# 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_14-lu_sq
_database_code_depnum_ccdc_archive 'CCDC 1487118'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 F6 Lu O8'
_chemical_formula_sum            'C12 H4 F6 Lu O8'
_chemical_formula_weight         565.12
_chemical_melting_point          ?
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'
Lu Lu -0.4720 5.8584 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.848(5)
_cell_length_b                   10.927(5)
_cell_length_c                   11.517(5)
_cell_angle_alpha                90
_cell_angle_beta                 120.340(5)
_cell_angle_gamma                90
_cell_volume                     1504.0(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1595
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0121
_cell_measurement_theta_min      3.2546
_shelx_estimated_absorpt_T_max   0.379
_shelx_estimated_absorpt_T_min   0.286
_exptl_absorpt_coefficient_mu    6.678
_exptl_absorpt_correction_T_max  0.301
_exptl_absorpt_correction_T_min  0.205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.496
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0234
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2794
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         3.409
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1337
_reflns_number_total             1404
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         1404
_refine_ls_number_restraints     87
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0202
_refine_ls_restrained_S_all      0.997
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0120P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0373
_refine_ls_wR_factor_ref         0.0383
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Rigid bond restraints
 C1, O4, O5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim O4 \\sim O5: within 3.8A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 C2, F2B, F3A, C3A, C4A, C3B, C4B, F2A, F3B, C0AA, C3A, C2, C3B, C2, F2B, C3A,
 C4A, C3A, C4B, C3B, F2A, C3B, F3A, C4A, C4A, C0AA, F3B, C4B, C4B, C0AA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: F2B(0.5) F3A(0.5) C3A(0.5) C4A(0.5) C3B(0.5) C4B(0.5) F2A(0.5)
 F3B(0.5)
6.a Riding coordinates:
 O2(H2A,H2B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.3882(5) 0.000000 0.2473(5) 0.0255(13) Uani 1 2 d S TU P . .
C2 C 0.3686(4) 0.000000 0.1051(5) 0.0230(12) Uani 1 2 d S TU P . .
C5 C 0.3182(5) 0.000000 -0.2988(5) 0.0315(15) Uani 1 2 d S T P . .
C7 C 0.500000 0.2339(5) 0.500000 0.0289(14) Uani 1 2 d S T P . .
C8 C 0.500000 0.3710(5) 0.500000 0.0269(14) Uani 1 2 d S T P . .
C9 C 0.4636(3) 0.4378(4) 0.3825(4) 0.0278(10) Uani 1 1 d . . . . .
O1 O 0.3130(2) -0.1000(3) -0.3548(3) 0.0396(8) Uani 1 1 d . . . . .
O2 O 0.1845(2) -0.1292(2) 0.3632(2) 0.0329(7) Uani 1 1 d . . . . .
H2A H 0.194818 -0.199561 0.339716 0.040 Uiso 1 1 d R . . . .
H2B H 0.115558 -0.123081 0.338206 0.040 Uiso 1 1 d R . . . .
O3 O 0.4104(2) 0.1850(3) 0.4764(3) 0.0349(7) Uani 1 1 d . . . . .
O4 O 0.3036(3) 0.000000 0.2600(3) 0.0360(11) Uani 1 2 d S TU P . .
O5 O 0.4863(3) 0.000000 0.3407(3) 0.0369(11) Uani 1 2 d S TU P . .
Lu1 Lu 0.33880(2) 0.000000 0.47934(2) 0.01672(9) Uani 1 2 d S T P . .
F1 F 0.4302(2) 0.3780(2) 0.2666(2) 0.0448(7) Uani 1 1 d . . . . .
F2B F 0.4303(5) 0.2020(5) 0.1241(4) 0.0498(15) Uani 0.5 1 d . U . A 2
F3A F 0.3969(5) 0.2008(5) -0.1210(5) 0.0502(15) Uani 0.5 1 d . U . A 2
C3A C 0.3908(8) 0.0997(10) 0.0504(10) 0.026(2) Uani 0.5 1 d . U . A 2
C4A C 0.3731(8) 0.0983(11) -0.0785(10) 0.027(2) Uani 0.5 1 d . U . A 2
C3B C 0.3318(7) -0.1050(10) 0.0259(10) 0.025(2) Uani 0.5 1 d . U . A -1
C4B C 0.3164(7) -0.1080(11) -0.1006(10) 0.024(2) Uani 0.5 1 d . U . A -1
F2A F 0.3085(5) -0.2052(5) 0.0744(5) 0.0501(15) Uani 0.5 1 d . U . A -1
F3B F 0.2831(5) -0.2147(5) -0.1673(4) 0.0430(13) Uani 0.5 1 d . U . A -1
C0AA C 0.3354(4) 0.000000 -0.1587(5) 0.0231(12) Uani 1 2 d S TU P . .


_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
C1 C2 1.519(6) . ?
C1 O4 1.252(6) . ?
C1 O5 1.234(6) . ?
C2 C3A 1.368(11) 6 ?
C2 C3A 1.368(11) . ?
C2 C3B 1.392(11) . ?
C5 O1 1.252(3) 6 ?
C5 O1 1.252(3) . ?
C5 Lu1 2.710(6) 1_554 ?
C5 C0AA 1.508(7) . ?
C7 C8 1.499(7) . ?
C7 O3 1.248(3) 2_656 ?
C7 O3 1.248(3) . ?
C8 C9 1.389(5) . ?
C8 C9 1.389(5) 2_656 ?
C9 C9 1.360(8) 6_565 ?
C9 F1 1.341(4) . ?
O1 Lu1 2.379(3) 1_554 ?
O2 Lu1 2.337(3) . ?
O3 Lu1 2.259(3) . ?
O4 Lu1 2.319(4) . ?
O5 Lu1 2.257(4) 5_656 ?
F2B C3A 1.341(11) . ?
F3A C4A 1.329(12) . ?
C3A C4A 1.378(13) . ?
C4A C0AA 1.339(11) . ?
C3B C4B 1.362(13) . ?
C3B F2A 1.340(12) . ?
C4B F3B 1.344(12) . ?
C4B C0AA 1.445(11) . ?

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
O4 C1 C2 117.2(5) . . ?
O5 C1 C2 117.3(5) . . ?
O5 C1 O4 125.5(5) . . ?
C3A C2 C1 122.4(5) 6 . ?
C3A C2 C1 122.4(5) . . ?
C3B C2 C1 120.9(5) . . ?
O1 C5 O1 121.6(5) . 6 ?
O1 C5 Lu1 61.4(3) 6 1_554 ?
O1 C5 Lu1 61.4(3) . 1_554 ?
O1 C5 C0AA 119.2(3) . . ?
O1 C5 C0AA 119.2(3) 6 . ?
C0AA C5 Lu1 166.9(4) . 1_554 ?
O3 C7 C8 115.4(3) 2_656 . ?
O3 C7 C8 115.4(3) . . ?
O3 C7 O3 129.3(5) . 2_656 ?
C9 C8 C7 121.7(3) 2_656 . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 C9 116.6(5) . 2_656 ?
C9 C9 C8 121.7(3) 6_565 . ?
F1 C9 C8 119.1(4) . . ?
F1 C9 C9 119.2(2) . 6_565 ?
C5 O1 Lu1 91.1(3) . 1_554 ?
C7 O3 Lu1 140.9(3) . . ?
C1 O4 Lu1 115.6(3) . . ?
C1 O5 Lu1 176.3(4) . 5_656 ?
O1 Lu1 C5 27.51(7) 6_556 1_556 ?
O1 Lu1 C5 27.51(7) 1_556 1_556 ?
O1 Lu1 O1 54.68(14) 6_556 1_556 ?
O2 Lu1 C5 92.22(11) 6 1_556 ?
O2 Lu1 C5 92.22(11) . 1_556 ?
O2 Lu1 O1 73.60(9) . 1_556 ?
O2 Lu1 O1 105.83(10) 6 1_556 ?
O2 Lu1 O1 105.83(10) . 6_556 ?
O2 Lu1 O1 73.60(9) 6 6_556 ?
O2 Lu1 O2 74.36(14) 6 . ?
O3 Lu1 C5 105.69(8) . 1_556 ?
O3 Lu1 C5 105.69(8) 6 1_556 ?
O3 Lu1 O1 81.17(10) . 6_556 ?
O3 Lu1 O1 131.93(10) . 1_556 ?
O3 Lu1 O1 81.17(10) 6 1_556 ?
O3 Lu1 O1 131.93(10) 6 6_556 ?
O3 Lu1 O2 74.47(10) . 6 ?
O3 Lu1 O2 144.43(9) . . ?
O3 Lu1 O2 74.47(10) 6 . ?
O3 Lu1 O2 144.43(9) 6 6 ?
O3 Lu1 O3 126.89(14) 6 . ?
O3 Lu1 O4 80.54(8) . . ?
O3 Lu1 O4 80.54(8) 6 . ?
O4 Lu1 C5 164.34(15) . 1_556 ?
O4 Lu1 O1 147.22(9) . 1_556 ?
O4 Lu1 O1 147.22(9) . 6_556 ?
O4 Lu1 O2 75.40(10) . . ?
O4 Lu1 O2 75.40(10) . 6 ?
O5 Lu1 C5 73.11(16) 5_656 1_556 ?
O5 Lu1 O1 77.84(11) 5_656 1_556 ?
O5 Lu1 O1 77.84(11) 5_656 6_556 ?
O5 Lu1 O2 140.60(7) 5_656 6 ?
O5 Lu1 O2 140.60(7) 5_656 . ?
O5 Lu1 O3 74.81(8) 5_656 6 ?
O5 Lu1 O3 74.81(8) 5_656 . ?
O5 Lu1 O4 122.55(14) 5_656 . ?
C2 C3A C4A 121.9(9) . . ?
F2B C3A C2 119.2(7) . . ?
F2B C3A C4A 119.0(9) . . ?
F3A C4A C3A 116.5(9) . . ?
F3A C4A C0AA 120.3(8) . . ?
C0AA C4A C3A 123.2(9) . . ?
C4B C3B C2 121.9(9) . . ?
F2A C3B C2 119.1(7) . . ?
F2A C3B C4B 119.0(9) . . ?
C3B C4B C0AA 120.6(9) . . ?
F3B C4B C3B 117.1(9) . . ?
F3B C4B C0AA 122.3(8) . . ?
C4A C0AA C5 122.3(5) . . ?
C4A C0AA C5 122.3(5) 6 . ?
C4A C0AA C4A 106.7(9) 6 . ?
C4B C0AA C5 121.9(5) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_13-yb_sq
_database_code_depnum_ccdc_archive 'CCDC 1486542'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9.95 H4 F2 O8 Yb, 4.006(F), 1.94(C)'
_chemical_formula_sum            'C11.89 H4 F6 O8 Yb'
_chemical_formula_weight         561.98
_chemical_melting_point          ?
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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.827(5)
_cell_length_b                   10.957(5)
_cell_length_c                   11.517(5)
_cell_angle_alpha                90
_cell_angle_beta                 120.416(5)
_cell_angle_gamma                90
_cell_volume                     1504.7(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1302
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9150
_cell_measurement_theta_min      2.9579
_shelx_estimated_absorpt_T_max   0.493
_shelx_estimated_absorpt_T_min   0.364
_exptl_absorpt_coefficient_mu    6.329
_exptl_absorpt_correction_T_max  0.439
_exptl_absorpt_correction_T_min  0.359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.481
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2835
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.964
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1303
_reflns_number_total             1403
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         0.627
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         1403
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0268
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0216P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0551
_refine_ls_wR_factor_ref         0.0575
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Rigid bond restraints
 C5B, C8B, F1B, F2B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C5B \\sim C8B \\sim F1B \\sim F2B: within 3.8A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C4, C5B, C7, C8B, F1B, F2B, C5A, C8A, F1A, F2A, C5B, C4, C5A, C4, C8B, C5B,
 F1B, C5B, C8A, C5A, F1A, C5A, C8B, C7, F2B, C8B, C8A, C7, F2A, C8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Riding coordinates:
 O3(H3A,H3B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.500000 -0.2355(7) 0.500000 0.0241(18) Uani 1 2 d S T P . .
C2 C 0.500000 -0.3712(7) 0.500000 0.0238(18) Uani 1 2 d S T P . .
C3 C 0.3860(6) 0.000000 0.2453(7) 0.029(2) Uani 1 2 d S T P A .
C4 C 0.3695(6) 0.000000 0.1060(7) 0.024(2) Uani 1.00(2) 2 d S TU P . .
C5B C 0.394(5) -0.100(2) 0.0518(19) 0.027(7) Uani 0.42(9) 1 d . U . A -1
C6 C 0.3210(6) 0.000000 -0.2982(7) 0.027(2) Uani 1 2 d S T P . .
C7 C 0.3363(6) 0.000000 -0.1569(7) 0.021(2) Uani 0.99(2) 2 d S TU P . .
C8B C 0.371(5) -0.0998(18) -0.079(2) 0.027(7) Uani 0.53(9) 1 d . U . A .
C9 C 0.5371(4) -0.4376(5) 0.6181(5) 0.0262(13) Uani 1 1 d . . . . .
O1 O 0.5896(3) -0.1855(4) 0.5238(4) 0.0332(10) Uani 1 1 d . . . . .
O2 O 0.4831(4) 0.000000 0.3423(5) 0.0378(16) Uani 1 2 d S T P . .
O3 O 0.8176(3) 0.1303(4) 0.6352(4) 0.0306(10) Uani 1 1 d . . . . .
H3A H 0.808241 0.207003 0.638718 0.037 Uiso 1 1 d R . . A .
H3B H 0.853881 0.105253 0.716148 0.037 Uiso 1 1 d R . . . .
O4 O 0.3151(4) -0.0995(4) -0.3535(4) 0.0405(11) Uani 1 1 d . . . . .
O5 O 0.3006(4) 0.000000 0.2571(5) 0.0321(14) Uani 1 2 d S T P . .
F1B F 0.4281(7) -0.2011(7) 0.1252(7) 0.051(3) Uani 0.504(11) 1 d . U . A -1
F2B F 0.3962(8) -0.2032(7) -0.1199(7) 0.050(3) Uani 0.496(12) 1 d . U . A -1
F3 F 0.5722(3) -0.3778(3) 0.7342(3) 0.0443(10) Uani 1 1 d . . . . .
Yb1 Yb 0.66073(2) 0.000000 0.52085(3) 0.01526(12) Uani 1 2 d S T P A .
C5A C 0.337(5) 0.1028(13) 0.030(3) 0.030(8) Uani 0.56(9) 1 d . U . A -1
C8A C 0.317(5) 0.1096(16) -0.102(3) 0.021(6) Uani 0.44(9) 1 d . U . A -1
F1A F 0.3106(7) 0.2057(7) 0.0753(7) 0.051(3) Uani 0.511(12) 1 d . U . A -1
F2A F 0.2870(8) 0.2131(7) -0.1660(7) 0.042(3) Uani 0.492(12) 1 d . U . A -1


_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
C1 C2 1.487(11) . ?
C1 O1 1.251(5) 2_656 ?
C1 O1 1.251(5) . ?
C2 C9 1.392(7) . ?
C2 C9 1.392(7) 2_656 ?
C3 C4 1.502(10) . ?
C3 O2 1.238(8) . ?
C3 O5 1.255(9) . ?
C3 Yb1 3.072(8) 5_656 ?
C4 C5B 1.38(2) . ?
C4 C5A 1.354(17) . ?
C5B C8B 1.37(2) . ?
C5B F1B 1.33(2) . ?
C6 C7 1.530(10) . ?
C6 O4 1.244(5) 6 ?
C6 O4 1.244(5) . ?
C6 Yb1 2.702(8) 5_655 ?
C7 C8B 1.343(14) 6 ?
C7 C8B 1.343(14) . ?
C7 C8A 1.44(2) . ?
C8B F2B 1.339(16) . ?
C9 C9 1.367(11) 6_545 ?
C9 F3 1.340(6) . ?
O1 Yb1 2.266(4) . ?
O2 Yb1 2.269(5) . ?
O3 Yb1 2.363(3) . ?
O4 Yb1 2.381(4) 5_655 ?
O5 Yb1 2.332(5) 5_656 ?
Yb1 Yb1 4.2221(17) 5_656 ?
C5A C8A 1.41(2) . ?
C5A F1A 1.37(2) . ?
C8A F2A 1.30(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 115.9(4) 2_656 . ?
O1 C1 C2 115.9(4) . . ?
O1 C1 O1 128.1(7) 2_656 . ?
C9 C2 C1 121.5(4) . . ?
C9 C2 C1 121.5(4) 2_656 . ?
C9 C2 C9 116.9(7) 2_656 . ?
C4 C3 Yb1 162.0(5) . 5_656 ?
O2 C3 C4 118.2(7) . . ?
O2 C3 O5 123.5(7) . . ?
O2 C3 Yb1 79.8(4) . 5_656 ?
O5 C3 C4 118.3(6) . . ?
O5 C3 Yb1 43.7(3) . 5_656 ?
C5B C4 C3 122.9(9) . . ?
C5A C4 C3 120.7(6) . . ?
C5A C4 C5B 116.2(13) . . ?
C8B C5B C4 121.6(15) . . ?
F1B C5B C4 117.4(19) . . ?
F1B C5B C8B 120.5(16) . . ?
C7 C6 Yb1 168.5(5) . 5_655 ?
O4 C6 C7 118.8(4) . . ?
O4 C6 C7 118.8(4) 6 . ?
O4 C6 O4 122.4(7) . 6 ?
O4 C6 Yb1 61.8(4) 6 5_655 ?
O4 C6 Yb1 61.8(4) . 5_655 ?
C8B C7 C6 121.6(7) . . ?
C8B C7 C6 121.6(7) 6 . ?
C8B C7 C8B 109(2) 6 . ?
C8B C7 C8A 27.4(7) 6 . ?
C8B C7 C8A 117.9(8) . . ?
C8A C7 C6 120.5(8) . . ?
C7 C8B C5B 122.7(13) . . ?
F2B C8B C5B 115.7(14) . . ?
F2B C8B C7 121.3(12) . . ?
C9 C9 C2 121.5(4) 6_545 . ?
F3 C9 C2 119.2(5) . . ?
F3 C9 C9 119.3(3) . 6_545 ?
C1 O1 Yb1 141.1(4) . . ?
C3 O2 Yb1 179.6(6) . . ?
C6 O4 Yb1 90.8(4) . 5_655 ?
C3 O5 Yb1 114.4(4) . 5_656 ?
C3 Yb1 Yb1 54.76(14) 5_656 5_656 ?
C6 Yb1 C3 174.2(2) 5_655 5_656 ?
C6 Yb1 Yb1 119.41(15) 5_655 5_656 ?
O1 Yb1 C3 72.63(12) . 5_656 ?
O1 Yb1 C3 72.62(12) 6 5_656 ?
O1 Yb1 C6 105.31(12) 6 5_655 ?
O1 Yb1 C6 105.31(12) . 5_655 ?
O1 Yb1 O1 127.56(19) 6 . ?
O1 Yb1 O2 74.61(10) . . ?
O1 Yb1 O2 74.61(10) 6 . ?
O1 Yb1 O3 74.50(13) 6 . ?
O1 Yb1 O3 144.74(13) . . ?
O1 Yb1 O3 74.50(13) . 6 ?
O1 Yb1 O3 144.74(13) 6 6 ?
O1 Yb1 O4 131.51(14) 6 2_655 ?
O1 Yb1 O4 131.51(14) . 5_655 ?
O1 Yb1 O4 80.86(15) . 2_655 ?
O1 Yb1 O4 80.86(15) 6 5_655 ?
O1 Yb1 O5 81.02(12) . 5_656 ?
O1 Yb1 O5 81.02(12) 6 5_656 ?
O1 Yb1 Yb1 64.01(9) . 5_656 ?
O1 Yb1 Yb1 64.01(9) 6 5_656 ?
O2 Yb1 C3 100.6(2) . 5_656 ?
O2 Yb1 C6 73.6(2) . 5_655 ?
O2 Yb1 O3 140.54(11) . 6 ?
O2 Yb1 O3 140.54(11) . . ?
O2 Yb1 O4 78.30(17) . 5_655 ?
O2 Yb1 O4 78.30(17) . 2_655 ?
O2 Yb1 O5 122.41(19) . 5_656 ?
O2 Yb1 Yb1 45.80(15) . 5_656 ?
O3 Yb1 C3 93.00(14) . 5_656 ?
O3 Yb1 C3 93.00(14) 6 5_656 ?
O3 Yb1 C6 91.64(15) 6 5_655 ?
O3 Yb1 C6 91.64(15) . 5_655 ?
O3 Yb1 O3 74.32(19) . 6 ?
O3 Yb1 O4 73.09(13) 6 2_655 ?
O3 Yb1 O4 105.21(14) . 2_655 ?
O3 Yb1 O4 105.21(14) 6 5_655 ?
O3 Yb1 O4 73.09(13) . 5_655 ?
O3 Yb1 Yb1 132.82(9) . 5_656 ?
O3 Yb1 Yb1 132.82(9) 6 5_656 ?
O4 Yb1 C3 152.63(11) 2_655 5_656 ?
O4 Yb1 C3 152.63(11) 5_655 5_656 ?
O4 Yb1 C6 27.42(10) 5_655 5_655 ?
O4 Yb1 C6 27.42(10) 2_655 5_655 ?
O4 Yb1 O4 54.5(2) 2_655 5_655 ?
O4 Yb1 Yb1 118.64(11) 5_655 5_656 ?
O4 Yb1 Yb1 118.64(11) 2_655 5_656 ?
O5 Yb1 C3 21.84(17) 5_656 5_656 ?
O5 Yb1 C6 164.0(2) 5_656 5_655 ?
O5 Yb1 O3 75.69(13) 5_656 6 ?
O5 Yb1 O3 75.69(13) 5_656 . ?
O5 Yb1 O4 147.08(12) 5_656 2_655 ?
O5 Yb1 O4 147.08(12) 5_656 5_655 ?
O5 Yb1 Yb1 76.60(12) 5_656 5_656 ?
C4 C5A C8A 124.2(15) . . ?
C4 C5A F1A 120.4(10) . . ?
F1A C5A C8A 115.0(18) . . ?
C5A C8A C7 116.7(18) . . ?
F2A C8A C7 123.7(12) . . ?
F2A C8A C5A 119.5(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4-pr_sq
_database_code_depnum_ccdc_archive 'CCDC 1445656'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 F6 O8 Pr'
_chemical_formula_sum            'C12 H4 F6 O8 Pr'
_chemical_formula_weight         531.06
_chemical_melting_point          ?
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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.086(5)
_cell_length_b                   11.349(5)
_cell_length_c                   11.748(5)
_cell_angle_alpha                90
_cell_angle_beta                 125.951(5)
_cell_angle_gamma                90
_cell_volume                     1520.3(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1886
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4717
_cell_measurement_theta_min      3.5663
_shelx_estimated_absorpt_T_max   0.619
_shelx_estimated_absorpt_T_min   0.529
_exptl_absorpt_coefficient_mu    3.318
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_correction_T_min  0.487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.320
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2661
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.987
_diffrn_reflns_theta_max         24.987
_diffrn_reflns_theta_min         3.573
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1351
_reflns_number_total             1417
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.500  0.000  0.000        58        16 ' '
   2  1.000  0.500  0.000        58        16 ' '
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1417
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0228
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0196P)²+1.5081P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0500
_refine_ls_wR_factor_ref         0.0513
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O3(H3A,H3B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pr1 Pr 0.66328(2) 0.500000 0.53540(2) 0.01460(10) Uani 1 2 d S T P . .
F1 F 0.3679(2) 0.7059(2) 0.0966(2) 0.0535(7) Uani 1 1 d . . . . .
F2 F 0.3575(3) 0.7093(2) -0.1333(3) 0.0549(7) Uani 1 1 d . . . . .
O1 O 0.4527(3) 0.500000 0.3462(3) 0.0265(9) Uani 1 2 d S T P . .
O2 O 0.3384(2) 0.5963(3) -0.3397(3) 0.0396(7) Uani 1 1 d . . . . .
O3 O 0.8384(2) 0.6346(3) 0.6556(3) 0.0417(8) Uani 1 1 d . . . . .
H3A H 0.832452 0.705409 0.674456 0.050 Uiso 1 1 d R . . . .
H3B H 0.909832 0.622469 0.689046 0.050 Uiso 1 1 d R . . . .
O5 O 0.5905(2) 0.3045(2) 0.5264(3) 0.0367(7) Uani 1 1 d . . . . .
O4 O 0.2613(3) 0.500000 0.2030(4) 0.0462(13) Uani 1 2 d S T P . .
C1 C 0.3587(4) 0.500000 0.2251(5) 0.0257(12) Uani 1 2 d S T P . .
C2 C 0.3634(4) 0.500000 0.0992(5) 0.0252(13) Uani 1 2 d S T P . .
C3 C 0.3629(3) 0.6032(4) 0.0379(4) 0.0298(9) Uani 1 1 d . . . . .
C4 C 0.3580(3) 0.6041(4) -0.0830(4) 0.0268(9) Uani 1 1 d . . . . .
C5 C 0.3532(4) 0.500000 -0.1490(5) 0.0232(12) Uani 1 2 d S T P . .
C8 C 0.500000 0.2571(5) 0.500000 0.0264(12) Uani 1 2 d S T P . .
C9 C 0.500000 0.1232(5) 0.500000 0.0240(12) Uani 1 2 d S T P . .
C7 C 0.5512(3) 0.0612(3) 0.6226(4) 0.0246(8) Uani 1 1 d . . . . .
C6 C 0.3423(4) 0.500000 -0.2849(5) 0.0254(13) Uani 1 2 d S T P . .
F3 F 0.60110(19) 0.1188(2) 0.7450(2) 0.0400(6) 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
Pr1 O1 2.449(3) . ?
Pr1 O1 2.698(3) 5_666 ?
Pr1 O2 2.533(3) 5_665 ?
Pr1 O2 2.533(3) 2_655 ?
Pr1 O3 2.515(3) 6_565 ?
Pr1 O3 2.515(3) . ?
Pr1 O5 2.421(3) . ?
Pr1 O5 2.421(3) 6_565 ?
Pr1 O4 2.596(4) 5_666 ?
Pr1 C1 3.006(5) 5_666 ?
Pr1 C6 2.897(5) 5_665 ?
F1 C3 1.334(5) . ?
F2 C4 1.330(5) . ?
O1 C1 1.251(6) . ?
O2 C6 1.253(4) . ?
O3 H3A 0.8501 . ?
O3 H3B 0.8496 . ?
O5 C8 1.243(3) . ?
O4 C1 1.238(6) . ?
C1 C2 1.520(7) . ?
C2 C3 1.373(5) . ?
C2 C3 1.373(5) 6_565 ?
C3 C4 1.381(5) . ?
C4 C5 1.393(5) . ?
C5 C6 1.512(7) . ?
C8 C9 1.519(7) . ?
C9 C7 1.367(5) 2_656 ?
C9 C7 1.367(5) . ?
C7 C7 1.390(8) 6 ?
C7 F3 1.342(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
O1 Pr1 O1 71.98(12) . 5_666 ?
O1 Pr1 O2 79.34(10) . 5_665 ?
O1 Pr1 O2 79.34(10) . 2_655 ?
O1 Pr1 O3 140.87(8) . 6_565 ?
O1 Pr1 O3 140.88(8) . . ?
O1 Pr1 O4 120.70(11) . 5_666 ?
O1 Pr1 C1 24.58(11) 5_666 5_666 ?
O1 Pr1 C1 96.56(13) . 5_666 ?
O1 Pr1 C6 149.37(12) 5_666 5_665 ?
O1 Pr1 C6 77.39(12) . 5_665 ?
O2 Pr1 O1 141.48(9) 5_665 5_666 ?
O2 Pr1 O1 141.48(8) 2_655 5_666 ?
O2 Pr1 O2 51.13(14) 5_665 2_655 ?
O2 Pr1 O4 148.61(8) 5_665 5_666 ?
O2 Pr1 O4 148.61(8) 2_655 5_666 ?
O2 Pr1 C1 153.93(7) 2_655 5_666 ?
O2 Pr1 C1 153.93(7) 5_665 5_666 ?
O2 Pr1 C6 25.58(7) 2_655 5_665 ?
O2 Pr1 C6 25.58(7) 5_665 5_665 ?
O3 Pr1 O1 113.69(8) . 5_666 ?
O3 Pr1 O1 113.69(8) 6_565 5_666 ?
O3 Pr1 O2 74.39(9) 6_565 5_665 ?
O3 Pr1 O2 74.39(9) . 2_655 ?
O3 Pr1 O2 104.80(10) . 5_665 ?
O3 Pr1 O2 104.80(10) 6_565 2_655 ?
O3 Pr1 O3 74.84(14) . 6_565 ?
O3 Pr1 O4 75.54(9) . 5_666 ?
O3 Pr1 O4 75.54(9) 6_565 5_666 ?
O3 Pr1 C1 94.61(10) 6_565 5_666 ?
O3 Pr1 C1 94.61(10) . 5_666 ?
O3 Pr1 C6 90.19(10) . 5_665 ?
O3 Pr1 C6 90.19(10) 6_565 5_665 ?
O5 Pr1 O1 72.79(7) 6_565 . ?
O5 Pr1 O1 69.70(7) . 5_666 ?
O5 Pr1 O1 72.79(7) . . ?
O5 Pr1 O1 69.70(7) 6_565 5_666 ?
O5 Pr1 O2 77.69(10) 6_565 2_655 ?
O5 Pr1 O2 77.69(10) . 5_665 ?
O5 Pr1 O2 125.31(10) . 2_655 ?
O5 Pr1 O2 125.31(10) 6_565 5_665 ?
O5 Pr1 O3 73.63(9) . 6_565 ?
O5 Pr1 O3 73.63(9) 6_565 . ?
O5 Pr1 O3 146.33(10) . . ?
O5 Pr1 O3 146.33(10) 6_565 6_565 ?
O5 Pr1 O5 132.90(12) 6_565 . ?
O5 Pr1 O4 85.42(8) . 5_666 ?
O5 Pr1 O4 85.42(8) 6_565 5_666 ?
O5 Pr1 C1 76.53(8) 6_565 5_666 ?
O5 Pr1 C1 76.52(8) . 5_666 ?
O5 Pr1 C6 101.39(8) . 5_665 ?
O5 Pr1 C6 101.39(8) 6_565 5_665 ?
O4 Pr1 O1 48.72(10) 5_666 5_666 ?
O4 Pr1 C1 24.14(12) 5_666 5_666 ?
O4 Pr1 C6 161.92(12) 5_666 5_665 ?
C6 Pr1 C1 173.95(13) 5_665 5_666 ?
Pr1 O1 Pr1 108.02(12) . 5_666 ?
C1 O1 Pr1 160.3(3) . . ?
C1 O1 Pr1 91.7(3) . 5_666 ?
C6 O2 Pr1 93.7(3) . 5_665 ?
Pr1 O3 H3A 120.4 . . ?
Pr1 O3 H3B 131.7 . . ?
H3A O3 H3B 107.7 . . ?
C8 O5 Pr1 138.9(3) . . ?
C1 O4 Pr1 96.8(3) . 5_666 ?
O1 C1 Pr1 63.8(3) . 5_666 ?
O1 C1 C2 119.0(4) . . ?
O4 C1 Pr1 59.0(3) . 5_666 ?
O4 C1 O1 122.8(5) . . ?
O4 C1 C2 118.2(4) . . ?
C2 C1 Pr1 177.2(3) . 5_666 ?
C3 C2 C1 121.4(2) 6_565 . ?
C3 C2 C1 121.4(2) . . ?
C3 C2 C3 117.2(5) 6_565 . ?
F1 C3 C2 119.4(3) . . ?
F1 C3 C4 118.8(4) . . ?
C2 C3 C4 121.8(4) . . ?
F2 C4 C3 116.6(4) . . ?
F2 C4 C5 121.9(3) . . ?
C3 C4 C5 121.5(4) . . ?
C4 C5 C4 116.1(5) . 6_565 ?
C4 C5 C6 122.0(2) 6_565 . ?
C4 C5 C6 122.0(2) . . ?
O5 C8 O5 128.7(5) . 2_656 ?
O5 C8 C9 115.6(3) . . ?
O5 C8 C9 115.6(3) 2_656 . ?
C7 C9 C8 121.0(3) . . ?
C7 C9 C8 121.0(3) 2_656 . ?
C7 C9 C7 118.1(5) . 2_656 ?
C9 C7 C7 121.0(3) . 6 ?
F3 C7 C9 119.9(4) . . ?
F3 C7 C7 119.13(19) . 6 ?
O2 C6 Pr1 60.7(2) . 5_665 ?
O2 C6 Pr1 60.7(2) 6_565 5_665 ?
O2 C6 O2 121.4(5) . 6_565 ?
O2 C6 C5 119.3(2) . . ?
O2 C6 C5 119.3(2) 6_565 . ?
C5 C6 Pr1 176.6(3) . 5_665 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_6-sm_sq
_database_code_depnum_ccdc_archive 'CCDC 1486534'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 F6 O8 Sm'
_chemical_formula_sum            'C12 H4 F6 O8 Sm'
_chemical_formula_weight         540.50
_chemical_melting_point          ?
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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.931(5)
_cell_length_b                   11.283(5)
_cell_length_c                   11.654(5)
_cell_angle_alpha                90
_cell_angle_beta                 125.279(5)
_cell_angle_gamma                90
_cell_volume                     1495.4(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5285
_cell_measurement_theta_min      3.5759
_shelx_estimated_absorpt_T_max   0.602
_shelx_estimated_absorpt_T_min   0.444
_exptl_absorpt_coefficient_mu    4.042
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_correction_T_min  0.465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.401
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2740
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.994
_diffrn_reflns_theta_max         24.994
_diffrn_reflns_theta_min         3.583
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1324
_reflns_number_total             1397
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         2.130
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.168
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0608P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0882
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.000000 0.2423(7) 0.500000 0.0248(16) Uani 1 2 d S T P . .
C2 C 0.000000 0.3759(6) 0.500000 0.0237(16) Uani 1 2 d S T P . .
C3 C 0.0513(4) 0.4394(5) 0.6225(5) 0.0251(12) Uani 1 1 d . . . . .
C4 C 0.1387(7) 0.000000 0.7719(7) 0.0240(17) Uani 1 2 d S T P . .
C5 C 0.1359(6) 0.000000 0.8991(7) 0.0251(17) Uani 1 2 d S T P . .
C6 C 0.1360(5) 0.1039(5) 0.9614(6) 0.0290(13) Uani 1 1 d . . . . .
C7 C 0.1413(5) 0.1044(5) 1.0829(6) 0.0282(13) Uani 1 1 d . . . . .
C8 C 0.1469(6) 0.000000 1.1505(7) 0.0219(16) Uani 1 2 d S T P . .
C10 C 0.1580(6) 0.000000 1.2868(8) 0.0239(17) Uani 1 2 d S T P . .
O1 O -0.0911(3) 0.1944(3) 0.4726(4) 0.0346(10) Uani 1 1 d . . . . .
O2 O -0.3339(3) -0.1328(4) 0.3479(4) 0.0380(10) Uani 1 1 d . . . . .
H2A H -0.388200 -0.103092 0.268347 0.057 Uiso 1 1 d GR . . . .
H2B H -0.359741 -0.140631 0.398717 0.057 Uiso 1 1 d GR . . . .
O3 O 0.0446(4) 0.000000 0.6510(5) 0.0259(12) Uani 1 2 d S T P . .
O4 O 0.2367(5) 0.000000 0.7908(6) 0.0450(18) Uani 1 2 d S T P . .
O5 O 0.1616(4) 0.0972(4) 1.3418(4) 0.0385(11) Uani 1 1 d . . . . .
F1 F 0.1321(4) 0.2072(4) 0.9022(4) 0.0548(11) Uani 1 1 d . . . . .
F2 F 0.1426(4) 0.2105(4) 1.1338(4) 0.0546(12) Uani 1 1 d . . . . .
F5 F 0.1014(3) 0.3809(3) 0.7453(3) 0.0403(8) Uani 1 1 d . . . . .
Sm1 Sm -0.16120(3) 0.000000 0.46664(3) 0.01433(17) Uani 1 2 d S T P . .


_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
C1 C2 1.508(10) . ?
C1 O1 1.240(5) 2_556 ?
C1 O1 1.240(5) . ?
C2 C3 1.373(7) 2_556 ?
C2 C3 1.373(7) . ?
C3 C3 1.367(11) 6_565 ?
C3 F5 1.348(6) . ?
C4 C5 1.506(10) . ?
C4 O3 1.253(9) . ?
C4 O4 1.251(10) . ?
C4 Sm1 2.972(7) 5_556 ?
C5 C6 1.378(7) . ?
C5 C6 1.378(7) 6 ?
C6 C7 1.375(8) . ?
C6 F1 1.340(7) . ?
C7 C8 1.394(7) . ?
C7 F2 1.331(7) . ?
C8 C10 1.505(10) . ?
C10 O5 1.256(5) 6 ?
C10 O5 1.256(5) . ?
C10 Sm1 2.848(8) 5_557 ?
O1 Sm1 2.385(4) . ?
O2 Sm1 2.470(4) . ?
O3 Sm1 2.392(5) . ?
O3 Sm1 2.664(5) 5_556 ?
O4 Sm1 2.541(6) 5_556 ?
O5 Sm1 2.491(4) 5_557 ?
Sm1 Sm1 4.0919(17) 5_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 115.8(4) . . ?
O1 C1 C2 115.8(4) 2_556 . ?
O1 C1 O1 128.4(7) . 2_556 ?
C3 C2 C1 121.5(3) . . ?
C3 C2 C1 121.5(3) 2_556 . ?
C3 C2 C3 117.0(7) 2_556 . ?
C3 C3 C2 121.5(3) 6_565 . ?
F5 C3 C2 119.2(5) . . ?
F5 C3 C3 119.3(3) . 6_565 ?
C5 C4 Sm1 176.3(5) . 5_556 ?
O3 C4 C5 120.1(7) . . ?
O3 C4 Sm1 63.6(4) . 5_556 ?
O4 C4 C5 118.3(7) . . ?
O4 C4 O3 121.7(7) . . ?
O4 C4 Sm1 58.0(4) . 5_556 ?
C6 C5 C4 121.7(3) 6 . ?
C6 C5 C4 121.7(3) . . ?
C6 C5 C6 116.5(7) . 6 ?
C7 C6 C5 122.0(5) . . ?
F1 C6 C5 118.8(5) . . ?
F1 C6 C7 119.3(5) . . ?
C6 C7 C8 122.0(5) . . ?
F2 C7 C6 116.2(5) . . ?
F2 C7 C8 121.7(5) . . ?
C7 C8 C7 115.4(7) 6 . ?
C7 C8 C10 122.3(3) 6 . ?
C7 C8 C10 122.3(3) . . ?
C8 C10 Sm1 175.9(5) . 5_557 ?
O5 C10 C8 119.2(3) 6 . ?
O5 C10 C8 119.2(3) . . ?
O5 C10 O5 121.6(7) 6 . ?
O5 C10 Sm1 60.9(3) . 5_557 ?
O5 C10 Sm1 60.9(3) 6 5_557 ?
C1 O1 Sm1 138.5(4) . . ?
C4 O3 Sm1 91.4(4) . 5_556 ?
C4 O3 Sm1 160.6(5) . . ?
Sm1 O3 Sm1 107.96(18) . 5_556 ?
C4 O4 Sm1 97.3(4) . 5_556 ?
C10 O5 Sm1 93.0(4) . 5_557 ?
C4 Sm1 Sm1 58.72(15) 5_556 5_556 ?
C10 Sm1 C4 174.34(19) 5_557 5_556 ?
C10 Sm1 Sm1 115.62(15) 5_557 5_556 ?
O1 Sm1 C4 76.41(11) . 5_556 ?
O1 Sm1 C4 76.41(11) 6 5_556 ?
O1 Sm1 C10 101.70(11) 6 5_557 ?
O1 Sm1 C10 101.70(11) . 5_557 ?
O1 Sm1 O1 133.72(18) 6 . ?
O1 Sm1 O2 145.46(14) . . ?
O1 Sm1 O2 145.46(14) 6 6 ?
O1 Sm1 O2 73.05(13) . 6 ?
O1 Sm1 O2 73.05(13) 6 . ?
O1 Sm1 O3 73.50(10) . . ?
O1 Sm1 O3 73.49(10) 6 . ?
O1 Sm1 O3 69.76(10) . 5_556 ?
O1 Sm1 O3 69.77(10) 6 5_556 ?
O1 Sm1 O4 85.30(11) 6 5_556 ?
O1 Sm1 O4 85.30(11) . 5_556 ?
O1 Sm1 O5 77.39(14) . 2_557 ?
O1 Sm1 O5 77.39(14) 6 5_557 ?
O1 Sm1 O5 126.26(14) 6 2_557 ?
O1 Sm1 O5 126.26(14) . 5_557 ?
O1 Sm1 Sm1 66.97(9) . 5_556 ?
O1 Sm1 Sm1 66.97(9) 6 5_556 ?
O2 Sm1 C4 94.06(15) 6 5_556 ?
O2 Sm1 C4 94.06(15) . 5_556 ?
O2 Sm1 C10 90.44(16) . 5_557 ?
O2 Sm1 C10 90.44(16) 6 5_557 ?
O2 Sm1 O2 74.7(2) 6 . ?
O2 Sm1 O3 113.46(13) . 5_556 ?
O2 Sm1 O3 113.46(13) 6 5_556 ?
O2 Sm1 O4 74.55(14) 6 5_556 ?
O2 Sm1 O4 74.55(14) . 5_556 ?
O2 Sm1 O5 74.29(14) 6 2_557 ?
O2 Sm1 O5 105.26(15) 6 5_557 ?
O2 Sm1 O5 105.26(15) . 2_557 ?
O2 Sm1 O5 74.29(14) . 5_557 ?
O2 Sm1 Sm1 135.53(10) . 5_556 ?
O2 Sm1 Sm1 135.53(10) 6 5_556 ?
O3 Sm1 C4 24.94(18) 5_556 5_556 ?
O3 Sm1 C4 96.98(19) . 5_556 ?
O3 Sm1 C10 77.36(19) . 5_557 ?
O3 Sm1 C10 149.40(18) 5_556 5_557 ?
O3 Sm1 O2 141.03(11) . 6 ?
O3 Sm1 O2 141.03(11) . . ?
O3 Sm1 O3 72.04(18) . 5_556 ?
O3 Sm1 O4 121.66(17) . 5_556 ?
O3 Sm1 O5 79.43(15) . 5_557 ?
O3 Sm1 O5 79.43(15) . 2_557 ?
O3 Sm1 Sm1 33.78(10) 5_556 5_556 ?
O3 Sm1 Sm1 38.26(12) . 5_556 ?
O4 Sm1 C4 24.69(19) 5_556 5_556 ?
O4 Sm1 C10 161.0(2) 5_556 5_557 ?
O4 Sm1 O3 49.62(16) 5_556 5_556 ?
O4 Sm1 Sm1 83.40(12) 5_556 5_556 ?
O5 Sm1 C4 153.47(11) 2_557 5_556 ?
O5 Sm1 C4 153.47(10) 5_557 5_556 ?
O5 Sm1 C10 26.14(10) 5_557 5_557 ?
O5 Sm1 C10 26.14(10) 2_557 5_557 ?
O5 Sm1 O3 141.22(13) 2_557 5_556 ?
O5 Sm1 O3 141.22(13) 5_557 5_556 ?
O5 Sm1 O4 147.60(12) 2_557 5_556 ?
O5 Sm1 O4 147.60(12) 5_557 5_556 ?
O5 Sm1 O5 52.2(2) 2_557 5_557 ?
O5 Sm1 Sm1 113.60(11) 2_557 5_556 ?
O5 Sm1 Sm1 113.60(11) 5_557 5_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_11-ho_sq
_database_code_depnum_ccdc_archive 'CCDC 1486539'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 F6 Ho O8'
_chemical_formula_sum            'C12 H4 F6 Ho O8'
_chemical_formula_weight         555.08
_chemical_melting_point          ?
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'
Ho Ho -0.2175 4.6783 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.782(5)
_cell_length_b                   11.192(5)
_cell_length_c                   11.547(5)
_cell_angle_alpha                90
_cell_angle_beta                 124.208(5)
_cell_angle_gamma                90
_cell_volume                     1473.0(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1867
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4364
_cell_measurement_theta_min      3.5680
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.488
_exptl_absorpt_correction_T_max  0.416
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.503
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2683
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.575
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1288
_reflns_number_total             1380
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
    1    1    0     2.550
   -2    0    1     2.958
    0    0    1     2.133
   -1    1    1     2.602
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.723
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1376
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0309P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0656
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2. Restrained distances
 H5B-O5
 0.85 with sigma of 0.02
 H5A-O5
 0.85 with sigma of 0.02
 H5B-H5A
 1.373 with sigma of 0.04
3.a Riding coordinates:
 O5(H5A,H5B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Ho1 Ho 0.65888(2) 0.500000 0.53047(3) 0.01470(13) Uani 1 2 d S T P . .
F1 F 0.3688(4) 0.7085(3) 0.0990(4) 0.0552(11) Uani 1 1 d . . . . .
F2 F 0.3561(4) 0.7125(4) -0.1360(4) 0.0557(11) Uani 1 1 d . . . . .
F3 F 0.3989(3) 0.1196(3) 0.2550(3) 0.0437(9) Uani 1 1 d . . . . .
O1 O 0.4614(4) 0.500000 0.3519(5) 0.0254(12) Uani 1 2 d S T P . .
O2 O 0.2684(5) 0.500000 0.2201(5) 0.0385(16) Uani 1 2 d S T P . .
O3 O 0.3377(4) 0.4020(4) -0.3450(4) 0.0356(10) Uani 1 1 d . . . . .
O4 O 0.5925(3) 0.3088(3) 0.5290(4) 0.0286(9) Uani 1 1 d . . . . .
O5 O 0.8292(3) 0.3725(4) 0.6437(4) 0.0341(10) Uani 1 1 d D . . . .
H5A H 0.813716 0.298262 0.636507 0.041 Uiso 1 1 d DR . . . .
H5B H 0.868216 0.388132 0.729837 0.041 Uiso 1 1 d DR . . . .
C1 C 0.3655(6) 0.500000 0.2343(7) 0.0250(17) Uani 1 2 d S T P . .
C2 C 0.3651(6) 0.500000 0.1029(7) 0.0247(18) Uani 1 2 d S T P . .
C3 C 0.3637(5) 0.6045(5) 0.0398(5) 0.0289(13) Uani 1 1 d . . . . .
C4 C 0.3578(5) 0.6048(5) -0.0837(5) 0.0282(13) Uani 1 1 d . . . . .
C5 C 0.3513(6) 0.500000 -0.1512(7) 0.0236(17) Uani 1 2 d S T P . .
C6 C 0.3411(6) 0.500000 -0.2895(7) 0.0243(18) Uani 1 2 d S T P . .
C7 C 0.500000 0.2621(7) 0.500000 0.0255(17) Uani 1 2 d S T P . .
C8 C 0.500000 0.1257(6) 0.500000 0.0217(16) Uani 1 2 d S T P . .
C9 C 0.4489(4) 0.0615(5) 0.3782(5) 0.0260(12) 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
Ho1 O1 2.313(5) . ?
Ho1 O1 2.669(5) 5_666 ?
Ho1 O2 2.460(5) 5_666 ?
Ho1 O3 2.430(3) 2_655 ?
Ho1 O3 2.430(3) 5_665 ?
Ho1 O4 2.323(4) 6_565 ?
Ho1 O4 2.323(4) . ?
Ho1 O5 2.409(4) 6_565 ?
Ho1 O5 2.409(4) . ?
Ho1 C1 2.918(7) 5_666 ?
Ho1 C6 2.782(7) 5_665 ?
F1 C3 1.331(6) . ?
F2 C4 1.342(7) . ?
F3 C9 1.349(6) . ?
O1 C1 1.254(8) . ?
O2 C1 1.254(8) . ?
O3 C6 1.257(5) . ?
O4 C7 1.237(5) . ?
O5 H5A 0.8499 . ?
O5 H5B 0.8416 . ?
C1 C2 1.515(9) . ?
C2 C3 1.373(6) . ?
C2 C3 1.373(6) 6_565 ?
C3 C4 1.382(7) . ?
C4 C5 1.383(6) . ?
C5 C6 1.522(9) . ?
C7 C8 1.526(10) . ?
C8 C9 1.370(6) . ?
C8 C9 1.370(6) 2_656 ?
C9 C9 1.377(11) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ho1 O1 72.38(17) . 5_666 ?
O1 Ho1 O2 122.97(16) . 5_666 ?
O1 Ho1 O3 79.08(14) . 2_655 ?
O1 Ho1 O3 79.08(14) . 5_665 ?
O1 Ho1 O4 74.46(10) . 6_565 ?
O1 Ho1 O4 74.46(10) . . ?
O1 Ho1 O5 141.53(10) . 6_565 ?
O1 Ho1 O5 141.53(11) . . ?
O1 Ho1 C1 97.82(19) . 5_666 ?
O1 Ho1 C1 25.44(17) 5_666 5_666 ?
O1 Ho1 C6 149.09(17) 5_666 5_665 ?
O1 Ho1 C6 76.72(18) . 5_665 ?
O2 Ho1 O1 50.59(15) 5_666 5_666 ?
O2 Ho1 C1 25.15(18) 5_666 5_666 ?
O2 Ho1 C6 160.31(19) 5_666 5_665 ?
O3 Ho1 O1 140.70(12) 2_655 5_666 ?
O3 Ho1 O1 140.70(12) 5_665 5_666 ?
O3 Ho1 O2 146.59(12) 5_665 5_666 ?
O3 Ho1 O2 146.59(12) 2_655 5_666 ?
O3 Ho1 O3 53.63(19) 2_655 5_665 ?
O3 Ho1 C1 152.85(10) 5_665 5_666 ?
O3 Ho1 C1 152.85(10) 2_655 5_666 ?
O3 Ho1 C6 26.83(10) 5_665 5_665 ?
O3 Ho1 C6 26.83(10) 2_655 5_665 ?
O4 Ho1 O1 69.46(9) . 5_666 ?
O4 Ho1 O1 69.46(9) 6_565 5_666 ?
O4 Ho1 O2 84.74(10) 6_565 5_666 ?
O4 Ho1 O2 84.74(10) . 5_666 ?
O4 Ho1 O3 77.33(13) . 2_655 ?
O4 Ho1 O3 127.70(13) 6_565 2_655 ?
O4 Ho1 O3 77.33(13) 6_565 5_665 ?
O4 Ho1 O3 127.70(13) . 5_665 ?
O4 Ho1 O4 134.12(16) 6_565 . ?
O4 Ho1 O5 144.01(14) . 6_565 ?
O4 Ho1 O5 144.01(14) 6_565 . ?
O4 Ho1 O5 73.62(13) . . ?
O4 Ho1 O5 73.62(13) 6_565 6_565 ?
O4 Ho1 C1 75.88(10) . 5_666 ?
O4 Ho1 C1 75.88(10) 6_565 5_666 ?
O4 Ho1 C6 102.35(10) 6_565 5_665 ?
O4 Ho1 C6 102.35(10) . 5_665 ?
O5 Ho1 O1 114.72(11) . 5_666 ?
O5 Ho1 O1 114.72(11) 6_565 5_666 ?
O5 Ho1 O2 74.54(12) . 5_666 ?
O5 Ho1 O2 74.54(12) 6_565 5_666 ?
O5 Ho1 O3 73.46(13) 6_565 5_665 ?
O5 Ho1 O3 104.47(14) . 5_665 ?
O5 Ho1 O3 104.46(14) 6_565 2_655 ?
O5 Ho1 O3 73.46(13) . 2_655 ?
O5 Ho1 O5 72.66(19) . 6_565 ?
O5 Ho1 C1 94.69(14) 6_565 5_666 ?
O5 Ho1 C1 94.69(14) . 5_666 ?
O5 Ho1 C6 89.71(14) 6_565 5_665 ?
O5 Ho1 C6 89.71(14) . 5_665 ?
C6 Ho1 C1 174.53(19) 5_665 5_666 ?
Ho1 O1 Ho1 107.62(17) . 5_666 ?
C1 O1 Ho1 163.9(5) . . ?
C1 O1 Ho1 88.5(4) . 5_666 ?
C1 O2 Ho1 98.3(4) . 5_666 ?
C6 O3 Ho1 92.4(3) . 5_665 ?
C7 O4 Ho1 137.2(4) . . ?
Ho1 O5 H5A 114.3 . . ?
Ho1 O5 H5B 107.4 . . ?
H5A O5 H5B 106.1 . . ?
O1 C1 Ho1 66.1(4) . 5_666 ?
O1 C1 C2 119.6(6) . . ?
O2 C1 Ho1 56.5(3) . 5_666 ?
O2 C1 O1 122.6(6) . . ?
O2 C1 C2 117.8(6) . . ?
C2 C1 Ho1 174.3(5) . 5_666 ?
C3 C2 C1 121.5(3) 6_565 . ?
C3 C2 C1 121.5(3) . . ?
C3 C2 C3 116.9(6) . 6_565 ?
F1 C3 C2 119.5(4) . . ?
F1 C3 C4 118.9(5) . . ?
C2 C3 C4 121.7(5) . . ?
F2 C4 C3 116.2(5) . . ?
F2 C4 C5 121.9(4) . . ?
C3 C4 C5 121.8(5) . . ?
C4 C5 C4 116.0(6) 6_565 . ?
C4 C5 C6 122.0(3) . . ?
C4 C5 C6 122.0(3) 6_565 . ?
O3 C6 Ho1 60.8(3) . 5_665 ?
O3 C6 Ho1 60.8(3) 6_565 5_665 ?
O3 C6 O3 121.4(6) 6_565 . ?
O3 C6 C5 119.3(3) 6_565 . ?
O3 C6 C5 119.3(3) . . ?
C5 C6 Ho1 175.6(5) . 5_665 ?
O4 C7 O4 129.9(7) . 2_656 ?
O4 C7 C8 115.0(4) . . ?
O4 C7 C8 115.0(4) 2_656 . ?
C9 C8 C7 121.7(3) . . ?
C9 C8 C7 121.7(3) 2_656 . ?
C9 C8 C9 116.7(7) . 2_656 ?
F3 C9 C8 119.5(5) . . ?
F3 C9 C9 118.8(3) . 6 ?
C8 C9 C9 121.7(3) . 6 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_12-er_sq
_database_code_depnum_ccdc_archive 'CCDC 1486540'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 Er F6 O8'
_chemical_formula_sum            'C12 H4 Er F6 O8'
_chemical_formula_weight         557.41
_chemical_melting_point          ?
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'
Er Er -0.2586 4.9576 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.754(5)
_cell_length_b                   11.149(5)
_cell_length_c                   11.518(5)
_cell_angle_alpha                90
_cell_angle_beta                 123.933(5)
_cell_angle_gamma                90
_cell_volume                     1465.4(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1493
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7812
_cell_measurement_theta_min      3.5636
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.844
_exptl_absorpt_correction_T_max  0.370
_exptl_absorpt_correction_T_min  0.225
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1048.0
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0487
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2837
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.972
_diffrn_reflns_theta_max         24.972
_diffrn_reflns_theta_min         3.571
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1293
_reflns_number_total             1377
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
    1    1    0     2.554
   -2    0    1     2.965
    0    0    1     2.131
   -1    1    1     2.611
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         1.394
_refine_diff_density_min         -1.399
_refine_diff_density_rms         0.160
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1373
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0278
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0299P)²+1.3512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0656
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O5(H5A,H5B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Er1 Er -0.15862(3) 0.500000 -0.02984(3) 0.01373(13) Uani 1 2 d S T P . .
F1 F 0.1302(4) 0.7093(3) 0.4005(4) 0.0552(12) Uani 1 1 d . . . . .
F2 F 0.1437(4) 0.7124(3) 0.6361(4) 0.0541(12) Uani 1 1 d . . . . .
O3 O 0.1633(4) 0.5971(4) 0.8447(4) 0.0348(10) Uani 1 1 d . . . . .
O1 O 0.0371(4) 0.500000 0.1474(5) 0.0237(12) Uani 1 2 d S T P . .
O4 O -0.0927(3) 0.3099(3) -0.0301(4) 0.0261(9) Uani 1 1 d . . . . .
O2 O 0.2291(5) 0.500000 0.2765(5) 0.0365(15) Uani 1 2 d S T P . .
O5 O -0.3275(3) 0.6271(4) -0.1441(4) 0.0327(9) Uani 1 1 d . . . . .
H5A H -0.310196 0.697354 -0.155620 0.039 Uiso 1 1 d R . . . .
H5B H -0.348556 0.632144 -0.087520 0.039 Uiso 1 1 d R . . . .
C1 C 0.1339(7) 0.500000 0.2654(7) 0.0248(18) Uani 1 2 d S T P . .
C2 C 0.1340(6) 0.500000 0.3966(7) 0.0220(17) Uani 1 2 d S T P . .
C3 C 0.1350(5) 0.6046(5) 0.4599(6) 0.0276(13) Uani 1 1 d . . . . .
C4 C 0.1419(5) 0.6052(5) 0.5829(6) 0.0285(13) Uani 1 1 d . . . . .
C5 C 0.1476(6) 0.500000 0.6516(7) 0.0216(17) Uani 1 2 d S T P . .
C6 C 0.1590(7) 0.500000 0.7889(7) 0.0233(18) Uani 1 2 d S T P . .
F3 F -0.1020(3) 0.1197(3) -0.2444(3) 0.0401(9) Uani 1 1 d . . . . .
C8 C -0.0522(4) 0.0609(5) -0.1216(5) 0.0233(12) Uani 1 1 d . . . . .
C9 C 0.000000 0.1272(6) 0.000000 0.0162(15) Uani 1 2 d S T P . .
C12 C 0.000000 0.2625(6) 0.000000 0.0200(16) Uani 1 2 d S T P . .


_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
Er1 O3 2.424(3) 2_556 ?
Er1 O3 2.424(3) 5_566 ?
Er1 O1 2.674(5) 5_565 ?
Er1 O1 2.298(5) . ?
Er1 O4 2.306(3) . ?
Er1 O4 2.306(3) 6_565 ?
Er1 O2 2.437(5) 5_565 ?
Er1 O5 2.392(4) . ?
Er1 O5 2.392(4) 6_565 ?
Er1 C1 2.917(7) 5_565 ?
Er1 C6 2.777(7) 5_566 ?
F1 C3 1.336(6) . ?
F2 C4 1.337(6) . ?
O3 C6 1.243(5) . ?
O1 C1 1.264(9) . ?
O4 C12 1.238(4) . ?
O2 C1 1.242(9) . ?
O5 H5A 0.8500 . ?
O5 H5B 0.8501 . ?
C1 C2 1.510(9) . ?
C2 C3 1.372(7) 6_565 ?
C2 C3 1.372(7) . ?
C3 C4 1.366(8) . ?
C4 C5 1.392(7) . ?
C5 C6 1.501(9) . ?
F3 C8 1.348(6) . ?
C8 C8 1.357(10) 6 ?
C8 C9 1.379(6) . ?
C9 C12 1.508(9) . ?

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
O3 Er1 O3 53.04(19) 2_556 5_566 ?
O3 Er1 O1 140.93(13) 2_556 5_565 ?
O3 Er1 O1 140.93(13) 5_566 5_565 ?
O3 Er1 O2 146.84(12) 2_556 5_565 ?
O3 Er1 O2 146.84(12) 5_566 5_565 ?
O3 Er1 C1 153.18(10) 5_566 5_565 ?
O3 Er1 C1 153.18(10) 2_556 5_565 ?
O3 Er1 C6 26.55(9) 5_566 5_566 ?
O3 Er1 C6 26.55(9) 2_556 5_566 ?
O1 Er1 O3 79.16(15) . 5_566 ?
O1 Er1 O3 79.16(15) . 2_556 ?
O1 Er1 O1 72.32(17) . 5_565 ?
O1 Er1 O4 74.61(10) . 6_565 ?
O1 Er1 O4 74.61(10) . . ?
O1 Er1 O2 122.81(18) . 5_565 ?
O1 Er1 O5 141.72(10) . 6_565 ?
O1 Er1 O5 141.72(10) . . ?
O1 Er1 C1 98.0(2) . 5_565 ?
O1 Er1 C1 25.67(19) 5_565 5_565 ?
O1 Er1 C6 148.86(19) 5_565 5_566 ?
O1 Er1 C6 76.5(2) . 5_566 ?
O4 Er1 O3 78.11(13) . 5_566 ?
O4 Er1 O3 127.95(13) 6_565 5_566 ?
O4 Er1 O3 127.94(13) . 2_556 ?
O4 Er1 O3 78.11(13) 6_565 2_556 ?
O4 Er1 O1 69.04(9) . 5_565 ?
O4 Er1 O1 69.04(9) 6_565 5_565 ?
O4 Er1 O4 133.62(17) . 6_565 ?
O4 Er1 O2 84.23(10) . 5_565 ?
O4 Er1 O2 84.23(10) 6_565 5_565 ?
O4 Er1 O5 143.67(14) 6_565 6_565 ?
O4 Er1 O5 73.52(13) 6_565 . ?
O4 Er1 O5 143.67(14) . . ?
O4 Er1 O5 73.52(13) . 6_565 ?
O4 Er1 C1 75.46(10) . 5_565 ?
O4 Er1 C1 75.46(10) 6_565 5_565 ?
O4 Er1 C6 102.77(10) . 5_566 ?
O4 Er1 C6 102.77(10) 6_565 5_566 ?
O2 Er1 O1 50.48(16) 5_565 5_565 ?
O2 Er1 C1 24.8(2) 5_565 5_565 ?
O2 Er1 C6 160.7(2) 5_565 5_566 ?
O5 Er1 O3 74.03(13) 6_565 5_566 ?
O5 Er1 O3 74.03(13) . 2_556 ?
O5 Er1 O3 104.72(14) 6_565 2_556 ?
O5 Er1 O3 104.72(14) . 5_566 ?
O5 Er1 O1 114.24(12) . 5_565 ?
O5 Er1 O1 114.24(12) 6_565 5_565 ?
O5 Er1 O2 74.14(13) 6_565 5_565 ?
O5 Er1 O2 74.14(13) . 5_565 ?
O5 Er1 O5 72.7(2) 6_565 . ?
O5 Er1 C1 94.01(15) . 5_565 ?
O5 Er1 C1 94.01(15) 6_565 5_565 ?
O5 Er1 C6 90.40(16) . 5_566 ?
O5 Er1 C6 90.40(16) 6_565 5_566 ?
C6 Er1 C1 174.5(2) 5_566 5_565 ?
C6 O3 Er1 92.8(4) . 5_566 ?
Er1 O1 Er1 107.68(17) . 5_565 ?
C1 O1 Er1 87.9(4) . 5_565 ?
C1 O1 Er1 164.4(5) . . ?
C12 O4 Er1 137.4(4) . . ?
C1 O2 Er1 99.8(4) . 5_565 ?
Er1 O5 H5A 111.2 . . ?
Er1 O5 H5B 105.0 . . ?
H5A O5 H5B 107.7 . . ?
O1 C1 Er1 66.4(4) . 5_565 ?
O1 C1 C2 119.2(7) . . ?
O2 C1 Er1 55.4(4) . 5_565 ?
O2 C1 O1 121.8(6) . . ?
O2 C1 C2 118.9(7) . . ?
C2 C1 Er1 174.4(5) . 5_565 ?
C3 C2 C1 121.8(3) . . ?
C3 C2 C1 121.8(3) 6_565 . ?
C3 C2 C3 116.4(6) 6_565 . ?
F1 C3 C2 119.2(5) . . ?
F1 C3 C4 118.8(5) . . ?
C4 C3 C2 122.0(5) . . ?
F2 C4 C3 116.9(5) . . ?
F2 C4 C5 120.8(5) . . ?
C3 C4 C5 122.3(5) . . ?
C4 C5 C4 114.8(6) . 6_565 ?
C4 C5 C6 122.6(3) 6_565 . ?
C4 C5 C6 122.6(3) . . ?
O3 C6 Er1 60.7(3) . 5_566 ?
O3 C6 Er1 60.7(3) 6_565 5_566 ?
O3 C6 O3 121.1(6) 6_565 . ?
O3 C6 C5 119.5(3) 6_565 . ?
O3 C6 C5 119.5(3) . . ?
C5 C6 Er1 175.0(5) . 5_566 ?
F3 C8 C8 119.1(3) . 6 ?
F3 C8 C9 118.4(5) . . ?
C8 C8 C9 122.4(3) 6 . ?
C8 C9 C8 115.1(6) 2 . ?
C8 C9 C12 122.4(3) 2 . ?
C8 C9 C12 122.4(3) . . ?
O4 C12 O4 129.5(7) 2 . ?
O4 C12 C9 115.3(3) . . ?
O4 C12 C9 115.3(3) 2 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_1-pr-3d_sq
_database_code_depnum_ccdc_archive 'CCDC 1445653'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 F6 O7 Pr'
_chemical_formula_sum            'C12 F6 O7 Pr'
_chemical_formula_weight         511.03
_chemical_melting_point          ?
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'
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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.212(5)
_cell_length_b                   21.288(5)
_cell_length_c                   7.905(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.851(5)
_cell_angle_gamma                90
_cell_volume                     1698.0(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2022
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5060
_cell_measurement_theta_min      3.2285
_shelx_estimated_absorpt_T_max   0.649
_shelx_estimated_absorpt_T_min   0.537
_exptl_absorpt_coefficient_mu    2.962
_exptl_absorpt_correction_T_max  0.623
_exptl_absorpt_correction_T_min  0.496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.999
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            5858
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.235
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2354
_reflns_number_total             2988
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.030  0.000 -0.019       206        55 ' '
   2  0.480  0.500 -0.061       206        55 ' '
The unit cells of complex contains two water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         2.867
_refine_diff_density_min         -1.441
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2983
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0531
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+3.5993P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1256
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 C3-C1
 1.395 with sigma of 0.02
 C3-C2
 1.395 with sigma of 0.02
 C2-C1
 2.4 with sigma of 0.04
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Pr1 Pr 0.01055(4) 0.21505(2) 0.00493(6) 0.01566(18) Uani 1 1 d . . . . .
O4 O -0.1291(6) 0.2595(3) -0.2515(8) 0.0310(15) Uani 1 1 d . . . . .
O1 O 0.2464(6) 0.1899(3) -0.0297(8) 0.0355(16) Uani 1 1 d . . . . .
O3 O -0.2245(6) 0.1838(3) 0.0338(8) 0.0398(17) Uani 1 1 d . . . . .
F3 F -0.4106(6) 0.1227(3) 0.2416(9) 0.0526(17) Uani 1 1 d . . . . .
C5 C -0.2309(8) 0.2167(4) 0.1617(11) 0.0215(18) Uani 1 1 d . . . . .
O2 O 0.1522(5) 0.2580(3) -0.2171(8) 0.0307(15) Uani 1 1 d . . . . .
F6 F -0.3340(5) 0.3388(2) 0.1775(8) 0.0428(15) Uani 1 1 d . . . . .
C10 C 0.2529(8) 0.2280(4) -0.1430(11) 0.025(2) Uani 1 1 d . . . . .
O6 O -0.0102(6) 0.1328(3) -0.2089(7) 0.0328(16) Uani 1 1 d . . . . .
O5 O 0.0432(7) 0.1187(3) 0.1806(9) 0.0464(19) Uani 1 1 d . . . . .
F5 F 0.4319(6) 0.1356(3) -0.2275(9) 0.0492(16) Uani 1 1 d . . . . .
F4 F -0.6437(5) 0.1478(3) 0.3378(9) 0.0540(18) Uani 1 1 d . . . . .
F2 F 0.2302(7) 0.0590(4) -0.3877(14) 0.107(3) Uani 1 1 d . . . . .
C6 C -0.3637(8) 0.2301(4) 0.2116(11) 0.024(2) Uani 1 1 d . . . . .
C7 C -0.4480(9) 0.1829(4) 0.2503(12) 0.029(2) Uani 1 1 d . . . . .
C3 C 0.0003(9) 0.0602(4) -0.4333(11) 0.031(2) Uani 1 1 d D . . . .
C9 C 0.3874(8) 0.2434(5) -0.1940(11) 0.027(2) Uani 1 1 d . . . . .
C4 C 0.0007(10) 0.1272(4) -0.3636(12) 0.031(2) Uani 1 1 d . . . . .
C8 C -0.5690(8) 0.1963(5) 0.2948(12) 0.031(2) Uani 1 1 d . . . . .
C12 C -0.4089(9) 0.2920(4) 0.2216(11) 0.027(2) Uani 1 1 d . . . . .
O7 O 0.0145(9) 0.3302(3) 0.0307(9) 0.058(2) Uani 1 1 d . . . . .
C2 C 0.1175(10) 0.0296(5) -0.4422(14) 0.044(3) Uani 1 1 d D . . . .
F1 F -0.2307(7) 0.0592(3) -0.4845(13) 0.102(3) Uani 1 1 d . . . . .
C1 C -0.1169(10) 0.0299(4) -0.4916(13) 0.041(3) Uani 1 1 d D . . . .
C11 C 0.4706(8) 0.1964(5) -0.2324(12) 0.031(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
Pr1 O4 2.479(6) . ?
Pr1 O4 2.623(6) 4_566 ?
Pr1 O1 2.523(6) . ?
Pr1 O3 2.535(6) . ?
Pr1 C5 2.925(8) . ?
Pr1 O2 2.504(6) 4_566 ?
Pr1 O2 2.606(6) . ?
Pr1 C10 2.909(8) . ?
Pr1 O6 2.421(6) . ?
Pr1 O5 2.471(6) . ?
Pr1 O7 2.459(6) . ?
O4 C5 1.261(10) 4_565 ?
O1 C10 1.217(10) . ?
O3 C5 1.240(10) . ?
F3 C7 1.342(10) . ?
C5 C6 1.497(11) . ?
O2 C10 1.274(10) . ?
F6 C12 1.335(10) . ?
C10 C9 1.525(11) . ?
O6 C4 1.250(10) . ?
F5 C11 1.356(11) . ?
F4 C8 1.359(9) . ?
F2 C2 1.323(11) . ?
C6 C7 1.388(12) . ?
C6 C12 1.401(12) . ?
C7 C8 1.366(12) . ?
C3 C4 1.529(11) . ?
C3 C2 1.374(11) . ?
C3 C1 1.375(11) . ?
C9 C8 1.365(13) 4_665 ?
C9 C11 1.377(13) . ?
C4 O7 1.256(11) 4_565 ?
C12 C11 1.359(12) 4_466 ?
C2 C1 1.369(13) 3_554 ?
F1 C1 1.329(11) . ?

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
O4 Pr1 O4 102.25(18) . 4_566 ?
O4 Pr1 O1 115.51(19) . . ?
O4 Pr1 O3 75.0(2) . . ?
O4 Pr1 C5 25.5(2) 4_566 . ?
O4 Pr1 C5 85.7(2) . . ?
O4 Pr1 O2 67.94(18) . . ?
O4 Pr1 O2 144.3(2) . 4_566 ?
O4 Pr1 C10 150.2(2) 4_566 . ?
O4 Pr1 C10 93.0(2) . . ?
O1 Pr1 O4 139.4(2) . 4_566 ?
O1 Pr1 O3 152.5(2) . . ?
O1 Pr1 C5 158.4(2) . . ?
O1 Pr1 O2 50.44(19) . . ?
O1 Pr1 C10 24.6(2) . . ?
O3 Pr1 O4 50.14(19) . 4_566 ?
O3 Pr1 C5 25.0(2) . . ?
O3 Pr1 O2 141.7(2) . . ?
O3 Pr1 C10 159.6(2) . . ?
O2 Pr1 O4 67.32(19) 4_566 4_566 ?
O2 Pr1 O4 147.4(2) . 4_566 ?
O2 Pr1 O1 73.2(2) 4_566 . ?
O2 Pr1 O3 114.11(19) 4_566 . ?
O2 Pr1 C5 150.8(2) . . ?
O2 Pr1 C5 92.1(2) 4_566 . ?
O2 Pr1 O2 101.83(17) 4_566 . ?
O2 Pr1 C10 26.0(2) . . ?
O2 Pr1 C10 85.3(2) 4_566 . ?
C10 Pr1 C5 173.8(2) . . ?
O6 Pr1 O4 74.2(2) . . ?
O6 Pr1 O4 131.6(2) . 4_566 ?
O6 Pr1 O1 75.7(2) . . ?
O6 Pr1 O3 83.7(2) . . ?
O6 Pr1 C5 108.4(2) . . ?
O6 Pr1 O2 77.4(2) . . ?
O6 Pr1 O2 139.0(2) . 4_566 ?
O6 Pr1 C10 77.1(2) . . ?
O6 Pr1 O5 77.4(2) . . ?
O6 Pr1 O7 141.0(2) . . ?
O5 Pr1 O4 78.5(2) . 4_566 ?
O5 Pr1 O4 141.9(2) . . ?
O5 Pr1 O1 80.6(2) . . ?
O5 Pr1 O3 77.2(2) . . ?
O5 Pr1 C5 79.7(2) . . ?
O5 Pr1 O2 71.8(2) . 4_566 ?
O5 Pr1 O2 129.0(2) . . ?
O5 Pr1 C10 104.8(2) . . ?
O7 Pr1 O4 74.7(2) . 4_566 ?
O7 Pr1 O4 71.8(2) . . ?
O7 Pr1 O1 102.5(3) . . ?
O7 Pr1 O3 105.0(3) . . ?
O7 Pr1 C5 87.5(2) . . ?
O7 Pr1 O2 72.5(2) . 4_566 ?
O7 Pr1 O2 72.7(2) . . ?
O7 Pr1 C10 86.3(3) . . ?
O7 Pr1 O5 141.4(2) . . ?
Pr1 O4 Pr1 111.7(2) . 4_565 ?
C5 O4 Pr1 90.7(5) 4_565 4_565 ?
C5 O4 Pr1 157.0(5) 4_565 . ?
C10 O1 Pr1 95.7(5) . . ?
C5 O3 Pr1 95.4(5) . . ?
O4 C5 Pr1 63.7(4) 4_566 . ?
O4 C5 C6 118.9(7) 4_566 . ?
O3 C5 Pr1 59.6(4) . . ?
O3 C5 O4 121.9(7) . 4_566 ?
O3 C5 C6 119.1(8) . . ?
C6 C5 Pr1 166.1(6) . . ?
Pr1 O2 Pr1 111.5(2) 4_565 . ?
C10 O2 Pr1 146.6(5) . 4_565 ?
C10 O2 Pr1 90.4(5) . . ?
O1 C10 Pr1 59.7(4) . . ?
O1 C10 O2 122.7(8) . . ?
O1 C10 C9 119.4(8) . . ?
O2 C10 Pr1 63.6(4) . . ?
O2 C10 C9 117.8(7) . . ?
C9 C10 Pr1 169.4(6) . . ?
C4 O6 Pr1 137.8(5) . . ?
C7 C6 C5 122.5(8) . . ?
C7 C6 C12 116.6(7) . . ?
C12 C6 C5 121.0(7) . . ?
F3 C7 C6 119.3(8) . . ?
F3 C7 C8 119.2(8) . . ?
C8 C7 C6 121.4(8) . . ?
C2 C3 C4 120.4(8) . . ?
C2 C3 C1 118.7(8) . . ?
C1 C3 C4 120.9(8) . . ?
C8 C9 C10 122.4(8) 4_665 . ?
C8 C9 C11 116.8(8) 4_665 . ?
C11 C9 C10 120.8(8) . . ?
O6 C4 C3 116.4(8) . . ?
O6 C4 O7 128.1(8) . 4_565 ?
O7 C4 C3 115.4(8) 4_565 . ?
F4 C8 C7 118.1(8) . . ?
F4 C8 C9 119.8(8) . 4_466 ?
C9 C8 C7 122.0(8) 4_466 . ?
F6 C12 C6 118.7(7) . . ?
F6 C12 C11 120.8(8) . 4_466 ?
C11 C12 C6 120.4(9) 4_466 . ?
C4 O7 Pr1 140.7(6) 4_566 . ?
F2 C2 C3 118.7(8) . . ?
F2 C2 C1 121.0(9) . 3_554 ?
C1 C2 C3 120.3(9) 3_554 . ?
C2 C1 C3 120.9(9) 3_554 . ?
F1 C1 C3 119.1(8) . . ?
F1 C1 C2 119.9(9) . 3_554 ?
F5 C11 C9 119.7(7) . . ?
F5 C11 C12 117.5(8) . 4_665 ?
C12 C11 C9 122.8(9) 4_665 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_7-eu_sq
_database_code_depnum_ccdc_archive 'CCDC 1486535'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 Eu F6 O8'
_chemical_formula_sum            'C12 H4 Eu F6 O8'
_chemical_formula_weight         542.12
_chemical_melting_point          ?
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'
Eu Eu -0.1578 3.6682 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.896(5)
_cell_length_b                   11.257(5)
_cell_length_c                   11.628(5)
_cell_angle_alpha                90
_cell_angle_beta                 125.141(5)
_cell_angle_gamma                90
_cell_volume                     1487.4(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1762
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1219
_cell_measurement_theta_min      3.5788
_shelx_estimated_absorpt_T_max   0.603
_shelx_estimated_absorpt_T_min   0.509
_exptl_absorpt_coefficient_mu    4.332
_exptl_absorpt_correction_T_max  0.569
_exptl_absorpt_correction_T_min  0.488
_exptl_absorpt_correction_type   multi-scan'
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2750
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.586
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1314
_reflns_number_total             1391
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.500        58        14 ' '
   2  0.500  0.500  0.500        58        14 ' '
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         0.786
_refine_diff_density_min         -1.204
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0275
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+0.3872P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0702
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O4(H4A,H4B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.000000 0.2591(6) 0.000000 0.0202(15) Uani 1 2 d S T P . .
C2 C 0.000000 0.1251(6) 0.000000 0.0197(15) Uani 1 2 d S T P . .
C3 C 0.0518(4) 0.0613(4) 0.1232(5) 0.0227(11) Uani 1 1 d . . . . .
C4 C 0.1385(6) 0.500000 0.2702(7) 0.0224(16) Uani 1 2 d S T P . .
C5 C 0.1360(6) 0.500000 0.3989(7) 0.0215(16) Uani 1 2 d S T P . .
C6 C 0.1359(4) 0.6041(5) 0.4611(5) 0.0251(12) Uani 1 1 d . . . . .
C7 C 0.1411(4) 0.6053(5) 0.5826(5) 0.0244(12) Uani 1 1 d . . . . .
C8 C 0.1468(6) 0.500000 0.6503(7) 0.0204(16) Uani 1 2 d S T P . .
Eu1 Eu 0.16076(2) 0.500000 0.03298(3) 0.01060(14) Uani 1 2 d S T P . .
F1 F 0.1009(3) 0.1193(3) 0.2453(3) 0.0376(8) Uani 1 1 d . . . . .
F2 F 0.1312(4) 0.7071(3) 0.4014(4) 0.0502(10) Uani 1 1 d . . . . .
F3 F 0.1429(4) 0.7109(3) 0.6345(4) 0.0501(10) Uani 1 1 d . . . . .
O1 O -0.0432(4) 0.500000 -0.1501(5) 0.0214(11) Uani 1 2 d S T P . .
O2 O 0.2363(4) 0.500000 0.2888(5) 0.0390(15) Uani 1 2 d S T P . .
O3 O 0.0917(3) 0.3063(3) 0.0289(4) 0.0275(9) Uani 1 1 d . . . . .
O4 O 0.3334(3) 0.6296(3) 0.1504(4) 0.0328(9) Uani 1 1 d . . . . .
H4A H 0.351393 0.672228 0.104164 0.039 Uiso 1 1 d R . . . .
H4B H 0.345563 0.673278 0.218054 0.039 Uiso 1 1 d R . . . .
O5 O 0.1618(4) 0.5970(3) -0.1576(4) 0.0342(10) Uani 1 1 d . . . . .
C9 C 0.1584(6) 0.500000 -0.2129(7) 0.0205(16) Uani 1 2 d S T P . .


_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
C1 C2 1.508(9) . ?
C1 O3 1.236(4) 2 ?
C1 O3 1.236(4) . ?
C2 C3 1.378(6) 2 ?
C2 C3 1.378(6) . ?
C3 C3 1.379(10) 6 ?
C3 F1 1.338(6) . ?
C4 C5 1.518(9) . ?
C4 Eu1 2.947(7) . ?
C4 O1 1.254(8) 5_565 ?
C4 O2 1.246(8) . ?
C5 C6 1.377(6) 6_565 ?
C5 C6 1.377(6) . ?
C6 C7 1.372(7) . ?
C6 F2 1.333(6) . ?
C7 C8 1.401(6) . ?
C7 F3 1.327(6) . ?
C8 C9 1.503(9) 1_556 ?
Eu1 Eu1 4.0749(17) 5_565 ?
Eu1 O1 2.371(4) . ?
Eu1 O1 2.662(5) 5_565 ?
Eu1 O2 2.521(5) . ?
Eu1 O3 2.371(3) . ?
Eu1 O3 2.371(3) 6_565 ?
Eu1 O4 2.445(3) . ?
Eu1 O4 2.445(3) 6_565 ?
Eu1 O5 2.478(3) 6_565 ?
Eu1 O5 2.478(3) . ?
Eu1 C9 2.840(7) . ?
O4 H4A 0.8586 . ?
O4 H4B 0.8580 . ?
O5 C9 1.254(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
O3 C1 C2 115.5(3) 2 . ?
O3 C1 C2 115.5(3) . . ?
O3 C1 O3 129.0(6) 2 . ?
C3 C2 C1 121.4(3) . . ?
C3 C2 C1 121.4(3) 2 . ?
C3 C2 C3 117.1(6) 2 . ?
C2 C3 C3 121.4(3) . 6 ?
F1 C3 C2 119.4(5) . . ?
F1 C3 C3 119.2(3) . 6 ?
C5 C4 Eu1 176.2(5) . . ?
O1 C4 C5 119.2(6) 5_565 . ?
O1 C4 Eu1 64.6(4) 5_565 . ?
O2 C4 C5 118.1(6) . . ?
O2 C4 Eu1 58.1(4) . . ?
O2 C4 O1 122.7(6) . 5_565 ?
C6 C5 C4 121.7(3) 6_565 . ?
C6 C5 C4 121.7(3) . . ?
C6 C5 C6 116.7(6) 6_565 . ?
C7 C6 C5 122.2(5) . . ?
F2 C6 C5 118.8(4) . . ?
F2 C6 C7 119.0(4) . . ?
C6 C7 C8 121.6(5) . . ?
F3 C7 C6 117.0(4) . . ?
F3 C7 C8 121.5(4) . . ?
C7 C8 C7 115.7(6) 6_565 . ?
C7 C8 C9 122.2(3) . 1_556 ?
C7 C8 C9 122.2(3) 6_565 1_556 ?
C4 Eu1 Eu1 58.79(14) . 5_565 ?
O1 Eu1 C4 25.20(17) 5_565 . ?
O1 Eu1 C4 97.20(18) . . ?
O1 Eu1 Eu1 33.60(9) 5_565 5_565 ?
O1 Eu1 Eu1 38.41(11) . 5_565 ?
O1 Eu1 O1 72.00(17) . 5_565 ?
O1 Eu1 O2 122.02(15) . . ?
O1 Eu1 O3 73.81(9) . 6_565 ?
O1 Eu1 O3 73.81(9) . . ?
O1 Eu1 O4 141.56(10) . . ?
O1 Eu1 O4 141.56(10) . 6_565 ?
O1 Eu1 O5 79.41(14) . 6_565 ?
O1 Eu1 O5 79.41(14) . . ?
O1 Eu1 C9 149.34(16) 5_565 . ?
O1 Eu1 C9 77.34(17) . . ?
O2 Eu1 C4 24.82(17) . . ?
O2 Eu1 Eu1 83.61(11) . 5_565 ?
O2 Eu1 O1 50.01(14) . 5_565 ?
O2 Eu1 C9 160.64(17) . . ?
O3 Eu1 C4 76.08(10) 6_565 . ?
O3 Eu1 C4 76.08(10) . . ?
O3 Eu1 Eu1 66.99(8) . 5_565 ?
O3 Eu1 Eu1 66.99(8) 6_565 5_565 ?
O3 Eu1 O1 69.50(9) . 5_565 ?
O3 Eu1 O1 69.50(9) 6_565 5_565 ?
O3 Eu1 O2 84.97(10) . . ?
O3 Eu1 O2 84.97(10) 6_565 . ?
O3 Eu1 O3 133.67(16) . 6_565 ?
O3 Eu1 O4 144.62(13) . . ?
O3 Eu1 O4 144.62(13) 6_565 6_565 ?
O3 Eu1 O4 73.64(12) . 6_565 ?
O3 Eu1 O4 73.64(12) 6_565 . ?
O3 Eu1 O5 126.71(12) . . ?
O3 Eu1 O5 126.71(12) 6_565 6_565 ?
O3 Eu1 O5 77.74(13) 6_565 . ?
O3 Eu1 O5 77.74(12) . 6_565 ?
O3 Eu1 C9 102.11(10) 6_565 . ?
O3 Eu1 C9 102.11(10) . . ?
O4 Eu1 C4 94.30(14) 6_565 . ?
O4 Eu1 C4 94.31(14) . . ?
O4 Eu1 Eu1 136.24(9) . 5_565 ?
O4 Eu1 Eu1 136.24(9) 6_565 5_565 ?
O4 Eu1 O1 114.08(11) . 5_565 ?
O4 Eu1 O1 114.08(11) 6_565 5_565 ?
O4 Eu1 O2 74.50(12) 6_565 . ?
O4 Eu1 O2 74.50(12) . . ?
O4 Eu1 O4 73.26(18) 6_565 . ?
O4 Eu1 O5 74.20(12) 6_565 6_565 ?
O4 Eu1 O5 104.68(13) . 6_565 ?
O4 Eu1 O5 74.20(12) . . ?
O4 Eu1 O5 104.68(13) 6_565 . ?
O4 Eu1 C9 90.08(13) . . ?
O4 Eu1 C9 90.08(13) 6_565 . ?
O5 Eu1 C4 153.49(9) . . ?
O5 Eu1 C4 153.49(9) 6_565 . ?
O5 Eu1 Eu1 113.70(10) 6_565 5_565 ?
O5 Eu1 Eu1 113.70(10) . 5_565 ?
O5 Eu1 O1 141.17(12) . 5_565 ?
O5 Eu1 O1 141.17(12) 6_565 5_565 ?
O5 Eu1 O2 147.40(11) 6_565 . ?
O5 Eu1 O2 147.40(11) . . ?
O5 Eu1 O5 52.28(17) 6_565 . ?
O5 Eu1 C9 26.15(9) . . ?
O5 Eu1 C9 26.15(9) 6_565 . ?
C9 Eu1 C4 174.54(18) . . ?
C9 Eu1 Eu1 115.75(13) . 5_565 ?
C4 O1 Eu1 90.2(4) 5_565 5_565 ?
C4 O1 Eu1 161.8(5) 5_565 . ?
Eu1 O1 Eu1 108.00(17) . 5_565 ?
C4 O2 Eu1 97.1(4) . . ?
C1 O3 Eu1 138.0(4) . . ?
Eu1 O4 H4A 122.0 . . ?
Eu1 O4 H4B 117.8 . . ?
H4A O4 H4B 106.2 . . ?
C9 O5 Eu1 93.3(3) . . ?
C8 C9 Eu1 175.5(5) 1_554 . ?
O5 C9 C8 119.5(3) 6_565 1_554 ?
O5 C9 C8 119.5(3) . 1_554 ?
O5 C9 Eu1 60.6(3) 6_565 . ?
O5 C9 Eu1 60.6(3) . . ?
O5 C9 O5 121.1(6) 6_565 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_9-tb_sq
_database_code_depnum_ccdc_archive 'CCDC 1486537'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 F6 O8 Tb'
_chemical_formula_sum            'C12 H4 F6 O8 Tb'
_chemical_formula_weight         549.08
_chemical_melting_point          ?
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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.833(5)
_cell_length_b                   11.226(5)
_cell_length_c                   11.579(5)
_cell_angle_alpha                90
_cell_angle_beta                 124.600(5)
_cell_angle_gamma                90
_cell_volume                     1480.1(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1730
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4639
_cell_measurement_theta_min      3.5716
_shelx_estimated_absorpt_T_max   0.490
_shelx_estimated_absorpt_T_min   0.412
_exptl_absorpt_coefficient_mu    4.894
_exptl_absorpt_correction_T_max  0.435
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.464
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'not measured'
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2704
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         3.578
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1294
_reflns_number_total             1390
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.500  0.000  0.000        58        15 ' '
   2  0.000  0.500  0.000        58        15 ' '
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.942
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1386
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0244
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0117P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0528
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 H5A-O5
 0.85 with sigma of 0.02
 H5B-O5
 0.85 with sigma of 0.02
 H5B-H5A
 1.373 with sigma of 0.04
 H5B-Tb1
 2.7 with sigma of 0.04
 H5A-Tb1
 2.7 with sigma of 0.04
2. Rigid bond restraints
 Tb1, O5, H5A, H5B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Tb1 \\sim O5 \\sim H5A \\sim H5B: within 3.8A with sigma of 0.04 and sigma for
terminal atoms of 0.08
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Tb1 Tb 0.34029(2) 0.500000 0.46829(3) 0.01328(11) Uani 1 2 d DS TU P . .
F1 F 0.3576(3) 0.7115(3) -0.1347(3) 0.0535(10) Uani 1 1 d . . . . .
F2 F 0.3691(3) 0.7080(3) 0.0986(3) 0.0520(9) Uani 1 1 d . . . . .
F3 F 0.3987(2) 0.1195(2) 0.2550(3) 0.0398(7) Uani 1 1 d . . . . .
O1 O 0.3379(3) 0.5970(3) -0.3432(3) 0.0355(9) Uani 1 1 d . . . . .
O2 O 0.2667(4) 0.500000 0.2159(5) 0.0382(13) Uani 1 2 d S T P . .
O3 O 0.4586(4) 0.500000 0.3513(4) 0.0229(10) Uani 1 2 d S T P . .
O4 O 0.4080(3) 0.3079(3) 0.4712(3) 0.0286(8) Uani 1 1 d . . . . .
O5 O 0.1683(3) 0.3716(3) 0.3513(4) 0.0346(8) Uani 1 1 d D U . . .
C1 C 0.3634(6) 0.500000 0.2315(7) 0.0227(14) Uani 1 2 d S T P . .
C2 C 0.3655(5) 0.500000 0.1026(6) 0.0210(14) Uani 1 2 d S T P . .
C3 C 0.3640(4) 0.6043(4) 0.0390(5) 0.0282(11) Uani 1 1 d . . . . .
C4 C 0.3579(4) 0.6043(4) -0.0843(5) 0.0263(11) Uani 1 1 d . . . . .
C5 C 0.3524(5) 0.500000 -0.1518(7) 0.0213(14) Uani 1 2 d S T P . .
C6 C 0.3406(5) 0.500000 -0.2883(7) 0.0235(15) Uani 1 2 d S T P . .
C7 C 0.500000 0.2594(5) 0.500000 0.0231(15) Uani 1 2 d S T P . .
C8 C 0.500000 0.1258(5) 0.500000 0.0204(14) Uani 1 2 d S T P . .
C9 C 0.4477(4) 0.0607(4) 0.3782(5) 0.0245(10) Uani 1 1 d . . . . .
H5A H 0.169(4) 0.353(5) 0.421(3) 0.085(15) Uiso 1 1 d D U . . .
H5B H 0.187(4) 0.314(3) 0.322(6) 0.080(15) Uiso 1 1 d D U . . .


_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
Tb1 O1 2.457(3) 1_556 ?
Tb1 O1 2.457(3) 6_566 ?
Tb1 O2 2.490(5) . ?
Tb1 O3 2.651(4) . ?
Tb1 O3 2.346(4) 5_666 ?
Tb1 O4 2.343(3) 6_565 ?
Tb1 O4 2.344(3) . ?
Tb1 O5 2.432(3) . ?
Tb1 O5 2.432(3) 6_565 ?
Tb1 C1 2.935(6) . ?
Tb1 C6 2.816(6) 1_556 ?
F1 C4 1.336(5) . ?
F2 C3 1.335(5) . ?
F3 C9 1.354(5) . ?
O1 C6 1.251(4) . ?
O2 C1 1.244(7) . ?
O3 C1 1.258(7) . ?
O4 C7 1.243(4) . ?
O5 H5A 0.822(19) . ?
O5 H5B 0.835(19) . ?
C1 C2 1.509(8) . ?
C2 C3 1.377(5) 6_565 ?
C2 C3 1.377(5) . ?
C3 C4 1.382(6) . ?
C4 C5 1.385(5) . ?
C5 C6 1.494(8) . ?
C7 C8 1.500(8) . ?
C8 C9 1.375(5) 2_656 ?
C8 C9 1.375(5) . ?
C9 C9 1.362(9) 6 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 52.62(16) 1_556 6_566 ?
O1 Tb1 O2 147.17(10) 6_566 . ?
O1 Tb1 O2 147.17(10) 1_556 . ?
O1 Tb1 O3 141.06(11) 6_566 . ?
O1 Tb1 O3 141.06(11) 1_556 . ?
O1 Tb1 C1 153.34(8) 6_566 . ?
O1 Tb1 C1 153.34(8) 1_556 . ?
O1 Tb1 C6 26.32(8) 6_566 1_556 ?
O1 Tb1 C6 26.32(8) 1_556 1_556 ?
O2 Tb1 O3 50.19(14) . . ?
O2 Tb1 C1 24.81(16) . . ?
O2 Tb1 C6 160.42(16) . 1_556 ?
O3 Tb1 O1 79.43(12) 5_666 1_556 ?
O3 Tb1 O1 79.43(12) 5_666 6_566 ?
O3 Tb1 O2 122.18(14) 5_666 . ?
O3 Tb1 O3 71.99(16) 5_666 . ?
O3 Tb1 O5 141.86(9) 5_666 6_565 ?
O3 Tb1 O5 141.86(9) 5_666 . ?
O3 Tb1 C1 25.38(15) . . ?
O3 Tb1 C1 97.37(17) 5_666 . ?
O3 Tb1 C6 77.40(16) 5_666 1_556 ?
O3 Tb1 C6 149.39(16) . 1_556 ?
O4 Tb1 O1 77.67(11) . 6_566 ?
O4 Tb1 O1 127.02(11) . 1_556 ?
O4 Tb1 O1 77.67(11) 6_565 1_556 ?
O4 Tb1 O1 127.02(11) 6_565 6_566 ?
O4 Tb1 O2 84.86(9) 6_565 . ?
O4 Tb1 O2 84.86(9) . . ?
O4 Tb1 O3 74.04(8) 6_565 5_666 ?
O4 Tb1 O3 74.04(8) . 5_666 ?
O4 Tb1 O3 69.50(8) 6_565 . ?
O4 Tb1 O3 69.50(8) . . ?
O4 Tb1 O4 133.88(15) 6_565 . ?
O4 Tb1 O5 144.10(12) . 6_565 ?
O4 Tb1 O5 73.69(11) . . ?
O4 Tb1 O5 144.10(12) 6_565 . ?
O4 Tb1 O5 73.69(11) 6_565 6_565 ?
O4 Tb1 C1 76.04(9) 6_565 . ?
O4 Tb1 C1 76.04(9) . . ?
O4 Tb1 C6 102.25(9) . 1_556 ?
O4 Tb1 C6 102.25(9) 6_565 1_556 ?
O5 Tb1 O1 74.30(12) 6_565 1_556 ?
O5 Tb1 O1 104.77(12) 6_565 6_566 ?
O5 Tb1 O1 104.77(12) . 1_556 ?
O5 Tb1 O1 74.30(12) . 6_566 ?
O5 Tb1 O2 74.21(11) . . ?
O5 Tb1 O2 74.21(11) 6_565 . ?
O5 Tb1 O3 114.08(11) . . ?
O5 Tb1 O3 114.08(11) 6_565 . ?
O5 Tb1 O5 72.71(18) . 6_565 ?
O5 Tb1 C1 94.07(13) 6_565 . ?
O5 Tb1 C1 94.07(13) . . ?
O5 Tb1 C6 90.14(13) 6_565 1_556 ?
O5 Tb1 C6 90.14(13) . 1_556 ?
C6 Tb1 C1 174.77(18) 1_556 . ?
C6 O1 Tb1 93.1(3) . 1_554 ?
C1 O2 Tb1 98.1(4) . . ?
Tb1 O3 Tb1 108.01(15) 5_666 . ?
C1 O3 Tb1 90.1(4) . . ?
C1 O3 Tb1 161.9(4) . 5_666 ?
C7 O4 Tb1 138.3(3) . . ?
Tb1 O5 H5A 98(3) . . ?
Tb1 O5 H5B 105(3) . . ?
H5A O5 H5B 112(4) . . ?
O2 C1 Tb1 57.1(3) . . ?
O2 C1 O3 121.7(6) . . ?
O2 C1 C2 118.6(6) . . ?
O3 C1 Tb1 64.6(3) . . ?
O3 C1 C2 119.7(5) . . ?
C2 C1 Tb1 175.7(4) . . ?
C3 C2 C1 121.7(3) . . ?
C3 C2 C1 121.7(3) 6_565 . ?
C3 C2 C3 116.5(5) 6_565 . ?
F2 C3 C2 119.1(4) . . ?
F2 C3 C4 119.2(4) . . ?
C2 C3 C4 121.8(4) . . ?
F1 C4 C3 115.7(4) . . ?
F1 C4 C5 122.0(4) . . ?
C3 C4 C5 122.3(4) . . ?
C4 C5 C4 115.4(5) 6_565 . ?
C4 C5 C6 122.3(3) . . ?
C4 C5 C6 122.3(3) 6_565 . ?
O1 C6 Tb1 60.6(3) . 1_554 ?
O1 C6 Tb1 60.6(3) 6_565 1_554 ?
O1 C6 O1 121.1(6) 6_565 . ?
O1 C6 C5 119.4(3) 6_565 . ?
O1 C6 C5 119.4(3) . . ?
C5 C6 Tb1 174.9(4) . 1_554 ?
O4 C7 O4 128.1(6) . 2_656 ?
O4 C7 C8 116.0(3) . . ?
O4 C7 C8 116.0(3) 2_656 . ?
C9 C8 C7 122.2(3) 2_656 . ?
C9 C8 C7 122.2(3) . . ?
C9 C8 C9 115.7(6) 2_656 . ?
F3 C9 C8 118.6(4) . . ?
F3 C9 C9 119.2(2) . 6 ?
C9 C9 C8 122.2(3) 6 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_2-nd-3d_sq
_database_code_depnum_ccdc_archive 'CCDC 1445654'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 F6 Nd O7'
_chemical_formula_sum            'C12 F6 Nd O7'
_chemical_formula_weight         514.36
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.205(5)
_cell_length_b                   21.215(5)
_cell_length_c                   7.866(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.642(5)
_cell_angle_gamma                90
_cell_volume                     1683.6(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.5262
_cell_measurement_theta_min      3.1985
_shelx_estimated_absorpt_T_max   0.630
_shelx_estimated_absorpt_T_min   0.529
_exptl_absorpt_coefficient_mu    3.178
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.029
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5706
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.205
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2481
_reflns_number_total             2959
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.030  0.000 -0.019       206        55 ' '
   2  0.480  0.500 -0.061       206        55 ' '
The unit cells of complex contains two water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         4.379
_refine_diff_density_min         -1.415
_refine_diff_density_rms         0.243
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2953
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0487
_refine_ls_restrained_S_all      1.105
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0747P)²+4.5505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1350
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.5000(9) 0.1269(4) -0.3651(10) 0.034(2) Uani 1 1 d . . . . .
C2 C 0.4991(8) 0.0608(4) -0.4302(10) 0.0293(18) Uani 1 1 d . . . . .
C3 C 0.6151(10) 0.0299(5) -0.4438(14) 0.048(2) Uani 1 1 d . . . . .
C4 C 0.3835(10) 0.0302(5) -0.4928(13) 0.046(2) Uani 1 1 d . . . . .
C5 C 1.0898(8) 0.2083(4) -0.2794(11) 0.0272(19) Uani 1 1 d . . . . .
C6 C 1.1352(7) 0.2705(4) -0.2862(10) 0.0265(18) Uani 1 1 d . . . . .
C7 C 1.0520(8) 0.3178(4) -0.2514(11) 0.0324(19) Uani 1 1 d . . . . .
C8 C 0.9293(8) 0.3042(4) -0.2070(11) 0.0304(19) Uani 1 1 d . . . . .
C9 C 0.8850(7) 0.2433(4) -0.1951(10) 0.0265(18) Uani 1 1 d . . . . .
C10 C 0.9694(7) 0.1950(4) -0.2333(10) 0.0293(18) Uani 1 1 d . . . . .
C11 C 0.7515(8) 0.2280(4) -0.1430(10) 0.0260(18) Uani 1 1 d . . . . .
C12 C 0.2685(8) 0.2163(3) 0.1598(11) 0.0245(18) Uani 1 1 d . . . . .
O1 O 0.7453(5) 0.1897(3) -0.0306(7) 0.0371(14) Uani 1 1 d . . . . .
O2 O 0.6506(5) 0.2423(3) 0.2830(7) 0.0316(13) Uani 1 1 d . . . . .
O3 O 0.5128(8) 0.3304(3) 0.0297(8) 0.056(2) Uani 1 1 d . . . . .
O4 O 0.4884(6) 0.1333(2) -0.2086(6) 0.0317(13) Uani 1 1 d . . . . .
O5 O 0.3703(5) 0.2595(3) -0.2534(7) 0.0313(13) Uani 1 1 d . . . . .
O6 O 0.5402(7) 0.1195(3) 0.1782(8) 0.0457(16) Uani 1 1 d . . . . .
O7 O 0.2755(5) 0.1842(3) 0.0339(7) 0.0392(15) Uani 1 1 d . . . . .
F1 F 0.2678(7) 0.0587(4) -0.4836(12) 0.108(3) Uani 1 1 d . . . . .
F2 F 0.7309(7) 0.0590(3) -0.3873(13) 0.115(3) Uani 1 1 d . . . . .
F3 F 0.9312(5) 0.1352(2) -0.2275(8) 0.0470(14) Uani 1 1 d . . . . .
F4 F 1.1646(5) 0.1611(2) -0.3236(7) 0.0434(13) Uani 1 1 d . . . . .
F5 F 0.8539(5) 0.3521(3) -0.1641(8) 0.0505(15) Uani 1 1 d . . . . .
F6 F 1.0892(5) 0.3781(2) -0.2574(8) 0.0520(15) Uani 1 1 d . . . . .
Nd1 Nd 0.50925(3) 0.21527(2) 0.00420(4) 0.01541(19) 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
C1 C2 1.493(11) . ?
C1 O3 1.247(10) 4_565 ?
C1 O4 1.261(9) . ?
C2 C3 1.371(13) . ?
C2 C4 1.372(12) . ?
C3 C4 1.370(13) 3_654 ?
C3 F2 1.348(11) . ?
C4 F1 1.338(11) . ?
C5 C6 1.402(12) . ?
C5 C10 1.362(11) . ?
C5 F4 1.336(9) . ?
C6 C7 1.368(12) . ?
C6 C12 1.511(11) 4_665 ?
C7 C8 1.380(11) . ?
C7 F6 1.339(10) . ?
C8 C9 1.376(13) . ?
C8 F5 1.349(10) . ?
C9 C10 1.400(12) . ?
C9 C11 1.516(10) . ?
C10 F3 1.329(10) . ?
C11 O1 1.210(10) . ?
C11 O2 1.271(9) 4_565 ?
C11 Nd1 2.895(8) . ?
C12 O5 1.264(9) 4_566 ?
C12 O7 1.213(10) . ?
C12 Nd1 2.905(8) . ?
O1 Nd1 2.524(5) . ?
O2 Nd1 2.504(5) . ?
O2 Nd1 2.583(5) 4_566 ?
O3 Nd1 2.450(6) . ?
O4 Nd1 2.401(5) . ?
O5 Nd1 2.476(5) . ?
O5 Nd1 2.597(5) 4_565 ?
O6 Nd1 2.444(6) . ?
O7 Nd1 2.519(6) . ?

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
O3 C1 C2 116.7(7) 4_565 . ?
O3 C1 O4 127.2(7) 4_565 . ?
O4 C1 C2 116.1(7) . . ?
C3 C2 C1 121.0(8) . . ?
C3 C2 C4 116.9(8) . . ?
C4 C2 C1 121.9(8) . . ?
C4 C3 C2 122.0(8) 3_654 . ?
F2 C3 C2 118.6(8) . . ?
F2 C3 C4 119.3(9) . 3_654 ?
C3 C4 C2 121.0(8) 3_654 . ?
F1 C4 C2 119.0(8) . . ?
F1 C4 C3 119.8(9) . 3_654 ?
C10 C5 C6 121.4(8) . . ?
F4 C5 C6 119.4(7) . . ?
F4 C5 C10 119.2(8) . . ?
C5 C6 C12 120.1(7) . 4_665 ?
C7 C6 C5 117.7(7) . . ?
C7 C6 C12 122.1(8) . 4_665 ?
C6 C7 C8 120.7(8) . . ?
F6 C7 C6 120.5(7) . . ?
F6 C7 C8 118.8(8) . . ?
C9 C8 C7 122.3(8) . . ?
F5 C8 C7 118.6(8) . . ?
F5 C8 C9 119.0(7) . . ?
C8 C9 C10 117.0(7) . . ?
C8 C9 C11 122.5(7) . . ?
C10 C9 C11 120.6(8) . . ?
C5 C10 C9 120.9(8) . . ?
F3 C10 C5 119.2(8) . . ?
F3 C10 C9 119.9(7) . . ?
C9 C11 Nd1 169.8(6) . . ?
O1 C11 C9 119.3(7) . . ?
O1 C11 O2 122.7(7) . 4_565 ?
O1 C11 Nd1 60.2(4) . . ?
O2 C11 C9 118.0(7) 4_565 . ?
O2 C11 Nd1 63.1(4) 4_565 . ?
C6 C12 Nd1 166.9(5) 4_466 . ?
O5 C12 C6 118.3(7) 4_566 4_466 ?
O5 C12 Nd1 63.3(4) 4_566 . ?
O7 C12 C6 120.0(7) . 4_466 ?
O7 C12 O5 121.6(7) . 4_566 ?
O7 C12 Nd1 59.6(4) . . ?
C11 O1 Nd1 95.2(5) . . ?
C11 O2 Nd1 146.6(5) 4_566 . ?
C11 O2 Nd1 90.8(5) 4_566 4_566 ?
Nd1 O2 Nd1 111.29(19) . 4_566 ?
C1 O3 Nd1 140.9(5) 4_566 . ?
C1 O4 Nd1 138.3(5) . . ?
C12 O5 Nd1 90.9(5) 4_565 4_565 ?
C12 O5 Nd1 156.8(5) 4_565 . ?
Nd1 O5 Nd1 111.74(19) . 4_565 ?
C12 O7 Nd1 95.9(5) . . ?
C11 Nd1 C12 174.1(2) . . ?
O1 Nd1 C11 24.6(2) . . ?
O1 Nd1 C12 158.2(2) . . ?
O1 Nd1 O2 50.46(17) . 4_565 ?
O1 Nd1 O5 139.39(18) . 4_566 ?
O2 Nd1 C11 26.0(2) 4_565 . ?
O2 Nd1 C11 85.1(2) . . ?
O2 Nd1 C12 92.4(2) . . ?
O2 Nd1 C12 150.97(19) 4_565 . ?
O2 Nd1 O1 73.17(18) . . ?
O2 Nd1 O2 101.75(16) . 4_565 ?
O2 Nd1 O5 147.6(2) 4_565 4_566 ?
O2 Nd1 O5 67.42(17) . 4_566 ?
O2 Nd1 O7 114.06(18) . . ?
O3 Nd1 C11 86.4(2) . . ?
O3 Nd1 C12 87.8(2) . . ?
O3 Nd1 O1 102.8(2) . . ?
O3 Nd1 O2 72.6(2) . . ?
O3 Nd1 O2 72.8(2) . 4_565 ?
O3 Nd1 O5 71.9(2) . . ?
O3 Nd1 O5 74.8(2) . 4_566 ?
O3 Nd1 O7 104.8(2) . . ?
O4 Nd1 C11 77.3(2) . . ?
O4 Nd1 C12 107.9(2) . . ?
O4 Nd1 O1 75.8(2) . . ?
O4 Nd1 O2 139.07(19) . . ?
O4 Nd1 O2 77.44(19) . 4_565 ?
O4 Nd1 O3 141.04(19) . . ?
O4 Nd1 O5 73.97(19) . . ?
O4 Nd1 O5 131.34(18) . 4_566 ?
O4 Nd1 O6 77.2(2) . . ?
O4 Nd1 O7 83.64(19) . . ?
O5 Nd1 C11 150.2(2) 4_566 . ?
O5 Nd1 C11 93.2(2) . . ?
O5 Nd1 C12 25.8(2) 4_566 . ?
O5 Nd1 C12 85.7(2) . . ?
O5 Nd1 O1 115.54(18) . . ?
O5 Nd1 O2 68.02(17) . 4_565 ?
O5 Nd1 O2 144.5(2) . . ?
O5 Nd1 O5 102.37(16) . 4_566 ?
O5 Nd1 O7 75.03(19) . . ?
O6 Nd1 C11 104.8(2) . . ?
O6 Nd1 C12 79.4(2) . . ?
O6 Nd1 O1 80.6(2) . . ?
O6 Nd1 O2 72.0(2) . . ?
O6 Nd1 O2 129.0(2) . 4_565 ?
O6 Nd1 O3 141.6(2) . . ?
O6 Nd1 O5 78.4(2) . 4_566 ?
O6 Nd1 O5 141.5(2) . . ?
O6 Nd1 O7 77.0(2) . . ?
O7 Nd1 C11 159.8(2) . . ?
O7 Nd1 C12 24.5(2) . . ?
O7 Nd1 O1 152.4(2) . . ?
O7 Nd1 O2 141.82(18) . 4_565 ?
O7 Nd1 O5 49.99(17) . 4_566 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3-ce_sq
_database_code_depnum_ccdc_archive 'CCDC 1445655'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 Ce F6 O8'
_chemical_formula_sum            'C12 H4 Ce F6 O8'
_chemical_formula_weight         530.27
_chemical_melting_point          ?
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'
Ce Ce -0.2486 2.6331 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.140(5)
_cell_length_b                   11.358(5)
_cell_length_c                   11.783(5)
_cell_angle_alpha                90
_cell_angle_beta                 126.176(5)
_cell_angle_gamma                90
_cell_volume                     1527.5(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2646
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6057
_cell_measurement_theta_min      3.5804
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.092
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_correction_T_min  0.463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.306
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3035
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.587
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1334
_reflns_number_total             1428
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         1.267
_refine_diff_density_min         -0.989
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1374
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0201
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0303P)²+4.0347P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0521
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O3(H3A,H3B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Ce1 Ce 0.66423(2) 0.500000 0.53608(2) 0.01325(10) Uani 1 2 d S T P . .
F1 F 0.3682(3) 0.7057(2) 0.0968(2) 0.0541(7) Uani 1 1 d . . . . .
F2 F 0.3572(3) 0.7090(2) -0.1328(3) 0.0544(7) Uani 1 1 d . . . . .
O1 O 0.5900(2) 0.3034(2) 0.5266(3) 0.0382(6) Uani 1 1 d . . . . .
O2 O 0.3387(3) 0.5966(2) -0.3384(3) 0.0400(7) Uani 1 1 d . . . . .
O3 O 0.8399(2) 0.6365(3) 0.6583(3) 0.0416(7) Uani 1 1 d . . . . .
H3A H 0.845125 0.671004 0.596637 0.062 Uiso 1 1 d GR . . . .
H3B H 0.903756 0.597123 0.715416 0.062 Uiso 1 1 d GR . . . .
O5 O 0.4523(3) 0.500000 0.3456(3) 0.0269(7) Uani 1 2 d S T P . .
O8 O 0.2609(3) 0.500000 0.2013(4) 0.0466(11) Uani 1 2 d S T P . .
C1 C 0.500000 0.2562(4) 0.500000 0.0266(10) Uani 1 2 d S T P . .
C2 C 0.3587(4) 0.500000 0.2241(5) 0.0249(10) Uani 1 2 d S T P . .
C3 C 0.3635(4) 0.500000 0.0991(4) 0.0235(10) Uani 1 2 d S T P . .
C4 C 0.3634(3) 0.6030(3) 0.0383(3) 0.0289(7) Uani 1 1 d . . . . .
C5 C 0.3580(3) 0.6038(3) -0.0825(3) 0.0274(7) Uani 1 1 d . . . . .
C6 C 0.3530(4) 0.500000 -0.1491(4) 0.0229(10) Uani 1 2 d S T P . .
C8 C 0.500000 0.1228(4) 0.500000 0.0241(10) Uani 1 2 d S T P . .
C9 C 0.5511(3) 0.0603(3) 0.6229(3) 0.0247(7) Uani 1 1 d . . . . .
F3 F 0.60047(19) 0.11823(18) 0.7449(2) 0.0402(5) Uani 1 1 d . . . . .
C11 C 0.3417(4) 0.500000 -0.2848(5) 0.0239(10) Uani 1 2 d S T P . .


_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
Ce1 O1 2.442(2) . ?
Ce1 O1 2.442(2) 6_565 ?
Ce1 O2 2.553(3) 5_665 ?
Ce1 O2 2.553(3) 2_655 ?
Ce1 O3 2.535(3) . ?
Ce1 O3 2.535(3) 6_565 ?
Ce1 O5 2.465(3) . ?
Ce1 O5 2.715(3) 5_666 ?
Ce1 O8 2.613(4) 5_666 ?
Ce1 C2 3.028(5) 5_666 ?
Ce1 C11 2.913(5) 5_665 ?
F1 C4 1.336(4) . ?
F2 C5 1.331(4) . ?
O1 C1 1.238(3) . ?
O2 C11 1.254(3) . ?
O3 H3A 0.8660 . ?
O3 H3B 0.8663 . ?
O5 C2 1.251(5) . ?
O8 C2 1.243(6) . ?
C1 C8 1.514(6) . ?
C2 C3 1.514(6) . ?
C3 C4 1.372(4) 6_565 ?
C3 C4 1.372(4) . ?
C4 C5 1.380(5) . ?
C5 C6 1.395(4) . ?
C6 C11 1.509(6) . ?
C8 C9 1.375(4) 2_656 ?
C8 C9 1.375(4) . ?
C9 C9 1.369(7) 6 ?
C9 F3 1.342(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
O1 Ce1 O1 132.23(12) . 6_565 ?
O1 Ce1 O2 77.91(10) . 5_665 ?
O1 Ce1 O2 125.21(9) 6_565 5_665 ?
O1 Ce1 O2 125.21(9) . 2_655 ?
O1 Ce1 O2 77.91(10) 6_565 2_655 ?
O1 Ce1 O3 73.60(9) . 6_565 ?
O1 Ce1 O3 146.73(9) 6_565 6_565 ?
O1 Ce1 O3 146.73(9) . . ?
O1 Ce1 O3 73.60(9) 6_565 . ?
O1 Ce1 O5 69.41(7) 6_565 5_666 ?
O1 Ce1 O5 72.51(7) . . ?
O1 Ce1 O5 69.41(7) . 5_666 ?
O1 Ce1 O5 72.51(7) 6_565 . ?
O1 Ce1 O8 85.23(8) . 5_666 ?
O1 Ce1 O8 85.23(8) 6_565 5_666 ?
O1 Ce1 C2 76.26(8) . 5_666 ?
O1 Ce1 C2 76.26(8) 6_565 5_666 ?
O1 Ce1 C11 101.55(8) . 5_665 ?
O1 Ce1 C11 101.55(8) 6_565 5_665 ?
O2 Ce1 O2 50.91(12) 5_665 2_655 ?
O2 Ce1 O5 141.33(8) 2_655 5_666 ?
O2 Ce1 O5 141.33(8) 5_665 5_666 ?
O2 Ce1 O8 149.02(7) 5_665 5_666 ?
O2 Ce1 O8 149.02(7) 2_655 5_666 ?
O2 Ce1 C2 153.94(6) 2_655 5_666 ?
O2 Ce1 C2 153.94(7) 5_665 5_666 ?
O2 Ce1 C11 25.46(6) 5_665 5_665 ?
O2 Ce1 C11 25.46(6) 2_655 5_665 ?
O3 Ce1 O2 105.29(10) . 5_665 ?
O3 Ce1 O2 74.81(9) . 2_655 ?
O3 Ce1 O2 74.81(9) 6_565 5_665 ?
O3 Ce1 O2 105.29(10) 6_565 2_655 ?
O3 Ce1 O3 75.41(14) 6_565 . ?
O3 Ce1 O5 113.36(8) 6_565 5_666 ?
O3 Ce1 O5 113.36(8) . 5_666 ?
O3 Ce1 O8 75.58(9) . 5_666 ?
O3 Ce1 O8 75.58(9) 6_565 5_666 ?
O3 Ce1 C2 94.51(10) . 5_666 ?
O3 Ce1 C2 94.51(9) 6_565 5_666 ?
O3 Ce1 C11 90.46(10) 6_565 5_665 ?
O3 Ce1 C11 90.45(10) . 5_665 ?
O5 Ce1 O2 79.22(10) . 5_665 ?
O5 Ce1 O2 79.22(10) . 2_655 ?
O5 Ce1 O3 140.73(7) . 6_565 ?
O5 Ce1 O3 140.73(7) . . ?
O5 Ce1 O5 71.80(12) . 5_666 ?
O5 Ce1 O8 120.22(11) . 5_666 ?
O5 Ce1 C2 96.18(12) . 5_666 ?
O5 Ce1 C2 24.38(11) 5_666 5_666 ?
O5 Ce1 C11 77.54(12) . 5_665 ?
O5 Ce1 C11 149.35(11) 5_666 5_665 ?
O8 Ce1 O5 48.42(10) 5_666 5_666 ?
O8 Ce1 C2 24.05(12) 5_666 5_666 ?
O8 Ce1 C11 162.23(12) 5_666 5_665 ?
C11 Ce1 C2 173.72(12) 5_665 5_666 ?
C1 O1 Ce1 139.3(2) . . ?
C11 O2 Ce1 93.5(2) . 5_665 ?
Ce1 O3 H3A 109.9 . . ?
Ce1 O3 H3B 110.4 . . ?
H3A O3 H3B 108.7 . . ?
Ce1 O5 Ce1 108.20(12) . 5_666 ?
C2 O5 Ce1 92.0(3) . 5_666 ?
C2 O5 Ce1 159.8(3) . . ?
C2 O8 Ce1 97.0(3) . 5_666 ?
O1 C1 O1 128.6(4) 2_656 . ?
O1 C1 C8 115.7(2) 2_656 . ?
O1 C1 C8 115.7(2) . . ?
O5 C2 Ce1 63.6(3) . 5_666 ?
O5 C2 C3 119.2(4) . . ?
O8 C2 Ce1 58.9(3) . 5_666 ?
O8 C2 O5 122.6(5) . . ?
O8 C2 C3 118.2(4) . . ?
C3 C2 Ce1 177.1(3) . 5_666 ?
C4 C3 C2 121.4(2) 6_565 . ?
C4 C3 C2 121.4(2) . . ?
C4 C3 C4 117.1(4) 6_565 . ?
F1 C4 C3 119.4(3) . . ?
F1 C4 C5 118.8(3) . . ?
C3 C4 C5 121.8(3) . . ?
F2 C5 C4 116.5(3) . . ?
F2 C5 C6 121.6(3) . . ?
C4 C5 C6 121.9(3) . . ?
C5 C6 C5 115.4(4) . 6_565 ?
C5 C6 C11 122.3(2) 6_565 . ?
C5 C6 C11 122.3(2) . . ?
C9 C8 C1 121.1(2) 2_656 . ?
C9 C8 C1 121.1(2) . . ?
C9 C8 C9 117.7(4) . 2_656 ?
C9 C9 C8 121.1(2) 6 . ?
F3 C9 C8 119.5(3) . . ?
F3 C9 C9 119.38(17) . 6 ?
O2 C11 Ce1 61.0(2) 6_565 5_665 ?
O2 C11 Ce1 61.0(2) . 5_665 ?
O2 C11 O2 122.0(4) . 6_565 ?
O2 C11 C6 119.0(2) 6_565 . ?
O2 C11 C6 119.0(2) . . ?
C6 C11 Ce1 176.4(3) . 5_665 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_8-gd_sq
_database_code_depnum_ccdc_archive 'CCDC 1486536'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 F6 Gd O8)'
_chemical_formula_sum            'C12 H4 F6 Gd O8'
_chemical_formula_weight         547.40
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.886(5)
_cell_length_b                   11.220(5)
_cell_length_c                   11.590(5)
_cell_angle_alpha                90
_cell_angle_beta                 124.941(5)
_cell_angle_gamma                90
_cell_volume                     1480.2(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1702
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6488
_cell_measurement_theta_min      3.6244
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.596
_exptl_absorpt_correction_T_max  0.550
_exptl_absorpt_correction_T_min  0.442
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2885
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.988
_diffrn_reflns_theta_max         24.988
_diffrn_reflns_theta_min         3.632
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1305
_reflns_number_total             1384
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.500  0.000  0.500        59        11 ' '
   2  0.000  0.500  0.500        59        11 ' '
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         1.194
_refine_diff_density_min         -2.200
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1379
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0484P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0837
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O3(H3A,H3B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.16028(3) 0.000000 0.03246(3) 0.01034(16) Uani 1 2 d S T P . .
O2 O -0.0417(4) 0.000000 -0.1497(5) 0.0200(12) Uani 1 2 d S T P . .
O3 O 0.3325(3) 0.1295(4) 0.1499(4) 0.0328(11) Uani 1 1 d . . . . .
H3A H 0.330619 0.197254 0.179281 0.039 Uiso 1 1 d R . . . .
H3B H 0.340899 0.131174 0.085761 0.039 Uiso 1 1 d R . . . .
O5 O 0.0920(3) -0.1934(3) 0.0291(4) 0.0270(10) Uani 1 1 d . . . . .
F1 F -0.1008(3) -0.3807(3) -0.2453(4) 0.0380(9) Uani 1 1 d . . . . .
O4 O 0.2345(5) 0.000000 0.2865(6) 0.0392(18) Uani 1 2 d S T P . .
C2 C 0.000000 -0.3754(7) 0.000000 0.0202(18) Uani 1 2 d S T P . .
O1 O 0.1627(4) -0.0970(4) -0.1572(4) 0.0357(12) Uani 1 1 d . . . . .
C3 C -0.0517(5) -0.4385(5) -0.1222(6) 0.0225(13) Uani 1 1 d . . . . .
C1 C 0.000000 -0.2404(7) 0.000000 0.0208(18) Uani 1 2 d S T P . .
C4 C 0.1371(7) 0.000000 0.2688(8) 0.0233(19) Uani 1 2 d S T P . .
C5 C 0.1586(7) 0.000000 -0.2122(8) 0.0197(18) Uani 1 2 d S T P . .
C7 C 0.1341(6) 0.000000 0.3969(8) 0.0226(19) Uani 1 2 d S T P . .
C6 C 0.1473(7) 0.000000 -0.3486(8) 0.0210(19) Uani 1 2 d S T P . .
F2 F 0.1311(5) 0.2076(4) 0.4017(4) 0.0514(12) Uani 1 1 d . . . . .
F3 F 0.1430(5) 0.2110(4) -0.3656(4) 0.0511(12) Uani 1 1 d . . . . .
C8 C 0.1357(5) 0.1044(6) 0.4601(6) 0.0249(14) Uani 1 1 d . . . . .
C9 C 0.1412(5) 0.1045(6) -0.4161(6) 0.0255(14) 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
Gd1 Gd1 4.0674(17) 5 ?
Gd1 O2 2.354(5) . ?
Gd1 O2 2.668(5) 5 ?
Gd1 O3 2.440(4) 6 ?
Gd1 O3 2.440(4) . ?
Gd1 O5 2.359(4) 6 ?
Gd1 O5 2.359(4) . ?
Gd1 O4 2.500(6) . ?
Gd1 O1 2.470(4) 6 ?
Gd1 O1 2.470(4) . ?
Gd1 C4 2.936(8) . ?
Gd1 C5 2.822(8) . ?
O2 C4 1.251(9) 5 ?
O5 C1 1.237(5) . ?
F1 C3 1.345(6) . ?
O4 C4 1.247(10) . ?
C2 C3 1.363(7) . ?
C2 C3 1.363(7) 2 ?
C2 C1 1.516(11) . ?
O1 C5 1.246(6) . ?
C3 C3 1.379(12) 6_545 ?
C4 C7 1.508(11) . ?
C5 C6 1.497(10) . ?
C7 C8 1.375(7) . ?
C7 C8 1.375(7) 6 ?
C6 C9 1.385(7) 6 ?
C6 C9 1.385(7) . ?
F2 C8 1.324(7) . ?
F3 C9 1.324(7) . ?
C8 C9 1.393(9) 1_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Gd1 Gd1 33.39(11) 5 5 ?
O2 Gd1 Gd1 38.60(12) . 5 ?
O2 Gd1 O2 71.99(19) . 5 ?
O2 Gd1 O3 141.63(11) . 6 ?
O2 Gd1 O3 141.63(11) . . ?
O2 Gd1 O5 73.99(10) . . ?
O2 Gd1 O5 73.98(10) . 6 ?
O2 Gd1 O4 122.13(18) . . ?
O2 Gd1 O1 79.54(16) . . ?
O2 Gd1 O1 79.54(16) . 6 ?
O2 Gd1 C4 25.23(19) 5 . ?
O2 Gd1 C4 97.2(2) . . ?
O2 Gd1 C5 77.2(2) . . ?
O2 Gd1 C5 149.21(19) 5 . ?
O3 Gd1 Gd1 136.23(10) . 5 ?
O3 Gd1 Gd1 136.23(10) 6 5 ?
O3 Gd1 O2 114.16(13) 6 5 ?
O3 Gd1 O2 114.16(13) . 5 ?
O3 Gd1 O3 73.1(2) 6 . ?
O3 Gd1 O4 74.43(14) . . ?
O3 Gd1 O4 74.43(14) 6 . ?
O3 Gd1 O1 74.09(15) 6 . ?
O3 Gd1 O1 104.51(16) 6 6 ?
O3 Gd1 O1 74.09(15) . 6 ?
O3 Gd1 O1 104.51(16) . . ?
O3 Gd1 C4 94.33(16) . . ?
O3 Gd1 C4 94.33(16) 6 . ?
O3 Gd1 C5 90.13(16) 6 . ?
O3 Gd1 C5 90.13(16) . . ?
O5 Gd1 Gd1 67.05(9) 6 5 ?
O5 Gd1 Gd1 67.05(9) . 5 ?
O5 Gd1 O2 69.45(10) . 5 ?
O5 Gd1 O2 69.45(10) 6 5 ?
O5 Gd1 O3 144.39(14) 6 6 ?
O5 Gd1 O3 144.39(14) . . ?
O5 Gd1 O3 73.60(14) 6 . ?
O5 Gd1 O3 73.60(14) . 6 ?
O5 Gd1 O5 133.76(18) . 6 ?
O5 Gd1 O4 84.84(11) 6 . ?
O5 Gd1 O4 84.84(11) . . ?
O5 Gd1 O1 77.90(15) . . ?
O5 Gd1 O1 126.92(15) . 6 ?
O5 Gd1 O1 77.90(15) 6 6 ?
O5 Gd1 O1 126.92(15) 6 . ?
O5 Gd1 C4 75.97(11) . . ?
O5 Gd1 C4 75.97(11) 6 . ?
O5 Gd1 C5 102.21(12) 6 . ?
O5 Gd1 C5 102.21(12) . . ?
O4 Gd1 Gd1 83.53(13) . 5 ?
O4 Gd1 O2 50.14(16) . 5 ?
O4 Gd1 C4 24.9(2) . . ?
O4 Gd1 C5 160.6(2) . . ?
O1 Gd1 Gd1 113.99(12) 6 5 ?
O1 Gd1 Gd1 113.99(11) . 5 ?
O1 Gd1 O2 141.26(14) 6 5 ?
O1 Gd1 O2 141.25(14) . 5 ?
O1 Gd1 O4 147.26(13) . . ?
O1 Gd1 O4 147.26(13) 6 . ?
O1 Gd1 O1 52.3(2) 6 . ?
O1 Gd1 C4 153.51(12) 6 . ?
O1 Gd1 C4 153.51(12) . . ?
O1 Gd1 C5 26.16(11) 6 . ?
O1 Gd1 C5 26.16(11) . . ?
C4 Gd1 Gd1 58.62(16) . 5 ?
C5 Gd1 Gd1 115.82(16) . 5 ?
C5 Gd1 C4 174.4(2) . . ?
Gd1 O2 Gd1 108.01(19) . 5 ?
C4 O2 Gd1 162.5(5) 5 . ?
C4 O2 Gd1 89.4(5) 5 5 ?
C1 O5 Gd1 137.6(4) . . ?
C4 O4 Gd1 97.5(5) . . ?
C3 C2 C3 117.4(8) 2 . ?
C3 C2 C1 121.3(4) 2 . ?
C3 C2 C1 121.3(4) . . ?
C5 O1 Gd1 92.9(4) . . ?
F1 C3 C2 119.8(5) . . ?
F1 C3 C3 118.9(3) . 6_545 ?
C2 C3 C3 121.3(4) . 6_545 ?
O5 C1 O5 129.6(8) 2 . ?
O5 C1 C2 115.2(4) 2 . ?
O5 C1 C2 115.2(4) . . ?
O2 C4 Gd1 65.3(4) 5 . ?
O2 C4 C7 118.6(7) 5 . ?
O4 C4 Gd1 57.6(4) . . ?
O4 C4 O2 122.9(7) . 5 ?
O4 C4 C7 118.5(7) . . ?
C7 C4 Gd1 176.1(5) . . ?
O1 C5 Gd1 60.9(3) 6 . ?
O1 C5 Gd1 60.9(3) . . ?
O1 C5 O1 121.7(7) 6 . ?
O1 C5 C6 119.1(3) 6 . ?
O1 C5 C6 119.1(3) . . ?
C6 C5 Gd1 175.5(6) . . ?
C8 C7 C4 121.6(4) 6 . ?
C8 C7 C4 121.6(4) . . ?
C8 C7 C8 116.8(7) . 6 ?
C9 C6 C5 122.1(4) . . ?
C9 C6 C5 122.1(4) 6 . ?
C9 C6 C9 115.7(7) 6 . ?
C7 C8 C9 121.6(5) . 1_556 ?
F2 C8 C7 119.4(5) . . ?
F2 C8 C9 119.0(5) . 1_556 ?
C6 C9 C8 122.0(5) . 1_554 ?
F3 C9 C6 122.4(5) . . ?
F3 C9 C8 115.6(5) . 1_554 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_10-dy_sq
_database_code_depnum_ccdc_archive 'CCDC 1486538'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 Dy F6 O8'
_chemical_formula_sum            'C12 H4 Dy F6 O8'
_chemical_formula_weight         552.65
_chemical_melting_point          ?
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'
Dy Dy -0.1892 4.4098 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   13.804(5)
_cell_length_b                   11.198(5)
_cell_length_c                   11.558(5)
_cell_angle_alpha                90
_cell_angle_beta                 124.377(5)
_cell_angle_gamma                90
_cell_volume                     1474.6(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1583
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.4063
_cell_measurement_theta_min      3.5695
_shelx_estimated_absorpt_T_max   0.491
_shelx_estimated_absorpt_T_min   0.325
_exptl_absorpt_coefficient_mu    5.184
_exptl_absorpt_correction_T_max  0.436
_exptl_absorpt_correction_T_min  0.244
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2611
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.576
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1302
_reflns_number_total             1382
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.000  0.000  0.000        54        15 ' '
   2  0.500  0.500  0.000        54        15 ' '
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1378
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0253
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0291P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0615
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O2(H2A,H2B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
C1 C 0.0524(4) 0.0611(4) 0.6230(5) 0.0237(11) Uani 1 1 d . . . . .
C2 C 0.000000 0.1252(5) 0.500000 0.0198(14) Uani 1 2 d S T P . .
C3 C 0.000000 0.2609(6) 0.500000 0.0211(14) Uani 1 2 d S T P . .
C4 C 0.1580(6) 0.500000 0.2880(7) 0.0261(17) Uani 1 2 d S T P . .
C5 C 0.1473(6) 0.500000 0.1507(7) 0.0250(16) Uani 1 2 d S T P . .
C6 C 0.1418(4) 0.3954(5) 0.0838(5) 0.0255(11) Uani 1 1 d . . . . .
C7 C 0.1355(5) 0.3958(5) -0.0400(5) 0.0282(12) Uani 1 1 d . . . . .
C8 C 0.1343(6) 0.500000 -0.1036(6) 0.0230(15) Uani 1 2 d S T P . .
C9 C 0.1355(6) 0.500000 -0.2331(7) 0.0253(16) Uani 1 2 d S T P . .
Dy1 Dy 0.15927(2) 0.500000 0.53113(3) 0.01375(12) Uani 1 2 d S T P . .
F1 F 0.1011(3) 0.1194(3) 0.7445(3) 0.0391(8) Uani 1 1 d . . . . .
F2 F 0.1434(4) 0.2884(3) 0.1352(3) 0.0515(10) Uani 1 1 d . . . . .
F3 F 0.1309(4) 0.2915(3) -0.0991(3) 0.0538(10) Uani 1 1 d . . . . .
O1 O 0.0928(3) 0.3087(3) 0.5293(4) 0.0274(8) Uani 1 1 d . . . . .
O2 O 0.3288(3) 0.6291(3) 0.6456(4) 0.0338(9) Uani 1 1 d . . . . .
H2A H 0.337106 0.704413 0.654853 0.041 Uiso 1 1 d R . . . .
H2B H 0.396846 0.598083 0.690023 0.041 Uiso 1 1 d R . . . .
O3 O 0.1628(4) 0.5968(3) 0.3442(4) 0.0363(9) Uani 1 1 d . . . . .
O4 O 0.2323(4) 0.500000 -0.2181(5) 0.0373(14) Uani 1 2 d S T P . .
O5 O 0.0405(4) 0.500000 -0.3512(4) 0.0250(11) Uani 1 2 d S T P . .


_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
C1 C1 1.369(10) 6 ?
C1 C2 1.377(6) . ?
C1 F1 1.336(5) . ?
C2 C3 1.519(9) . ?
C3 O1 1.245(4) . ?
C3 O1 1.245(4) 2_556 ?
C4 C5 1.509(9) . ?
C4 Dy1 2.800(6) . ?
C4 O3 1.246(5) 6_565 ?
C4 O3 1.246(5) . ?
C5 C6 1.382(6) 6_565 ?
C5 C6 1.382(6) . ?
C6 C7 1.383(7) . ?
C6 F2 1.332(6) . ?
C7 C8 1.374(6) . ?
C7 F3 1.335(6) . ?
C8 C9 1.507(9) . ?
C9 Dy1 2.923(6) 1_554 ?
C9 O4 1.247(9) . ?
C9 O5 1.250(8) . ?
Dy1 O1 2.326(3) 6_565 ?
Dy1 O1 2.326(3) . ?
Dy1 O2 2.412(3) . ?
Dy1 O2 2.412(3) 6_565 ?
Dy1 O3 2.442(3) . ?
Dy1 O3 2.442(3) 6_565 ?
Dy1 O4 2.473(5) 1_556 ?
Dy1 O5 2.656(4) 1_556 ?
Dy1 O5 2.335(5) 5_565 ?
O2 H2A 0.8498 . ?
O2 H2B 0.8500 . ?

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
C1 C1 C2 121.4(3) 6 . ?
F1 C1 C1 119.2(2) . 6 ?
F1 C1 C2 119.3(4) . . ?
C1 C2 C1 117.2(6) . 2_556 ?
C1 C2 C3 121.4(3) . . ?
C1 C2 C3 121.4(3) 2_556 . ?
O1 C3 C2 115.5(3) 2_556 . ?
O1 C3 C2 115.5(3) . . ?
O1 C3 O1 129.1(6) 2_556 . ?
C5 C4 Dy1 175.7(5) . . ?
O3 C4 C5 119.6(3) 6_565 . ?
O3 C4 C5 119.6(3) . . ?
O3 C4 Dy1 60.6(3) . . ?
O3 C4 Dy1 60.6(3) 6_565 . ?
O3 C4 O3 120.9(6) . 6_565 ?
C6 C5 C4 122.0(3) . . ?
C6 C5 C4 122.0(3) 6_565 . ?
C6 C5 C6 115.9(6) 6_565 . ?
C5 C6 C7 121.9(5) . . ?
F2 C6 C5 122.0(4) . . ?
F2 C6 C7 116.1(4) . . ?
C8 C7 C6 122.0(5) . . ?
F3 C7 C6 118.9(4) . . ?
F3 C7 C8 119.1(4) . . ?
C7 C8 C7 116.3(6) . 6_565 ?
C7 C8 C9 121.8(3) . . ?
C7 C8 C9 121.8(3) 6_565 . ?
C8 C9 Dy1 175.2(5) . 1_554 ?
O4 C9 C8 118.4(6) . . ?
O4 C9 Dy1 56.9(3) . 1_554 ?
O4 C9 O5 122.2(6) . . ?
O5 C9 C8 119.4(6) . . ?
O5 C9 Dy1 65.3(3) . 1_554 ?
C4 Dy1 C9 174.38(19) . 1_556 ?
O1 Dy1 C4 102.25(9) . . ?
O1 Dy1 C4 102.25(9) 6_565 . ?
O1 Dy1 C9 75.93(9) 6_565 1_556 ?
O1 Dy1 C9 75.93(9) . 1_556 ?
O1 Dy1 O1 134.11(16) . 6_565 ?
O1 Dy1 O2 73.07(12) 6_565 . ?
O1 Dy1 O2 73.07(12) . 6_565 ?
O1 Dy1 O2 144.35(13) 6_565 6_565 ?
O1 Dy1 O2 144.35(12) . . ?
O1 Dy1 O3 77.77(12) 6_565 . ?
O1 Dy1 O3 127.29(12) 6_565 6_565 ?
O1 Dy1 O3 77.77(12) . 6_565 ?
O1 Dy1 O3 127.29(12) . . ?
O1 Dy1 O4 84.73(9) . 1_556 ?
O1 Dy1 O4 84.73(9) 6_565 1_556 ?
O1 Dy1 O5 74.35(9) . 5_565 ?
O1 Dy1 O5 74.35(9) 6_565 5_565 ?
O1 Dy1 O5 69.51(8) 6_565 1_556 ?
O1 Dy1 O5 69.51(8) . 1_556 ?
O2 Dy1 C4 90.29(14) 6_565 . ?
O2 Dy1 C4 90.29(14) . . ?
O2 Dy1 C9 94.21(14) 6_565 1_556 ?
O2 Dy1 C9 94.21(14) . 1_556 ?
O2 Dy1 O2 73.64(18) . 6_565 ?
O2 Dy1 O3 73.83(12) . . ?
O2 Dy1 O3 104.69(13) 6_565 . ?
O2 Dy1 O3 73.83(12) 6_565 6_565 ?
O2 Dy1 O3 104.69(13) . 6_565 ?
O2 Dy1 O4 74.33(12) 6_565 1_556 ?
O2 Dy1 O4 74.33(12) . 1_556 ?
O2 Dy1 O5 114.03(11) 6_565 1_556 ?
O2 Dy1 O5 114.03(11) . 1_556 ?
O3 Dy1 C4 26.39(9) 6_565 . ?
O3 Dy1 C4 26.39(9) . . ?
O3 Dy1 C9 153.33(9) 6_565 1_556 ?
O3 Dy1 C9 153.33(9) . 1_556 ?
O3 Dy1 O3 52.71(17) 6_565 . ?
O3 Dy1 O4 146.94(11) . 1_556 ?
O3 Dy1 O4 146.94(11) 6_565 1_556 ?
O3 Dy1 O5 141.20(12) . 1_556 ?
O3 Dy1 O5 141.20(12) 6_565 1_556 ?
O4 Dy1 C4 160.64(18) 1_556 . ?
O4 Dy1 C9 24.98(18) 1_556 1_556 ?
O4 Dy1 O5 50.29(14) 1_556 1_556 ?
O5 Dy1 C4 149.07(17) 1_556 . ?
O5 Dy1 C4 76.75(17) 5_565 . ?
O5 Dy1 C9 97.63(18) 5_565 1_556 ?
O5 Dy1 C9 25.31(17) 1_556 1_556 ?
O5 Dy1 O2 141.29(10) 5_565 . ?
O5 Dy1 O2 141.30(10) 5_565 6_565 ?
O5 Dy1 O3 79.36(13) 5_565 6_565 ?
O5 Dy1 O3 79.36(13) 5_565 . ?
O5 Dy1 O4 122.61(15) 5_565 1_556 ?
O5 Dy1 O5 72.31(16) 5_565 1_556 ?
C3 O1 Dy1 137.6(3) . . ?
Dy1 O2 H2A 133.2 . . ?
Dy1 O2 H2B 119.1 . . ?
H2A O2 H2B 107.7 . . ?
C4 O3 Dy1 93.1(3) . . ?
C9 O4 Dy1 98.1(4) . 1_554 ?
C9 O5 Dy1 89.3(4) . 1_554 ?
C9 O5 Dy1 163.0(4) . 5_565 ?
Dy1 O5 Dy1 107.69(15) 5_565 1_554 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_5-nd_sq
_database_code_depnum_ccdc_archive 'CCDC 1445657'
_audit_update_record             
;
2017-03-08 deposited with the CCDC.
2017-03-09 downloaded from the CCDC.
;
_audit_creation_date             2017-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H4 F6 Nd O8'
_chemical_formula_sum            'C12 H4 F6 Nd O8'
_chemical_formula_weight         534.39
_chemical_melting_point          ?
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'
Nd Nd -0.1943 3.0179 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 2/m'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   14.025(5)
_cell_length_b                   11.325(5)
_cell_length_c                   11.715(5)
_cell_angle_alpha                90
_cell_angle_beta                 125.732(5)
_cell_angle_gamma                90
_cell_volume                     1510.5(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1547
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.3584
_cell_measurement_theta_min      3.5720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.551
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_correction_T_min  0.469
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0510
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            2773
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.579
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1325
_reflns_number_total             1410
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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.
loop_
  _platon_missing_refln_index_h
  _platon_missing_refln_index_k
  _platon_missing_refln_index_l
  _platon_missing_refln_theta
    1    1    0     2.537
   -2    0    1     2.905
    0    0    1     2.141
   -1    1    1     2.559
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details
The unit cells of complex contains one water molecule which have been treated as diffuse contributions to the overall scattering without specific atom positions using the SQUEEZE/PLATON tools. The SQUEEZE results were consistent with TG-DSC and elemental analysis.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
'CrysAlisPro, Agilent Technologies,Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)(compiled Jan 23 2012,18:06:46)'
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2015)'
_refine_diff_density_max         0.931
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         1406
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0274
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0278P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0639
_refine_ls_wR_factor_ref         0.0657
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H,H) groups
2.a Riding coordinates:
 O1(H1A,H1B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Nd1 Nd -0.16251(2) 0.000000 -0.03462(3) 0.01356(13) Uani 1 2 d S T P . .
F3 F 0.1423(3) 0.2103(3) 0.6333(3) 0.0523(9) Uani 1 1 d . . . . .
F2 F 0.1313(3) 0.2065(3) 0.4024(3) 0.0528(9) Uani 1 1 d . . . . .
O2 O -0.0907(3) 0.1955(3) -0.0273(4) 0.0353(8) Uani 1 1 d . . . . .
O5 O 0.1613(3) 0.0967(3) 0.8400(3) 0.0391(9) Uani 1 1 d . . . . .
O1 O -0.3366(3) -0.1331(3) -0.1542(3) 0.0387(9) Uani 1 1 d . . . . .
H1A H -0.410861 -0.128430 -0.208958 0.046 Uiso 1 1 d R . . . .
H1B H -0.319961 -0.207770 -0.152198 0.046 Uiso 1 1 d R . . . .
O3 O 0.0458(3) 0.000000 0.1530(4) 0.0248(10) Uani 1 2 d S T P . .
O4 O 0.2378(4) 0.000000 0.2948(5) 0.0453(15) Uani 1 2 d S T P . .
C1 C 0.000000 0.2423(5) 0.000000 0.0245(14) Uani 1 2 d S T P . .
C2 C 0.000000 0.3752(5) 0.000000 0.0237(14) Uani 1 2 d S T P . .
C4 C 0.1412(5) 0.000000 0.2741(6) 0.0228(14) Uani 1 2 d S T P . .
C5 C 0.1357(5) 0.000000 0.4002(6) 0.0250(15) Uani 1 2 d S T P . .
C6 C 0.1362(4) 0.1040(4) 0.4618(5) 0.0281(11) Uani 1 1 d . . . . .
C7 C 0.1418(4) 0.1034(4) 0.5830(4) 0.0283(11) Uani 1 1 d . . . . .
C8 C 0.1461(5) 0.000000 0.6493(6) 0.0241(15) Uani 1 2 d S T P . .
C3 C 0.0518(4) 0.4392(4) 0.1228(5) 0.0244(10) Uani 1 1 d . . . . .
C9 C 0.1574(5) 0.000000 0.7858(6) 0.0246(15) Uani 1 2 d S T P . .
F1 F 0.1009(2) 0.3816(2) 0.2451(3) 0.0392(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
Nd1 O2 2.413(3) 6 ?
Nd1 O2 2.413(3) . ?
Nd1 O5 2.520(3) 2_556 ?
Nd1 O5 2.520(3) 5_556 ?
Nd1 O1 2.490(3) 6 ?
Nd1 O1 2.490(3) . ?
Nd1 O3 2.422(4) . ?
Nd1 O3 2.693(4) 5 ?
Nd1 O4 2.578(5) 5 ?
Nd1 C4 2.990(6) 5 ?
Nd1 C9 2.873(6) 5_556 ?
F3 C7 1.345(6) . ?
F2 C6 1.335(5) . ?
O2 C1 1.235(4) . ?
O5 C9 1.251(4) . ?
O1 H1A 0.8481 . ?
O1 H1B 0.8734 . ?
O3 C4 1.260(7) . ?
O4 C4 1.230(7) . ?
C1 C2 1.506(8) . ?
C2 C3 1.380(5) 2 ?
C2 C3 1.380(5) . ?
C4 C5 1.523(8) . ?
C5 C6 1.379(6) . ?
C5 C6 1.379(6) 6 ?
C6 C7 1.375(7) . ?
C7 C8 1.387(6) . ?
C8 C9 1.512(9) . ?
C3 C3 1.377(9) 6_565 ?
C3 F1 1.342(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
O2 Nd1 O2 133.13(15) 6 . ?
O2 Nd1 O5 125.77(11) 6 2_556 ?
O2 Nd1 O5 77.71(12) . 2_556 ?
O2 Nd1 O5 77.71(12) 6 5_556 ?
O2 Nd1 O5 125.77(11) . 5_556 ?
O2 Nd1 O1 73.50(11) 6 . ?
O2 Nd1 O1 145.81(11) . . ?
O2 Nd1 O1 145.81(11) 6 6 ?
O2 Nd1 O1 73.50(11) . 6 ?
O2 Nd1 O3 69.61(9) . 5 ?
O2 Nd1 O3 73.18(8) 6 . ?
O2 Nd1 O3 69.61(9) 6 5 ?
O2 Nd1 O3 73.18(8) . . ?
O2 Nd1 O4 85.19(9) 6 5 ?
O2 Nd1 O4 85.19(9) . 5 ?
O2 Nd1 C4 76.40(9) 6 5 ?
O2 Nd1 C4 76.40(9) . 5 ?
O2 Nd1 C9 101.63(10) 6 5_556 ?
O2 Nd1 C9 101.63(10) . 5_556 ?
O5 Nd1 O5 51.52(16) 2_556 5_556 ?
O5 Nd1 O3 141.32(10) 5_556 5 ?
O5 Nd1 O3 141.32(10) 2_556 5 ?
O5 Nd1 O4 148.33(10) 2_556 5 ?
O5 Nd1 O4 148.33(10) 5_556 5 ?
O5 Nd1 C4 153.79(9) 5_556 5 ?
O5 Nd1 C4 153.79(9) 2_556 5 ?
O5 Nd1 C9 25.77(8) 2_556 5_556 ?
O5 Nd1 C9 25.77(8) 5_556 5_556 ?
O1 Nd1 O5 74.47(11) 6 2_556 ?
O1 Nd1 O5 104.98(12) 6 5_556 ?
O1 Nd1 O5 104.98(12) . 2_556 ?
O1 Nd1 O5 74.47(11) . 5_556 ?
O1 Nd1 O1 74.53(17) . 6 ?
O1 Nd1 O3 113.66(10) . 5 ?
O1 Nd1 O3 113.66(10) 6 5 ?
O1 Nd1 O4 75.20(11) 6 5 ?
O1 Nd1 O4 75.20(11) . 5 ?
O1 Nd1 C4 94.27(12) 6 5 ?
O1 Nd1 C4 94.27(12) . 5 ?
O1 Nd1 C9 90.35(12) . 5_556 ?
O1 Nd1 C9 90.35(12) 6 5_556 ?
O3 Nd1 O5 79.16(12) . 2_556 ?
O3 Nd1 O5 79.16(12) . 5_556 ?
O3 Nd1 O1 141.01(9) . . ?
O3 Nd1 O1 141.01(9) . 6 ?
O3 Nd1 O3 72.14(15) . 5 ?
O3 Nd1 O4 121.14(15) . 5 ?
O3 Nd1 C4 97.06(16) . 5 ?
O3 Nd1 C4 24.92(13) 5 5 ?
O3 Nd1 C9 77.14(16) . 5_556 ?
O3 Nd1 C9 149.28(14) 5 5_556 ?
O4 Nd1 O3 49.00(13) 5 5 ?
O4 Nd1 C4 24.09(14) 5 5 ?
O4 Nd1 C9 161.72(16) 5 5_556 ?
C9 Nd1 C4 174.19(15) 5_556 5 ?
C1 O2 Nd1 138.4(3) . . ?
C9 O5 Nd1 93.1(3) . 5_556 ?
Nd1 O1 H1A 139.0 . . ?
Nd1 O1 H1B 114.4 . . ?
H1A O1 H1B 105.8 . . ?
Nd1 O3 Nd1 107.86(15) . 5 ?
C4 O3 Nd1 161.3(4) . . ?
C4 O3 Nd1 90.8(4) . 5 ?
C4 O4 Nd1 97.1(4) . 5 ?
O2 C1 O2 129.3(6) . 2 ?
O2 C1 C2 115.4(3) 2 . ?
O2 C1 C2 115.4(3) . . ?
C3 C2 C1 121.7(3) . . ?
C3 C2 C1 121.7(3) 2 . ?
C3 C2 C3 116.6(6) . 2 ?
O3 C4 Nd1 64.2(3) . 5 ?
O3 C4 C5 118.1(5) . . ?
O4 C4 Nd1 58.8(3) . 5 ?
O4 C4 O3 123.0(6) . . ?
O4 C4 C5 118.9(5) . . ?
C5 C4 Nd1 177.7(4) . 5 ?
C6 C5 C4 121.3(3) . . ?
C6 C5 C4 121.3(3) 6 . ?
C6 C5 C6 117.2(6) . 6 ?
F2 C6 C5 119.1(4) . . ?
F2 C6 C7 119.9(4) . . ?
C7 C6 C5 121.1(5) . . ?
F3 C7 C6 115.5(4) . . ?
F3 C7 C8 121.8(4) . . ?
C6 C7 C8 122.7(5) . . ?
C7 C8 C7 115.1(6) . 6 ?
C7 C8 C9 122.4(3) . . ?
C7 C8 C9 122.4(3) 6 . ?
C3 C3 C2 121.7(3) 6_565 . ?
F1 C3 C2 119.2(4) . . ?
F1 C3 C3 119.1(2) . 6_565 ?
O5 C9 Nd1 61.1(3) . 5_556 ?
O5 C9 Nd1 61.1(3) 6 5_556 ?
O5 C9 O5 122.2(6) 6 . ?
O5 C9 C8 118.9(3) . . ?
O5 C9 C8 118.9(3) 6 . ?
C8 C9 Nd1 176.2(4) . 5_556 ?

_olex2_submission_special_instructions 'No special instructions were received'
