 1 d D U . . .
H2B' H 0.627(3) 0.470(3) 0.190(3) 0.021 Uiso 1 1 d D U . . .
O3W O 0.2423(3) 0.4455(2) 0.5576(2) 0.0153(4) Uani 1 1 d D . . . .
H3 H 0.294(4) 0.438(3) 0.613(3) 0.023 Uiso 1 1 d D U . . .
H3' H 0.187(4) 0.385(3) 0.567(3) 0.023 Uiso 1 1 d D U . . .
O1 O 0.3070(2) 0.74446(18) 0.53310(18) 0.0133(4) Uani 1 1 d . . . . .
O2 O 0.2138(2) 0.97713(18) 0.44734(19) 0.0186(4) Uani 1 1 d . . . . .
C1 C 0.2619(3) 0.8914(3) 0.5382(3) 0.0142(6) Uani 1 1 d . . . . .
C2 C 0.2612(4) 0.9744(3) 0.6795(3) 0.0208(6) Uani 1 1 d . . . . .
F1 F 0.3194(2) 1.09865(16) 0.64015(18) 0.0298(4) Uani 1 1 d . . . . .
F2 F 0.0818(2) 1.02927(19) 0.79596(18) 0.0415(5) Uani 1 1 d . . . . .
F3 F 0.3734(3) 0.88175(17) 0.7389(2) 0.0406(5) Uani 1 1 d . . . . .
O1' O 0.2219(2) 0.44631(18) 0.25627(18) 0.0138(4) Uani 1 1 d . . . . .
O2' O 0.2611(2) 0.55261(19) 0.02979(19) 0.0180(4) Uani 1 1 d . . . . .
C1' C 0.2339(3) 0.4505(3) 0.1174(3) 0.0135(6) Uani 1 1 d . . . . .
C2' C 0.2082(4) 0.3067(3) 0.0556(3) 0.0197(6) Uani 1 1 d . . . . .
F1' F 0.2213(2) 0.31384(19) -0.09043(16) 0.0357(4) Uani 1 1 d . . . . .
F2' F 0.3402(2) 0.17348(17) 0.0537(2) 0.0390(5) Uani 1 1 d . . . . .
F3' F 0.0351(2) 0.29730(18) 0.14829(17) 0.0329(4) 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
Mg1 O1W 2.0259(18) . ?
Mg1 O3W 2.0405(18) . ?
Mg1 O2W' 2.0672(18) . ?
Mg1 O2W 2.0819(18) . ?
Mg1 O1 2.0946(16) . ?
Mg1 O1' 2.0995(16) . ?
O1W H1 0.82(2) . ?
O1W H1' 0.79(2) . ?
O2W H2B 0.83(2) . ?
O2W H2A 0.82(2) . ?
O2W' H2A' 0.81(2) . ?
O2W' H2B' 0.84(2) . ?
O3W H3 0.78(2) . ?
O3W H3' 0.79(2) . ?
O1 C1 1.256(3) . ?
O2 C1 1.234(3) . ?
C1 C2 1.537(3) . ?
C2 F3 1.321(3) . ?
C2 F2 1.331(3) . ?
C2 F1 1.339(3) . ?
O1' C1' 1.262(3) . ?
O2' C1' 1.228(3) . ?
C1' C2' 1.546(3) . ?
C2' F2' 1.322(3) . ?
C2' F1' 1.327(3) . ?
C2' F3' 1.331(3) . ?

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
O1W Mg1 O3W 177.23(8) . . ?
O1W Mg1 O2W' 89.56(8) . . ?
O3W Mg1 O2W' 87.69(8) . . ?
O1W Mg1 O2W 94.14(8) . . ?
O3W Mg1 O2W 88.62(8) . . ?
O2W' Mg1 O2W 176.20(8) . . ?
O1W Mg1 O1 91.11(7) . . ?
O3W Mg1 O1 89.11(7) . . ?
O2W' Mg1 O1 88.62(7) . . ?
O2W Mg1 O1 90.42(7) . . ?
O1W Mg1 O1' 91.17(7) . . ?
O3W Mg1 O1' 88.67(7) . . ?
O2W' Mg1 O1' 92.60(7) . . ?
O2W Mg1 O1' 88.22(7) . . ?
O1 Mg1 O1' 177.42(7) . . ?
Mg1 O1W H1 117.0(19) . . ?
Mg1 O1W H1' 115.9(19) . . ?
H1 O1W H1' 113(3) . . ?
Mg1 O2W H2B 123.1(17) . . ?
Mg1 O2W H2A 113.8(18) . . ?
H2B O2W H2A 111(2) . . ?
Mg1 O2W' H2A' 117.9(18) . . ?
Mg1 O2W' H2B' 118.4(17) . . ?
H2A' O2W' H2B' 109(2) . . ?
Mg1 O3W H3 122.2(19) . . ?
Mg1 O3W H3' 123.3(19) . . ?
H3 O3W H3' 114(3) . . ?
C1 O1 Mg1 126.12(15) . . ?
O2 C1 O1 128.5(2) . . ?
O2 C1 C2 116.3(2) . . ?
O1 C1 C2 115.1(2) . . ?
F3 C2 F2 107.6(2) . . ?
F3 C2 F1 107.1(2) . . ?
F2 C2 F1 106.53(19) . . ?
F3 C2 C1 113.5(2) . . ?
F2 C2 C1 110.0(2) . . ?
F1 C2 C1 111.8(2) . . ?
C1' O1' Mg1 129.90(15) . . ?
O2' C1' O1' 128.4(2) . . ?
O2' C1' C2' 118.1(2) . . ?
O1' C1' C2' 113.5(2) . . ?
F2' C2' F1' 107.52(19) . . ?
F2' C2' F3' 107.3(2) . . ?
F1' C2' F3' 107.10(19) . . ?
F2' C2' C1' 111.51(19) . . ?
F1' C2' C1' 112.4(2) . . ?
F3' C2' C1' 110.80(19) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 O2 -11.7(4) . . . . ?
Mg1 O1 C1 C2 166.26(15) . . . . ?
O2 C1 C2 F3 -157.8(2) . . . . ?
O1 C1 C2 F3 24.0(3) . . . . ?
O2 C1 C2 F2 81.7(3) . . . . ?
O1 C1 C2 F2 -96.5(2) . . . . ?
O2 C1 C2 F1 -36.5(3) . . . . ?
O1 C1 C2 F1 145.3(2) . . . . ?
Mg1 O1' C1' O2' -6.5(4) . . . . ?
Mg1 O1' C1' C2' 174.10(14) . . . . ?
O2' C1' C2' F2' 121.3(2) . . . . ?
O1' C1' C2' F2' -59.2(3) . . . . ?
O2' C1' C2' F1' 0.5(3) . . . . ?
O1' C1' C2' F1' 180.0(2) . . . . ?
O2' C1' C2' F3' -119.3(2) . . . . ?
O1' C1' C2' F3' 60.2(3) . . . . ?

_refine_diff_density_max         0.263
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.044


#END MgTFA2_100K   

# start Validation Reply Form
_vrf_PLAT234_MgTFA2_300K         
;
PROBLEM: Large Hirshfeld Difference F1B -- C2 .. 0.16 Ang.
RESPONSE: Atoms F1, F2 and F3 were refined in three split positions to model 
most of the observed disordered electron density and the third compomponent
of the model, with very low occupancy, shows some slightly distorted ADPs that
produce this error.
;
_vrf_PLAT250_MgTFA2_300K         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.4 Note
RESPONSE: The disorder observed in F1, F2 and F3 strongly influences the
average U(i,j) tensor producing this deviation from the expected isotropic
behaviour.
;
_vrf_PLAT480_MgTFA2_300K         
;
PROBLEM: Long H...A H-Bond Reported H2B .. F1 .. 2.72 Ang.
RESPONSE: This weak interaction is important for comparison purposes with
the structures described at lower temperatures.
;
_vrf_PLAT480_MgTFA2_200K         
;
PROBLEM: Long H...A H-Bond Reported H2B .. F1 .. 2.64 Ang.
RESPONSE: This weak interaction is important for comparison purposes with
the structures described at lower temperatures.
;
_vrf_PLAT905_MgTFA2_200K         
;
PROBLEM: Negative K value in the Analysis of Variance ... -0.409 Report
RESPONSE: Data collection at 200 K showed significantly anisotropic peak
shapes, probably coming from the non-perfect reconstruction of the original
single crystal after a low temperature phase transition where splitting of the
crystal into two-domains was observed. Integration of intensities was affected
by this anisotropy and very low intensity reflections show abnormally low K 
values. 
;
_vrf_DIFMN03_MgTFA2_160K_tri     
;
PROBLEM: The minimum difference density is < -0.1*ZMAX*0.75
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_DIFMX02_MgTFA2_160K_tri     
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_RFACG01_MgTFA2_160K_tri     
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_RFACR01_MgTFA2_160K_tri     
;
PROBLEM: The value of the weighted R factor is > 0.25
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_PLAT082_MgTFA2_160K_tri     
;
PROBLEM: High R1 Value .................................. 0.11 Report
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_PLAT084_MgTFA2_160K_tri     
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.31 Report
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_PLAT213_MgTFA2_160K_tri     
;
PROBLEM: Atom F1' has ADP max-min Ratio ..... 3.4 prolat
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_PLAT250_MgTFA2_160K_tri     
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.7 Note
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_PLAT480_MgTFA2_160K_tri     
;
PROBLEM: Long H...A H-Bond Reported H2A .. F3' .. 2.58 Ang.
RESPONSE: This weak interaction is important for comparison purposes with
the structures described at lower temperatures.

;
_vrf_PLAT905_MgTFA2_160K_tri     
;
PROBLEM: Negative K value in the Analysis of Variance ... -1.064 Report
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_PLAT911_MgTFA2_160K_tri     
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 144 Report
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a two-domain twin of triclinic components was barely 
sucessful, the dataset has low redundancy due to the large number of failed 
reflections and is full of inconsistent equivalents, with a high R(int) and 
R(sigma). The low quality of the data prevents the triclinic structural model 
to accurately represent the observed electron density, that contains a large 
number of peaks away from expected atom positions. This explains this and most 
of the other errors detected by checkcif. 
;
_vrf_RFACG01_MgTFA2_160k_mon     
;
PROBLEM: The value of the R factor is > 0.10
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_RFACR01_MgTFA2_160k_mon     
;
PROBLEM: The value of the weighted R factor is > 0.25
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT029_MgTFA2_160k_mon     
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.967 Note
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT031_MgTFA2_160k_mon     
;
PROBLEM: Refined Extinction Parameter within Range ...... 3.000 Sigma
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. SHELXL refinement program requests the inclusion of this parameter
in the final model if supressed.
;
_vrf_PLAT082_MgTFA2_160k_mon     
;
PROBLEM: High R1 Value .................................. 0.11 Report
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT084_MgTFA2_160k_mon     
;
PROBLEM: High wR2 Value (i.e. > 0.25) ................... 0.32 Report
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT250_MgTFA2_160k_mon     
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.3 Note
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT906_MgTFA2_160k_mon     
;
PROBLEM: Large K value in the Analysis of Variance ...... 9.236 Check
RESPONSE: It is well known that integration of low intensity data is usually
underestimated due to an overestimation of the background in 2D detectors.
Additionally the available data is of low quality (see other responses).
This explains this error that only affects a small group of the lowest
observed intensities, not significant for the structural model.
;
_vrf_PLAT911_MgTFA2_160k_mon     
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 36 Report
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT976_MgTFA2_160k_mon     
;
PROBLEM: Check Calcd Residual Density 0.85A From O2W -0.41 eA-3
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT978_MgTFA2_160k_mon     
;
PROBLEM: Number C-C Bonds with Positive Residual Density 0 Note
RESPONSE: The phase transition form monoclinic C2/c to trilclinic P-1 
structure seems to occur at this temperature. Integration of the diffraction 
frames considering a single monoclinic crystal was barely sucessful. Most of 
the reflections show clear splitting and peakshapes vary strongly in different 
frames of the same run. The dataset is full of inconsistent equivalents, with 
a high R(int) and R(sigma). The low quality of the data also prevents the 
monoclinic structural model to accurately represent the observed electron 
density, that contains a large number of peaks away from expected atomic 
positions. This explains this and most of the other errors detected by 
checkcif.
;
_vrf_PLAT340_MgTFA2_143k         
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.005 Ang.
RESPONSE: The available data, obtained from the integration of a two-component
twin does not allow for better bond precision.
;
_vrf_PLAT911_MgTFA2_143k         
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 15 Report
RESPONSE: The available data comes from an integratio of a dataset obtained
with a strategy designed to collect redundant data for a monoclinic compound
observed above 160K, this made some reflections been missing for a triclinic
dataset. A better model for the triclinic structure was obtained at 100K.
;
_vrf_PLAT250_MgTFA2_100k         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.1 Note
RESPONSE: The large ADPs observed for F atoms strongly influence the average
U(i,j) tensor and a slight deviation of these ADPs, that contain a small,
unmodelled, disorder component (as observed at higher temperatures above
the phase transition), produces this aparent error.
;
_vrf_PLAT417_MgTFA2_100k         
;
PROBLEM: Short Inter D-H..H-D H2A .. H3' .. 2.13 Ang.
RESPONSE: H-atom positions were determined from the difference Fourier maps
but were modelled as riding on the parent O atom using dfix and dang to 
define initial reasonable O-H bond distances and H-O-H bond angles. The
subsequent rigid refinement leads to H atom positions that may not be
perfectly consistent with the real positions in the crysta. This may explain
this error in the H2A and/or H3' atom positions.
;
_vrf_PLAT911_MgTFA2_100k         
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 21 Report
RESPONSE: The low-temperature system prevented the orientation of the crystal
in certain directions to prevent freezing of the mechanical system that made 
some reflections to be impossible to measure therefore are missing in the
dataset.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_MgTFA2_300K
_database_code_depnum_ccdc_archive 'CCDC 1505493'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        magnesium(ii)-tetraaquo-bistrifluoroacetate
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mg, 2 C2 O2 F3, 4 H2 O'
_chemical_formula_sum            'C4 H8 F6 Mg O8'
_chemical_formula_weight         322.41

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-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                   13.2064(6)
_cell_length_b                   12.6063(6)
_cell_length_c                   8.3132(4)
_cell_angle_alpha                90
_cell_angle_beta                 118.849(2)
_cell_angle_gamma                90
_cell_volume                     1212.24(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9955
_cell_measurement_theta_min      2.395
_cell_measurement_theta_max      33.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.259
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            31593
_diffrn_reflns_av_unetI/netI     0.0073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.390
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1511
_reflns_number_gt                1313
_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          ', Twin'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0433P)²+0.3461P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0059(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1511
_refine_ls_number_parameters     149
_refine_ls_number_restraints     100
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0266
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0741
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.178
_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
Mg1 Mg 0.5000 0.60404(3) 0.7500 0.03179(15) Uani 1 2 d S T P . .
O1W O 0.5000 0.76438(9) 0.7500 0.0574(3) Uani 1 2 d S T P . .
H1 H 0.4445 0.7985 0.7448 0.086 Uiso 1 1 d R U . . .
O2W O 0.39192(6) 0.59973(5) 0.46705(10) 0.03848(19) Uani 1 1 d . . . . .
H2A H 0.3648 0.5400 0.4249 0.058 Uiso 1 1 d R U . . .
H2B H 0.3447 0.6488 0.4153 0.058 Uiso 1 1 d R U . . .
O3W O 0.5000 0.44119(8) 0.7500 0.0414(3) Uani 1 2 d S T P . .
H3 H 0.5252 0.4058 0.6938 0.062 Uiso 1 1 d R U . . .
O1 O 0.35844(6) 0.59883(5) 0.79884(11) 0.0401(2) Uani 1 1 d . . . . .
O2 O 0.28049(7) 0.75922(7) 0.70991(14) 0.0576(3) Uani 1 1 d . . . . .
C1 C 0.28211(8) 0.66778(9) 0.75993(14) 0.0398(2) Uani 1 1 d D . . . .
C2 C 0.17672(12) 0.63029(13) 0.7767(2) 0.0640(4) Uani 1 1 d D U . . .
F1 F 0.1259(5) 0.7150(3) 0.8122(11) 0.0847(14) Uani 0.533(11) 1 d D U P A 1
F2 F 0.1018(4) 0.5850(6) 0.6201(9) 0.1192(19) Uani 0.533(11) 1 d D U P A 1
F3 F 0.2014(5) 0.5654(5) 0.9080(12) 0.100(2) Uani 0.533(11) 1 d D U P A 1
F1A F 0.0920(5) 0.6945(6) 0.7110(18) 0.080(3) Uani 0.302(11) 1 d D U P A 2
F2A F 0.1384(9) 0.5376(8) 0.6998(17) 0.099(3) Uani 0.302(11) 1 d D U P A 2
F3A F 0.2180(10) 0.6064(10) 0.9613(11) 0.097(3) Uani 0.302(11) 1 d D U P A 2
F1B F 0.1642(13) 0.6695(17) 0.906(2) 0.115(5) Uani 0.165(7) 1 d D U P A 3
F2B F 0.0796(7) 0.6452(12) 0.6172(14) 0.075(3) Uani 0.165(7) 1 d D U P A 3
F3B F 0.1728(9) 0.5229(8) 0.801(2) 0.075(3) Uani 0.165(7) 1 d D U P A 3


_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 O1W 2.0212(12) . ?
Mg1 O3W 2.0530(11) . ?
Mg1 O2W 2.0816(7) 2_656 ?
Mg1 O2W 2.0816(7) . ?
Mg1 O1 2.0969(7) . ?
Mg1 O1 2.0969(7) 2_656 ?
O1W H1 0.8321 . ?
O2W H2A 0.8352 . ?
O2W H2B 0.8355 . ?
O3W H3 0.8239 . ?
O1 C1 1.2496(12) . ?
O2 C1 1.2221(14) . ?
C1 C2 1.5384(16) . ?
C2 F1B 1.262(7) . ?
C2 F1A 1.272(5) . ?
C2 F3 1.274(5) . ?
C2 F2A 1.311(7) . ?
C2 F2 1.325(5) . ?
C2 F2B 1.341(8) . ?
C2 F1 1.367(4) . ?
C2 F3B 1.372(10) . ?
C2 F3A 1.392(8) . ?

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
O1W Mg1 O3W 180.0 . . ?
O1W Mg1 O2W 91.50(2) . 2_656 ?
O3W Mg1 O2W 88.50(2) . 2_656 ?
O1W Mg1 O2W 91.50(2) . . ?
O3W Mg1 O2W 88.50(2) . . ?
O2W Mg1 O2W 177.01(4) 2_656 . ?
O1W Mg1 O1 91.80(2) . . ?
O3W Mg1 O1 88.20(2) . . ?
O2W Mg1 O1 88.26(3) 2_656 . ?
O2W Mg1 O1 91.64(3) . . ?
O1W Mg1 O1 91.80(2) . 2_656 ?
O3W Mg1 O1 88.20(2) . 2_656 ?
O2W Mg1 O1 91.64(3) 2_656 2_656 ?
O2W Mg1 O1 88.26(3) . 2_656 ?
O1 Mg1 O1 176.41(4) . 2_656 ?
Mg1 O1W H1 121.1 . . ?
Mg1 O2W H2A 114.8 . . ?
Mg1 O2W H2B 119.8 . . ?
H2A O2W H2B 112.9 . . ?
Mg1 O3W H3 122.8 . . ?
C1 O1 Mg1 127.68(7) . . ?
O2 C1 O1 128.59(10) . . ?
O2 C1 C2 116.90(10) . . ?
O1 C1 C2 114.51(10) . . ?
F1A C2 F2A 107.8(4) . . ?
F3 C2 F2 109.0(3) . . ?
F1B C2 F2B 109.3(8) . . ?
F3 C2 F1 105.4(3) . . ?
F2 C2 F1 109.7(3) . . ?
F1B C2 F3B 103.4(8) . . ?
F2B C2 F3B 101.3(6) . . ?
F1A C2 F3A 114.0(5) . . ?
F2A C2 F3A 101.4(5) . . ?
F1B C2 C1 116.9(5) . . ?
F1A C2 C1 114.4(3) . . ?
F3 C2 C1 114.0(2) . . ?
F2A C2 C1 112.5(3) . . ?
F2 C2 C1 108.8(2) . . ?
F2B C2 C1 110.1(4) . . ?
F1 C2 C1 109.8(2) . . ?
F3B C2 C1 114.5(4) . . ?
F3A C2 C1 106.0(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 O2 -11.70(18) . . . . ?
Mg1 O1 C1 C2 167.71(9) . . . . ?
O2 C1 C2 F1B -70.0(13) . . . . ?
O1 C1 C2 F1B 110.5(13) . . . . ?
O2 C1 C2 F1A 9.6(7) . . . . ?
O1 C1 C2 F1A -169.9(7) . . . . ?
O2 C1 C2 F3 -145.1(5) . . . . ?
O1 C1 C2 F3 35.4(5) . . . . ?
O2 C1 C2 F2A 133.1(7) . . . . ?
O1 C1 C2 F2A -46.4(7) . . . . ?
O2 C1 C2 F2 93.0(4) . . . . ?
O1 C1 C2 F2 -86.5(4) . . . . ?
O2 C1 C2 F2B 55.4(8) . . . . ?
O1 C1 C2 F2B -124.1(8) . . . . ?
O2 C1 C2 F1 -27.1(4) . . . . ?
O1 C1 C2 F1 153.4(4) . . . . ?
O2 C1 C2 F3B 168.8(8) . . . . ?
O1 C1 C2 F3B -10.6(8) . . . . ?
O2 C1 C2 F3A -116.9(6) . . . . ?
O1 C1 C2 F3A 63.6(6) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2W H2A O1 0.84 2.02 2.7963(10) 154.2 6_565
O2W H2B O2 0.84 1.87 2.6978(10) 170.1 7_566
O1W H1 O2 0.83 2.10 2.7545(8) 135.1 .
O3W H3 O2W 0.82 2.10 2.8363(7) 149.0 5_666
O1W H1 O2 0.83 2.10 2.7545(8) 135.1 .
O2W H2B O2 0.84 1.87 2.6978(10) 170.1 7_566
O2W H2B F1 0.84 2.72 3.220(5) 120.3 7_566
O3W H3 O2W 0.82 2.10 2.8363(7) 149.0 5_666

_refine_diff_density_max         0.272
_refine_diff_density_min         -0.177
_refine_diff_density_rms         0.030

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water'
_chemical_properties_physical    ', Deliquescent'
####################################################################### 
# 
# 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_MnTFA2-final-100k-5-model2
_database_code_depnum_ccdc_archive 'CCDC 1505498'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-10-20 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Mn2+ 3, C2O2F3 6, H2O 4'
_chemical_formula_sum            'C12 H8 F18 Mn3 O16'
_chemical_formula_weight         915.00

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'
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'
Mn Mn 0.3368 0.7283 '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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   9.0195(5)
_cell_length_b                   9.0431(5)
_cell_length_c                   15.9167(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.694(3)
_cell_angle_gamma                90
_cell_volume                     1298.14(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1456
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      29.74

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.341
_exptl_crystal_F_000             890
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.491
_exptl_crystal_size_mid          0.289
_exptl_crystal_size_min          0.125
_exptl_absorpt_coefficient_mu    1.641
_shelx_estimated_absorpt_T_min   0.500
_shelx_estimated_absorpt_T_max   0.821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.641
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker D8 APEX'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            4315
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.559
_diffrn_reflns_theta_max         28.785
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4315
_reflns_number_gt                3639
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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          
'Refined as a 4-component twin., Twin,pseudo-tetragonal monoclinic structure with non-crystallographic mirror symmetry'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+4.9290P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4315
_refine_ls_number_parameters     368
_refine_ls_number_restraints     586
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0515
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1140
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.119
_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
Mn1 Mn 0.70458(8) 0.44189(6) 0.29357(3) 0.00863(14) Uani 1 1 d D . . . .
Mn2 Mn 0.5179(9) 0.4968(14) 0.5061(7) 0.0163(10) Uani 0.5 1 d . . P . .
O1A O 0.4164(8) 0.3488(8) 0.4183(5) 0.0183(11) Uani 0.513(8) 1 d D U P A 1
O2A O 0.5043(12) 0.3073(14) 0.2845(6) 0.0118(12) Uani 0.513(8) 1 d D U P A 1
C1A C 0.4120(11) 0.2989(13) 0.3454(6) 0.0183(14) Uani 0.513(8) 1 d D U P A 1
C2A C 0.2649(15) 0.2294(16) 0.3117(9) 0.0280(12) Uani 0.513(8) 1 d D U P A 1
F1A F 0.2391(9) 0.1015(8) 0.3535(6) 0.0280(17) Uani 0.513(8) 1 d D U P A 1
F2A F 0.1472(11) 0.3105(12) 0.3234(7) 0.046(2) Uani 0.513(8) 1 d D U P A 1
F3A F 0.2702(11) 0.1742(13) 0.2302(6) 0.037(2) Uani 0.513(8) 1 d D U P A 1
O1AA O 0.3657(9) 0.3884(9) 0.3976(5) 0.0183(11) Uani 0.487(8) 1 d D U P A 2
O2AA O 0.5136(12) 0.2970(15) 0.2999(6) 0.0118(12) Uani 0.487(8) 1 d D U P A 2
C1AA C 0.3900(12) 0.3143(14) 0.3333(7) 0.0183(14) Uani 0.487(8) 1 d D U P A 2
C2AA C 0.2579(16) 0.2156(16) 0.3094(9) 0.0280(12) Uani 0.487(8) 1 d D U P A 2
F1AA F 0.2137(14) 0.1315(13) 0.3736(7) 0.052(3) Uani 0.487(8) 1 d D U P A 2
F2AA F 0.2821(14) 0.1284(12) 0.2463(7) 0.044(3) Uani 0.487(8) 1 d D U P A 2
F3AA F 0.1450(12) 0.3048(11) 0.2889(6) 0.041(2) Uani 0.487(8) 1 d D U P A 2
O1B O 0.7240(10) 0.3889(9) 0.5133(5) 0.0238(14) Uani 0.551(8) 1 d D U P A 3
O2B O 0.8156(16) 0.305(3) 0.3886(8) 0.0125(17) Uani 0.551(8) 1 d D U P A 3
C1B C 0.8037(18) 0.311(3) 0.4672(8) 0.0267(14) Uani 0.551(8) 1 d D U P A 3
C2B C 0.9332(14) 0.2305(14) 0.5142(7) 0.0361(19) Uani 0.551(8) 1 d D U P A 3
F1B F 0.9046(10) 0.2034(10) 0.5930(5) 0.0356(19) Uani 0.551(8) 1 d D U P A 3
F2B F 0.9716(9) 0.1051(9) 0.4775(5) 0.047(2) Uani 0.551(8) 1 d D U P A 3
F3B F 1.0524(9) 0.3150(9) 0.5148(5) 0.049(2) Uani 0.551(8) 1 d D U P A 3
O1BA O 0.6670(12) 0.3586(12) 0.5045(7) 0.0238(14) Uani 0.449(8) 1 d D U P A 4
O2BA O 0.789(2) 0.299(3) 0.3903(10) 0.0125(17) Uani 0.449(8) 1 d D U P A 4
C1BA C 0.780(2) 0.318(3) 0.4683(10) 0.0267(14) Uani 0.449(8) 1 d D U P A 4
C2BA C 0.9142(16) 0.2674(16) 0.5225(9) 0.0361(19) Uani 0.449(8) 1 d D U P A 4
F1BA F 1.0162(9) 0.1931(12) 0.4773(5) 0.040(2) Uani 0.449(8) 1 d D U P A 4
F2BA F 0.9965(13) 0.3785(12) 0.5499(7) 0.065(3) Uani 0.449(8) 1 d D U P A 4
F3BA F 0.8639(13) 0.1740(14) 0.5839(7) 0.046(3) Uani 0.449(8) 1 d D U P A 4
O1C O 0.7900(5) 0.2707(3) 0.2061(2) 0.0198(6) Uani 1 1 d D U . . .
O2C O 0.8865(5) 0.1122(3) 0.1149(2) 0.0192(6) Uani 1 1 d D U . . .
C1C C 0.8580(7) 0.2401(4) 0.1419(3) 0.0156(6) Uani 1 1 d D U . . .
C2C C 0.9141(6) 0.3710(4) 0.0887(3) 0.0160(7) Uani 1 1 d D U . . .
F1C F 0.8311(7) 0.4901(6) 0.0968(4) 0.0252(15) Uani 0.505(7) 1 d D U P B 5
F2C F 1.0477(7) 0.3972(7) 0.1162(4) 0.0282(16) Uani 0.505(7) 1 d D U P B 5
F3C F 0.9204(7) 0.3389(7) 0.0059(3) 0.0255(15) Uani 0.505(7) 1 d D U P B 5
F1CA F 0.9458(7) 0.4946(6) 0.1356(4) 0.0207(14) Uani 0.495(7) 1 d . U P B 6
F2CA F 1.0375(7) 0.3455(7) 0.0452(4) 0.0245(15) Uani 0.495(7) 1 d . U P B 6
F3CA F 0.8086(7) 0.4096(7) 0.0366(4) 0.0238(15) Uani 0.495(7) 1 d . U P B 6
O1W O 0.9137(9) 0.5520(11) 0.3106(6) 0.0132(12) Uani 0.529(11) 1 d D . P A 7
H1WA H 0.982(5) 0.522(7) 0.342(6) 0.020 Uiso 0.529(11) 1 d D U P A 7
H1WB H 0.941(6) 0.625(8) 0.284(6) 0.020 Uiso 0.529(11) 1 d D U P A 7
O2W O 0.6067(14) 0.543(2) 0.1826(8) 0.016(2) Uani 0.529(11) 1 d D . P A 7
H2WA H 0.652(6) 0.601(10) 0.152(4) 0.024 Uiso 0.529(11) 1 d D U P A 7
H2WB H 0.530(8) 0.515(10) 0.160(5) 0.024 Uiso 0.529(11) 1 d D U P A 7
O1WA O 0.9247(11) 0.5283(11) 0.2776(7) 0.0132(12) Uani 0.471(11) 1 d D . P A 8
H1WC H 0.943(4) 0.616(5) 0.265(8) 0.020 Uiso 0.471(11) 1 d D U P A 8
H1WD H 0.999(3) 0.498(9) 0.304(6) 0.020 Uiso 0.471(11) 1 d D U P A 8
O2WA O 0.5689(17) 0.548(3) 0.2019(11) 0.016(2) Uani 0.471(11) 1 d D . P A 8
H2WC H 0.580(9) 0.630(6) 0.180(6) 0.024 Uiso 0.471(11) 1 d D U P A 8
H2WD H 0.548(13) 0.496(9) 0.150(5) 0.024 Uiso 0.471(11) 1 d D U P A 8


_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
Mn1 O2WA 2.121(19) . ?
Mn1 O2BA 2.14(2) . ?
Mn1 O1W 2.147(9) . ?
Mn1 O1WA 2.152(10) . ?
Mn1 O2AA 2.167(12) . ?
Mn1 O2W 2.168(16) . ?
Mn1 O2A 2.182(11) . ?
Mn1 O2B 2.188(18) . ?
Mn1 O1C 2.226(3) . ?
Mn1 O2C 2.280(3) 2_655 ?
Mn2 Mn2 0.380(10) 3_666 ?
Mn2 O1BA 1.836(15) . ?
Mn2 O1A 1.930(13) 3_666 ?
Mn2 O1B 2.101(13) . ?
Mn2 O1AA 2.118(12) 3_666 ?
Mn2 O1BA 2.125(14) 3_666 ?
Mn2 O1A 2.133(13) . ?
Mn2 O2C 2.328(14) 4_566 ?
Mn2 O2C 2.362(13) 2_655 ?
Mn2 O1AA 2.402(12) . ?
Mn2 O1B 2.431(12) 3_666 ?
O1A C1A 1.246(10) . ?
O1A Mn2 1.930(13) 3_666 ?
O2A C1A 1.287(11) . ?
C1A C2A 1.558(11) . ?
C2A F2A 1.305(16) . ?
C2A F1A 1.355(12) . ?
C2A F3A 1.390(14) . ?
O1AA C1AA 1.246(11) . ?
O1AA Mn2 2.118(12) 3_666 ?
O2AA C1AA 1.250(11) . ?
C1AA C2AA 1.533(12) . ?
C2AA F2AA 1.298(15) . ?
C2AA F3AA 1.337(15) . ?
C2AA F1AA 1.338(13) . ?
O1B C1B 1.249(12) . ?
O1B Mn2 2.431(12) 3_666 ?
O2B C1B 1.258(11) . ?
C1B C2B 1.562(11) . ?
C2B F1B 1.306(12) . ?
C2B F3B 1.319(14) . ?
C2B F2B 1.324(12) . ?
O1BA C1BA 1.230(13) . ?
O1BA Mn2 2.125(14) 3_666 ?
O2BA C1BA 1.258(13) . ?
C1BA C2BA 1.549(13) . ?
C2BA F2BA 1.320(15) . ?
C2BA F1BA 1.352(14) . ?
C2BA F3BA 1.374(15) . ?
O1C C1C 1.230(4) . ?
O2C C1C 1.262(5) . ?
O2C Mn1 2.280(3) 2_645 ?
O2C Mn2 2.328(14) 4_665 ?
O2C Mn2 2.362(13) 2_645 ?
C1C C2C 1.544(5) . ?
C2C F2C 1.299(8) . ?
C2C F3CA 1.302(8) . ?
C2C F1C 1.318(7) . ?
C2C F2CA 1.338(7) . ?
C2C F3C 1.352(7) . ?
C2C F1CA 1.372(7) . ?
O1W H1WA 0.83(2) . ?
O1W H1WB 0.82(2) . ?
O2W H2WA 0.83(2) . ?
O2W H2WB 0.82(2) . ?
O1WA H1WC 0.83(2) . ?
O1WA H1WD 0.83(2) . ?
O2WA H2WC 0.827(17) . ?
O2WA H2WD 0.96(7) . ?

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
O2WA Mn1 O1WA 106.3(5) . . ?
O1W Mn1 O2W 104.8(5) . . ?
O2WA Mn1 O1C 94.9(6) . . ?
O2BA Mn1 O1C 84.6(6) . . ?
O1W Mn1 O1C 95.2(3) . . ?
O1WA Mn1 O1C 81.5(3) . . ?
O2AA Mn1 O1C 83.7(3) . . ?
O2W Mn1 O1C 85.7(4) . . ?
O2A Mn1 O1C 82.1(3) . . ?
O2B Mn1 O1C 83.1(5) . . ?
O2WA Mn1 O2C 85.7(5) . 2_655 ?
O2BA Mn1 O2C 94.4(6) . 2_655 ?
O1W Mn1 O2C 85.9(3) . 2_655 ?
O1WA Mn1 O2C 99.8(3) . 2_655 ?
O2AA Mn1 O2C 94.9(3) . 2_655 ?
O2W Mn1 O2C 95.1(4) . 2_655 ?
O2A Mn1 O2C 96.6(3) . 2_655 ?
O2B Mn1 O2C 96.1(5) . 2_655 ?
O1C Mn1 O2C 178.38(10) . 2_655 ?
Mn2 Mn2 O1BA 136(4) 3_666 . ?
Mn2 Mn2 O1A 118(4) 3_666 3_666 ?
Mn2 Mn2 O1B 148(4) 3_666 . ?
Mn2 Mn2 O1AA 135(4) 3_666 3_666 ?
Mn2 Mn2 O1BA 37(4) 3_666 3_666 ?
O1BA Mn2 O1BA 172.8(6) . 3_666 ?
Mn2 Mn2 O1A 53(4) 3_666 . ?
O1A Mn2 O1A 170.9(5) 3_666 . ?
Mn2 Mn2 O2C 91(4) 3_666 4_566 ?
O1BA Mn2 O2C 95.9(6) . 4_566 ?
O1A Mn2 O2C 89.9(5) 3_666 4_566 ?
O1B Mn2 O2C 102.8(5) . 4_566 ?
O1AA Mn2 O2C 85.5(5) 3_666 4_566 ?
O1BA Mn2 O2C 85.0(5) 3_666 4_566 ?
O1A Mn2 O2C 90.2(5) . 4_566 ?
Mn2 Mn2 O2C 80(4) 3_666 2_655 ?
O1BA Mn2 O2C 90.8(6) . 2_655 ?
O1A Mn2 O2C 94.4(6) 3_666 2_655 ?
O1B Mn2 O2C 85.3(5) . 2_655 ?
O1AA Mn2 O2C 101.0(5) 3_666 2_655 ?
O1BA Mn2 O2C 87.5(5) 3_666 2_655 ?
O1A Mn2 O2C 84.3(5) . 2_655 ?
O2C Mn2 O2C 170.7(3) 4_566 2_655 ?
Mn2 Mn2 O1AA 39(4) 3_666 . ?
O1AA Mn2 O1AA 173.6(6) 3_666 . ?
O2C Mn2 O1AA 94.0(4) 4_566 . ?
O2C Mn2 O1AA 78.8(4) 2_655 . ?
Mn2 Mn2 O1B 28(4) 3_666 3_666 ?
O1B Mn2 O1B 175.2(6) . 3_666 ?
O2C Mn2 O1B 79.1(4) 4_566 3_666 ?
O2C Mn2 O1B 92.5(4) 2_655 3_666 ?
C1A O1A Mn2 148.0(8) . 3_666 ?
C1A O1A Mn2 147.8(8) . . ?
C1A O2A Mn1 121.7(8) . . ?
O1A C1A O2A 131.8(10) . . ?
O1A C1A C2A 119.0(9) . . ?
O2A C1A C2A 108.7(9) . . ?
F2A C2A F1A 105.3(11) . . ?
F2A C2A F3A 111.8(11) . . ?
F1A C2A F3A 99.2(10) . . ?
F2A C2A C1A 114.5(11) . . ?
F1A C2A C1A 109.0(10) . . ?
F3A C2A C1A 115.3(11) . . ?
C1AA O1AA Mn2 140.2(8) . 3_666 ?
C1AA O1AA Mn2 134.9(7) . . ?
C1AA O2AA Mn1 131.1(10) . . ?
O1AA C1AA O2AA 125.6(10) . . ?
O1AA C1AA C2AA 111.9(10) . . ?
O2AA C1AA C2AA 121.1(11) . . ?
F2AA C2AA F3AA 108.2(11) . . ?
F2AA C2AA F1AA 107.5(12) . . ?
F3AA C2AA F1AA 107.2(13) . . ?
F2AA C2AA C1AA 114.1(12) . . ?
F3AA C2AA C1AA 107.3(11) . . ?
F1AA C2AA C1AA 112.3(11) . . ?
C1B O1B Mn2 138.1(9) . . ?
C1B O1B Mn2 133.3(8) . 3_666 ?
C1B O2B Mn1 128.1(14) . . ?
O1B C1B O2B 131.8(14) . . ?
O1B C1B C2B 114.4(10) . . ?
O2B C1B C2B 112.5(11) . . ?
F1B C2B F3B 105.8(10) . . ?
F1B C2B F2B 108.6(10) . . ?
F3B C2B F2B 106.4(10) . . ?
F1B C2B C1B 113.1(10) . . ?
F3B C2B C1B 109.7(12) . . ?
F2B C2B C1B 112.8(11) . . ?
C1BA O1BA Mn2 145.0(14) . . ?
C1BA O1BA Mn2 143.0(12) . 3_666 ?
C1BA O2BA Mn1 126.7(19) . . ?
O1BA C1BA O2BA 124.7(14) . . ?
O1BA C1BA C2BA 118.3(12) . . ?
O2BA C1BA C2BA 116.6(13) . . ?
F2BA C2BA F1BA 99.8(12) . . ?
F2BA C2BA F3BA 114.9(12) . . ?
F1BA C2BA F3BA 107.8(12) . . ?
F2BA C2BA C1BA 113.2(15) . . ?
F1BA C2BA C1BA 112.6(11) . . ?
F3BA C2BA C1BA 108.3(15) . . ?
C1C O1C Mn1 148.9(3) . . ?
C1C O2C Mn1 109.0(2) . 2_645 ?
C1C O2C Mn2 138.5(4) . 4_665 ?
C1C O2C Mn2 139.5(4) . 2_645 ?
O1C C1C O2C 126.5(3) . . ?
O1C C1C C2C 116.9(3) . . ?
O2C C1C C2C 116.5(3) . . ?
F2C C2C F1C 110.1(5) . . ?
F3CA C2C F2CA 108.8(5) . . ?
F2C C2C F3C 108.5(5) . . ?
F1C C2C F3C 107.5(5) . . ?
F3CA C2C F1CA 105.9(5) . . ?
F2CA C2C F1CA 104.7(5) . . ?
F2C C2C C1C 105.3(5) . . ?
F3CA C2C C1C 108.2(5) . . ?
F1C C2C C1C 112.5(4) . . ?
F2CA C2C C1C 115.6(4) . . ?
F3C C2C C1C 112.8(4) . . ?
F1CA C2C C1C 113.2(4) . . ?
Mn1 O1W H1WA 125(3) . . ?
Mn1 O1W H1WB 126(3) . . ?
H1WA O1W H1WB 110(4) . . ?
Mn1 O2W H2WA 123(3) . . ?
Mn1 O2W H2WB 124(3) . . ?
H2WA O2W H2WB 111(4) . . ?
Mn1 O1WA H1WC 124(3) . . ?
Mn1 O1WA H1WD 124(3) . . ?
H1WC O1WA H1WD 106(4) . . ?
Mn1 O2WA H2WC 129(4) . . ?
Mn1 O2WA H2WD 118(4) . . ?
H2WC O2WA H2WD 96(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn2 O1A C1A O2A 32(2) 3_666 . . . ?
Mn2 O1A C1A O2A 15(3) . . . . ?
Mn2 O1A C1A C2A -138.8(13) 3_666 . . . ?
Mn2 O1A C1A C2A -156.0(12) . . . . ?
Mn1 O2A C1A O1A -6(2) . . . . ?
Mn1 O2A C1A C2A 165.6(8) . . . . ?
O1A C1A C2A F2A 49.1(16) . . . . ?
O2A C1A C2A F2A -123.5(13) . . . . ?
O1A C1A C2A F1A -68.6(16) . . . . ?
O2A C1A C2A F1A 118.8(13) . . . . ?
O1A C1A C2A F3A -179.0(11) . . . . ?
O2A C1A C2A F3A 8.3(16) . . . . ?
Mn2 O1AA C1AA O2AA -8(2) 3_666 . . . ?
Mn2 O1AA C1AA O2AA -13(2) . . . . ?
Mn2 O1AA C1AA C2AA 159.0(11) 3_666 . . . ?
Mn2 O1AA C1AA C2AA 153.5(9) . . . . ?
Mn1 O2AA C1AA O1AA -31(2) . . . . ?
Mn1 O2AA C1AA C2AA 162.8(9) . . . . ?
O1AA C1AA C2AA F2AA -175.3(12) . . . . ?
O2AA C1AA C2AA F2AA -7.7(19) . . . . ?
O1AA C1AA C2AA F3AA 64.8(14) . . . . ?
O2AA C1AA C2AA F3AA -127.6(14) . . . . ?
O1AA C1AA C2AA F1AA -52.7(17) . . . . ?
O2AA C1AA C2AA F1AA 114.9(15) . . . . ?
Mn2 O1B C1B O2B 27(4) . . . . ?
Mn2 O1B C1B O2B 28(4) 3_666 . . . ?
Mn2 O1B C1B C2B -166.6(11) . . . . ?
Mn2 O1B C1B C2B -165.6(10) 3_666 . . . ?
Mn1 O2B C1B O1B 4(4) . . . . ?
Mn1 O2B C1B C2B -162.6(13) . . . . ?
O1B C1B C2B F1B 27(2) . . . . ?
O2B C1B C2B F1B -163.7(19) . . . . ?
O1B C1B C2B F3B -90(2) . . . . ?
O2B C1B C2B F3B 78(2) . . . . ?
O1B C1B C2B F2B 151.2(17) . . . . ?
O2B C1B C2B F2B -40(3) . . . . ?
Mn2 Mn2 O1BA C1BA 79(7) 3_666 . . . ?
O2C Mn2 O1BA C1BA 175(2) 4_566 . . . ?
O2C Mn2 O1BA C1BA 2(3) 2_655 . . . ?
O2C Mn2 O1BA Mn2 97(6) 4_566 . . 3_666 ?
O2C Mn2 O1BA Mn2 -77(6) 2_655 . . 3_666 ?
Mn2 O1BA C1BA O2BA -50(5) . . . . ?
Mn2 O1BA C1BA O2BA -39(5) 3_666 . . . ?
Mn2 O1BA C1BA C2BA 137.8(16) . . . . ?
Mn2 O1BA C1BA C2BA 149.5(14) 3_666 . . . ?
Mn1 O2BA C1BA O1BA 44(5) . . . . ?
Mn1 O2BA C1BA C2BA -143.9(17) . . . . ?
O1BA C1BA C2BA F2BA -83(3) . . . . ?
O2BA C1BA C2BA F2BA 105(3) . . . . ?
O1BA C1BA C2BA F1BA 165(2) . . . . ?
O2BA C1BA C2BA F1BA -7(3) . . . . ?
O1BA C1BA C2BA F3BA 46(3) . . . . ?
O2BA C1BA C2BA F3BA -126(3) . . . . ?
Mn1 O1C C1C O2C 177.2(5) . . . . ?
Mn1 O1C C1C C2C -2.9(13) . . . . ?
Mn1 O2C C1C O1C -1.2(9) 2_645 . . . ?
Mn2 O2C C1C O1C -175.3(5) 4_665 . . . ?
Mn2 O2C C1C O1C 170.6(5) 2_645 . . . ?
Mn1 O2C C1C C2C 178.9(4) 2_645 . . . ?
Mn2 O2C C1C C2C 4.8(10) 4_665 . . . ?
Mn2 O2C C1C C2C -9.3(11) 2_645 . . . ?
O1C C1C C2C F2C 92.0(7) . . . . ?
O2C C1C C2C F2C -88.1(7) . . . . ?
O1C C1C C2C F3CA -87.3(7) . . . . ?
O2C C1C C2C F3CA 92.6(7) . . . . ?
O1C C1C C2C F1C -28.0(9) . . . . ?
O2C C1C C2C F1C 151.9(6) . . . . ?
O1C C1C C2C F2CA 150.5(6) . . . . ?
O2C C1C C2C F2CA -29.6(9) . . . . ?
O1C C1C C2C F3C -149.8(6) . . . . ?
O2C C1C C2C F3C 30.1(8) . . . . ?
O1C C1C C2C F1CA 29.8(9) . . . . ?
O2C C1C C2C F1CA -150.3(6) . . . . ?

_refine_diff_density_max         1.199
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.131


# start Validation Reply Form
_vrf_PLAT088_MnTFA2-final-100k-5-model2 
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.07 Note  
RESPONSE: The structure presents masive disorder that obligued to split
the majority of the atoms, almost duplicating the number of variables
needed for the fit. This large number of parameters is accompanied by
a large number of restraints and constraints imposed to keep molecular
geometry and reasonable thermal parameters of all the split atoms.
;
_vrf_PLAT220_MnTFA2-final-100k-5-model2 
;
PROBLEM: Non-Solvent Resd 1   F   Ueq(max)/Ueq(min) Range        3.1 Ratio 
RESPONSE: Data quality is very affected by multiple component twinning
probably cause by the monoclinic but pseudo-tetragonal unit cell and 
the observation of high degree of structural disorder. This may explain
the large Ueq(max) to Ueq(min) range of values observed.
;
_vrf_PLAT911_MnTFA2-final-100k-5-model2 
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600          2 Report
RESPONSE: Since the crystal was a multiple-component twin but was modeled
as four-component, disregarding twin members below 5% weight, some reflections 
may have been lost on integration due to partial twin overlap with unmodelled 
components that degraded reflection quality.
;
# end Validation Reply Form

_exptl_crystal_recrystallization_method 'Crystallized from synthesis flask'
_chemical_properties_physical    ', Deliquescent'
####################################################################### 
# 
# 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_MnMgTFA2_final_twin5
_database_code_depnum_ccdc_archive 'CCDC 1507757'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-10-02 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H8 F6 Mg0.45 Mn0.55 O8'
_chemical_formula_weight         339.19

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'
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'
Mn Mn 0.3368 0.7283 '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                   8.1926(6)
_cell_length_b                   9.0995(7)
_cell_length_c                   9.4154(7)
_cell_angle_alpha                88.761(4)
_cell_angle_beta                 63.982(3)
_cell_angle_gamma                71.251(4)
_cell_volume                     591.40(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9845
_cell_measurement_theta_min      3.085
_cell_measurement_theta_max      30.42

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_F_000             338
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.144
_exptl_absorpt_coefficient_mu    0.794
_shelx_estimated_absorpt_T_min   0.765
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_process_details   'TWINABS (Bruker, 2012)'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            6410
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.387
_diffrn_reflns_theta_max         30.653
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6410
_reflns_number_gt                5166
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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          
'Refined as a 2-component twin. R(int) for unmerged HKLF 4 style dataset:0.0202, Twin,Site occupation factor of Mn/Mg was refined constraining the total site occupation to 1'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0257P)²+0.1582P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6410
_refine_ls_number_parameters     198
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0304
_refine_ls_wR_factor_ref         0.0662
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.033
_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
Mg1 Mg 0.27111(4) 0.59533(3) 0.38853(3) 0.01203(10) Uani 0.452(2) 1 d . . P . .
Mn1 Mn 0.27111(4) 0.59533(3) 0.38853(3) 0.01203(10) Uani 0.548(2) 1 d . . P . .
O1W O 0.31870(17) 0.73863(12) 0.20809(13) 0.0208(2) Uani 1 1 d D . . . .
H1 H 0.281(3) 0.8308(14) 0.242(2) 0.031 Uiso 1 1 d D U . . .
H1' H 0.278(3) 0.727(2) 0.1454(19) 0.031 Uiso 1 1 d D U . . .
O2W O -0.03737(15) 0.71507(12) 0.50793(12) 0.0158(2) Uani 1 1 d D . . . .
H2B H -0.092(2) 0.8127(13) 0.519(2) 0.024 Uiso 1 1 d D U . . .
H2A H -0.095(2) 0.6871(18) 0.5951(16) 0.024 Uiso 1 1 d D U . . .
O2W' O 0.57533(15) 0.47150(12) 0.28536(12) 0.0162(2) Uani 1 1 d D . . . .
H2A' H 0.612(2) 0.3880(16) 0.3159(18) 0.024 Uiso 1 1 d D U . . .
H2B' H 0.640(2) 0.463(2) 0.1869(13) 0.024 Uiso 1 1 d D U . . .
O3W O 0.23889(17) 0.44289(13) 0.56241(13) 0.0182(2) Uani 1 1 d D . . . .
H3 H 0.291(2) 0.434(2) 0.619(2) 0.027 Uiso 1 1 d D U . . .
H3' H 0.185(2) 0.3798(19) 0.575(2) 0.027 Uiso 1 1 d D U . . .
O1 O 0.30682(15) 0.74625(11) 0.53615(12) 0.0159(2) Uani 1 1 d . . . . .
O2 O 0.21436(17) 0.97336(12) 0.44744(13) 0.0211(2) Uani 1 1 d . . . . .
C1 C 0.2603(2) 0.89200(17) 0.53936(18) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.2544(3) 0.98008(18) 0.6805(2) 0.0229(3) Uani 1 1 d . . . . .
F1 F 0.31719(16) 1.10021(11) 0.63726(13) 0.0338(3) Uani 1 1 d . . . . .
F2 F 0.07298(17) 1.03956(14) 0.79515(13) 0.0464(3) Uani 1 1 d . . . . .
F3 F 0.35985(19) 0.89023(12) 0.74322(14) 0.0445(3) Uani 1 1 d . . . . .
O1' O 0.22717(15) 0.43810(12) 0.25268(12) 0.0162(2) Uani 1 1 d . . . . .
O2' O 0.25168(16) 0.55195(12) 0.03457(12) 0.0201(2) Uani 1 1 d . . . . .
C1' C 0.2328(2) 0.44647(17) 0.11691(17) 0.0151(3) Uani 1 1 d . . . . .
C2' C 0.2087(2) 0.30361(18) 0.05281(18) 0.0210(3) Uani 1 1 d . . . . .
F1' F 0.22924(17) 0.30964(13) -0.09470(11) 0.0368(3) Uani 1 1 d . . . . .
F2' F 0.33632(16) 0.17011(11) 0.05238(14) 0.0391(3) Uani 1 1 d . . . . .
F3' F 0.03308(15) 0.29806(13) 0.14419(12) 0.0342(3) 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
Mg1 O1W 2.0949(11) . ?
Mg1 O3W 2.1053(10) . ?
Mg1 O2W' 2.1314(11) . ?
Mg1 O1 2.1450(10) . ?
Mg1 O1' 2.1510(10) . ?
Mg1 O2W 2.1514(11) . ?
O1W H1 0.813(11) . ?
O1W H1' 0.816(11) . ?
O2W H2B 0.841(10) . ?
O2W H2A 0.831(11) . ?
O2W' H2A' 0.819(10) . ?
O2W' H2B' 0.832(10) . ?
O3W H3 0.811(10) . ?
O3W H3' 0.808(10) . ?
O1 C1 1.2537(17) . ?
O2 C1 1.2320(18) . ?
C1 C2 1.541(2) . ?
C2 F3 1.3177(18) . ?
C2 F2 1.329(2) . ?
C2 F1 1.3358(19) . ?
O1' C1' 1.2604(17) . ?
O2' C1' 1.2265(18) . ?
C1' C2' 1.548(2) . ?
C2' F2' 1.3226(19) . ?
C2' F1' 1.3258(18) . ?
C2' F3' 1.3307(19) . ?

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
O1W Mg1 O3W 176.87(5) . . ?
O1W Mg1 O2W' 89.40(4) . . ?
O3W Mg1 O2W' 87.56(4) . . ?
O1W Mg1 O1 91.95(4) . . ?
O3W Mg1 O1 88.70(4) . . ?
O2W' Mg1 O1 88.02(4) . . ?
O1W Mg1 O1' 91.24(4) . . ?
O3W Mg1 O1' 88.17(4) . . ?
O2W' Mg1 O1' 93.03(4) . . ?
O1 Mg1 O1' 176.65(4) . . ?
O1W Mg1 O2W 94.20(4) . . ?
O3W Mg1 O2W 88.86(4) . . ?
O2W' Mg1 O2W 176.08(4) . . ?
O1 Mg1 O2W 90.30(4) . . ?
O1' Mg1 O2W 88.46(4) . . ?
Mg1 O1W H1 113.0(14) . . ?
Mg1 O1W H1' 114.6(13) . . ?
H1 O1W H1' 110.8(15) . . ?
Mg1 O2W H2B 124.4(12) . . ?
Mg1 O2W H2A 114.8(12) . . ?
H2B O2W H2A 106.1(14) . . ?
Mg1 O2W' H2A' 117.6(12) . . ?
Mg1 O2W' H2B' 118.2(12) . . ?
H2A' O2W' H2B' 109.3(14) . . ?
Mg1 O3W H3 122.6(12) . . ?
Mg1 O3W H3' 126.1(12) . . ?
H3 O3W H3' 111.0(14) . . ?
C1 O1 Mg1 124.44(9) . . ?
O2 C1 O1 128.59(13) . . ?
O2 C1 C2 116.32(13) . . ?
O1 C1 C2 115.07(13) . . ?
F3 C2 F2 107.84(14) . . ?
F3 C2 F1 107.22(13) . . ?
F2 C2 F1 106.88(13) . . ?
F3 C2 C1 113.22(13) . . ?
F2 C2 C1 109.80(13) . . ?
F1 C2 C1 111.61(13) . . ?
C1' O1' Mg1 128.64(9) . . ?
O2' C1' O1' 128.35(13) . . ?
O2' C1' C2' 118.32(13) . . ?
O1' C1' C2' 113.33(13) . . ?
F2' C2' F1' 107.70(13) . . ?
F2' C2' F3' 107.43(13) . . ?
F1' C2' F3' 107.34(13) . . ?
F2' C2' C1' 111.62(13) . . ?
F1' C2' C1' 112.14(13) . . ?
F3' C2' C1' 110.39(12) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 O2 -11.6(2) . . . . ?
Mg1 O1 C1 C2 166.35(10) . . . . ?
O2 C1 C2 F3 -159.68(15) . . . . ?
O1 C1 C2 F3 22.1(2) . . . . ?
O2 C1 C2 F2 79.74(18) . . . . ?
O1 C1 C2 F2 -98.46(16) . . . . ?
O2 C1 C2 F1 -38.6(2) . . . . ?
O1 C1 C2 F1 143.21(13) . . . . ?
Mg1 O1' C1' O2' -5.5(2) . . . . ?
Mg1 O1' C1' C2' 175.65(9) . . . . ?
O2' C1' C2' F2' 126.56(15) . . . . ?
O1' C1' C2' F2' -54.43(17) . . . . ?
O2' C1' C2' F1' 5.6(2) . . . . ?
O1' C1' C2' F1' -175.38(13) . . . . ?
O2' C1' C2' F3' -114.03(15) . . . . ?
O1' C1' C2' F3' 64.98(17) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1 O2 0.813(11) 2.107(13) 2.7777(15) 139.8(17) .
O1W H1' O2' 0.816(11) 2.039(13) 2.7134(14) 139.7(17) .
O2W H2B O2 0.841(10) 1.841(11) 2.6817(14) 177.8(16) 2_576
O2W H2A O1' 0.831(11) 1.971(11) 2.7610(15) 158.6(17) 2_566
O2W' H2A' O1 0.819(10) 2.022(12) 2.7807(15) 153.8(17) 2_666
O2W' H2A' F3 0.819(10) 2.519(15) 3.1588(15) 135.8(15) 2_666
O2W' H2B' O2' 0.832(10) 1.862(11) 2.6863(14) 171.1(18) 2_665
O3W H3 O2W' 0.811(10) 2.057(12) 2.7753(15) 147.4(17) 2_666
O3W H3' O2W 0.808(10) 2.086(12) 2.7849(15) 144.7(17) 2_566

_refine_diff_density_max         0.442
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.063


# start Validation Reply Form
_vrf_PLAT077_MnMgTFA2_final_twin5 
;
PROBLEM: Unitcell contains non-integer number of atoms .. Please Check
RESPONSE: The unit cell does contain an integer number of atom but the 
proportion of Mn2+ and Mg2+ in the crystal has been determined by 
refinement of atomic site occupancies to 55% and 45% respectively. 
;
_vrf_PLAT250_MnMgTFA2_final_twin5 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.2 Note
RESPONSE: The crystal used for structure determination and refinement is a 
two-component twin and we attribute this error to defective modelling of 
the crystal components during integration, absorption correction and scaling.
 
;
_vrf_PLAT911_MnMgTFA2_final_twin5 
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L= 0.600 13 Report
RESPONSE: A number of intensities have been lost due to geometrical restrictions
in the orientation of the crystal during data collection at low temperature. 
;
_vrf_PLAT155_MnMgTFA2_final_twin5 
;
PROBLEM: The Triclinic Unitcell is NOT Reduced .......... Please Do !
RESPONSE: Reduced cell can be obtained by applying the transformation
matrix [[-1 0 0][0 -1 0][-1 0 1]]. A non-conventional unit cell
was chosen for consistency with Mg(tfa)2.4H2O compound described
in a conventional cell with a=8.0985 b=9.0458 c=9.3604 
alpha=88.324 beta=65.021 gamma=71.131.
;
# end Validation Reply Form 

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_chemical_properties_physical    ', Deliquescent'
####################################################################### 
# 
# 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_MnCaTFA2-100k-final-5
_database_code_depnum_ccdc_archive 'CCDC 1510812'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-10-20 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ca 2+ 1.72, Mn2+ 1.28, C2O2F3 6, H2O 4'
_chemical_formula_sum            'C12 H8 Ca1.72 F18 Mn1.28 O16'
_chemical_formula_weight         889.46

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'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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/n'
_space_group_name_Hall           '-P 2yn'

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

_cell_length_a                   9.0523(5)
_cell_length_b                   9.1619(5)
_cell_length_c                   16.3326(10)
_cell_angle_alpha                90
_cell_angle_beta                 92.621(3)
_cell_angle_gamma                90
_cell_volume                     1353.15(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9973
_cell_measurement_theta_min      2.549
_cell_measurement_theta_max      32.135

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.183
_exptl_crystal_F_000             873
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.442
_exptl_crystal_size_mid          0.361
_exptl_crystal_size_min          0.205
_exptl_absorpt_coefficient_mu    1.134
_shelx_estimated_absorpt_T_min   0.634
_shelx_estimated_absorpt_T_max   0.801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_T_max  0.801
_exptl_absorpt_process_details   
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            8732
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.497
_diffrn_reflns_theta_max         34.839
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8732
_reflns_number_gt                6192
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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          
'Refined as a 2-component twin., Twin,pseudo-tetragonal monoclinic structure with non-crystallographic mirror symmetry'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0553P)²+0.3102P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8732
_refine_ls_number_parameters     397
_refine_ls_number_restraints     288
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.1128
_refine_ls_wR_factor_gt          0.1008
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.115
_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
Mn1 Mn 0.70709(3) 0.43612(3) 0.29193(2) 0.01504(7) Uani 0.625(7) 1 d . . P . .
Ca1 Ca 0.70709(3) 0.43612(3) 0.29193(2) 0.01504(7) Uani 0.375(7) 1 d . . P . .
Ca2 Ca 0.51953(18) 0.4997(3) 0.50606(16) 0.0169(3) Uani 0.481(4) 1 d . . P . .
Mn2 Mn 0.51953(18) 0.4997(3) 0.50606(16) 0.0169(3) Uani 0.019(4) 1 d . . P . .
O1W O 0.58812(15) 0.53994(14) 0.18801(9) 0.0313(3) Uani 1 1 d D . . . .
H1WA H 0.608(3) 0.615(2) 0.1645(17) 0.047 Uiso 1 1 d D U . . .
H1WB H 0.532(3) 0.500(3) 0.1553(15) 0.047 Uiso 1 1 d D U . . .
O2W O 0.92648(19) 0.53700(16) 0.29604(14) 0.0491(5) Uani 1 1 d D . . . .
H2WA H 1.004(3) 0.507(4) 0.317(2) 0.074 Uiso 1 1 d D U . . .
H2WB H 0.947(4) 0.616(3) 0.276(2) 0.074 Uiso 1 1 d D U . . .
O1A O 0.4034(5) 0.3595(4) 0.4019(3) 0.0361(9) Uani 0.697(11) 1 d D U P A 1
O2A O 0.5057(10) 0.2946(10) 0.2866(7) 0.0186(14) Uani 0.697(11) 1 d D U P A 1
C1A C 0.3958(7) 0.3041(9) 0.3302(5) 0.0282(14) Uani 0.697(11) 1 d D U P A 1
C2A C 0.2618(6) 0.2103(7) 0.3010(4) 0.0278(10) Uani 0.697(11) 1 d D U P A 1
F1A F 0.2397(4) 0.1040(4) 0.3553(3) 0.0459(9) Uani 0.697(11) 1 d D U P A 1
F2A F 0.1398(4) 0.2909(4) 0.2942(4) 0.0579(12) Uani 0.697(11) 1 d D U P A 1
F3A F 0.2740(3) 0.1460(6) 0.2298(2) 0.0647(12) Uani 0.697(11) 1 d D U P A 1
O1AA O 0.3608(7) 0.3877(6) 0.3781(4) 0.0190(11) Uani 0.303(11) 1 d D U P A 2
O2AA O 0.511(2) 0.293(3) 0.2821(17) 0.023(4) Uani 0.303(11) 1 d D U P A 2
C1AA C 0.4102(15) 0.298(2) 0.3293(10) 0.021(3) Uani 0.303(11) 1 d D U P A 2
C2AA C 0.2585(17) 0.2365(17) 0.3022(11) 0.037(3) Uani 0.303(11) 1 d D U P A 2
F1AA F 0.2385(11) 0.2349(19) 0.2242(5) 0.080(4) Uani 0.303(11) 1 d D U P A 2
F2AA F 0.2523(9) 0.0949(7) 0.3193(8) 0.051(2) Uani 0.303(11) 1 d D U P A 2
F3AA F 0.1474(8) 0.2983(10) 0.3340(7) 0.0469(19) Uani 0.303(11) 1 d D U P A 2
O1B O 0.7389(9) 0.3809(5) 0.5071(3) 0.0281(9) Uani 0.594(18) 1 d D U P A 3
O2B O 0.8144(10) 0.2906(14) 0.3876(5) 0.0265(18) Uani 0.594(18) 1 d D U P A 3
C1B C 0.8230(9) 0.3151(10) 0.4640(5) 0.0196(12) Uani 0.594(18) 1 d D U P A 3
C2B C 0.9542(10) 0.2435(10) 0.5122(5) 0.0329(15) Uani 0.594(18) 1 d D U P A 3
F1B F 0.9176(8) 0.1997(7) 0.5860(3) 0.0508(11) Uani 0.594(18) 1 d D U P A 3
F2B F 0.9999(10) 0.1252(8) 0.4750(5) 0.062(2) Uani 0.594(18) 1 d D U P A 3
F3B F 1.0583(6) 0.3403(5) 0.5201(4) 0.0540(13) Uani 0.594(18) 1 d D U P A 3
O1BA O 0.6883(11) 0.3606(8) 0.4991(5) 0.0278(13) Uani 0.406(18) 1 d D U P A 4
O2BA O 0.8146(11) 0.3011(19) 0.3884(7) 0.0160(17) Uani 0.406(18) 1 d D U P A 4
C1BA C 0.7920(12) 0.3012(14) 0.4638(7) 0.0184(17) Uani 0.406(18) 1 d D U P A 4
C2BA C 0.9221(15) 0.2453(17) 0.5162(9) 0.039(3) Uani 0.406(18) 1 d D U P A 4
F1BA F 1.0266(12) 0.1708(14) 0.4736(7) 0.055(2) Uani 0.406(18) 1 d D U P A 4
F2BA F 1.0085(16) 0.3499(8) 0.5534(10) 0.085(3) Uani 0.406(18) 1 d D U P A 4
F3BA F 0.8802(15) 0.1593(13) 0.5754(6) 0.059(2) Uani 0.406(18) 1 d D U P A 4
O1C O 0.79163(14) 0.26556(12) 0.20497(7) 0.0208(2) Uani 1 1 d . . . . .
O2C O 0.88281(13) 0.10668(11) 0.11762(7) 0.0208(2) Uani 1 1 d . . . . .
C1C C 0.85612(17) 0.23351(14) 0.14249(9) 0.0154(3) Uani 1 1 d . . . . .
C2C C 0.90899(18) 0.35985(16) 0.08920(10) 0.0203(3) Uani 1 1 d . . . . .
F1C F 0.9434(3) 0.4807(2) 0.13259(14) 0.0397(8) Uani 0.520(3) 1 d . . P B 5
F2C F 1.0238(3) 0.3276(3) 0.04565(17) 0.0417(8) Uani 0.520(3) 1 d . . P B 5
F3C F 0.7988(3) 0.3983(3) 0.03716(16) 0.0380(7) Uani 0.520(3) 1 d . . P B 5
F4C F 0.8228(4) 0.4727(3) 0.0868(2) 0.0460(10) Uani 0.480(3) 1 d . . P B 6
F5C F 1.0422(3) 0.3953(3) 0.11781(19) 0.0448(9) Uani 0.480(3) 1 d . . P B 6
F6C F 0.9239(4) 0.3147(3) 0.01141(15) 0.0413(8) Uani 0.480(3) 1 d . . P B 6


_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
Mn1 O1W 2.1860(13) . ?
Mn1 O2W 2.1888(18) . ?
Mn1 O2BA 2.196(11) . ?
Mn1 O2AA 2.20(2) . ?
Mn1 O2A 2.236(8) . ?
Mn1 O2B 2.241(9) . ?
Mn1 O1C 2.2681(11) . ?
Mn1 O2C 2.3231(12) 2_655 ?
Ca2 Mn2 0.397(2) 3_666 ?
Ca2 Ca2 0.397(2) 3_666 ?
Ca2 O1BA 1.996(7) . ?
Ca2 O1A 2.078(4) 3_666 ?
Ca2 O1B 2.264(7) . ?
Ca2 O1BA 2.273(8) 3_666 ?
Ca2 O1A 2.343(4) . ?
Ca2 O1AA 2.372(7) 3_666 ?
Ca2 O2C 2.447(3) 2_655 ?
Ca2 O2C 2.451(3) 4_566 ?
Ca2 O1B 2.583(7) 3_666 ?
Ca2 O1AA 2.685(7) . ?
O1W H1WA 0.816(19) . ?
O1W H1WB 0.808(19) . ?
O2W H2WA 0.81(2) . ?
O2W H2WB 0.82(2) . ?
O1A C1A 1.275(7) . ?
O1A Mn2 2.078(4) 3_666 ?
O1A Ca2 2.078(4) 3_666 ?
O2A C1A 1.252(7) . ?
C1A C2A 1.544(6) . ?
C2A F3A 1.312(7) . ?
C2A F2A 1.329(6) . ?
C2A F1A 1.338(7) . ?
O1AA C1AA 1.244(14) . ?
O1AA Mn2 2.372(7) 3_666 ?
O1AA Ca2 2.372(7) 3_666 ?
O2AA C1AA 1.225(15) . ?
C1AA C2AA 1.530(14) . ?
C2AA F1AA 1.278(18) . ?
C2AA F3AA 1.284(16) . ?
C2AA F2AA 1.329(15) . ?
O1B C1B 1.220(8) . ?
O1B Ca2 2.583(7) 3_666 ?
O2B C1B 1.267(9) . ?
C1B C2B 1.541(8) . ?
C2B F3B 1.297(10) . ?
C2B F2B 1.318(10) . ?
C2B F1B 1.327(9) . ?
O1BA C1BA 1.248(10) . ?
O1BA Mn2 2.273(8) 3_666 ?
O1BA Ca2 2.273(8) 3_666 ?
O2BA C1BA 1.258(12) . ?
C1BA C2BA 1.513(12) . ?
C2BA F3BA 1.316(15) . ?
C2BA F2BA 1.362(15) . ?
C2BA F1BA 1.380(14) . ?
O1C C1C 1.2340(18) . ?
O1C Ca1 3.0188(11) 2_645 ?
O2C C1C 1.2580(16) . ?
O2C Ca1 2.3231(12) 2_645 ?
O2C Mn1 2.3231(12) 2_645 ?
O2C Mn2 2.447(3) 2_645 ?
O2C Ca2 2.447(3) 2_645 ?
O2C Mn2 2.451(3) 4_665 ?
O2C Ca2 2.451(3) 4_665 ?
C1C C2C 1.538(2) . ?
C1C Ca1 2.9924(13) 2_645 ?
C2C F4C 1.295(3) . ?
C2C F5C 1.314(3) . ?
C2C F2C 1.319(3) . ?
C2C F3C 1.328(3) . ?
C2C F1C 1.344(3) . ?
C2C F6C 1.349(3) . ?
F2C Ca2 3.068(4) 4_665 ?
F6C Ca2 2.947(4) 2_645 ?
F6C Ca2 3.010(4) 4_665 ?

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
O1W Mn1 O2W 104.73(6) . . ?
O1W Mn1 O2BA 171.5(4) . . ?
O2W Mn1 O2BA 81.0(4) . . ?
O1W Mn1 O2AA 80.6(8) . . ?
O2W Mn1 O2AA 168.1(6) . . ?
O1W Mn1 O2A 81.4(3) . . ?
O2W Mn1 O2A 169.5(3) . . ?
O1W Mn1 O2B 169.3(3) . . ?
O2W Mn1 O2B 82.3(3) . . ?
O1W Mn1 O1C 88.96(5) . . ?
O2W Mn1 O1C 88.77(6) . . ?
O2BA Mn1 O1C 84.8(3) . . ?
O2AA Mn1 O1C 80.6(5) . . ?
O2A Mn1 O1C 82.8(2) . . ?
O2B Mn1 O1C 83.0(3) . . ?
O1W Mn1 O2C 91.52(5) . 2_655 ?
O2W Mn1 O2C 92.30(6) . 2_655 ?
O2BA Mn1 O2C 94.6(3) . 2_655 ?
O2AA Mn1 O2C 98.2(5) . 2_655 ?
O2A Mn1 O2C 96.1(2) . 2_655 ?
O2B Mn1 O2C 96.3(2) . 2_655 ?
O1C Mn1 O2C 178.67(4) . 2_655 ?
Mn2 Ca2 O1BA 130.2(9) 3_666 . ?
Ca2 Ca2 O1BA 130.2(9) 3_666 . ?
Mn2 Ca2 O1A 127.9(9) 3_666 3_666 ?
Ca2 Ca2 O1A 127.9(9) 3_666 3_666 ?
Mn2 Ca2 O1B 140.4(9) 3_666 . ?
Ca2 Ca2 O1B 140.4(9) 3_666 . ?
Mn2 Ca2 O1BA 42.1(8) 3_666 3_666 ?
Ca2 Ca2 O1BA 42.1(8) 3_666 3_666 ?
O1BA Ca2 O1BA 172.33(13) . 3_666 ?
Mn2 Ca2 O1A 44.4(8) 3_666 . ?
Ca2 Ca2 O1A 44.4(8) 3_666 . ?
O1A Ca2 O1A 172.31(11) 3_666 . ?
Mn2 Ca2 O1AA 139.1(9) 3_666 3_666 ?
Ca2 Ca2 O1AA 139.1(9) 3_666 3_666 ?
Mn2 Ca2 O2C 86.0(8) 3_666 2_655 ?
Ca2 Ca2 O2C 86.0(8) 3_666 2_655 ?
O1BA Ca2 O2C 84.4(2) . 2_655 ?
O1A Ca2 O2C 103.12(15) 3_666 2_655 ?
O1B Ca2 O2C 81.30(15) . 2_655 ?
O1BA Ca2 O2C 94.23(19) 3_666 2_655 ?
O1A Ca2 O2C 77.70(12) . 2_655 ?
O1AA Ca2 O2C 108.36(17) 3_666 2_655 ?
Mn2 Ca2 O2C 84.7(8) 3_666 4_566 ?
Ca2 Ca2 O2C 84.7(8) 3_666 4_566 ?
O1BA Ca2 O2C 101.7(2) . 4_566 ?
O1A Ca2 O2C 82.71(13) 3_666 4_566 ?
O1B Ca2 O2C 106.01(17) . 4_566 ?
O1BA Ca2 O2C 78.82(19) 3_666 4_566 ?
O1A Ca2 O2C 95.56(12) . 4_566 ?
O1AA Ca2 O2C 78.93(17) 3_666 4_566 ?
O2C Ca2 O2C 170.69(5) 2_655 4_566 ?
Mn2 Ca2 O1B 34.0(8) 3_666 3_666 ?
Ca2 Ca2 O1B 34.0(8) 3_666 3_666 ?
O1B Ca2 O1B 174.37(12) . 3_666 ?
O2C Ca2 O1B 97.00(14) 2_655 3_666 ?
O2C Ca2 O1B 75.16(13) 4_566 3_666 ?
Mn2 Ca2 O1AA 35.4(8) 3_666 . ?
Ca2 Ca2 O1AA 35.4(8) 3_666 . ?
O1AA Ca2 O1AA 174.43(11) 3_666 . ?
O2C Ca2 O1AA 73.22(15) 2_655 . ?
O2C Ca2 O1AA 98.97(15) 4_566 . ?
Mn1 O1W H1WA 128(2) . . ?
Mn1 O1W H1WB 126(2) . . ?
H1WA O1W H1WB 103(3) . . ?
Mn1 O2W H2WA 130(3) . . ?
Mn1 O2W H2WB 126(2) . . ?
H2WA O2W H2WB 105(3) . . ?
C1A O1A Mn2 156.1(4) . 3_666 ?
C1A O1A Ca2 156.1(4) . 3_666 ?
C1A O1A Ca2 152.7(3) . . ?
C1A O2A Mn1 127.2(6) . . ?
O2A C1A O1A 122.6(7) . . ?
O2A C1A C2A 114.8(6) . . ?
O1A C1A C2A 120.9(5) . . ?
F3A C2A F2A 106.2(5) . . ?
F3A C2A F1A 106.4(5) . . ?
F2A C2A F1A 108.1(4) . . ?
F3A C2A C1A 115.2(4) . . ?
F2A C2A C1A 110.8(5) . . ?
F1A C2A C1A 109.9(6) . . ?
C1AA O1AA Mn2 129.4(8) . 3_666 ?
C1AA O1AA Ca2 129.4(8) . 3_666 ?
C1AA O1AA Ca2 123.9(8) . . ?
C1AA O2AA Mn1 123.7(17) . . ?
O2AA C1AA O1AA 136.7(18) . . ?
O2AA C1AA C2AA 119.5(16) . . ?
O1AA C1AA C2AA 94.9(11) . . ?
F1AA C2AA F3AA 109.3(13) . . ?
F1AA C2AA F2AA 101.1(11) . . ?
F3AA C2AA F2AA 107.7(13) . . ?
F1AA C2AA C1AA 112.1(13) . . ?
F3AA C2AA C1AA 115.5(12) . . ?
F2AA C2AA C1AA 110.1(14) . . ?
C1B O1B Ca2 143.5(5) . . ?
C1B O1B Ca2 138.4(5) . 3_666 ?
C1B O2B Mn1 125.9(8) . . ?
O1B C1B O2B 130.2(8) . . ?
O1B C1B C2B 113.7(7) . . ?
O2B C1B C2B 116.0(7) . . ?
F3B C2B F2B 111.5(8) . . ?
F3B C2B F1B 109.1(7) . . ?
F2B C2B F1B 105.5(7) . . ?
F3B C2B C1B 107.5(6) . . ?
F2B C2B C1B 111.4(7) . . ?
F1B C2B C1B 112.0(7) . . ?
C1BA O1BA Ca2 153.9(7) . . ?
C1BA O1BA Mn2 150.1(7) . 3_666 ?
C1BA O1BA Ca2 150.1(7) . 3_666 ?
C1BA O2BA Mn1 128.0(9) . . ?
O1BA C1BA O2BA 127.7(10) . . ?
O1BA C1BA C2BA 118.0(10) . . ?
O2BA C1BA C2BA 113.3(9) . . ?
O2BA C1BA Ca2 112.2(8) . . ?
C2BA C1BA Ca2 131.7(8) . . ?
F3BA C2BA F2BA 105.8(11) . . ?
F3BA C2BA F1BA 107.6(11) . . ?
F2BA C2BA F1BA 100.4(10) . . ?
F3BA C2BA C1BA 112.0(11) . . ?
F2BA C2BA C1BA 115.5(11) . . ?
F1BA C2BA C1BA 114.6(11) . . ?
C1C O1C Mn1 150.20(10) . . ?
C1C O1C Ca1 76.96(8) . 2_645 ?
Mn1 O1C Ca1 132.8 . 2_645 ?
C1C O2C Ca1 109.75(9) . 2_645 ?
C1C O2C Mn1 109.75(9) . 2_645 ?
C1C O2C Mn2 135.93(12) . 2_645 ?
Ca1 O2C Mn2 113.95(8) 2_645 2_645 ?
Mn1 O2C Mn2 113.95(8) 2_645 2_645 ?
C1C O2C Ca2 135.93(12) . 2_645 ?
Ca1 O2C Ca2 113.95(8) 2_645 2_645 ?
Mn1 O2C Ca2 113.95(8) 2_645 2_645 ?
C1C O2C Mn2 135.92(12) . 4_665 ?
Ca1 O2C Mn2 114.12(8) 2_645 4_665 ?
Mn1 O2C Mn2 114.12(8) 2_645 4_665 ?
C1C O2C Ca2 135.92(12) . 4_665 ?
Ca1 O2C Ca2 114.12(8) 2_645 4_665 ?
Mn1 O2C Ca2 114.12(8) 2_645 4_665 ?
O1C C1C O2C 126.29(13) . . ?
O1C C1C C2C 117.40(12) . . ?
O2C C1C C2C 116.31(12) . . ?
O1C C1C Ca1 79.36(8) . 2_645 ?
O2C C1C Ca1 46.94(7) . 2_645 ?
C2C C1C Ca1 163.25(9) . 2_645 ?
F4C C2C F5C 110.8(2) . . ?
F2C C2C F3C 107.5(2) . . ?
F2C C2C F1C 107.4(2) . . ?
F3C C2C F1C 105.6(2) . . ?
F4C C2C F6C 107.6(2) . . ?
F5C C2C F6C 106.3(2) . . ?
F4C C2C C1C 114.55(16) . . ?
F5C C2C C1C 106.82(17) . . ?
F2C C2C C1C 114.20(16) . . ?
F3C C2C C1C 108.52(16) . . ?
F1C C2C C1C 113.11(15) . . ?
F6C C2C C1C 110.45(16) . . ?
C2C F2C Ca2 109.26(17) . 4_665 ?
C2C F6C Ca2 114.64(17) . 2_645 ?
C2C F6C Ca2 111.23(17) . 4_665 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mn1 O2A C1A O1A -26.1(17) . . . . ?
Mn1 O2A C1A C2A 168.7(7) . . . . ?
Mn2 O1A C1A O2A 33(2) 3_666 . . . ?
Ca2 O1A C1A O2A 33(2) 3_666 . . . ?
Ca2 O1A C1A O2A 17(2) . . . . ?
Mn2 O1A C1A C2A -162.9(9) 3_666 . . . ?
Ca2 O1A C1A C2A -162.9(9) 3_666 . . . ?
Ca2 O1A C1A C2A -179.0(7) . . . . ?
O2A C1A C2A F3A -7.3(12) . . . . ?
O1A C1A C2A F3A -172.8(8) . . . . ?
O2A C1A C2A F2A -127.9(10) . . . . ?
O1A C1A C2A F2A 66.7(11) . . . . ?
O2A C1A C2A F1A 112.8(10) . . . . ?
O1A C1A C2A F1A -52.6(11) . . . . ?
Mn1 O2AA C1AA O1AA 21(4) . . . . ?
Mn1 O2AA C1AA C2AA 158.6(17) . . . . ?
Mn2 O1AA C1AA O2AA -59(4) 3_666 . . . ?
Ca2 O1AA C1AA O2AA -59(4) 3_666 . . . ?
Ca2 O1AA C1AA O2AA -59(3) . . . . ?
Mn2 O1AA C1AA C2AA 156.8(8) 3_666 . . . ?
Ca2 O1AA C1AA C2AA 156.8(8) 3_666 . . . ?
Ca2 O1AA C1AA C2AA 156.6(8) . . . . ?
O2AA C1AA C2AA F1AA -24(3) . . . . ?
O1AA C1AA C2AA F1AA 128.6(15) . . . . ?
O2AA C1AA C2AA F3AA -150(2) . . . . ?
O1AA C1AA C2AA F3AA 3(2) . . . . ?
O2AA C1AA C2AA F2AA 88(3) . . . . ?
O1AA C1AA C2AA F2AA -119.6(17) . . . . ?
Ca2 O1B C1B O2B 3.0(16) . . . . ?
Ca2 O1B C1B O2B 7.0(15) 3_666 . . . ?
Ca2 O1B C1B C2B -172.7(6) . . . . ?
Ca2 O1B C1B C2B -168.8(6) 3_666 . . . ?
Mn1 O2B C1B O1B 30.9(16) . . . . ?
Mn1 O2B C1B C2B -153.5(7) . . . . ?
O1B C1B C2B F3B -87.0(8) . . . . ?
O2B C1B C2B F3B 96.7(10) . . . . ?
O1B C1B C2B F2B 150.7(9) . . . . ?
O2B C1B C2B F2B -25.7(12) . . . . ?
O1B C1B C2B F1B 32.8(10) . . . . ?
O2B C1B C2B F1B -143.6(10) . . . . ?
Ca2 O1BA C1BA O2BA -17(3) . . . . ?
Mn2 O1BA C1BA O2BA -2(2) 3_666 . . . ?
Ca2 O1BA C1BA O2BA -2(2) 3_666 . . . ?
Ca2 O1BA C1BA C2BA 151.2(16) . . . . ?
Mn2 O1BA C1BA C2BA 165.4(12) 3_666 . . . ?
Ca2 O1BA C1BA C2BA 165.4(12) 3_666 . . . ?
Mn2 O1BA C1BA Ca2 14.2(6) 3_666 . . . ?
Ca2 O1BA C1BA Ca2 14.2(6) 3_666 . . . ?
Mn1 O2BA C1BA O1BA 12(2) . . . . ?
Mn1 O2BA C1BA C2BA -156.0(11) . . . . ?
Mn1 O2BA C1BA Ca2 7.4(17) . . . . ?
O1BA C1BA C2BA F3BA 52.2(17) . . . . ?
O2BA C1BA C2BA F3BA -138.3(14) . . . . ?
Ca2 C1BA C2BA F3BA 62.5(18) . . . . ?
O1BA C1BA C2BA F2BA -69.0(16) . . . . ?
O2BA C1BA C2BA F2BA 100.5(15) . . . . ?
Ca2 C1BA C2BA F2BA -58.7(17) . . . . ?
O1BA C1BA C2BA F1BA 175.1(12) . . . . ?
O2BA C1BA C2BA F1BA -15.4(18) . . . . ?
Ca2 C1BA C2BA F1BA -174.6(11) . . . . ?
Mn1 O1C C1C O2C 177.51(15) . . . . ?
Ca1 O1C C1C O2C 0.23(16) 2_645 . . . ?
Mn1 O1C C1C C2C -2.7(3) . . . . ?
Ca1 O1C C1C C2C 179.98(15) 2_645 . . . ?
Mn1 O1C C1C Ca1 177.3(2) . . . 2_645 ?
Ca1 O2C C1C O1C -0.3(2) 2_645 . . . ?
Mn1 O2C C1C O1C -0.3(2) 2_645 . . . ?
Mn2 O2C C1C O1C 172.08(13) 2_645 . . . ?
Ca2 O2C C1C O1C 172.08(13) 2_645 . . . ?
Mn2 O2C C1C O1C -174.52(13) 4_665 . . . ?
Ca2 O2C C1C O1C -174.52(13) 4_665 . . . ?
Ca1 O2C C1C C2C 179.94(11) 2_645 . . . ?
Mn1 O2C C1C C2C 179.94(11) 2_645 . . . ?
Mn2 O2C C1C C2C -7.7(2) 2_645 . . . ?
Ca2 O2C C1C C2C -7.7(2) 2_645 . . . ?
Mn2 O2C C1C C2C 5.7(2) 4_665 . . . ?
Ca2 O2C C1C C2C 5.7(2) 4_665 . . . ?
Mn1 O2C C1C Ca1 0.0 2_645 . . 2_645 ?
Mn2 O2C C1C Ca1 172.39(19) 2_645 . . 2_645 ?
Ca2 O2C C1C Ca1 172.39(19) 2_645 . . 2_645 ?
Mn2 O2C C1C Ca1 -174.21(19) 4_665 . . 2_645 ?
Ca2 O2C C1C Ca1 -174.21(19) 4_665 . . 2_645 ?
O1C C1C C2C F4C -34.8(3) . . . . ?
O2C C1C C2C F4C 145.0(2) . . . . ?
Ca1 C1C C2C F4C 145.2(4) 2_645 . . . ?
O1C C1C C2C F5C 88.3(2) . . . . ?
O2C C1C C2C F5C -91.9(2) . . . . ?
Ca1 C1C C2C F5C -91.7(4) 2_645 . . . ?
O1C C1C C2C F2C 153.5(2) . . . . ?
O2C C1C C2C F2C -26.7(3) . . . . ?
Ca1 C1C C2C F2C -26.6(5) 2_645 . . . ?
O1C C1C C2C F3C -86.6(2) . . . . ?
O2C C1C C2C F3C 93.2(2) . . . . ?
Ca1 C1C C2C F3C 93.3(4) 2_645 . . . ?
O1C C1C C2C F1C 30.2(3) . . . . ?
O2C C1C C2C F1C -150.0(2) . . . . ?
Ca1 C1C C2C F1C -149.9(3) 2_645 . . . ?
O1C C1C C2C F6C -156.5(2) . . . . ?
O2C C1C C2C F6C 23.3(3) . . . . ?
Ca1 C1C C2C F6C 23.5(5) 2_645 . . . ?
F3C C2C F2C Ca2 -91.47(19) . . . 4_665 ?
F1C C2C F2C Ca2 155.32(16) . . . 4_665 ?
C1C C2C F2C Ca2 29.0(2) . . . 4_665 ?
F4C C2C F6C Ca2 -151.3(2) . . . 2_645 ?
F5C C2C F6C Ca2 89.9(2) . . . 2_645 ?
C1C C2C F6C Ca2 -25.6(3) . . . 2_645 ?
F4C C2C F6C Ca2 -158.6(2) . . . 4_665 ?
F5C C2C F6C Ca2 82.6(2) . . . 4_665 ?
C1C C2C F6C Ca2 -32.9(2) . . . 4_665 ?

_refine_diff_density_max         0.822
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.131


# start Validation Reply Form
_vrf_PLAT077_MnCaTFA2-100k-final-5 
;
PROBLEM: Unitcell contains non-integer number of atoms .. Please Check
RESPONSE: The number of Mn and Ca atoms and the ration Ca/Mn are not integer,
but Ca and Mn add to 6 atoms/unit cell as expected for a partial
substitution of Ca for Mn (or viceversa) in the stoichiometric 
Ca(tfa)2.4/3H2O or Mn(tfa)2.4/3H2O.
;
_vrf_PLAT241_MnCaTFA2-100k-final-5 
;
PROBLEM: High MainMol Ueq as Compared to Neighbors of O1W Check
RESPONSE: The crystal used for data collection was a multiple twin that was
modelled as two-component (disregarding minor components), additionally
the unit cell is pseudo-hexagonal and the structure shows more than 80% of
the atoms disordered. This adds to a structural model that required the use
of a significant number of restraints. O1W is a coordinated water molecule
and one of the few ordered atoms in the model, so it is probably affected by 
lower scale disorder that was not considered reasonable to model. 
;
_vrf_PLAT242_MnCaTFA2-100k-final-5 
;
PROBLEM: Low MainMol Ueq as Compared to Neighbors of C2C Check
RESPONSE: C2C is bonded to three F atoms that show rotational disorder, that
was modelled in two different positions 180 deg apart from each-other.
Therefore it is expected it shows a much lower Ueq than the neighbours. This
may also be a consequence of the mayor disorder observed in this crystal 
structure.
;
_vrf_PLAT250_MnCaTFA2-100k-final-5 
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.4 Note
RESPONSE: The crystal used for data collection was a multiple twin that was
modelled as two-component (disregarding minor components), additionally
the unit cell is pseudo-hexagonal and the structure shows more than 80% of
the atoms disordered. This adds to a structural model that required the use
of a significant number of restraints. The observed Uij ellipsoids are 
probably affected by these problems in the crystal structue yielding 
sinificantly elongaded average ellipsoids consistent with the twinning
direction.
;
_vrf_PLAT041_MnCaTFA2-100k-final-5 
;
PROBLEM: Calc. and Reported SumFormula Strings Differ Please Check
RESPONSE: This compound is isostructural with Ca3(tfa)6.4H2O and 
Mn3(tfa)6.4H2O and has been described with the same formulation of
Ca1.72Mn1.28(tfa)6.4H2O with Z=2, Z'=0.5. Checkcif interprets the first two 
compounds automatically with Z=2 but this one with Z=4 for no good 
crystallographic reason so this alert implies no error in our interpretation
of this structure.
;
# end Validation Reply Form # end Validation Reply Form
# END of CIF file
_exptl_crystal_recrystallization_method 'crystallized from synthesis flask'
_chemical_properties_physical    ', Deliquescent'
####################################################################### 
# 
# 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_MgTFA2_143k
_database_code_depnum_ccdc_archive 'CCDC 1505497'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H8 F6 Mg O8'
_chemical_formula_weight         322.41

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'
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'

_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                   8.1395(4)
_cell_length_b                   9.0727(5)
_cell_length_c                   9.3369(5)
_cell_angle_alpha                88.102(3)
_cell_angle_beta                 65.910(2)
_cell_angle_gamma                70.795(2)
_cell_volume                     590.32(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    143(2)
_cell_measurement_reflns_used    9967
_cell_measurement_theta_min      2.394
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.814
_exptl_crystal_F_000             324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.266
_shelx_estimated_absorpt_T_min   0.896
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   'TWINABS (Bruker, 2012)'

_diffrn_ambient_temperature      143(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 8.3333
_diffrn_reflns_number            9250
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.394
_diffrn_reflns_theta_max         28.378
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9250
_reflns_number_gt                7136
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1059P)²+0.2653P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9250
_refine_ls_number_parameters     173
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0603
_refine_ls_wR_factor_ref         0.1773
_refine_ls_wR_factor_gt          0.1581
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_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
Mg1 Mg 0.26488(12) 0.59875(10) 0.39174(11) 0.0211(2) Uani 1 1 d . . . . .
O1W O 0.2968(3) 0.7464(2) 0.2233(3) 0.0310(5) Uani 1 1 d . . . . .
H1 H 0.2622 0.8418 0.2485 0.046 Uiso 1 1 d R U . . .
H1' H 0.2671 0.7311 0.1533 0.046 Uiso 1 1 d R U . . .
O2W O -0.0324(3) 0.7101(2) 0.5063(2) 0.0239(4) Uani 1 1 d . . . . .
H2B H -0.0822 0.8062 0.5112 0.036 Uiso 1 1 d R U . . .
H2A H -0.0824 0.6823 0.5939 0.036 Uiso 1 1 d R U . . .
O2W' O 0.5591(3) 0.4797(2) 0.2904(2) 0.0237(4) Uani 1 1 d . . . . .
H2A' H 0.5941 0.3922 0.3174 0.036 Uiso 1 1 d R U . . .
H2B' H 0.6092 0.4696 0.1915 0.036 Uiso 1 1 d R U . . .
O3W O 0.2441(3) 0.4445(2) 0.5571(2) 0.0253(4) Uani 1 1 d . . . . .
H3 H 0.2989 0.4342 0.6152 0.038 Uiso 1 1 d R U . . .
H3' H 0.1885 0.3821 0.5699 0.038 Uiso 1 1 d R U . . .
O1 O 0.3044(3) 0.7443(2) 0.5354(2) 0.0241(4) Uani 1 1 d . . . . .
O2 O 0.2135(3) 0.9783(2) 0.4501(3) 0.0313(5) Uani 1 1 d . . . . .
C1 C 0.2614(4) 0.8903(3) 0.5405(3) 0.0242(6) Uani 1 1 d . . . . .
C2 C 0.2645(5) 0.9710(4) 0.6823(4) 0.0347(7) Uani 1 1 d . . . . .
F1 F 0.3172(4) 1.0960(3) 0.6452(3) 0.0526(6) Uani 1 1 d . . . . .
F2 F 0.0891(4) 1.0222(4) 0.7988(3) 0.0723(8) Uani 1 1 d . . . . .
F3 F 0.3810(5) 0.8773(3) 0.7366(4) 0.0702(9) Uani 1 1 d . . . . .
O1' O 0.2178(3) 0.4494(2) 0.2569(2) 0.0252(5) Uani 1 1 d . . . . .
O2' O 0.2677(3) 0.5508(2) 0.0276(3) 0.0316(5) Uani 1 1 d . . . . .
C1' C 0.2351(4) 0.4522(3) 0.1171(3) 0.0246(6) Uani 1 1 d . . . . .
C2' C 0.2093(5) 0.3084(4) 0.0536(4) 0.0343(7) Uani 1 1 d . . . . .
F1' F 0.2196(4) 0.3177(3) -0.0905(3) 0.0616(7) Uani 1 1 d . . . . .
F2' F 0.3427(4) 0.1767(3) 0.0509(4) 0.0700(8) Uani 1 1 d . . . . .
F3' F 0.0392(3) 0.2982(3) 0.1455(3) 0.0566(7) 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
Mg1 O1W 2.023(2) . ?
Mg1 O3W 2.042(2) . ?
Mg1 O2W' 2.077(2) . ?
Mg1 O2W 2.090(2) . ?
Mg1 O1 2.097(2) . ?
Mg1 O1' 2.101(2) . ?
O1W H1 0.8262 . ?
O1W H1' 0.8137 . ?
O2W H2B 0.8254 . ?
O2W H2A 0.8247 . ?
O2W' H2A' 0.8200 . ?
O2W' H2B' 0.8366 . ?
O3W H3 0.8179 . ?
O3W H3' 0.8119 . ?
O1 C1 1.251(3) . ?
O2 C1 1.233(4) . ?
C1 C2 1.547(4) . ?
C2 F3 1.309(4) . ?
C2 F1 1.328(4) . ?
C2 F2 1.329(4) . ?
O1' C1' 1.255(4) . ?
O2' C1' 1.222(4) . ?
C1' C2' 1.559(4) . ?
C2' F1' 1.315(4) . ?
C2' F2' 1.316(4) . ?
C2' F3' 1.331(4) . ?

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
O1W Mg1 O3W 177.70(9) . . ?
O1W Mg1 O2W' 89.96(9) . . ?
O3W Mg1 O2W' 87.75(8) . . ?
O1W Mg1 O2W 93.74(9) . . ?
O3W Mg1 O2W 88.55(8) . . ?
O2W' Mg1 O2W 176.25(9) . . ?
O1W Mg1 O1 91.02(9) . . ?
O3W Mg1 O1 89.16(9) . . ?
O2W' Mg1 O1 88.70(8) . . ?
O2W Mg1 O1 90.61(8) . . ?
O1W Mg1 O1' 91.24(9) . . ?
O3W Mg1 O1' 88.62(8) . . ?
O2W' Mg1 O1' 92.48(8) . . ?
O2W Mg1 O1' 88.06(8) . . ?
O1 Mg1 O1' 177.45(8) . . ?
Mg1 O1W H1 120.1 . . ?
Mg1 O1W H1' 116.1 . . ?
H1 O1W H1' 110.0 . . ?
Mg1 O2W H2B 121.2 . . ?
Mg1 O2W H2A 114.1 . . ?
H2B O2W H2A 108.8 . . ?
Mg1 O2W' H2A' 115.3 . . ?
Mg1 O2W' H2B' 114.1 . . ?
H2A' O2W' H2B' 107.0 . . ?
Mg1 O3W H3 122.9 . . ?
Mg1 O3W H3' 125.6 . . ?
H3 O3W H3' 111.4 . . ?
C1 O1 Mg1 126.60(19) . . ?
O2 C1 O1 128.9(3) . . ?
O2 C1 C2 115.9(3) . . ?
O1 C1 C2 115.1(3) . . ?
F3 C2 F1 107.2(3) . . ?
F3 C2 F2 108.4(3) . . ?
F1 C2 F2 106.5(3) . . ?
F3 C2 C1 112.9(3) . . ?
F1 C2 C1 111.9(3) . . ?
F2 C2 C1 109.7(3) . . ?
C1' O1' Mg1 129.5(2) . . ?
O2' C1' O1' 129.0(3) . . ?
O2' C1' C2' 117.4(3) . . ?
O1' C1' C2' 113.6(3) . . ?
F1' C2' F2' 107.6(3) . . ?
F1' C2' F3' 107.4(3) . . ?
F2' C2' F3' 108.1(3) . . ?
F1' C2' C1' 112.4(3) . . ?
F2' C2' C1' 110.7(3) . . ?
F3' C2' C1' 110.6(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 O2 -11.4(4) . . . . ?
Mg1 O1 C1 C2 166.92(19) . . . . ?
O2 C1 C2 F3 -155.3(3) . . . . ?
O1 C1 C2 F3 26.2(4) . . . . ?
O2 C1 C2 F1 -34.2(4) . . . . ?
O1 C1 C2 F1 147.2(3) . . . . ?
O2 C1 C2 F2 83.8(4) . . . . ?
O1 C1 C2 F2 -94.8(3) . . . . ?
Mg1 O1' C1' O2' -7.1(4) . . . . ?
Mg1 O1' C1' C2' 173.24(17) . . . . ?
O2' C1' C2' F1' -2.5(4) . . . . ?
O1' C1' C2' F1' 177.1(3) . . . . ?
O2' C1' C2' F2' 117.8(3) . . . . ?
O1' C1' C2' F2' -62.5(3) . . . . ?
O2' C1' C2' F3' -122.5(3) . . . . ?
O1' C1' C2' F3' 57.2(4) . . . . ?

_refine_diff_density_max         0.729
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.107

####################################################################### 
# 
# 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_MgTFA2_160K_tri
_database_code_depnum_ccdc_archive 'CCDC 1505495'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H8 F6 Mg O8'
_chemical_formula_weight         322.41

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'
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'

_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                   8.142(2)
_cell_length_b                   9.099(3)
_cell_length_c                   9.250(3)
_cell_angle_alpha                87.850(16)
_cell_angle_beta                 67.112(14)
_cell_angle_gamma                69.439(14)
_cell_volume                     587.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    1982
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      23.27

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_F_000             324
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.267
_shelx_estimated_absorpt_T_min   0.896
_shelx_estimated_absorpt_T_max   0.966
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   'TWINABS (Bruker, 2013)'

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 120
_diffrn_reflns_number            5346
_diffrn_reflns_av_unetI/netI     0.0829
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.406
_diffrn_reflns_theta_max         28.383
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.863
_diffrn_measured_fraction_theta_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.863
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.863
_diffrn_reflns_point_group_measured_fraction_full 0.952
_reflns_number_total             5346
_reflns_number_gt                3230
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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          
;
 Refined as a 2-component twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5346
_refine_ls_number_parameters     173
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1512
_refine_ls_R_factor_gt           0.1057
_refine_ls_wR_factor_ref         0.3099
_refine_ls_wR_factor_gt          0.2782
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.083
_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
Mg1 Mg 0.2605(4) 0.5998(3) 0.3930(3) 0.0248(6) Uani 1 1 d . . . . .
O1W O 0.2829(10) 0.7498(6) 0.2290(6) 0.0411(16) Uani 1 1 d . . . . .
H1 H 0.2484 0.8452 0.2541 0.062 Uiso 1 1 d R U . . .
H1' H 0.2532 0.7345 0.1589 0.062 Uiso 1 1 d R U . . .
O2W O -0.0361(8) 0.7087(6) 0.5081(6) 0.0268(13) Uani 1 1 d . . . . .
H2B H -0.0860 0.8048 0.5130 0.040 Uiso 1 1 d R U . . .
H2A H -0.0861 0.6810 0.5957 0.040 Uiso 1 1 d R U . . .
O2W' O 0.5537(7) 0.4824(6) 0.2898(6) 0.0268(13) Uani 1 1 d . . . . .
H2A' H 0.5887 0.3948 0.3168 0.040 Uiso 1 1 d R U . . .
H2B' H 0.6038 0.4723 0.1910 0.040 Uiso 1 1 d R U . . .
O3W O 0.2463(9) 0.4443(6) 0.5575(6) 0.0297(12) Uani 1 1 d . . . . .
H3 H 0.3011 0.4341 0.6157 0.045 Uiso 1 1 d R U . . .
H3' H 0.1907 0.3820 0.5703 0.045 Uiso 1 1 d R U . . .
O1 O 0.2994(8) 0.7444(7) 0.5383(6) 0.0281(14) Uani 1 1 d . . . . .
O2 O 0.2150(9) 0.9774(6) 0.4519(7) 0.0334(15) Uani 1 1 d . . . . .
C1 C 0.2566(12) 0.8894(10) 0.5429(10) 0.028(2) Uani 1 1 d . . . . .
C2 C 0.2671(16) 0.9667(11) 0.6846(13) 0.044(3) Uani 1 1 d . . . . .
F1 F 0.3111(11) 1.0940(7) 0.6522(8) 0.067(2) Uani 1 1 d . . . . .
F2 F 0.0972(11) 1.0085(10) 0.8058(8) 0.098(3) Uani 1 1 d . . . . .
F3 F 0.3912(12) 0.8725(7) 0.7324(9) 0.083(3) Uani 1 1 d . U . . .
O1' O 0.2142(8) 0.4515(6) 0.2574(7) 0.0287(14) Uani 1 1 d . . . . .
O2' O 0.2716(9) 0.5502(7) 0.0259(7) 0.0387(17) Uani 1 1 d . . . . .
C1' C 0.2340(12) 0.4524(10) 0.1172(10) 0.025(2) Uani 1 1 d . . . . .
C2' C 0.2118(15) 0.3098(12) 0.0503(11) 0.039(2) Uani 1 1 d . . . . .
F1' F 0.2169(12) 0.3226(8) -0.0914(7) 0.079(3) Uani 1 1 d . . . . .
F2' F 0.3495(12) 0.1821(8) 0.0436(11) 0.096(3) Uani 1 1 d . . . . .
F3' F 0.0482(10) 0.2975(8) 0.1422(7) 0.073(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
Mg1 O1W 2.000(5) . ?
Mg1 O3W 2.037(5) . ?
Mg1 O2W' 2.065(6) . ?
Mg1 O2W 2.085(6) . ?
Mg1 O1 2.095(5) . ?
Mg1 O1' 2.095(5) . ?
O1W H1 0.8242 . ?
O1W H1' 0.8059 . ?
O2W H2B 0.8188 . ?
O2W H2A 0.8285 . ?
O2W' H2A' 0.8121 . ?
O2W' H2B' 0.8369 . ?
O3W H3 0.8064 . ?
O3W H3' 0.8214 . ?
O1 C1 1.238(10) . ?
O2 C1 1.203(10) . ?
C1 C2 1.555(12) . ?
C2 F3 1.289(12) . ?
C2 F1 1.319(12) . ?
C2 F2 1.331(13) . ?
O1' C1' 1.243(10) . ?
O2' C1' 1.238(10) . ?
C1' C2' 1.553(11) . ?
C2' F2' 1.284(13) . ?
C2' F1' 1.297(12) . ?
C2' F3' 1.313(12) . ?

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
O1W Mg1 O3W 178.3(3) . . ?
O1W Mg1 O2W' 89.5(3) . . ?
O3W Mg1 O2W' 88.8(3) . . ?
O1W Mg1 O2W 94.1(3) . . ?
O3W Mg1 O2W 87.6(3) . . ?
O2W' Mg1 O2W 176.4(2) . . ?
O1W Mg1 O1 90.7(2) . . ?
O3W Mg1 O1 89.1(2) . . ?
O2W' Mg1 O1 89.0(2) . . ?
O2W Mg1 O1 90.8(2) . . ?
O1W Mg1 O1' 91.7(2) . . ?
O3W Mg1 O1' 88.5(2) . . ?
O2W' Mg1 O1' 92.3(2) . . ?
O2W Mg1 O1' 87.7(2) . . ?
O1 Mg1 O1' 177.3(2) . . ?
Mg1 O1W H1 120.9 . . ?
Mg1 O1W H1' 115.6 . . ?
H1 O1W H1' 110.9 . . ?
Mg1 O2W H2B 119.4 . . ?
Mg1 O2W H2A 116.0 . . ?
H2B O2W H2A 108.6 . . ?
Mg1 O2W' H2A' 113.3 . . ?
Mg1 O2W' H2B' 115.9 . . ?
H2A' O2W' H2B' 106.9 . . ?
Mg1 O3W H3 122.7 . . ?
Mg1 O3W H3' 125.5 . . ?
H3 O3W H3' 111.7 . . ?
C1 O1 Mg1 127.0(6) . . ?
O2 C1 O1 129.7(8) . . ?
O2 C1 C2 115.7(7) . . ?
O1 C1 C2 114.5(8) . . ?
F3 C2 F1 106.7(10) . . ?
F3 C2 F2 107.1(10) . . ?
F1 C2 F2 108.1(8) . . ?
F3 C2 C1 113.1(7) . . ?
F1 C2 C1 112.9(9) . . ?
F2 C2 C1 108.8(9) . . ?
C1' O1' Mg1 129.4(6) . . ?
O2' C1' O1' 128.3(7) . . ?
O2' C1' C2' 117.1(7) . . ?
O1' C1' C2' 114.6(8) . . ?
F2' C2' F1' 107.2(8) . . ?
F2' C2' F3' 109.1(10) . . ?
F1' C2' F3' 108.4(9) . . ?
F2' C2' C1' 109.7(9) . . ?
F1' C2' C1' 112.5(9) . . ?
F3' C2' C1' 110.0(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 O2 -14.0(14) . . . . ?
Mg1 O1 C1 C2 168.9(6) . . . . ?
O2 C1 C2 F3 -148.9(10) . . . . ?
O1 C1 C2 F3 28.7(14) . . . . ?
O2 C1 C2 F1 -27.7(13) . . . . ?
O1 C1 C2 F1 149.9(8) . . . . ?
O2 C1 C2 F2 92.3(11) . . . . ?
O1 C1 C2 F2 -90.2(10) . . . . ?
Mg1 O1' C1' O2' -6.5(14) . . . . ?
Mg1 O1' C1' C2' 172.3(6) . . . . ?
O2' C1' C2' F2' 112.5(11) . . . . ?
O1' C1' C2' F2' -66.4(12) . . . . ?
O2' C1' C2' F1' -6.7(13) . . . . ?
O1' C1' C2' F1' 174.4(8) . . . . ?
O2' C1' C2' F3' -127.5(10) . . . . ?
O1' C1' C2' F3' 53.5(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1 O2 0.82 2.10 2.735(7) 133.4 .
O1W H1' O2' 0.81 2.05 2.710(7) 139.5 .
O2W H2B O2 0.82 1.86 2.674(8) 173.5 2_576
O2W H2A O1' 0.83 2.01 2.781(9) 154.3 2_566
O2W H2A F3' 0.83 2.58 3.198(9) 132.0 2_566
O2W' H2A' O1 0.81 2.06 2.778(8) 147.3 2_666
O2W' H2A' F3 0.81 2.43 3.104(8) 141.2 2_666
O2W' H2B' O2' 0.84 1.84 2.679(8) 176.3 2_665
O3W H3 O2W' 0.81 2.06 2.777(7) 148.8 2_666
O3W H3' O2W 0.82 2.07 2.790(7) 146.5 2_566

_refine_diff_density_max         1.508
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.247

####################################################################### 
# 
# 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_MgTFA2_200K
_database_code_depnum_ccdc_archive 'CCDC 1505494'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H4 F3 Mg0.50 O4'
_chemical_formula_weight         161.21

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-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                   13.2595(9)
_cell_length_b                   12.7856(9)
_cell_length_c                   8.1950(7)
_cell_angle_alpha                90
_cell_angle_beta                 120.562(6)
_cell_angle_gamma                90
_cell_volume                     1196.30(17)
_cell_formula_units_Z            8
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    9997
_cell_measurement_theta_min      2.392
_cell_measurement_theta_max      25.95

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.262
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'

_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 120
_diffrn_reflns_number            31440
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.392
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1480
_reflns_number_gt                1159
_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)+(0.1187P)²+0.7162P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1480
_refine_ls_number_parameters     148
_refine_ls_number_restraints     107
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1762
_refine_ls_wR_factor_gt          0.1519
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.391
_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
Mg1 Mg 0.5000 0.60300(7) 0.7500 0.0293(3) Uani 1 2 d S T P . .
O1W O 0.5000 0.76098(17) 0.7500 0.0510(7) Uani 1 2 d DS T P . .
H1 H 0.4486 0.7932 0.7447 0.076 Uiso 1 1 d DR U . . .
O2W O 0.38926(12) 0.59818(10) 0.4568(2) 0.0334(4) Uani 1 1 d D . . . .
H2A H 0.3758 0.5373 0.4430 0.050 Uiso 1 1 d DR U . . .
H2B H 0.3477 0.6473 0.4126 0.050 Uiso 1 1 d DR U . . .
O3W O 0.5000 0.44311(15) 0.7500 0.0349(5) Uani 1 2 d DS T P . .
H3 H 0.5202 0.4092 0.6921 0.052 Uiso 1 1 d DR U . . .
O1 O 0.35689(13) 0.59960(10) 0.7929(2) 0.0339(4) Uani 1 1 d . . . . .
O2 O 0.28465(14) 0.76170(12) 0.7179(3) 0.0451(5) Uani 1 1 d . . . . .
C1 C 0.28340(17) 0.66990(17) 0.7602(3) 0.0339(5) Uani 1 1 d D . . . .
C2 C 0.1772(2) 0.6337(2) 0.7759(4) 0.0495(6) Uani 1 1 d D U . . .
F1 F 0.1228(6) 0.7156(4) 0.8007(13) 0.0686(16) Uani 0.688(17) 1 d D U P A 1
F2 F 0.1016(5) 0.5845(7) 0.6206(9) 0.089(2) Uani 0.688(17) 1 d D U P A 1
F3 F 0.2089(5) 0.5729(6) 0.9238(11) 0.073(2) Uani 0.688(17) 1 d D U P A 1
F1A F 0.0911(12) 0.6984(13) 0.708(3) 0.064(4) Uani 0.205(14) 1 d D U P A 2
F2A F 0.2139(19) 0.615(2) 0.9589(19) 0.080(5) Uani 0.205(14) 1 d D U P A 2
F3A F 0.1361(18) 0.5413(14) 0.692(4) 0.077(5) Uani 0.205(14) 1 d D U P A 2
F1B F 0.0803(15) 0.640(2) 0.606(2) 0.055(5) Uani 0.108(9) 1 d D U P A 3
F2B F 0.155(3) 0.693(3) 0.885(5) 0.086(8) Uani 0.108(9) 1 d D U P A 3
F3B F 0.1782(16) 0.5332(14) 0.821(4) 0.055(5) Uani 0.108(9) 1 d D U P A 3


_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 O1W 2.020(2) . ?
Mg1 O3W 2.044(2) . ?
Mg1 O2W 2.0842(15) . ?
Mg1 O2W 2.0842(15) 2_656 ?
Mg1 O1 2.0987(14) . ?
Mg1 O1 2.0987(14) 2_656 ?
Mg1 H2A 2.3526 . ?
O1W H1 0.7781 . ?
O2W H2A 0.7939 . ?
O2W H2B 0.7914 . ?
O3W H3 0.7836 . ?
O1 C1 1.251(2) . ?
O2 C1 1.226(3) . ?
C1 C2 1.548(3) . ?
C2 F1A 1.285(11) . ?
C2 F2 1.312(5) . ?
C2 F3 1.315(5) . ?
C2 F2B 1.316(16) . ?
C2 F1B 1.332(13) . ?
C2 F3A 1.336(11) . ?
C2 F3B 1.336(14) . ?
C2 F2A 1.343(13) . ?
C2 F1 1.346(5) . ?

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
O1W Mg1 O3W 180.0 . . ?
O1W Mg1 O2W 91.70(4) . . ?
O3W Mg1 O2W 88.30(4) . . ?
O1W Mg1 O2W 91.70(4) . 2_656 ?
O3W Mg1 O2W 88.30(4) . 2_656 ?
O2W Mg1 O2W 176.61(9) . 2_656 ?
O1W Mg1 O1 91.19(4) . . ?
O3W Mg1 O1 88.81(4) . . ?
O2W Mg1 O1 91.45(6) . . ?
O2W Mg1 O1 88.48(6) 2_656 . ?
O1W Mg1 O1 91.19(4) . 2_656 ?
O3W Mg1 O1 88.81(4) . 2_656 ?
O2W Mg1 O1 88.48(6) . 2_656 ?
O2W Mg1 O1 91.45(6) 2_656 2_656 ?
O1 Mg1 O1 177.62(8) . 2_656 ?
O1W Mg1 H2A 110.9 . . ?
O3W Mg1 H2A 69.1 . . ?
O2W Mg1 H2A 19.4 . . ?
O2W Mg1 H2A 157.2 2_656 . ?
O1 Mg1 H2A 88.3 . . ?
O1 Mg1 H2A 90.8 2_656 . ?
Mg1 O1W H1 121.9 . . ?
Mg1 O2W H2A 99.7 . . ?
Mg1 O2W H2B 115.0 . . ?
H2A O2W H2B 131.2 . . ?
Mg1 O3W H3 123.6 . . ?
C1 O1 Mg1 128.44(14) . . ?
O2 C1 O1 128.9(2) . . ?
O2 C1 C2 117.0(2) . . ?
O1 C1 C2 114.2(2) . . ?
F2 C2 F3 109.9(4) . . ?
F2B C2 F1B 104.1(15) . . ?
F1A C2 F3A 107.9(10) . . ?
F2B C2 F3B 109.9(15) . . ?
F1B C2 F3B 102.5(11) . . ?
F1A C2 F2A 109.6(10) . . ?
F3A C2 F2A 103.7(10) . . ?
F2 C2 F1 108.4(3) . . ?
F3 C2 F1 105.4(3) . . ?
F1A C2 C1 114.7(7) . . ?
F2 C2 C1 110.0(3) . . ?
F3 C2 C1 112.0(3) . . ?
F2B C2 C1 114.2(12) . . ?
F1B C2 C1 109.3(9) . . ?
F3A C2 C1 111.8(7) . . ?
F3B C2 C1 115.5(8) . . ?
F2A C2 C1 108.6(9) . . ?
F1 C2 C1 111.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 O2 -10.0(3) . . . . ?
Mg1 O1 C1 C2 169.79(15) . . . . ?
O2 C1 C2 F1A 12.5(12) . . . . ?
O1 C1 C2 F1A -167.3(12) . . . . ?
O2 C1 C2 F2 99.8(6) . . . . ?
O1 C1 C2 F2 -80.0(5) . . . . ?
O2 C1 C2 F3 -137.7(5) . . . . ?
O1 C1 C2 F3 42.4(5) . . . . ?
O2 C1 C2 F2B -51(2) . . . . ?
O1 C1 C2 F2B 129(2) . . . . ?
O2 C1 C2 F1B 64.8(13) . . . . ?
O1 C1 C2 F1B -115.0(13) . . . . ?
O2 C1 C2 F3A 135.8(14) . . . . ?
O1 C1 C2 F3A -44.1(14) . . . . ?
O2 C1 C2 F3B 179.7(16) . . . . ?
O1 C1 C2 F3B -0.2(16) . . . . ?
O2 C1 C2 F2A -110.5(12) . . . . ?
O1 C1 C2 F2A 69.7(12) . . . . ?
O2 C1 C2 F1 -20.2(5) . . . . ?
O1 C1 C2 F1 160.0(4) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2W H2A O1 0.79 2.08 2.792(2) 149.4 6_565
O2W H2B O2 0.79 1.92 2.687(2) 164.8 7_566
O1W H1 O2 0.78 2.11 2.7313(16) 137.1 .
O3W H3 O2W 0.78 2.11 2.7999(16) 147.9 5_666
O1W H1 O2 0.78 2.11 2.7313(16) 137.1 .
O2W H2B O2 0.79 1.92 2.687(2) 164.8 7_566
O2W H2B F1 0.79 2.64 3.131(5) 121.7 7_566
O3W H3 O2W 0.78 2.11 2.7999(16) 147.9 5_666

_refine_diff_density_max         0.673
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_MgTFA2_160k_mon
_database_code_depnum_ccdc_archive 'CCDC 1505496'
loop_
_citation_id
_citation_doi
_citation_year
1 10.1039/C6DT04152C 2017
_audit_update_record             
;
2016-09-21 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H8 F6 Mg O8'
_chemical_formula_weight         322.41

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-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                   13.243(2)
_cell_length_b                   12.8685(19)
_cell_length_c                   8.1543(13)
_cell_angle_alpha                90
_cell_angle_beta                 120.701(7)
_cell_angle_gamma                90
_cell_volume                     1194.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    9503
_cell_measurement_theta_min      2.388
_cell_measurement_theta_max      25.37

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_F_000             648
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    0.263
_shelx_estimated_absorpt_T_min   0.898
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_T_max  0.967
_exptl_absorpt_process_details   'SADABS (Bruker, 2013)'

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker X8 Apex'
_diffrn_measurement_method       'ω and \j scans'
_diffrn_detector_area_resol_mean 120
_diffrn_reflns_number            16302
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         2.388
_diffrn_reflns_theta_max         28.272
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             1402
_reflns_number_gt                841
_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)+(0.0897P)²+22.3022P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.009(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1402
_refine_ls_number_parameters     120
_refine_ls_number_restraints     72
_refine_ls_R_factor_all          0.1612
_refine_ls_R_factor_gt           0.1095
_refine_ls_wR_factor_ref         0.3177
_refine_ls_wR_factor_gt          0.2842
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.095
_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
Mg1 Mg 0.5000 0.6025(2) 0.7500 0.0381(9) Uani 1 2 d S T P . .
O1W O 0.5000 0.7604(6) 0.7500 0.083(4) Uani 1 2 d S TU P . .
H1 H 0.4487 0.7991 0.7465 0.125 Uiso 1 1 d R U . . .
O2W O 0.3885(4) 0.5977(3) 0.4529(7) 0.0400(13) Uani 1 1 d . . . . .
H2A H 0.3586 0.5393 0.4173 0.060 Uiso 1 1 d R U . . .
H2B H 0.3335 0.6400 0.4081 0.060 Uiso 1 1 d R U . . .
O3W O 0.5000 0.4433(5) 0.7500 0.0387(17) Uani 1 2 d S T P . .
H3 H 0.4693 0.4049 0.7938 0.058 Uiso 1 1 d R U . . .
O1 O 0.3572(4) 0.5996(4) 0.7931(7) 0.0406(13) Uani 1 1 d . . . . .
O2 O 0.2863(4) 0.7630(4) 0.7208(9) 0.0520(16) Uani 1 1 d . . . . .
C1 C 0.2840(6) 0.6713(6) 0.7614(11) 0.0434(18) Uani 1 1 d D . . . .
C2 C 0.1768(6) 0.6364(6) 0.7728(12) 0.059(2) Uani 1 1 d D U . . .
F1 F 0.1101(16) 0.7120(13) 0.769(3) 0.083(5) Uani 0.62(4) 1 d D U P A 1
F2 F 0.1129(15) 0.5654(17) 0.645(3) 0.098(5) Uani 0.62(4) 1 d D U P A 1
F3 F 0.2153(11) 0.5826(11) 0.943(2) 0.068(4) Uani 0.62(4) 1 d D U P A 1
F1A F 0.134(2) 0.7153(16) 0.829(4) 0.058(5) Uani 0.38(4) 1 d D U P A 2
F2A F 0.0891(15) 0.613(2) 0.591(2) 0.071(5) Uani 0.38(4) 1 d D U P A 2
F3A F 0.187(2) 0.5514(18) 0.862(5) 0.087(7) Uani 0.38(4) 1 d D U P A 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
Mg1 O1W 2.032(8) . ?
Mg1 O3W 2.049(7) . ?
Mg1 O1 2.094(5) 2_656 ?
Mg1 O1 2.094(5) . ?
Mg1 O2W 2.098(5) 2_656 ?
Mg1 O2W 2.098(5) . ?
O1W H1 0.8306 . ?
O2W H2A 0.8292 . ?
O2W H2B 0.8302 . ?
O3W H3 0.8282 . ?
O1 C1 1.265(8) . ?
O2 C1 1.230(9) . ?
C1 C2 1.536(11) . ?
C2 F3A 1.281(15) . ?
C2 F1 1.304(13) . ?
C2 F2 1.315(12) . ?
C2 F1A 1.354(16) . ?
C2 F2A 1.371(14) . ?
C2 F3 1.391(13) . ?

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
O1W Mg1 O3W 180.0 . . ?
O1W Mg1 O1 91.01(15) . 2_656 ?
O3W Mg1 O1 88.99(15) . 2_656 ?
O1W Mg1 O1 91.01(15) . . ?
O3W Mg1 O1 88.99(15) . . ?
O1 Mg1 O1 178.0(3) 2_656 . ?
O1W Mg1 O2W 91.70(15) . 2_656 ?
O3W Mg1 O2W 88.30(15) . 2_656 ?
O1 Mg1 O2W 91.72(19) 2_656 2_656 ?
O1 Mg1 O2W 88.22(19) . 2_656 ?
O1W Mg1 O2W 91.70(15) . . ?
O3W Mg1 O2W 88.30(15) . . ?
O1 Mg1 O2W 88.22(19) 2_656 . ?
O1 Mg1 O2W 91.72(19) . . ?
O2W Mg1 O2W 176.6(3) 2_656 . ?
Mg1 O1W H1 126.8 . . ?
Mg1 O2W H2A 111.1 . . ?
Mg1 O2W H2B 115.5 . . ?
H2A O2W H2B 106.5 . . ?
Mg1 O3W H3 126.6 . . ?
C1 O1 Mg1 128.0(5) . . ?
O2 C1 O1 129.3(7) . . ?
O2 C1 C2 116.6(6) . . ?
O1 C1 C2 114.2(6) . . ?
F1 C2 F2 110.1(11) . . ?
F3A C2 F1A 112.9(17) . . ?
F3A C2 F2A 102.2(14) . . ?
F1A C2 F2A 105.2(13) . . ?
F1 C2 F3 107.1(11) . . ?
F2 C2 F3 101.6(10) . . ?
F3A C2 C1 116.7(12) . . ?
F1 C2 C1 114.6(11) . . ?
F2 C2 C1 113.4(10) . . ?
F1A C2 C1 111.3(12) . . ?
F2A C2 C1 107.3(10) . . ?
F3 C2 C1 109.0(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Mg1 O1 C1 O2 -10.0(12) . . . . ?
Mg1 O1 C1 C2 168.9(5) . . . . ?
O2 C1 C2 F3A -162(2) . . . . ?
O1 C1 C2 F3A 19(2) . . . . ?
O2 C1 C2 F1 -10.8(16) . . . . ?
O1 C1 C2 F1 170.1(13) . . . . ?
O2 C1 C2 F2 116.8(16) . . . . ?
O1 C1 C2 F2 -62.2(16) . . . . ?
O2 C1 C2 F1A -30.6(16) . . . . ?
O1 C1 C2 F1A 150.4(14) . . . . ?
O2 C1 C2 F2A 84.0(15) . . . . ?
O1 C1 C2 F2A -95.1(15) . . . . ?
O2 C1 C2 F3 -130.8(11) . . . . ?
O1 C1 C2 F3 50.1(12) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1 O2 0.83 2.10 2.717(5) 130.3 .
O2W H2A O1 0.83 2.05 2.786(7) 147.7 6_565
O2W H2A F3 0.83 2.55 3.233(13) 140.5 6_565
O2W H2A F3A 0.83 2.38 3.05(2) 138.5 6_565
O2W H2B O2 0.83 1.86 2.689(6) 171.9 7_566
O3W H3 O2W 0.83 2.06 2.773(5) 144.0 6_566

_refine_diff_density_max         0.544
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.133

