# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_compound_2b
_database_code_depnum_ccdc_archive 'CCDC 1846358'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;
#===================================================================
#===================================================================
# 5. CHEMICAL DATA
#===================================================================

_chemical_name_systematic        
;
 
;
_chemical_name_common            ?
_chemical_formula_moiety         'C11 H12 F3 O5 Re'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C11 H12 F3 O5 Re'
_chemical_formula_weight         467.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Re Re -1.0185 7.2310 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===================================================================
# 6. CRYSTAL DATA
#===================================================================

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_Int_Tables_number      15

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,y,1/2-z
3 -x,-y,-z
4 x,-y,1/2+z
5 1/2+x,1/2+y,z
6 1/2-x,1/2+y,1/2-z
7 1/2-x,1/2-y,-z
8 1/2+x,1/2-y,1/2+z

_cell_length_a                   16.0247(4)
_cell_length_b                   6.6973(1)
_cell_length_c                   24.9223(6)
_cell_angle_alpha                90
_cell_angle_beta                 91.1148(11)
_cell_angle_gamma                90
_cell_volume                     2674.21(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    9659
_cell_measurement_theta_min      1.63
_cell_measurement_theta_max      25.49

_exptl_crystal_description       fragment
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.322
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1760
_exptl_absorpt_coefficient_mu    9.139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5109
_exptl_absorpt_correction_T_max  0.7452

_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'

_exptl_special_details           
;
Diffractometer operator             E. Herdtweck
scanspeed                           5 s per frame
dx                                  50
3626 frames measured in 8 data sets
phi-scan with delta_phi         = 0.50
omega-scans with delta_omega    = 0.50
;

#===================================================================
# 7. EXPERIMENTAL DATA
#===================================================================

_diffrn_ambient_temperature      123(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16 # 8 for binned mode

_diffrn_standards_decay_%        0
# number of measured reflections (redundant set)
_diffrn_reflns_number            26944
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         25.49
_reflns_number_total             2496
_reflns_number_gt                2413

# number of observed reflections (> n sig(I))
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2010)'
_computing_publication_material  'PLATON (Spek, 2010)'

#===================================================================
# 8. REFINEMENT DATA
#===================================================================

_refine_special_details          
;
 Refinement on F² for ALL reflections except for 0 with very negative F²
 or flagged by the user for potential systematic errors.  Weighted R-factors
 wR and all goodnesses of fit S are based on F², conventional R-factors R
 are based on F, with F set to zero for negative F². The observed criterion
 of F² > 2sigma(F²) is used only for calculating  R_factor_obs etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0045P)²+8.3211P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000593(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2496
_refine_ls_number_parameters     182
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0138
_refine_ls_R_factor_gt           0.0130
_refine_ls_wR_factor_ref         0.0293
_refine_ls_wR_factor_gt          0.0290
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 1.000

_refine_diff_density_max         0.532
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.070

#===================================================================
# 9. ATOMIC COORDINATES AND THERMAL PARAMETERS
#===================================================================

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Re1 Re Uani 0.34897(1) 0.57113(1) 0.11518(1) 1.000 0.0151(1) . .
F1 F Uani 0.45529(14) 1.2692(3) 0.30521(7) 1.000 0.0516(7) . .
F2 F Uani 0.41546(11) 1.2526(3) 0.38686(7) 1.000 0.0360(6) . .
F3 F Uani 0.49210(12) 1.0259(3) 0.35439(8) 1.000 0.0449(7) . .
O1 O Uani 0.45259(13) 0.5823(3) 0.10249(9) 1.000 0.0346(7) . .
O2 O Uani 0.31192(14) 0.3509(3) 0.13972(8) 1.000 0.0281(6) . .
O3 O Uani 0.28426(13) 0.7246(3) 0.07895(7) 1.000 0.0277(6) . .
O4 O Uani 0.34305(12) 0.3835(3) 0.03403(7) 1.000 0.0207(6) . .
O5 O Uani 0.35929(12) 1.0507(3) 0.32983(8) 1.000 0.0248(6) . .
C1 C Uani 0.35011(16) 0.7312(4) 0.18639(10) 1.000 0.0166(8) . .
C2 C Uani 0.31574(17) 0.9212(4) 0.18958(11) 1.000 0.0194(8) . .
C3 C Uani 0.32060(17) 1.0286(4) 0.23707(11) 1.000 0.0203(8) . .
C4 C Uani 0.35917(17) 0.9427(4) 0.28113(11) 1.000 0.0199(8) . .
C5 C Uani 0.39268(17) 0.7533(4) 0.27982(11) 1.000 0.0219(9) . .
C6 C Uani 0.38812(17) 0.6487(4) 0.23218(11) 1.000 0.0210(8) . .
C7 C Uani 0.42929(18) 1.1476(4) 0.34312(11) 1.000 0.0221(8) . .
C8 C Uani 0.3824(2) 0.1900(4) 0.03305(12) 1.000 0.0303(10) . .
C9 C Uani 0.3889(3) 0.1339(5) -0.02509(13) 1.000 0.0430(13) . .
C10 C Uani 0.35949(19) 0.3130(5) -0.05654(11) 1.000 0.0282(10) . .
C11 C Uani 0.36210(19) 0.4804(4) -0.01618(11) 1.000 0.0247(9) . .
H21 H Uiso 0.28870 0.97800 0.15890 1.000 0.0230 calc R
H31 H Uiso 0.29770 1.15920 0.23920 1.000 0.0240 calc R
H51 H Uiso 0.41820 0.69620 0.31090 1.000 0.0260 calc R
H61 H Uiso 0.41120 0.51820 0.23050 1.000 0.0250 calc R
H81 H Uiso 0.34840 0.09080 0.05230 1.000 0.0360 calc R
H82 H Uiso 0.43850 0.19600 0.05030 1.000 0.0360 calc R
H91 H Uiso 0.35340 0.01660 -0.03340 1.000 0.0510 calc R
H92 H Uiso 0.44730 0.10110 -0.03380 1.000 0.0510 calc R
H101 H Uiso 0.30210 0.29260 -0.07090 1.000 0.0340 calc R
H102 H Uiso 0.39700 0.34090 -0.08670 1.000 0.0340 calc R
H111 H Uiso 0.41810 0.54300 -0.01440 1.000 0.0300 calc R
H112 H Uiso 0.32010 0.58390 -0.02530 1.000 0.0300 calc R

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.0173(1) 0.0133(1) 0.0146(1) 0.0008(1) 0.0000(1) 0.0006(1)
F1 0.0794(16) 0.0474(12) 0.0277(10) 0.0109(9) -0.0059(10) -0.0364(11)
F2 0.0427(11) 0.0363(10) 0.0290(10) -0.0176(8) 0.0020(8) -0.0062(8)
F3 0.0340(11) 0.0463(12) 0.0538(13) -0.0167(10) -0.0156(10) 0.0099(9)
O1 0.0207(11) 0.0490(14) 0.0342(13) -0.0190(10) 0.0049(10) -0.0031(10)
O2 0.0487(13) 0.0184(10) 0.0171(10) 0.0023(8) 0.0010(9) -0.0061(9)
O3 0.0407(12) 0.0246(11) 0.0177(10) 0.0001(8) -0.0054(9) 0.0120(9)
O4 0.0267(11) 0.0195(10) 0.0160(10) 0.0013(8) 0.0010(8) 0.0022(8)
O5 0.0223(11) 0.0305(11) 0.0216(11) -0.0111(8) 0.0038(8) -0.0041(8)
C1 0.0172(13) 0.0159(13) 0.0169(13) -0.0012(10) 0.0028(11) -0.0033(10)
C2 0.0208(14) 0.0185(13) 0.0189(14) 0.0027(11) 0.0007(12) 0.0004(11)
C3 0.0203(14) 0.0148(13) 0.0259(15) -0.0023(11) 0.0021(12) 0.0012(10)
C4 0.0158(14) 0.0243(15) 0.0196(14) -0.0064(11) 0.0037(11) -0.0046(11)
C5 0.0234(15) 0.0255(16) 0.0167(14) 0.0005(11) -0.0024(12) 0.0016(11)
C6 0.0225(14) 0.0181(13) 0.0223(15) -0.0011(11) -0.0021(12) 0.0034(11)
C7 0.0266(16) 0.0215(14) 0.0182(14) -0.0007(11) 0.0001(12) -0.0011(12)
C8 0.0428(19) 0.0233(15) 0.0249(16) -0.0040(12) 0.0015(14) 0.0107(14)
C9 0.064(3) 0.0365(19) 0.0286(18) -0.0112(15) 0.0054(17) 0.0092(18)
C10 0.0258(16) 0.0422(19) 0.0168(14) -0.0052(13) 0.0026(12) -0.0077(14)
C11 0.0296(16) 0.0272(15) 0.0171(14) 0.0052(12) -0.0007(12) -0.0004(13)

#==================================================================
# 10. MOLECULAR GEOMETRY
#===================================================================

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.698(2) . . yes
Re1 O2 1.708(2) . . yes
Re1 O3 1.706(2) . . yes
Re1 O4 2.3814(18) . . yes
Re1 C1 2.073(3) . . yes
F1 C7 1.321(3) . . yes
F2 C7 1.320(3) . . yes
F3 C7 1.321(3) . . yes
O4 C8 1.442(3) . . yes
O4 C11 1.447(3) . . yes
O5 C4 1.413(3) . . yes
O5 C7 1.332(3) . . yes
C1 C2 1.390(4) . . no
C1 C6 1.397(4) . . no
C2 C3 1.386(4) . . no
C3 C4 1.376(4) . . no
C4 C5 1.378(4) . . no
C5 C6 1.379(4) . . no
C8 C9 1.503(4) . . no
C9 C10 1.504(5) . . no
C10 C11 1.506(4) . . no
C2 H21 0.9500 . . no
C3 H31 0.9500 . . no
C5 H51 0.9500 . . no
C6 H61 0.9500 . . no
C8 H81 0.9900 . . no
C8 H82 0.9900 . . no
C9 H91 0.9900 . . no
C9 H92 0.9900 . . no
C10 H101 0.9900 . . no
C10 H102 0.9900 . . no
C11 H111 0.9900 . . no
C11 H112 0.9900 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Re1 O2 116.93(10) . . . yes
O1 Re1 O3 117.48(10) . . . yes
O1 Re1 O4 83.57(9) . . . yes
O1 Re1 C1 98.30(10) . . . yes
O2 Re1 O3 119.86(10) . . . yes
O2 Re1 O4 80.79(8) . . . yes
O2 Re1 C1 97.90(10) . . . yes
O3 Re1 O4 81.64(8) . . . yes
O3 Re1 C1 97.86(10) . . . yes
O4 Re1 C1 178.08(8) . . . yes
Re1 O4 C8 118.59(16) . . . yes
Re1 O4 C11 119.48(15) . . . yes
C8 O4 C11 106.8(2) . . . yes
C4 O5 C7 116.8(2) . . . yes
Re1 C1 C2 121.71(19) . . . yes
Re1 C1 C6 119.42(19) . . . yes
C2 C1 C6 118.9(2) . . . no
C1 C2 C3 120.6(2) . . . no
C2 C3 C4 118.8(2) . . . no
O5 C4 C3 117.7(2) . . . yes
O5 C4 C5 119.8(2) . . . yes
C3 C4 C5 122.4(3) . . . no
C4 C5 C6 118.3(3) . . . no
C1 C6 C5 121.2(2) . . . no
F1 C7 F2 108.8(2) . . . yes
F1 C7 F3 106.4(2) . . . yes
F1 C7 O5 113.5(2) . . . yes
F2 C7 F3 107.0(2) . . . yes
F2 C7 O5 108.1(2) . . . yes
F3 C7 O5 112.8(2) . . . yes
O4 C8 C9 106.2(2) . . . yes
C8 C9 C10 106.0(3) . . . no
C9 C10 C11 104.0(2) . . . no
O4 C11 C10 103.9(2) . . . yes
C1 C2 H21 120.00 . . . no
C3 C2 H21 120.00 . . . no
C2 C3 H31 121.00 . . . no
C4 C3 H31 121.00 . . . no
C4 C5 H51 121.00 . . . no
C6 C5 H51 121.00 . . . no
C1 C6 H61 119.00 . . . no
C5 C6 H61 119.00 . . . no
O4 C8 H81 111.00 . . . no
O4 C8 H82 110.00 . . . no
C9 C8 H81 110.00 . . . no
C9 C8 H82 110.00 . . . no
H81 C8 H82 109.00 . . . no
C8 C9 H91 110.00 . . . no
C8 C9 H92 111.00 . . . no
C10 C9 H91 111.00 . . . no
C10 C9 H92 111.00 . . . no
H91 C9 H92 109.00 . . . no
C9 C10 H101 111.00 . . . no
C9 C10 H102 111.00 . . . no
C11 C10 H101 111.00 . . . no
C11 C10 H102 111.00 . . . no
H101 C10 H102 109.00 . . . no
O4 C11 H111 111.00 . . . no
O4 C11 H112 111.00 . . . no
C10 C11 H111 111.00 . . . no
C10 C11 H112 111.00 . . . no
H111 C11 H112 109.00 . . . no

_iucr_refine_instructions_details 
;
;
# End of Crystallographic Information File

####################################################################### 
# 
# 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_compound_5
_database_code_depnum_ccdc_archive 'CCDC 1846359'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H18 N O3 Re'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C9 H18 N O3 Re'
_chemical_formula_iupac          ?
_chemical_formula_weight         374.45
_chemical_compound_source        'see text'

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'
N N 0.0061 0.0033 ' 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'
Re Re -1.0185 7.2310 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_symmetry_Int_Tables_number      62

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 1/2-x,-y,1/2+z
3 1/2+x,1/2-y,1/2-z
4 -x,1/2+y,-z
5 -x,-y,-z
6 1/2+x,y,1/2-z
7 1/2-x,1/2+y,1/2+z
8 x,1/2-y,z

_cell_length_a                   10.2640(3)
_cell_length_b                   13.0928(4)
_cell_length_c                   8.2318(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1106.23(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    123
_cell_measurement_reflns_used    9969
_cell_measurement_theta_min      2.4742
_cell_measurement_theta_max      36.3344
_cell_special_details            
;
;

_exptl_crystal_description       block
_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.300
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.248
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             712
_exptl_absorpt_coefficient_mu    10.968
_exptl_crystal_density_meas_temp ?

# Permitted for _exptl_absorpt_correction_type :
# analytical     'analytical from crystal shape'
#                Example: de Meulenaer&Tompa: ABST
# cylinder       'cylindrical'
# gaussian       'Gaussian from crystal shape'
#                Example: PLATON/ABSG
# integration    'integration from crystal shape'
# multi-scan     'symmetry-related measurements'
#                Example: SADABS, MULABS
# none           'no absorption corr. applied'
# numerical      'numerical from crystal shape'
# psi-scan       'psi-scan corrections'
#                Example: PLATON/ABSP
# refdelf        'refined from delta-F'
#                Example: SHELXA,
# sphere         'spherical'
#                Example: PLATON/ABSS
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.4420
_exptl_absorpt_correction_T_max  0.7471

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             M.Kaposi
scanspeed                           5 s per frame
dx                                  35 mm
6241 frames measured in 17 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            85048
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0150
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         36.46
_diffrn_reflns_theta_full        36.46
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             2782
# number of observed reflections (> n sig(I))
_reflns_number_gt                2641
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  
'SHELXL97 (Sheldrick, 2008), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+1.5148P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom


# Permitted for _refine_ls_hydrogen_treatment :
# refall            - refined all H-atom parameters
# refxyz            - refined H-atom coordinates only
# refU              - refined H-atom U only
# noref             - no refinement of H-atom parameters
# constr            - H-atom parameters constrained
# hetero            - H-atom parameters constrained for H on C,
#                     all H-atom parameters refined for H on
#                     heteroatoms
# heteroxyz         - H-atom parameters constrained for H on C,
#                     refined H-atom coordinates only for H
#                     on heteroatoms
# heteroU           - H-atom parameters constrained for H on C,
#                     refined H-atom U's only for H on
#                     heteroatoms
# heteronoref       - H-atom parameters constrained for H on C,
#                     no refinement of H-atom parameters for
#                     H on heteroatoms
# hetero-mixed      - H-atom parameters constrained for H on C
#                     and some heteroatoms, all H-atom
#                     parameters refined for H on remaining
#                     heteroatoms.
# heteroxyz-mixed   - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     coordinates only for H on remaining
#                     heteroatoms.
# heteroU-mixed     - H-atom parameters constrained for H on C
#                     and some heteroatoms, refined H-atom
#                     U's only for H on remaining heteroatoms
# heteronoref-mixed - H-atom parameters constrained for H on C
#                     and some heteroatoms, no refinement of
#                     H-atom parameters for H on remaining
#                     heteroatoms
# mixed   - some constrained, some independent
# undef   - H-atom parameters not defined
_refine_ls_hydrogen_treatment    noref

_refine_ls_extinction_method     shelxl
_refine_ls_extinction_coef       0.00792(12)
_refine_ls_extinction_expression FC^*^=KFC[1+0.001XFC²Λ³/SIN(2Θ)]^-1/4^
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         2782
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0154
_refine_ls_R_factor_gt           0.0138
_refine_ls_wR_factor_ref         0.0294
_refine_ls_wR_factor_gt          0.0290
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.515
_refine_diff_density_min         -1.726
_refine_diff_density_rms         0.111

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re1 Re Uani 0.86700(1) 0.25000 1.20788(1) 1.000 0.0115(1) d S . .
O1 O Uani 1.03407(16) 0.25000 1.1943(2) 1.000 0.0243(5) d S . .
O2 O Uani 0.81998(13) 0.35654(10) 1.31163(14) 1.000 0.0232(3) d . . .
N1 N Uani 0.79519(15) 0.25000 0.99447(18) 1.000 0.0088(3) d S . .
C1 C Uani 0.75953(13) 0.35208(10) 0.91705(16) 1.000 0.0113(3) d . . .
C2 C Uani 0.74844(15) 0.34268(13) 0.73225(18) 1.000 0.0179(4) d . . .
C3 C Uani 0.6734(2) 0.25000 0.6752(3) 1.000 0.0203(6) d S . .
C4 C Uani 0.86922(15) 0.42866(11) 0.9502(2) 1.000 0.0175(3) d . . .
C5 C Uani 0.63080(14) 0.39113(12) 0.98847(19) 1.000 0.0175(4) d . . .
H2A H Uiso 0.70530 0.40470 0.68950 1.000 0.0210 c R . .
H2B H Uiso 0.83720 0.34010 0.68550 1.000 0.0210 c R . .
H3A H Uiso 0.66610 0.25000 0.55530 1.000 0.0240 c SR . .
H3B H Uiso 0.58460 0.25000 0.72210 1.000 0.0240 c SR . .
H4A H Uiso 0.95180 0.40100 0.90980 1.000 0.0260 c R . .
H4B H Uiso 0.87590 0.44080 1.06740 1.000 0.0260 c R . .
H4C H Uiso 0.85010 0.49310 0.89470 1.000 0.0260 c R . .
H5A H Uiso 0.61120 0.45870 0.94350 1.000 0.0260 c R . .
H5B H Uiso 0.63850 0.39600 1.10690 1.000 0.0260 c R . .
H5C H Uiso 0.56050 0.34360 0.96060 1.000 0.0260 c R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.0106(1) 0.0167(1) 0.0071(1) 0.0000 -0.0018(1) 0.0000
O1 0.0120(6) 0.0465(11) 0.0144(7) 0.0000 -0.0034(5) 0.0000
O2 0.0272(6) 0.0262(6) 0.0163(5) -0.0093(4) -0.0009(4) 0.0008(5)
N1 0.0106(6) 0.0084(6) 0.0074(6) 0.0000 -0.0008(5) 0.0000
C1 0.0109(5) 0.0100(5) 0.0130(5) 0.0031(4) 0.0005(4) 0.0008(4)
C2 0.0179(6) 0.0231(7) 0.0126(6) 0.0073(5) -0.0012(5) -0.0002(5)
C3 0.0175(9) 0.0321(12) 0.0112(8) 0.0000 -0.0048(7) 0.0000
C4 0.0166(6) 0.0114(5) 0.0246(7) 0.0019(5) 0.0017(5) -0.0034(5)
C5 0.0134(6) 0.0167(6) 0.0224(7) 0.0030(5) 0.0025(5) 0.0049(5)

#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.7185(16) . . yes
Re1 O2 1.7053(13) . . yes
Re1 N1 1.9051(15) . . yes
Re1 O2 1.7053(13) . 8_555 yes
N1 C1 1.5253(15) . . yes
N1 C1 1.5253(15) . 8_555 yes
C1 C2 1.530(2) . . no
C1 C4 1.532(2) . . no
C1 C5 1.534(2) . . no
C2 C3 1.512(2) . . no
C2 H2A 0.9900 . . no
C2 H2B 0.9900 . . no
C3 H3A 0.9900 . . no
C3 H3B 0.9900 . . no
C4 H4A 0.9800 . . no
C4 H4B 0.9800 . . no
C4 H4C 0.9800 . . no
C5 H5A 0.9800 . . no
C5 H5B 0.9800 . . no
C5 H5C 0.9800 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Re1 O2 108.36(5) . . . yes
O1 Re1 N1 109.03(7) . . . yes
O1 Re1 O2 108.36(5) . . 8_555 yes
O2 Re1 N1 110.63(5) . . . yes
O2 Re1 O2 109.77(6) . . 8_555 yes
O2 Re1 N1 110.63(5) 8_555 . . yes
Re1 N1 C1 118.56(7) . . . yes
Re1 N1 C1 118.56(7) . . 8_555 yes
C1 N1 C1 122.39(12) . . 8_555 yes
N1 C1 C2 111.27(11) . . . yes
N1 C1 C4 108.83(11) . . . yes
N1 C1 C5 109.79(12) . . . yes
C2 C1 C4 106.52(12) . . . no
C2 C1 C5 110.10(12) . . . no
C4 C1 C5 110.28(11) . . . no
C1 C2 C3 114.28(14) . . . no
C2 C3 C2 106.75(16) . . 8_555 no
C1 C2 H2A 109.00 . . . no
C1 C2 H2B 109.00 . . . no
C3 C2 H2A 109.00 . . . no
C3 C2 H2B 109.00 . . . no
H2A C2 H2B 108.00 . . . no
C2 C3 H3A 110.00 . . . no
C2 C3 H3B 110.00 . . . no
H3A C3 H3B 109.00 . . . no
C2 C3 H3A 110.00 8_555 . . no
C2 C3 H3B 110.00 8_555 . . no
C1 C4 H4A 109.00 . . . no
C1 C4 H4B 109.00 . . . no
C1 C4 H4C 109.00 . . . no
H4A C4 H4B 109.00 . . . no
H4A C4 H4C 109.00 . . . no
H4B C4 H4C 109.00 . . . no
C1 C5 H5A 109.00 . . . no
C1 C5 H5B 109.00 . . . no
C1 C5 H5C 109.00 . . . no
H5A C5 H5B 109.00 . . . no
H5A C5 H5C 109.00 . . . no
H5B C5 H5C 109.00 . . . no

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
O1 Re1 N1 C1 -93.89(11) . . . . no
O2 Re1 N1 C1 25.18(13) . . . . no
O2 Re1 N1 C1 -147.04(11) . . . 8_555 no
O2 Re1 N1 C1 147.04(11) 8_555 . . . no
Re1 N1 C1 C2 160.59(10) . . . . no
C1 N1 C1 C2 -27.52(18) 8_555 . . . no
Re1 N1 C1 C4 43.52(15) . . . . no
C1 N1 C1 C4 -144.58(13) 8_555 . . . no
Re1 N1 C1 C5 -77.27(14) . . . . no
C1 N1 C1 C5 94.63(15) 8_555 . . . no
N1 C1 C2 C3 45.03(17) . . . . no
C4 C1 C2 C3 163.50(13) . . . . no
C5 C1 C2 C3 -76.93(16) . . . . no
C1 C2 C3 C2 -62.69(19) . . . 8_555 no

_iucr_refine_instructions_details 
;
TITL LiSu4_0ma in Pnma
CELL 0.71073 10.2640 13.0928 8.2318 90.000 90.000 90.000
ZERR 8.00 0.0003 0.0004 0.0002 0.000 0.000 0.000
LATT 1
SYMM x+1/2, -y+1/2, -z+1/2
SYMM -x, y+1/2, -z
SYMM -x+1/2, -y, z+1/2
SFAC C H N O RE
UNIT 36 72 4 12 4
LIST 4
TEMP -150.150
SIZE 0.297 0.342 0.411
ACTA
L.S. 4
FMAP 2
PLAN -20
HTAB
BOND $H
CONF
 WGHT      0.0000      1.5148 
WGHT      0.0000      1.5148 
EXTI    0.007925
FVAR       0.12321
RE1   5    0.866995    0.250000    1.207878    10.50000    0.01060    0.01673 =
         0.00712    0.00000   -0.00178    0.00000
O1    4    1.034070    0.250000    1.194312    10.50000    0.01202    0.04646 =
         0.01439    0.00000   -0.00343    0.00000
C1    1    0.759526    0.352080    0.917047    11.00000    0.01092    0.01004 =
         0.01303    0.00310    0.00054    0.00085
C2    1    0.748435    0.342681    0.732255    11.00000    0.01787    0.02308 =
         0.01258    0.00731   -0.00125   -0.00019
AFIX  23
H2A   2    0.705265    0.404733    0.689527    11.00000   -1.20000
H2B   2    0.837250    0.340056    0.685534    11.00000   -1.20000
AFIX   0
O2    4    0.819980    0.356537    1.311630    11.00000    0.02719    0.02617 =
         0.01626   -0.00927   -0.00093    0.00084
N1    3    0.795189    0.250000    0.994469    10.50000    0.01059    0.00843 =
         0.00743    0.00000   -0.00083    0.00000
C3    1    0.673425    0.250000    0.675231    10.50000    0.01755    0.03211 =
         0.01116    0.00000   -0.00482    0.00000
AFIX  23
H3A   2    0.666138    0.250000    0.555309    10.50000   -1.20000
H3B   2    0.584591    0.250000    0.722081    10.50000   -1.20000
AFIX   0
C4    1    0.869219    0.428657    0.950228    11.00000    0.01661    0.01136 =
         0.02459    0.00185    0.00170   -0.00342
AFIX 137
H4A   2    0.951809    0.401000    0.909814    11.00000   -1.50000
H4B   2    0.875927    0.440810    1.067401    11.00000   -1.50000
H4C   2    0.850083    0.493143    0.894693    11.00000   -1.50000
AFIX   0
C5    1    0.630800    0.391126    0.988467    11.00000    0.01344    0.01668 =
         0.02243    0.00298    0.00252    0.00490
AFIX 137
H5A   2    0.611173    0.458710    0.943530    11.00000   -1.50000
H5B   2    0.638510    0.395991    1.106876    11.00000   -1.50000
H5C   2    0.560471    0.343623    0.960625    11.00000   -1.50000
HKLF 4 1 1 0 0 0 1 0 0 0 1
 
REM  LiSu4_0ma in Pnma
REM R1 =  0.0138 for   2641 Fo > 4sig(Fo)  and  0.0154 for all   2782 data
REM     73 parameters refined using      0 restraints
 
END  
     
WGHT      0.0000      1.5148 
REM Highest difference peak  1.515,  deepest hole -1.726,  1-sigma level  0.111
Q1    1   0.8954  0.2843  1.1864  11.00000  0.05    1.51
Q2    1   0.8560  0.2500  1.2896  10.50000  0.05    1.11
Q3    1   0.8133  0.2765  1.1997  11.00000  0.05    0.77
Q4    1   0.8579  0.1836  1.2671  11.00000  0.05    0.73
Q5    1   0.8562  0.2500  1.1141  10.50000  0.05    0.69
Q6    1   0.9689  0.2500  1.1634  10.50000  0.05    0.64
Q7    1   0.8648  0.2500  1.0300  10.50000  0.05    0.61
Q8    1   0.9626  0.2500  1.2492  10.50000  0.05    0.52
Q9    1   0.8719  0.1688  1.3325  11.00000  0.05    0.51
Q10   1   0.6928  0.3713  0.9407  11.00000  0.05    0.49
Q11   1   0.7551  0.2500  1.2680  10.50000  0.05    0.48
Q12   1   0.7076  0.2944  0.7025  11.00000  0.05    0.47
Q13   1   0.8229  0.2132  1.2841  11.00000  0.05    0.46
Q14   1   0.8570  0.1228  1.2664  11.00000  0.05    0.43
Q15   1   0.9872  0.2500  1.0802  10.50000  0.05    0.41
Q16   1   0.8177  0.3890  0.9340  11.00000  0.05    0.41
Q17   1   0.7599  0.3329  0.8206  11.00000  0.05    0.38
Q18   1   0.7827  0.1693  1.2843  11.00000  0.05    0.37
Q19   1   0.8880  0.2500  1.4739  10.50000  0.05    0.34
Q20   1   0.8639  0.3277  1.1510  11.00000  0.05    0.33
;

#===END
####################################################################### 
# 
# 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_compound_1b
_database_code_depnum_ccdc_archive 'CCDC 1846360'
_audit_update_record             
;
2018-06-04 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;

#===============================================================================

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C11 H12 F3 O4 Re'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural     ?
_chemical_formula_sum            'C11 H12 F3 O4 Re'
_chemical_formula_iupac          ?
_chemical_formula_weight         451.47
_chemical_compound_source        'see text'

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'
F F 0.0171 0.0103 ' 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'
Re Re -1.0185 7.2310 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

#===============================================================================

# 6. CRYSTAL DATA

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   6.6339(6)
_cell_length_b                   9.8331(9)
_cell_length_c                   10.7312(10)
_cell_angle_alpha                106.871(4)
_cell_angle_beta                 94.897(4)
_cell_angle_gamma                94.758(4)
_cell_volume                     663.17(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    123
_cell_measurement_reflns_used    9888
_cell_measurement_theta_min      3.1018
_cell_measurement_theta_max      25.5015

_exptl_crystal_description       fragment
_exptl_crystal_colour            yellow

_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.130
_exptl_crystal_size_rad          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.261
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_F_000             424
_exptl_absorpt_coefficient_mu    9.204
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_absorpt_correction_T_min  0.157
_exptl_absorpt_correction_T_max  0.383

#===============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
;
Diffractometer operator             S. Haslinger
scanspeed                           20 s per frame
dx                                  35 mm
2690 frames measured in 7 data sets
phi-scans with delta_phi         = 0.5
omega-scans with delta_omega     = 0.5
;
_diffrn_ambient_temperature      123
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device       ' κ-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16

# number of measured reflections (redundant set)
_diffrn_reflns_number            16656
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_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         2.00
_diffrn_reflns_theta_max         25.53
_diffrn_reflns_theta_full        25.53
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             2446
# number of observed reflections (> n sig(I))
_reflns_number_gt                2323
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_computing_structure_refinement  
'SHELXL97 (Sheldrick, 1997), SHELXLE (Huebschle, 2011)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'

#===============================================================================

# 8. REFINEMENT DATA

_refine_special_details          
;
 Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs etc. and is not
 relevant to the choice of reflections for refinement.
 R-factors based on F² are statistically about twice
 as large as those based on F, and R-factors based on
 ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0309P)²+0.0768P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom


# Permitted for _refine_ls_hydrogen_treatment :
# refall  - refined all H parameters
# refxyz  - refined H coordinates only
# refU    - refined H U only
# noref   - no refinement of H parameters
# constr  - H parameters constrained
# mixed   - some constrained, some independent
# undef   - H-atom parameters not defined
_refine_ls_hydrogen_treatment    mixed

_refine_ls_extinction_method     none
_refine_ls_abs_structure_details ?
_refine_ls_abs_structure_Flack   .
_refine_ls_number_reflns         2446
_refine_ls_number_parameters     229
_refine_ls_number_restraints     97
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0203
_refine_ls_wR_factor_ref         0.0500
_refine_ls_wR_factor_gt          0.0491
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_restrained_S_all      1.192
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.003
_refine_diff_density_max         1.412
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.133

#===============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags

_atom_site_disorder_assembly
_atom_site_disorder_group

Re1 Re Uani 0.07965(2) 0.41085(1) 1.16655(1) 1.000 0.0203(1) d . . .
O1 O Uani 0.0510(5) 0.3010(3) 1.2640(3) 1.000 0.0378(10) d . . .
O2 O Uani 0.2790(5) 0.5427(3) 1.2073(3) 1.000 0.0340(10) d . . .
O3 O Uani -0.1371(4) 0.4323(3) 1.0801(3) 1.000 0.0297(9) d . . .
O4 O Uani -0.0447(5) 0.5730(3) 1.3440(3) 1.000 0.0287(10) d . . .
C1 C Uani 0.2036(6) 0.2691(4) 1.0159(4) 1.000 0.0208(12) d . . .
C2 C Uani 0.0925(7) 0.1396(4) 0.9439(4) 1.000 0.0241(12) d . . .
C3 C Uani 0.1788(7) 0.0399(4) 0.8494(4) 1.000 0.0259(14) d . . .
C4 C Uani 0.3769(7) 0.0713(4) 0.8257(4) 1.000 0.0259(12) d . A .
C5 C Uani 0.4893(7) 0.2010(5) 0.8963(4) 1.000 0.0307(16) d . . .
C6 C Uani 0.4016(7) 0.2986(5) 0.9893(4) 1.000 0.0269(12) d . . .
C7 C Uani 0.4746(8) -0.0377(5) 0.7290(4) 1.000 0.0337(14) d . . .
C8 C Uani -0.2353(8) 0.5356(6) 1.3882(5) 1.000 0.0448(17) d . . .
C9 C Uani -0.3210(9) 0.6762(7) 1.4453(6) 1.000 0.062(2) d . . .
C10 C Uani -0.1431(9) 0.7904(5) 1.4616(5) 1.000 0.0427(18) d . . .
C11 C Uani -0.0290(11) 0.7240(5) 1.3512(5) 1.000 0.054(2) d . . .
F2 F Uani 0.6582(12) 0.0063(9) 0.7073(9) 0.420(5) 0.0435(14) d UP A 1
F2A F Uani 0.5884(15) 0.0340(9) 0.6554(9) 0.365(5) 0.0417(14) d UP A 2
F2B F Uani 0.453(3) -0.0312(17) 0.6091(14) 0.216(4) 0.0427(16) d UP A 3
F3 F Uani 0.3558(17) -0.0849(10) 0.6107(8) 0.420(5) 0.0420(16) d UP A 1
F3A F Uani 0.3489(18) -0.1273(10) 0.6371(10) 0.365(5) 0.0442(16) d UP A 2
F3B F Uani 0.387(2) -0.1793(15) 0.7122(15) 0.216(4) 0.0427(14) d UP A 3
F1A F Uani 0.6061(18) -0.0998(11) 0.7820(8) 0.365(5) 0.0426(14) d UP A 2
F1B F Uani 0.677(2) -0.0402(18) 0.7619(16) 0.216(4) 0.0414(14) d UP A 3
F1 F Uani 0.4851(15) -0.1616(8) 0.7668(7) 0.420(5) 0.0406(14) d UP A 1
H10A H Uiso -0.19070 0.88070 1.45400 1.000 0.0510 c R . .
H11A H Uiso -0.09040 0.73670 1.26860 1.000 0.0650 c R . .
H11B H Uiso 0.11500 0.76630 1.36840 1.000 0.0650 c R . .
H10B H Uiso -0.05930 0.80950 1.54700 1.000 0.0510 c R . .
H9A H Uiso -0.37000 0.68080 1.53090 1.000 0.0750 c R . .
H9B H Uiso -0.43520 0.68800 1.38510 1.000 0.0750 c R . .
H2 H Uiso -0.04390 0.11920 0.95950 1.000 0.0290 c R . .
H3 H Uiso 0.10280 -0.04890 0.80160 1.000 0.0310 c R . .
H5 H Uiso 0.62540 0.22180 0.88040 1.000 0.0370 c R . .
H6 H Uiso 0.47750 0.38770 1.03630 1.000 0.0320 c R . .
H8A H Uiso -0.21270 0.48620 1.45570 1.000 0.0540 c R . .
H8B H Uiso -0.32990 0.47180 1.31400 1.000 0.0540 c R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re1 0.0210(1) 0.0214(1) 0.0167(1) 0.0024(1) 0.0019(1) 0.0041(1)
O1 0.061(2) 0.0326(16) 0.0253(16) 0.0106(13) 0.0173(15) 0.0167(15)
O2 0.0264(18) 0.0380(17) 0.0299(17) -0.0022(13) 0.0048(13) 0.0041(14)
O3 0.0263(17) 0.0369(16) 0.0235(15) 0.0032(13) 0.0057(12) 0.0091(13)
O4 0.0348(19) 0.0263(16) 0.0226(16) 0.0018(13) 0.0060(13) 0.0081(13)
C1 0.024(2) 0.022(2) 0.018(2) 0.0081(16) 0.0008(16) 0.0052(16)
C2 0.023(2) 0.026(2) 0.022(2) 0.0053(17) 0.0050(17) 0.0001(17)
C3 0.030(3) 0.023(2) 0.022(2) 0.0023(17) 0.0051(17) 0.0020(17)
C4 0.026(2) 0.029(2) 0.022(2) 0.0051(18) 0.0042(17) 0.0074(18)
C5 0.021(2) 0.036(3) 0.034(3) 0.007(2) 0.0064(19) 0.0061(19)
C6 0.023(2) 0.025(2) 0.029(2) 0.0029(18) 0.0007(18) 0.0027(17)
C7 0.036(3) 0.036(2) 0.025(2) 0.000(2) 0.005(2) 0.012(2)
C8 0.042(3) 0.053(3) 0.034(3) 0.000(2) 0.014(2) 0.013(2)
C9 0.044(4) 0.082(4) 0.040(3) -0.018(3) -0.006(3) 0.034(3)
C10 0.063(4) 0.040(3) 0.025(2) 0.004(2) 0.003(2) 0.028(3)
C11 0.097(5) 0.030(3) 0.038(3) 0.007(2) 0.022(3) 0.019(3)
F2 0.046(3) 0.046(2) 0.035(2) 0.0004(18) 0.012(2) 0.0205(19)
F2A 0.047(3) 0.044(2) 0.033(2) 0.0035(19) 0.013(2) 0.020(2)
F2B 0.047(3) 0.045(3) 0.033(2) 0.0011(19) 0.010(2) 0.021(2)
F3 0.048(3) 0.043(3) 0.032(2) 0.0017(19) 0.008(2) 0.020(2)
F3A 0.048(3) 0.045(3) 0.034(2) -0.002(2) 0.009(2) 0.020(2)
F3B 0.048(3) 0.043(2) 0.034(2) 0.0011(19) 0.009(2) 0.022(2)
F1A 0.047(3) 0.044(2) 0.035(2) 0.0028(18) 0.009(2) 0.024(2)
F1B 0.046(3) 0.043(2) 0.034(2) 0.0033(19) 0.010(2) 0.023(2)
F1 0.047(3) 0.042(2) 0.033(2) 0.0049(18) 0.008(2) 0.025(2)

#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re1 O1 1.718(3) . . yes
Re1 O2 1.706(3) . . yes
Re1 O3 1.706(3) . . yes
Re1 O4 2.361(3) . . yes
Re1 C1 2.084(4) . . yes
F1 C7 1.396(10) . . yes
F1A C7 1.289(12) . . yes
F1B C7 1.363(15) . . yes
F2 C7 1.321(10) . . yes
F2A C7 1.424(11) . . yes
F2B C7 1.303(15) . . yes
F3 C7 1.369(10) . . yes
F3A C7 1.295(12) . . yes
F3B C7 1.418(16) . . yes
O4 C8 1.444(6) . . yes
O4 C11 1.459(6) . . yes
C1 C2 1.392(6) . . no
C1 C6 1.393(6) . . no
C2 C3 1.390(6) . . no
C3 C4 1.387(7) . . no
C4 C7 1.493(6) . . no
C4 C5 1.393(6) . . no
C5 C6 1.375(6) . . no
C8 C9 1.519(9) . . no
C9 C10 1.522(9) . . no
C10 C11 1.480(8) . . no
C2 H2 0.9500 . . no
C3 H3 0.9500 . . no
C5 H5 0.9500 . . no
C6 H6 0.9500 . . no
C8 H8A 0.9900 . . no
C8 H8B 0.9900 . . no
C9 H9A 0.9900 . . no
C9 H9B 0.9900 . . no
C10 H10A 0.9900 . . no
C10 H10B 0.9900 . . no
C11 H11A 0.9900 . . no
C11 H11B 0.9900 . . no

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Re1 O2 119.05(15) . . . yes
O1 Re1 O3 116.16(15) . . . yes
O1 Re1 O4 81.57(13) . . . yes
O1 Re1 C1 97.60(15) . . . yes
O2 Re1 O3 119.26(15) . . . yes
O2 Re1 O4 81.14(13) . . . yes
O2 Re1 C1 96.87(15) . . . yes
O3 Re1 O4 83.70(13) . . . yes
O3 Re1 C1 99.18(15) . . . yes
O4 Re1 C1 177.06(14) . . . yes
Re1 O4 C8 120.4(3) . . . yes
Re1 O4 C11 118.6(3) . . . yes
C8 O4 C11 108.7(4) . . . yes
Re1 C1 C2 120.3(3) . . . yes
Re1 C1 C6 120.9(3) . . . yes
C2 C1 C6 118.7(4) . . . no
C1 C2 C3 120.8(4) . . . no
C2 C3 C4 119.3(4) . . . no
C3 C4 C5 120.5(4) . . . no
C3 C4 C7 119.8(4) . . . no
C5 C4 C7 119.6(4) . . . no
C4 C5 C6 119.5(4) . . . no
C1 C6 C5 121.2(4) . . . no
F1 C7 C4 110.9(5) . . . yes
F1A C7 C4 113.9(5) . . . yes
F1B C7 C4 114.8(8) . . . yes
F2 C7 C4 114.9(5) . . . yes
F2A C7 C4 108.1(5) . . . yes
F2B C7 C4 115.4(9) . . . yes
F3 C7 C4 110.8(6) . . . yes
F3A C7 C4 114.7(7) . . . yes
F3B C7 C4 112.5(7) . . . yes
F1 C7 F2 108.7(7) . . . yes
F1 C7 F3 103.3(6) . . . yes
F1A C7 F2A 104.8(7) . . . yes
F1A C7 F3A 112.7(8) . . . yes
F1B C7 F2B 107.0(12) . . . yes
F1B C7 F3B 104.3(10) . . . yes
F2 C7 F3 107.6(7) . . . yes
F2A C7 F3A 101.3(7) . . . yes
F2B C7 F3B 101.6(10) . . . yes
O4 C8 C9 105.7(5) . . . yes
C8 C9 C10 104.6(5) . . . no
C9 C10 C11 102.1(4) . . . no
O4 C11 C10 104.5(4) . . . yes
C1 C2 H2 120.00 . . . no
C3 C2 H2 120.00 . . . no
C2 C3 H3 120.00 . . . no
C4 C3 H3 120.00 . . . no
C4 C5 H5 120.00 . . . no
C6 C5 H5 120.00 . . . no
C1 C6 H6 119.00 . . . no
C5 C6 H6 119.00 . . . no
O4 C8 H8A 111.00 . . . no
O4 C8 H8B 111.00 . . . no
C9 C8 H8A 111.00 . . . no
C9 C8 H8B 111.00 . . . no
H8A C8 H8B 109.00 . . . no
C8 C9 H9A 111.00 . . . no
C8 C9 H9B 111.00 . . . no
C10 C9 H9A 111.00 . . . no
C10 C9 H9B 111.00 . . . no
H9A C9 H9B 109.00 . . . no
C9 C10 H10A 111.00 . . . no
C9 C10 H10B 111.00 . . . no
C11 C10 H10A 111.00 . . . no
C11 C10 H10B 111.00 . . . no
H10A C10 H10B 109.00 . . . no
O4 C11 H11A 111.00 . . . no
O4 C11 H11B 111.00 . . . no
C10 C11 H11A 111.00 . . . no
C10 C11 H11B 111.00 . . . no
H11A C11 H11B 109.00 . . . no

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
O1 Re1 O4 C8 -55.1(3) . . . . no
O1 Re1 O4 C11 167.0(4) . . . . no
O2 Re1 O4 C8 -176.4(3) . . . . no
O2 Re1 O4 C11 45.6(4) . . . . no
O3 Re1 O4 C8 62.6(3) . . . . no
O3 Re1 O4 C11 -75.4(4) . . . . no
O1 Re1 C1 C2 61.5(4) . . . . no
O1 Re1 C1 C6 -115.5(4) . . . . no
O2 Re1 C1 C2 -177.9(3) . . . . no
O2 Re1 C1 C6 5.1(4) . . . . no
O3 Re1 C1 C2 -56.7(4) . . . . no
O3 Re1 C1 C6 126.3(4) . . . . no
Re1 O4 C8 C9 -151.1(3) . . . . no
C11 O4 C8 C9 -9.5(5) . . . . no
Re1 O4 C11 C10 172.8(3) . . . . no
C8 O4 C11 C10 30.4(5) . . . . no
Re1 C1 C2 C3 -175.5(3) . . . . no
C6 C1 C2 C3 1.6(6) . . . . no
Re1 C1 C6 C5 175.3(3) . . . . no
C2 C1 C6 C5 -1.7(7) . . . . no
C1 C2 C3 C4 -0.9(6) . . . . no
C2 C3 C4 C5 0.4(6) . . . . no
C2 C3 C4 C7 177.1(4) . . . . no
C3 C4 C5 C6 -0.5(7) . . . . no
C7 C4 C5 C6 -177.2(4) . . . . no
C4 C5 C6 C1 1.2(7) . . . . no
O4 C8 C9 C10 -14.4(5) . . . . no
C8 C9 C10 C11 32.1(6) . . . . no
C9 C10 C11 O4 -38.0(6) . . . . no

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
_geom_hbond_publ_flag
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
C3 H3 O1 0.9500 2.4800 3.393(5) 162.00 2_557 yes
C6 H6 O2 0.9500 2.5600 3.047(5) 112.00 . yes
C6 H6 O3 0.9500 2.5400 3.182(5) 125.00 1_655 yes
C9 H9B O2 0.9900 2.5700 3.407(7) 142.00 1_455 yes
C10 H10B O1 0.9900 2.5600 3.343(6) 136.00 2_568 yes

# Loop Mechanism for Extra Tables(s)

#loop_
#_publ_manuscript_incl_extra_item
#'_geom_extra_tableA_col_1'
#'_geom_extra_tableA_col_2'
#'_geom_extra_tableA_col_3'
#'_geom_extra_table_head_A'
#'_geom_table_footnote_A'
#'_geom_extra_tableB_col_1'
#'_geom_extra_tableB_col_2'
#'_geom_extra_tableB_col_3'
#'_geom_extra_table_head_B'
#'_geom_table_footnote_B'


#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
# ? ? ?


#
#loop_
#_geom_extra_tableB_col_1
#_geom_extra_tableB_col_2
#_geom_extra_tableB_col_3
# ? ? ?


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;


#
#_geom_table_footnote_A
#;
# ?
#;


#
#_geom_table_footnote_B
#;
# ?
#;

_iucr_refine_instructions_details 
;
;

#===END
