# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_cei3ether
_database_code_depnum_ccdc_archive 'CCDC 1897950'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
_audit_creation_date             2017-08-28
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 Ce I3 O3'
_chemical_formula_sum            'C12 H30 Ce I3 O3'
_chemical_formula_weight         743.18
_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'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   10.1423(4)
_cell_length_b                   13.9652(6)
_cell_length_c                   15.8918(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2250.90(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.277
_cell_measurement_theta_min      2.79
_shelx_estimated_absorpt_T_max   0.460
_shelx_estimated_absorpt_T_min   0.091
_exptl_absorpt_coefficient_mu    6.139
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1744 before and 0.0592 after correction. The Ratio of minimum to maximum transmission is 0.6810. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.193
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.158
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24517
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.311
_diffrn_reflns_theta_min         2.793
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4012
_reflns_number_total             5427
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         1.423
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0291
_refine_ls_restrained_S_all      1.020
_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)+(0.0220P)²+2.8583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0645
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 O1, C1, C2, C1, C2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C4, C3, O2, C5, C6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 O2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C1(H1A,H1B)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.5000 0.37161(2) 0.2500 0.01089(4) Uani 1 2 d S T P . .
I1 I 0.72199(2) 0.37498(2) 0.38399(2) 0.01934(4) Uani 1 1 d . . . . .
I2 I 0.5000 0.59088(2) 0.2500 0.02122(6) Uani 1 2 d S T P . .
O1 O 0.5000 0.19031(19) 0.2500 0.0190(4) Uani 1 2 d S TU P . .
O2 O 0.33902(18) 0.35823(14) 0.36220(12) 0.0170(3) Uani 1 1 d . U . . .
C5 C 0.3456(3) 0.4202(2) 0.43684(16) 0.0180(3) Uani 1 1 d . U . . .
H5A H 0.2604 0.4540 0.4434 0.022 Uiso 1 1 calc R . . . .
H5B H 0.4150 0.4690 0.4282 0.022 Uiso 1 1 calc R . . . .
C3 C 0.2285(3) 0.2909(2) 0.36123(17) 0.0183(3) Uani 1 1 d . U . . .
H3A H 0.2330 0.2501 0.4121 0.022 Uiso 1 1 calc R . . . .
H3B H 0.2367 0.2487 0.3114 0.022 Uiso 1 1 calc R . . . .
C4 C 0.0969(3) 0.3406(2) 0.3587(2) 0.0251(5) Uani 1 1 d . U . . .
H4A H 0.0965 0.3877 0.3130 0.038 Uiso 1 1 calc GR . . . .
H4B H 0.0814 0.3731 0.4125 0.038 Uiso 1 1 calc GR . . . .
H4C H 0.0272 0.2932 0.3491 0.038 Uiso 1 1 calc GR . . . .
C6 C 0.3747(3) 0.3654(2) 0.51598(18) 0.0261(6) Uani 1 1 d . U . . .
H6A H 0.4559 0.3283 0.5085 0.039 Uiso 1 1 calc GR . . . .
H6B H 0.3014 0.3219 0.5283 0.039 Uiso 1 1 calc GR . . . .
H6C H 0.3859 0.4103 0.5628 0.039 Uiso 1 1 calc GR . . . .
C1 C 0.4201(3) 0.1315(2) 0.19291(18) 0.0220(5) Uani 1 1 d . U . . .
H1A H 0.3377 0.1660 0.1790 0.026 Uiso 1 1 calc R . . . .
H1B H 0.3961 0.0709 0.2213 0.026 Uiso 1 1 calc R . . . .
C2 C 0.4944(3) 0.1097(2) 0.1132(2) 0.0278(6) Uani 1 1 d . U . . .
H2A H 0.4419 0.0664 0.0781 0.042 Uiso 1 1 calc GR . . . .
H2B H 0.5785 0.0790 0.1272 0.042 Uiso 1 1 calc GR . . . .
H2C H 0.5111 0.1693 0.0825 0.042 Uiso 1 1 calc GR . . . .


_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 I1 3.09923(18) 4_655 ?
Ce1 I1 3.09924(18) . ?
Ce1 I2 3.0621(3) . ?
Ce1 O1 2.532(3) . ?
Ce1 O2 2.4248(18) . ?
Ce1 O2 2.4248(18) 4_655 ?
O1 C1 1.467(3) . ?
O1 C1 1.467(3) 4_655 ?
O2 C5 1.470(3) . ?
O2 C3 1.463(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.501(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.505(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.504(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

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
I1 Ce1 I1 178.265(10) 4_655 . ?
I2 Ce1 I1 89.132(5) . . ?
I2 Ce1 I1 89.133(5) . 4_655 ?
O1 Ce1 I1 90.868(5) . . ?
O1 Ce1 I1 90.867(5) . 4_655 ?
O1 Ce1 I2 180.0 . . ?
O2 Ce1 I1 90.99(5) 4_655 . ?
O2 Ce1 I1 90.99(5) . 4_655 ?
O2 Ce1 I1 89.15(5) 4_655 4_655 ?
O2 Ce1 I1 89.15(5) . . ?
O2 Ce1 I2 94.42(5) . . ?
O2 Ce1 I2 94.42(5) 4_655 . ?
O2 Ce1 O1 85.58(5) . . ?
O2 Ce1 O1 85.58(5) 4_655 . ?
O2 Ce1 O2 171.16(9) 4_655 . ?
C1 O1 Ce1 124.02(15) 4_655 . ?
C1 O1 Ce1 124.02(15) . . ?
C1 O1 C1 112.0(3) 4_655 . ?
C5 O2 Ce1 121.17(15) . . ?
C3 O2 Ce1 123.89(15) . . ?
C3 O2 C5 114.94(19) . . ?
O2 C5 H5A 109.1 . . ?
O2 C5 H5B 109.1 . . ?
O2 C5 C6 112.7(2) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
O2 C3 H3A 109.1 . . ?
O2 C3 H3B 109.1 . . ?
O2 C3 C4 112.5(2) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C1 H1A 109.4 . . ?
O1 C1 H1B 109.4 . . ?
O1 C1 C2 111.0(2) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_ntr-1-039
_database_code_depnum_ccdc_archive 'CCDC 1897951'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
_audit_creation_date             2019-01-18
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 I2.98 O3 Sm, 0.02(I)'
_chemical_formula_sum            'C12 H30 I3 O3 Sm'
_chemical_formula_weight         753.41
_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'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   10.0662(7)
_cell_length_b                   13.8437(10)
_cell_length_c                   15.8345(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2206.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9975
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.261
_cell_measurement_theta_min      2.502
_shelx_estimated_absorpt_T_max   0.519
_shelx_estimated_absorpt_T_min   0.180
_exptl_absorpt_coefficient_mu    6.860
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.4022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1306 before and 0.0780 after correction. The Ratio of minimum to maximum transmission is 0.5383. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1388
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50414
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.332
_diffrn_reflns_theta_min         2.573
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  "'Bruker D8 Venture"
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3816
_reflns_number_total             5322
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.687
_refine_diff_density_min         -1.771
_refine_diff_density_rms         0.284
_refine_ls_extinction_coef       0.00049(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         5322
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0341
_refine_ls_restrained_S_all      1.112
_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)+(0.0376P)²+11.7152P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.1045
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(I1') = Uanis(I1)
3. Rigid body (RIGU) restrains
 O2, C3, C5, H3A, H3B, C4, H5A, H5B, C6, H4A, H4B, H4C, H6A, H6B, H6C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O1, C1, H1A, H1B, C2, H2A, H2B, H2C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(I1')=1-FVAR(1)
 Sof(I1)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B)
5.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Sm1 Sm 0.500000 0.62925(2) 0.250000 0.01328(7) Uani 1 2 d S T P A 1
I1 I 0.72036(3) 0.62561(2) 0.11913(2) 0.02111(7) Uani 0.9914(10) 1 d . . . A 1
I2 I 0.500000 0.41245(2) 0.250000 0.02258(9) Uani 1 2 d S T P A 1
O1 O 0.500000 0.8084(3) 0.250000 0.0195(7) Uani 1 2 d S TU P A 1
O2 O 0.6570(3) 0.6423(2) 0.35985(19) 0.0174(5) Uani 1 1 d . U . A 1
C3 C 0.6517(4) 0.5795(3) 0.4350(3) 0.0201(6) Uani 1 1 d . U . A 1
H3A H 0.737370 0.545007 0.440655 0.024 Uiso 1 1 calc R U . A 1
H3B H 0.581104 0.530602 0.427054 0.024 Uiso 1 1 calc R U . A 1
C5 C 0.7689(4) 0.7099(3) 0.3592(3) 0.0213(7) Uani 1 1 d . U . A 1
H5A H 0.763634 0.751654 0.409835 0.026 Uiso 1 1 calc R U . A 1
H5B H 0.761698 0.752017 0.308824 0.026 Uiso 1 1 calc R U . A 1
C1 C 0.4198(5) 0.8677(3) 0.3071(3) 0.0245(7) Uani 1 1 d . U . A 1
H1A H 0.336740 0.832973 0.321210 0.029 Uiso 1 1 calc R U . A 1
H1B H 0.395523 0.928809 0.278518 0.029 Uiso 1 1 calc R U . A 1
C2 C 0.4948(6) 0.8900(4) 0.3870(3) 0.0315(9) Uani 1 1 d . U . A 1
H2A H 0.507865 0.830305 0.419263 0.047 Uiso 1 1 calc GR U . A 1
H2B H 0.443901 0.936117 0.420991 0.047 Uiso 1 1 calc GR U . A 1
H2C H 0.581342 0.917929 0.372748 0.047 Uiso 1 1 calc GR U . A 1
C4 C 0.6249(6) 0.6349(3) 0.5145(3) 0.0306(9) Uani 1 1 d . U . A 1
H4A H 0.696497 0.681651 0.523938 0.046 Uiso 1 1 calc GR U . A 1
H4B H 0.620676 0.590023 0.562328 0.046 Uiso 1 1 calc GR U . A 1
H4C H 0.540133 0.669129 0.509322 0.046 Uiso 1 1 calc GR U . A 1
C6 C 0.9021(4) 0.6600(4) 0.3580(3) 0.0287(9) Uani 1 1 d . U . A 1
H6A H 0.915697 0.626130 0.411633 0.043 Uiso 1 1 calc GR U . A 1
H6B H 0.972478 0.708088 0.350174 0.043 Uiso 1 1 calc GR U . A 1
H6C H 0.904524 0.613441 0.311429 0.043 Uiso 1 1 calc GR U . A 1
I1' I 0.715(3) 0.628(2) 0.380(2) 0.02111(7) Uani 0.0086(10) 1 d . . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 I1 3.0359(3) 4_655 ?
Sm1 I1 3.0360(3) . ?
Sm1 I2 3.0012(5) . ?
Sm1 O1 2.480(4) . ?
Sm1 O2 2.357(3) . ?
Sm1 O2 2.357(3) 4_655 ?
O1 C1 1.464(5) 4_655 ?
O1 C1 1.464(5) . ?
O2 C3 1.474(5) . ?
O2 C5 1.466(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.499(6) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.508(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.505(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
I1 Sm1 I1 178.102(13) 4_655 . ?
I2 Sm1 I1 89.051(7) . 4_655 ?
I2 Sm1 I1 89.051(7) . . ?
O1 Sm1 I1 90.949(7) . . ?
O1 Sm1 I1 90.949(7) . 4_655 ?
O1 Sm1 I2 180.0 . . ?
O2 Sm1 I1 90.87(8) . . ?
O2 Sm1 I1 90.87(8) 4_655 4_655 ?
O2 Sm1 I1 89.27(8) 4_655 . ?
O2 Sm1 I1 89.28(8) . 4_655 ?
O2 Sm1 I2 94.39(7) . . ?
O2 Sm1 I2 94.39(7) 4_655 . ?
O2 Sm1 O1 85.61(7) . . ?
O2 Sm1 O1 85.61(7) 4_655 . ?
O2 Sm1 O2 171.22(14) 4_655 . ?
C1 O1 Sm1 124.1(2) 4_655 . ?
C1 O1 Sm1 124.1(2) . . ?
C1 O1 C1 111.8(4) 4_655 . ?
C3 O2 Sm1 121.8(2) . . ?
C5 O2 Sm1 124.0(2) . . ?
C5 O2 C3 114.2(3) . . ?
O2 C3 H3A 109.1 . . ?
O2 C3 H3B 109.1 . . ?
O2 C3 C4 112.6(3) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
O2 C5 H5A 109.0 . . ?
O2 C5 H5B 109.0 . . ?
O2 C5 C6 113.0(3) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 C2 110.9(4) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id NTR-1-039
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_bjy-01-078
_database_code_depnum_ccdc_archive 'CCDC 1897955'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
_audit_creation_date             2019-01-15
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 I3 O3 Tb'
_chemical_formula_sum            'C12 H30 I3 O3 Tb'
_chemical_formula_weight         761.98
_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'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   10.0273(6)
_cell_length_b                   13.7816(9)
_cell_length_c                   15.7910(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2182.2(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9686
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.04
_cell_measurement_theta_min      2.512
_shelx_estimated_absorpt_T_max   0.400
_shelx_estimated_absorpt_T_min   0.071
_exptl_absorpt_coefficient_mu    7.487
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.0331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2016/2. (Krause, L. et al, 2015)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.319
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1400
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.747
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45138
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         2.512
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans with a narrow frame width'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2965
_reflns_number_total             3344
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         1.190
_refine_diff_density_min         -1.241
_refine_diff_density_rms         0.169
_refine_ls_extinction_coef       0.00025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         3344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0235
_refine_ls_restrained_S_all      1.073
_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)+(0.0283P)²+2.3149P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0571
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C3(H3A,H3B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.500000 0.36959(2) 0.250000 0.01079(6) Uani 1 2 d S T P . .
I1 I 0.71916(2) 0.37373(2) 0.37931(2) 0.01817(6) Uani 1 1 d . . . . .
I2 I 0.500000 0.58514(2) 0.250000 0.01878(7) Uani 1 2 d S T P . .
O1 O 0.500000 0.1933(2) 0.250000 0.0167(5) Uani 1 2 d S T P . .
O2 O 0.34415(19) 0.35742(13) 0.35904(12) 0.0156(4) Uani 1 1 d . . . . .
C5 C 0.3506(3) 0.42045(18) 0.43382(16) 0.0167(5) Uani 1 1 d . . . . .
H5A H 0.265902 0.456866 0.438882 0.020 Uiso 1 1 calc R . . . .
H5B H 0.423457 0.468148 0.426134 0.020 Uiso 1 1 calc R . . . .
C3 C 0.2332(3) 0.28922(19) 0.35784(18) 0.0175(5) Uani 1 1 d . . . . .
H3A H 0.238995 0.246643 0.408200 0.021 Uiso 1 1 calc R . . . .
H3B H 0.240458 0.247720 0.306876 0.021 Uiso 1 1 calc R . . . .
C4 C 0.0996(3) 0.3393(2) 0.3575(2) 0.0246(6) Uani 1 1 d . . . . .
H4A H 0.097138 0.387165 0.311608 0.037 Uiso 1 1 calc GR . . . .
H4B H 0.085763 0.372075 0.411834 0.037 Uiso 1 1 calc GR . . . .
H4C H 0.028932 0.291178 0.348717 0.037 Uiso 1 1 calc GR . . . .
C6 C 0.3743(4) 0.3647(2) 0.51405(18) 0.0260(6) Uani 1 1 d . . . . .
H6A H 0.458115 0.328515 0.509447 0.039 Uiso 1 1 calc GR . . . .
H6B H 0.300522 0.319226 0.523256 0.039 Uiso 1 1 calc GR . . . .
H6C H 0.379631 0.409867 0.561849 0.039 Uiso 1 1 calc GR . . . .
C1 C 0.4193(3) 0.13294(18) 0.19314(19) 0.0203(5) Uani 1 1 d . . . . .
H1A H 0.335483 0.167364 0.179245 0.024 Uiso 1 1 calc R . . . .
H1B H 0.395810 0.071581 0.222119 0.024 Uiso 1 1 calc R . . . .
C2 C 0.4938(3) 0.1105(2) 0.1127(2) 0.0278(7) Uani 1 1 d . . . . .
H2A H 0.442360 0.064138 0.078798 0.042 Uiso 1 1 calc GR . . . .
H2B H 0.580835 0.082331 0.126616 0.042 Uiso 1 1 calc GR . . . .
H2C H 0.506727 0.170383 0.080241 0.042 Uiso 1 1 calc GR . . . .


_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 I1 3.0003(2) . ?
Tb1 I1 3.0003(2) 4_655 ?
Tb1 I2 2.9706(3) . ?
Tb1 O1 2.430(3) . ?
Tb1 O2 2.3313(19) . ?
Tb1 O2 2.3313(19) 4_655 ?
O1 C1 1.467(3) 4_655 ?
O1 C1 1.467(3) . ?
O2 C5 1.467(3) . ?
O2 C3 1.457(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.501(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.507(4) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.506(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

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
I1 Tb1 I1 177.822(8) . 4_655 ?
I2 Tb1 I1 88.911(4) . . ?
I2 Tb1 I1 88.911(4) . 4_655 ?
O1 Tb1 I1 91.089(4) . 4_655 ?
O1 Tb1 I1 91.089(4) . . ?
O1 Tb1 I2 180.0 . . ?
O2 Tb1 I1 90.75(5) . 4_655 ?
O2 Tb1 I1 90.75(5) 4_655 . ?
O2 Tb1 I1 89.41(5) 4_655 4_655 ?
O2 Tb1 I1 89.41(5) . . ?
O2 Tb1 I2 94.13(4) . . ?
O2 Tb1 I2 94.13(4) 4_655 . ?
O2 Tb1 O1 85.87(4) . . ?
O2 Tb1 O1 85.87(4) 4_655 . ?
O2 Tb1 O2 171.75(9) 4_655 . ?
C1 O1 Tb1 124.52(14) 4_655 . ?
C1 O1 Tb1 124.52(14) . . ?
C1 O1 C1 111.0(3) 4_655 . ?
C5 O2 Tb1 121.47(14) . . ?
C3 O2 Tb1 123.29(15) . . ?
C3 O2 C5 115.23(19) . . ?
O2 C5 H5A 109.1 . . ?
O2 C5 H5B 109.1 . . ?
O2 C5 C6 112.5(2) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
O2 C3 H3A 109.1 . . ?
O2 C3 H3B 109.1 . . ?
O2 C3 C4 112.6(2) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C1 H1A 109.4 . . ?
O1 C1 H1B 109.4 . . ?
O1 C1 C2 111.1(2) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id BJY-01-078
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_tmi3c4h8o
_database_code_depnum_ccdc_archive 'CCDC 1897957'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT413_tmi3c4h8o           
;
PROBLEM: Short Inter XH3 .. XHn H10B_2 ..H2A_5 . 1.88 Ang.
RESPONSE: The [Tm(I)3(C4H10)3] system is highly disordered
unlike the other iodides which are highly ordered.
The value of Z' is 4 (5 if the disorder components are included).
The short distances are between disordered components.
;
_vrf_PLAT971_tmi3c4h8o           
;
PROBLEM: Check Calcd Resid. Dens. 0.89A From I2_3 5.04 eA-3
RESPONSE:  The crystal packing is highly irregular with the irregularity 
effected the Tm positions (and to a lesser extent the ligand atoms) 
The large residuals are due to the disorder.
The packing may have been partially disrupted due to partial 
decomposition of the crystal resulting in irregular bond distances and 
angles.
;
_vrf_PLAT972_tmi3c4h8o           
;
PROBLEM: Check Calcd Resid. Dens. 0.86A From I2_3 -4.03 eA-3
RESPONSE: The crystal packing is highly irregular with the irregularity 
effected the Tm positions (and to a lesser extent the ligand atoms) 
The large residuals are due to the disorder.
The packing may have been partially disrupted due to partial 
decomposition of the crystal resulting in irregular bond distances and 
angles.
;
_vrf_PLAT342_tmi3c4h8o           
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02372 Ang.
RESPONSE: The low precision reflects underlying static disorder 
in of the crystals. 
;
_vrf_PLAT910_tmi3c4h8o           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min). 12 Note
RESPONSE: These are reflections obscured by the beamstop or 
reflections that were badly measured or were overexposed on the 
detector.
;
# end Validation Reply Form

_audit_creation_date             2019-01-17
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 I3 O3 Tm'
_chemical_formula_sum            'C12 H30 I3 O3 Tm'
_chemical_formula_weight         771.99
_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'
I I -0.4742 1.8119 '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'
Tm Tm -0.3139 5.2483 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.695(2)
_cell_length_b                   17.532(3)
_cell_length_c                   20.912(4)
_cell_angle_alpha                65.386(7)
_cell_angle_beta                 87.540(7)
_cell_angle_gamma                87.044(7)
_cell_volume                     4557.7(15)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8965
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.465
_shelx_estimated_absorpt_T_max   0.448
_shelx_estimated_absorpt_T_min   0.210
_exptl_absorpt_coefficient_mu    7.959
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.4389
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1327 before and 0.0659 after correction. The Ratio of minimum to maximum transmission is 0.5998. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2832
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0207
_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       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            88713
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.143
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15297
_reflns_number_total             17277
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         5.396
_refine_diff_density_min         -4.347
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         17277
_refine_ls_number_restraints     1113
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0688
_refine_ls_restrained_S_all      1.039
_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)+(0.0437P)²+148.1951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1565
_refine_special_details          Twin
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C10_2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C2_4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(Tm1_5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of
0.004
Uanis(C2_4) = Uanis(C2_5)
Uanis(C1_4) = Uanis(C1_5)
Uanis(O1_4) = Uanis(O1_5)
Uanis(C4_4) = Uanis(C4_5)
Uanis(C10_4) = Uanis(C10_5)
Uanis(O3_4) = Uanis(O3_5)
Uanis(C8_4) = Uanis(C8_5)
Uanis(C12_4) = Uanis(C12_5)
Uanis(C11_4) = Uanis(C11_5)
Uanis(C6_4) = Uanis(C6_5)
Uanis(C9_4) = Uanis(C9_5)
Uanis(I3_4) = Uanis(I3_5)
Uanis(I2_4) = Uanis(I2_5)
Uanis(Tm1_5) = Uanis(Tm1_4)
Uanis(C3_5) = Uanis(C3_4)
Uanis(C5_5) = Uanis(C5_4)
Uanis(I1_4) = Uanis(I1_5)
3. Rigid body (RIGU) restrains
 Tm1_2, I1_2, I2_2, I3_2, O1_2, O2_2, O3_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2,
  C7_2, C8_2, C9_2, C10_2, C11_2, C12_2
 Tm1_3, I1_3, I2_3, I3_3, O1_3, O2_3, O3_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3,
  C7_3, C8_3, C9_3, C10_3, C11_3, C12_3
 Tm1_1, I1_1, I2_1, I3_1, O1_1, O2_1, O3_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1,
  C7_1, C8_1, C9_1, C10_1, C11_1, C12_1
 Tm1_4, I1_4, I2_4, I3_4, O1_4, O2_4, O3_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4,
  C7_4, C8_4, C9_4, C10_4, C11_4, C12_4
 Tm1_5, I1_5, I2_5, I3_5, O1_5, O2_5, O3_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5,
  C7_5, C8_5, C9_5, C10_5, C11_5, C12_5
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Tm1_3, I1_3, I2_3, I3_3, O1_3, O2_3, O3_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3,
C7_3, C8_3, C9_3, C10_3, C11_3, C12_3}
{Tm1_1, I1_1, I2_1, I3_1, O1_1, O2_1, O3_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1,
C7_1, C8_1, C9_1, C10_1, C11_1, C12_1}
{Tm1_4, I1_4, I2_4, I3_4, O1_4, O2_4, O3_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4,
C7_4, C8_4, C9_4, C10_4, C11_4, C12_4}
{Tm1_5, I1_5, I2_5, I3_5, O1_5, O2_5, O3_5, C1_5, C2_5, C3_5, C4_5, C5_5, C6_5,
C7_5, C8_5, C9_5, C10_5, C11_5, C12_5}
as
{Tm1_2, I1_2, I2_2, I3_2, O1_2, O2_2, O3_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2,
C7_2, C8_2, C9_2, C10_2, C11_2, C12_2} sigma for 1-2: 0.002 1-3: 0.04
5. Others
 Sof(Tm1)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=1-FVAR(1)
 Sof(Tm1)=Sof(I1)=Sof(I2)=Sof(I3)=Sof(O1)=Sof(O2)=Sof(O3)=Sof(C1)=Sof(H1A)=
 Sof(H1B)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(H6C)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=
 Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B), C11(H11A,
 H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,H9B),
 C11(H11A,H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C9(H9A,
 H9B), C11(H11A,H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B),
 C9(H9A,H9B), C11(H11A,H11B), C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,
 H7B), C9(H9A,H9B), C11(H11A,H11B)
6.b Idealised Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,
 H10B,H10C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C2(H2A,
 H2B,H2C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,
 H12C)
6.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C),
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C2(H2A,H2B,H2C),
 C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C6(H6A,
 H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Tm1_2 Tm 0.25053(6) 0.69417(3) 0.61704(3) 0.05594(19) Uani 1 1 d D U . . .
I1_2 I 0.29857(14) 0.78043(7) 0.70564(6) 0.0969(5) Uani 1 1 d D U . . .
I2_2 I 0.05384(8) 0.77216(7) 0.60119(6) 0.0717(3) Uani 1 1 d D U . . .
I3_2 I 0.20463(8) 0.60906(5) 0.52687(5) 0.0555(2) Uani 1 1 d D U . . .
O1_2 O 0.4071(5) 0.6346(6) 0.6283(5) 0.080(3) Uani 1 1 d D U . . .
O2_2 O 0.3113(6) 0.8027(4) 0.5200(3) 0.046(2) Uani 1 1 d D U . . .
O3_2 O 0.2119(9) 0.5768(5) 0.7145(4) 0.096(4) Uani 1 1 d D U . . .
C1_2 C 0.4934(12) 0.6830(11) 0.6209(9) 0.122(8) Uani 1 1 d D U . . .
H1A_2 H 0.473828 0.743198 0.604240 0.146 Uiso 1 1 calc R . . . .
H1B_2 H 0.538968 0.676506 0.585345 0.146 Uiso 1 1 calc R . . . .
C2_2 C 0.5457(18) 0.6538(15) 0.6913(10) 0.125(9) Uani 1 1 d D U . . .
H2A_2 H 0.589591 0.697270 0.689270 0.188 Uiso 1 1 calc R . . . .
H2B_2 H 0.583802 0.601695 0.700119 0.188 Uiso 1 1 calc R . . . .
H2C_2 H 0.497100 0.643953 0.729469 0.188 Uiso 1 1 calc R . . . .
C3_2 C 0.4222(15) 0.5466(7) 0.6393(10) 0.101(6) Uani 1 1 d D U . . .
H3A_2 H 0.358458 0.521732 0.640581 0.122 Uiso 1 1 calc R . . . .
H3B_2 H 0.454409 0.514063 0.684668 0.122 Uiso 1 1 calc R . . . .
C4_2 C 0.486(2) 0.5433(12) 0.5790(10) 0.126(10) Uani 1 1 d D U . . .
H4A_2 H 0.459816 0.583274 0.534012 0.188 Uiso 1 1 calc R . . . .
H4B_2 H 0.487204 0.486472 0.580807 0.188 Uiso 1 1 calc R . . . .
H4C_2 H 0.553006 0.557977 0.583284 0.188 Uiso 1 1 calc R . . . .
C5_2 C 0.2899(12) 0.8895(7) 0.5078(11) 0.089(6) Uani 1 1 d D U . . .
H5A_2 H 0.246650 0.891253 0.546432 0.107 Uiso 1 1 calc R . . . .
H5B_2 H 0.254506 0.918301 0.463261 0.107 Uiso 1 1 calc R . . . .
C6_2 C 0.3814(13) 0.9352(9) 0.5040(10) 0.080(5) Uani 1 1 d D U . . .
H6A_2 H 0.383592 0.985699 0.459651 0.121 Uiso 1 1 calc R . . . .
H6B_2 H 0.438720 0.898450 0.506196 0.121 Uiso 1 1 calc R . . . .
H6C_2 H 0.381503 0.951329 0.543581 0.121 Uiso 1 1 calc R . . . .
C7_2 C 0.3739(10) 0.7873(10) 0.4671(6) 0.070(4) Uani 1 1 d D U . . .
H7A_2 H 0.385363 0.726147 0.482042 0.083 Uiso 1 1 calc R . . . .
H7B_2 H 0.438037 0.812766 0.463127 0.083 Uiso 1 1 calc R . . . .
C8_2 C 0.3251(12) 0.8251(10) 0.3961(6) 0.061(4) Uani 1 1 d D U . . .
H8A_2 H 0.371700 0.823550 0.359697 0.092 Uiso 1 1 calc R . . . .
H8B_2 H 0.304055 0.883392 0.385051 0.092 Uiso 1 1 calc R . . . .
H8C_2 H 0.268151 0.792647 0.397747 0.092 Uiso 1 1 calc R . . . .
C9_2 C 0.1179(11) 0.5358(10) 0.7225(12) 0.121(6) Uani 1 1 d D U . . .
H9A_2 H 0.078578 0.567636 0.680247 0.145 Uiso 1 1 calc R . . . .
H9B_2 H 0.081218 0.537734 0.763625 0.145 Uiso 1 1 calc R . . . .
C10_2 C 0.1303(18) 0.4447(11) 0.7322(13) 0.107(6) Uani 1 1 d D U . . .
H10A_2 H 0.098949 0.438153 0.693633 0.161 Uiso 1 1 calc R . . . .
H10B_2 H 0.099797 0.408121 0.777122 0.161 Uiso 1 1 calc R . . . .
H10C_2 H 0.200102 0.429351 0.732126 0.161 Uiso 1 1 calc R . . . .
C11_2 C 0.2685(14) 0.5378(12) 0.7769(7) 0.122(7) Uani 1 1 d D U . . .
H11A_2 H 0.332253 0.565096 0.767664 0.146 Uiso 1 1 calc R . . . .
H11B_2 H 0.281718 0.478255 0.785800 0.146 Uiso 1 1 calc R . . . .
C12_2 C 0.2226(19) 0.5410(12) 0.8434(7) 0.112(8) Uani 1 1 d D U . . .
H12A_2 H 0.195697 0.597806 0.832669 0.168 Uiso 1 1 calc GR . . . .
H12B_2 H 0.272536 0.526330 0.879215 0.168 Uiso 1 1 calc GR . . . .
H12C_2 H 0.170060 0.500987 0.861086 0.168 Uiso 1 1 calc GR . . . .
Tm1_3 Tm 0.79566(4) 0.82153(3) 0.88828(3) 0.03839(13) Uani 1 1 d D U . . .
I1_3 I 0.87805(8) 0.66208(6) 0.99227(8) 0.0844(4) Uani 1 1 d D U . . .
I2_3 I 0.97343(9) 0.91020(7) 0.88060(5) 0.0716(3) Uani 1 1 d D U . . .
I3_3 I 0.68669(8) 0.97502(6) 0.79443(5) 0.0632(3) Uani 1 1 d D U . . .
O1_3 O 0.6620(4) 0.7455(4) 0.8890(5) 0.049(2) Uani 1 1 d D U . . .
O2_3 O 0.8452(6) 0.7923(6) 0.7947(4) 0.060(2) Uani 1 1 d D U . . .
O3_3 O 0.7226(7) 0.8359(5) 0.9828(4) 0.060(2) Uani 1 1 d D U . . .
C1_3 C 0.6667(12) 0.6687(7) 0.8779(8) 0.067(4) Uani 1 1 d D U . . .
H1A_3 H 0.735555 0.656138 0.867939 0.080 Uiso 1 1 calc R . . . .
H1B_3 H 0.628299 0.677678 0.836208 0.080 Uiso 1 1 calc R . . . .
C2_3 C 0.6277(14) 0.5926(9) 0.9415(10) 0.082(5) Uani 1 1 d D U . . .
H2A_3 H 0.649806 0.540767 0.937374 0.123 Uiso 1 1 calc GR . . . .
H2B_3 H 0.556016 0.596334 0.942732 0.123 Uiso 1 1 calc GR . . . .
H2C_3 H 0.652286 0.592258 0.984964 0.123 Uiso 1 1 calc GR . . . .
C3_3 C 0.5608(7) 0.7683(10) 0.9019(7) 0.058(3) Uani 1 1 d D U . . .
H3A_3 H 0.559976 0.820731 0.909094 0.070 Uiso 1 1 calc R . . . .
H3B_3 H 0.534897 0.723450 0.945546 0.070 Uiso 1 1 calc R . . . .
C4_3 C 0.4950(11) 0.7810(12) 0.8411(8) 0.071(5) Uani 1 1 d D U . . .
H4A_3 H 0.527273 0.816331 0.796515 0.106 Uiso 1 1 calc GR . . . .
H4B_3 H 0.432873 0.808406 0.846402 0.106 Uiso 1 1 calc GR . . . .
H4C_3 H 0.482380 0.726398 0.841241 0.106 Uiso 1 1 calc GR . . . .
C5_3 C 0.9453(8) 0.7665(10) 0.7856(11) 0.087(6) Uani 1 1 d D U . . .
H5A_3 H 0.987879 0.778721 0.817014 0.105 Uiso 1 1 calc R . . . .
H5B_3 H 0.967703 0.799466 0.736513 0.105 Uiso 1 1 calc R . . . .
C6_3 C 0.9555(17) 0.6745(11) 0.8018(16) 0.128(10) Uani 1 1 d D U . . .
H6A_3 H 0.963225 0.667410 0.757730 0.192 Uiso 1 1 calc GR . . . .
H6B_3 H 0.896850 0.646283 0.827462 0.192 Uiso 1 1 calc GR . . . .
H6C_3 H 1.012995 0.649803 0.830656 0.192 Uiso 1 1 calc GR . . . .
C7_3 C 0.7846(12) 0.8059(13) 0.7340(7) 0.094(6) Uani 1 1 d D U . . .
H7A_3 H 0.715754 0.815706 0.745942 0.113 Uiso 1 1 calc R . . . .
H7B_3 H 0.787951 0.754022 0.726017 0.113 Uiso 1 1 calc R . . . .
C8_3 C 0.8137(16) 0.8789(13) 0.6659(8) 0.103(7) Uani 1 1 d D U . . .
H8A_3 H 0.768924 0.884122 0.628803 0.154 Uiso 1 1 calc GR . . . .
H8B_3 H 0.880639 0.868624 0.652006 0.154 Uiso 1 1 calc GR . . . .
H8C_3 H 0.810251 0.930854 0.672845 0.154 Uiso 1 1 calc GR . . . .
C9_3 C 0.7226(13) 0.9151(9) 0.9916(11) 0.102(7) Uani 1 1 d D U . . .
H9A_3 H 0.761541 0.956574 0.952986 0.122 Uiso 1 1 calc R . . . .
H9B_3 H 0.753124 0.904914 1.036692 0.122 Uiso 1 1 calc R . . . .
C10_3 C 0.6182(14) 0.9500(13) 0.9912(14) 0.125(9) Uani 1 1 d D U . . .
H10A_3 H 0.585922 0.954595 0.948780 0.187 Uiso 1 1 calc GR . . . .
H10B_3 H 0.619534 1.005652 0.991608 0.187 Uiso 1 1 calc GR . . . .
H10C_3 H 0.582154 0.912236 1.032972 0.187 Uiso 1 1 calc GR . . . .
C11_3 C 0.6712(11) 0.7701(9) 1.0380(6) 0.065(4) Uani 1 1 d D U . . .
H11A_3 H 0.673931 0.719800 1.027675 0.078 Uiso 1 1 calc R . . . .
H11B_3 H 0.601675 0.788269 1.038568 0.078 Uiso 1 1 calc R . . . .
C12_3 C 0.7130(17) 0.7466(15) 1.1104(7) 0.102(8) Uani 1 1 d D U . . .
H12A_3 H 0.783316 0.733764 1.109003 0.152 Uiso 1 1 calc GR . . . .
H12B_3 H 0.680422 0.697206 1.144869 0.152 Uiso 1 1 calc GR . . . .
H12C_3 H 0.701992 0.793650 1.123871 0.152 Uiso 1 1 calc GR . . . .
Tm1_1 Tm 0.24412(4) 0.19288(3) 0.62139(3) 0.04483(15) Uani 1 1 d D U . . .
I1_1 I 0.15412(8) 0.20054(7) 0.74876(5) 0.0640(3) Uani 1 1 d D U . . .
I2_1 I 0.40522(7) 0.30023(6) 0.61467(6) 0.0598(3) Uani 1 1 d D U . . .
I3_1 I 0.32168(8) 0.16918(6) 0.49618(5) 0.0596(3) Uani 1 1 d D U . . .
O1_1 O 0.1162(6) 0.1118(5) 0.6210(5) 0.065(3) Uani 1 1 d D U . . .
O2_1 O 0.1491(5) 0.3073(4) 0.5540(4) 0.050(2) Uani 1 1 d D U . . .
O3_1 O 0.3231(6) 0.0714(4) 0.6931(4) 0.060(2) Uani 1 1 d D U . . .
C1_1 C 0.0144(8) 0.1402(8) 0.6212(8) 0.074(4) Uani 1 1 d D U . . .
H1A_1 H -0.015213 0.148355 0.576360 0.089 Uiso 1 1 calc R . . . .
H1B_1 H 0.011643 0.195098 0.624368 0.089 Uiso 1 1 calc R . . . .
C2_1 C -0.0451(15) 0.0772(15) 0.6830(10) 0.125(10) Uani 1 1 d D U . . .
H2A_1 H -0.059782 0.029430 0.672660 0.187 Uiso 1 1 calc GR . . . .
H2B_1 H -0.106395 0.104763 0.689606 0.187 Uiso 1 1 calc GR . . . .
H2C_1 H -0.007158 0.057374 0.725941 0.187 Uiso 1 1 calc GR . . . .
C3_1 C 0.1304(14) 0.0293(7) 0.6190(9) 0.091(6) Uani 1 1 d D U . . .
H3A_1 H 0.101316 -0.013937 0.662189 0.109 Uiso 1 1 calc R . . . .
H3B_1 H 0.201256 0.015556 0.617866 0.109 Uiso 1 1 calc R . . . .
C4_1 C 0.083(2) 0.0277(12) 0.5547(10) 0.120(10) Uani 1 1 d D U . . .
H4A_1 H 0.091499 0.081854 0.514441 0.180 Uiso 1 1 calc GR . . . .
H4B_1 H 0.013638 0.017230 0.564665 0.180 Uiso 1 1 calc GR . . . .
H4C_1 H 0.115098 -0.017064 0.543872 0.180 Uiso 1 1 calc GR . . . .
C5_1 C 0.1385(9) 0.3815(7) 0.5685(9) 0.064(4) Uani 1 1 d D U . . .
H5A_1 H 0.161745 0.430571 0.526865 0.077 Uiso 1 1 calc R . . . .
H5B_1 H 0.179986 0.373750 0.608475 0.077 Uiso 1 1 calc R . . . .
C6_1 C 0.0343(10) 0.3986(10) 0.5857(10) 0.074(4) Uani 1 1 d D U . . .
H6A_1 H -0.006438 0.409729 0.545140 0.110 Uiso 1 1 calc GR . . . .
H6B_1 H 0.030802 0.447681 0.596973 0.110 Uiso 1 1 calc GR . . . .
H6C_1 H 0.010475 0.349714 0.626274 0.110 Uiso 1 1 calc GR . . . .
C7_1 C 0.1034(10) 0.3149(8) 0.4890(5) 0.056(3) Uani 1 1 d D U . . .
H7A_1 H 0.032973 0.329919 0.490840 0.068 Uiso 1 1 calc R . . . .
H7B_1 H 0.108935 0.259876 0.486063 0.068 Uiso 1 1 calc R . . . .
C8_1 C 0.1505(13) 0.3807(10) 0.4235(8) 0.078(5) Uani 1 1 d D U . . .
H8A_1 H 0.126014 0.376900 0.381588 0.118 Uiso 1 1 calc GR . . . .
H8B_1 H 0.221641 0.371025 0.425022 0.118 Uiso 1 1 calc GR . . . .
H8C_1 H 0.134208 0.436715 0.421551 0.118 Uiso 1 1 calc GR . . . .
C9_1 C 0.4291(8) 0.0582(8) 0.6836(8) 0.067(4) Uani 1 1 d D U . . .
H9A_1 H 0.462486 0.049505 0.727254 0.080 Uiso 1 1 calc R . . . .
H9B_1 H 0.454848 0.109268 0.645178 0.080 Uiso 1 1 calc R . . . .
C10_1 C 0.4524(15) -0.0169(9) 0.6660(9) 0.078(5) Uani 1 1 d D U . . .
H10A_1 H 0.423742 -0.006735 0.620908 0.117 Uiso 1 1 calc GR . . . .
H10B_1 H 0.425086 -0.067353 0.703059 0.117 Uiso 1 1 calc GR . . . .
H10C_1 H 0.523513 -0.025065 0.662810 0.117 Uiso 1 1 calc GR . . . .
C11_1 C 0.2812(12) 0.0054(8) 0.7537(6) 0.078(4) Uani 1 1 d D U . . .
H11A_1 H 0.291368 -0.048265 0.748713 0.093 Uiso 1 1 calc R . . . .
H11B_1 H 0.209775 0.016834 0.755362 0.093 Uiso 1 1 calc R . . . .
C12_1 C 0.3245(18) -0.0042(13) 0.8226(8) 0.102(7) Uani 1 1 d D U . . .
H12A_1 H 0.394614 -0.018548 0.822338 0.152 Uiso 1 1 calc GR . . . .
H12B_1 H 0.291843 -0.048934 0.861969 0.152 Uiso 1 1 calc GR . . . .
H12C_1 H 0.315024 0.048738 0.827771 0.152 Uiso 1 1 calc GR . . . .
Tm1_4 Tm 0.30441(7) 0.66795(6) 0.12694(5) 0.0429(2) Uani 0.789(2) 1 d D U P A 1
I1_4 I 0.3721(3) 0.82675(16) 0.01759(10) 0.0501(5) Uani 0.789(2) 1 d D U P A 1
I2_4 I 0.49307(10) 0.58324(7) 0.12188(7) 0.0423(3) Uani 0.789(2) 1 d D U P A 1
I3_4 I 0.22414(14) 0.50780(11) 0.22743(10) 0.1119(8) Uani 0.789(2) 1 d D U P A
1
O1_4 O 0.1606(6) 0.7392(7) 0.1350(6) 0.076(3) Uani 0.789(2) 1 d D U P A 1
O2_4 O 0.3570(9) 0.7009(6) 0.2144(4) 0.054(3) Uani 0.789(2) 1 d D U P A 1
O3_4 O 0.2332(8) 0.6478(7) 0.0389(4) 0.065(3) Uani 0.789(2) 1 d D U P A 1
C1_4 C 0.1111(15) 0.7268(14) 0.2014(9) 0.104(5) Uani 0.789(2) 1 d D U P A 1
H1A_4 H 0.135470 0.672997 0.238302 0.125 Uiso 0.789(2) 1 calc R . P A 1
H1B_4 H 0.040293 0.722022 0.196772 0.125 Uiso 0.789(2) 1 calc R . P A 1
C2_4 C 0.125(3) 0.7971(17) 0.2258(15) 0.124(7) Uani 0.789(2) 1 d D U P A 1
H2A_4 H 0.128064 0.851091 0.184754 0.186 Uiso 0.789(2) 1 calc GR . P A 1
H2B_4 H 0.185398 0.785886 0.251925 0.186 Uiso 0.789(2) 1 calc GR . P A 1
H2C_4 H 0.069215 0.799032 0.256412 0.186 Uiso 0.789(2) 1 calc GR . P A 1
C3_4 C 0.1065(15) 0.7964(10) 0.0732(9) 0.084(5) Uani 0.789(2) 1 d D U P A 1
H3A_4 H 0.039510 0.776567 0.075445 0.100 Uiso 0.789(2) 1 calc R . P A 1
H3B_4 H 0.139681 0.797705 0.029818 0.100 Uiso 0.789(2) 1 calc R . P A 1
C4_4 C 0.102(3) 0.8841(12) 0.0719(16) 0.130(12) Uani 0.789(2) 1 d D U P A 1
H4A_4 H 0.101129 0.926128 0.023001 0.195 Uiso 0.789(2) 1 calc GR . P A 1
H4B_4 H 0.158901 0.891307 0.095159 0.195 Uiso 0.789(2) 1 calc GR . P A 1
H4C_4 H 0.041970 0.891356 0.096634 0.195 Uiso 0.789(2) 1 calc GR . P A 1
C5_4 C 0.3715(15) 0.7858(8) 0.2067(10) 0.080(6) Uani 0.789(2) 1 d D U P A 1
H5A_4 H 0.350321 0.789918 0.251028 0.096 Uiso 0.789(2) 1 calc R . P A 1
H5B_4 H 0.328866 0.824919 0.169029 0.096 Uiso 0.789(2) 1 calc R . P A 1
C6_4 C 0.4750(16) 0.8137(14) 0.1894(13) 0.086(7) Uani 0.789(2) 1 d D U P A 1
H6A_4 H 0.496930 0.810121 0.145457 0.130 Uiso 0.789(2) 1 calc GR . P A 1
H6B_4 H 0.517552 0.777401 0.227557 0.130 Uiso 0.789(2) 1 calc GR . P A 1
H6C_4 H 0.478071 0.871891 0.183836 0.130 Uiso 0.789(2) 1 calc GR . P A 1
C7_4 C 0.3954(14) 0.6370(11) 0.2811(6) 0.065(5) Uani 0.789(2) 1 d D U P A 1
H7A_4 H 0.458366 0.655082 0.290628 0.078 Uiso 0.789(2) 1 calc R . P A 1
H7B_4 H 0.407916 0.583359 0.276468 0.078 Uiso 0.789(2) 1 calc R . P A 1
C8_4 C 0.3245(19) 0.623(2) 0.3425(9) 0.088(8) Uani 0.789(2) 1 d D U P A 1
H8A_4 H 0.257526 0.623617 0.327543 0.131 Uiso 0.789(2) 1 calc R . P A 1
H8B_4 H 0.330150 0.667948 0.358370 0.131 Uiso 0.789(2) 1 calc R . P A 1
H8C_4 H 0.340061 0.568735 0.381235 0.131 Uiso 0.789(2) 1 calc R . P A 1
C9_4 C 0.1327(10) 0.6176(10) 0.0493(12) 0.083(6) Uani 0.789(2) 1 d D U P A 1
H9A_4 H 0.088643 0.662458 0.017168 0.100 Uiso 0.789(2) 1 calc R . P A 1
H9B_4 H 0.110098 0.604684 0.098168 0.100 Uiso 0.789(2) 1 calc R . P A 1
C10_4 C 0.1270(16) 0.5393(12) 0.0353(19) 0.113(10) Uani 0.789(2) 1 d D U P A 1
H10A_4 H 0.147572 0.552343 -0.013532 0.169 Uiso 0.789(2) 1 calc R . P A 1
H10B_4 H 0.059592 0.520630 0.043086 0.169 Uiso 0.789(2) 1 calc R . P A 1
H10C_4 H 0.170229 0.494639 0.067221 0.169 Uiso 0.789(2) 1 calc R . P A 1
C11_4 C 0.2810(13) 0.6555(12) -0.0258(6) 0.075(5) Uani 0.789(2) 1 d D U P A 1
H11A_4 H 0.281619 0.600835 -0.029272 0.090 Uiso 0.789(2) 1 calc R . P A 1
H11B_4 H 0.349556 0.671138 -0.026534 0.090 Uiso 0.789(2) 1 calc R . P A 1
C12_4 C 0.2279(19) 0.7220(13) -0.0883(10) 0.081(6) Uani 0.789(2) 1 d D U P A 1
H12A_4 H 0.274476 0.747045 -0.127705 0.122 Uiso 0.789(2) 1 calc R . P A 1
H12B_4 H 0.198979 0.765799 -0.074999 0.122 Uiso 0.789(2) 1 calc R . P A 1
H12C_4 H 0.176144 0.696072 -0.102446 0.122 Uiso 0.789(2) 1 calc R . P A 1
Tm1_5 Tm 0.2828(3) 0.6735(2) 0.1121(2) 0.0429(2) Uani 0.211(2) 1 d D U P A 2
I1_5 I 0.3713(13) 0.8244(7) 0.0050(5) 0.0501(5) Uani 0.211(2) 1 d D U P A 2
I2_5 I 0.4581(4) 0.5641(3) 0.1303(3) 0.0423(3) Uani 0.211(2) 1 d D U P A 2
I3_5 I 0.1677(5) 0.5319(4) 0.2100(4) 0.1119(8) Uani 0.211(2) 1 d D U P A 2
O1_5 O 0.1448(10) 0.7574(11) 0.1075(15) 0.076(3) Uani 0.211(2) 1 d D U P A 2
O2_5 O 0.3273(19) 0.7077(12) 0.2008(8) 0.048(7) Uani 0.211(2) 1 d D U P A 2
O3_5 O 0.2210(16) 0.6552(16) 0.0202(8) 0.065(3) Uani 0.211(2) 1 d D U P A 2
C1_5 C 0.0455(14) 0.729(3) 0.113(2) 0.104(5) Uani 0.211(2) 1 d D U P A 2
H1A_5 H 0.036735 0.708201 0.076688 0.125 Uiso 0.211(2) 1 calc R . P A 2
H1B_5 H -0.000951 0.777144 0.104377 0.125 Uiso 0.211(2) 1 calc R . P A 2
C2_5 C 0.020(5) 0.659(5) 0.186(3) 0.124(7) Uani 0.211(2) 1 d D U P A 2
H2A_5 H 0.027422 0.604125 0.183070 0.186 Uiso 0.211(2) 1 calc R . P A 2
H2B_5 H -0.047311 0.667425 0.199297 0.186 Uiso 0.211(2) 1 calc R . P A 2
H2C_5 H 0.064675 0.659676 0.220873 0.186 Uiso 0.211(2) 1 calc R . P A 2
C3_5 C 0.149(3) 0.8420(15) 0.105(2) 0.084(5) Uani 0.211(2) 1 d D U P A 2
H3A_5 H 0.218251 0.854835 0.107520 0.100 Uiso 0.211(2) 1 calc R . P A 2
H3B_5 H 0.113054 0.844475 0.146261 0.100 Uiso 0.211(2) 1 calc R . P A 2
C4_5 C 0.105(8) 0.907(3) 0.038(3) 0.130(12) Uani 0.211(2) 1 d D U P A 2
H4A_5 H 0.136897 0.901039 -0.003040 0.195 Uiso 0.211(2) 1 calc R . P A 2
H4B_5 H 0.114954 0.963542 0.034329 0.195 Uiso 0.211(2) 1 calc R . P A 2
H4C_5 H 0.034847 0.898474 0.037933 0.195 Uiso 0.211(2) 1 calc R . P A 2
C5_5 C 0.327(3) 0.7938(15) 0.193(2) 0.080(6) Uani 0.211(2) 1 d D U P A 2
H5A_5 H 0.278530 0.801144 0.226970 0.096 Uiso 0.211(2) 1 calc R . P A 2
H5B_5 H 0.307309 0.831999 0.145269 0.096 Uiso 0.211(2) 1 calc R . P A 2
C6_5 C 0.426(3) 0.818(4) 0.207(5) 0.086(7) Uani 0.211(2) 1 d D U P A 2
H6A_5 H 0.476842 0.781940 0.197455 0.130 Uiso 0.211(2) 1 calc GR . P A 2
H6B_5 H 0.428477 0.809759 0.255846 0.130 Uiso 0.211(2) 1 calc GR . P A 2
H6C_5 H 0.436433 0.876535 0.175569 0.130 Uiso 0.211(2) 1 calc GR . P A 2
C7_5 C 0.368(4) 0.646(2) 0.2675(13) 0.10(2) Uani 0.211(2) 1 d D U P A 2
H7A_5 H 0.431807 0.664174 0.274633 0.118 Uiso 0.211(2) 1 calc R . P A 2
H7B_5 H 0.378589 0.591068 0.264310 0.118 Uiso 0.211(2) 1 calc R . P A 2
C8_5 C 0.301(6) 0.634(9) 0.3304(18) 0.088(8) Uani 0.211(2) 1 d D U P A 2
H8A_5 H 0.339841 0.618627 0.372377 0.131 Uiso 0.211(2) 1 calc R . P A 2
H8B_5 H 0.255413 0.589263 0.337970 0.131 Uiso 0.211(2) 1 calc R . P A 2
H8C_5 H 0.263226 0.686470 0.321485 0.131 Uiso 0.211(2) 1 calc R . P A 2
C9_5 C 0.1168(18) 0.638(2) 0.019(2) 0.083(6) Uani 0.211(2) 1 d D U P A 2
H9A_5 H 0.088250 0.678991 -0.025355 0.100 Uiso 0.211(2) 1 calc R . P A 2
H9B_5 H 0.081194 0.645648 0.058538 0.100 Uiso 0.211(2) 1 calc R . P A 2
C10_5 C 0.104(5) 0.549(3) 0.026(6) 0.113(10) Uani 0.211(2) 1 d D U P A 2
H10A_5 H 0.086724 0.551379 -0.019795 0.169 Uiso 0.211(2) 1 calc R . P A 2
H10B_5 H 0.051868 0.523048 0.060599 0.169 Uiso 0.211(2) 1 calc R . P A 2
H10C_5 H 0.165360 0.516339 0.041198 0.169 Uiso 0.211(2) 1 calc R . P A 2
C11_5 C 0.269(3) 0.682(3) -0.0478(11) 0.075(5) Uani 0.211(2) 1 d D U P A 2
H11A_5 H 0.274638 0.633642 -0.060988 0.090 Uiso 0.211(2) 1 calc R . P A 2
H11B_5 H 0.335354 0.698902 -0.044859 0.090 Uiso 0.211(2) 1 calc R . P A 2
C12_5 C 0.214(6) 0.754(4) -0.105(2) 0.081(6) Uani 0.211(2) 1 d D U P A 2
H12A_5 H 0.216696 0.745845 -0.148448 0.122 Uiso 0.211(2) 1 calc R . P A 2
H12B_5 H 0.244809 0.807154 -0.113458 0.122 Uiso 0.211(2) 1 calc R . P A 2
H12C_5 H 0.145734 0.757029 -0.089884 0.122 Uiso 0.211(2) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tm1_2 I1_2 2.9486(10) . ?
Tm1_2 I2_2 2.9248(13) . ?
Tm1_2 I3_2 2.9530(9) . ?
Tm1_2 O1_2 2.314(5) . ?
Tm1_2 O2_2 2.288(5) . ?
Tm1_2 O3_2 2.279(5) . ?
O1_2 C1_2 1.455(11) . ?
O1_2 C3_2 1.467(9) . ?
O2_2 C5_2 1.451(9) . ?
O2_2 C7_2 1.474(9) . ?
O3_2 C9_2 1.476(11) . ?
O3_2 C11_2 1.435(10) . ?
C1_2 H1A_2 0.9900 . ?
C1_2 H1B_2 0.9900 . ?
C1_2 C2_2 1.539(13) . ?
C2_2 H2A_2 0.9800 . ?
C2_2 H2B_2 0.9800 . ?
C2_2 H2C_2 0.9800 . ?
C3_2 H3A_2 0.9900 . ?
C3_2 H3B_2 0.9900 . ?
C3_2 C4_2 1.525(13) . ?
C4_2 H4A_2 0.9800 . ?
C4_2 H4B_2 0.9800 . ?
C4_2 H4C_2 0.9800 . ?
C5_2 H5A_2 0.9900 . ?
C5_2 H5B_2 0.9900 . ?
C5_2 C6_2 1.504(13) . ?
C6_2 H6A_2 0.9800 . ?
C6_2 H6B_2 0.9800 . ?
C6_2 H6C_2 0.9800 . ?
C7_2 H7A_2 0.9900 . ?
C7_2 H7B_2 0.9900 . ?
C7_2 C8_2 1.520(11) . ?
C8_2 H8A_2 0.9800 . ?
C8_2 H8B_2 0.9800 . ?
C8_2 H8C_2 0.9800 . ?
C9_2 H9A_2 0.9900 . ?
C9_2 H9B_2 0.9900 . ?
C9_2 C10_2 1.524(13) . ?
C10_2 H10A_2 0.9800 . ?
C10_2 H10B_2 0.9800 . ?
C10_2 H10C_2 0.9800 . ?
C11_2 H11A_2 0.9900 . ?
C11_2 H11B_2 0.9900 . ?
C11_2 C12_2 1.523(12) . ?
C12_2 H12A_2 0.9800 . ?
C12_2 H12B_2 0.9800 . ?
C12_2 H12C_2 0.9800 . ?
Tm1_3 I1_3 2.9392(10) . ?
Tm1_3 I2_3 2.9186(11) . ?
Tm1_3 I3_3 2.9595(10) . ?
Tm1_3 O1_3 2.316(5) . ?
Tm1_3 O2_3 2.289(5) . ?
Tm1_3 O3_3 2.279(5) . ?
O1_3 C1_3 1.456(11) . ?
O1_3 C3_3 1.467(9) . ?
O2_3 C5_3 1.451(9) . ?
O2_3 C7_3 1.475(9) . ?
O3_3 C9_3 1.475(11) . ?
O3_3 C11_3 1.436(10) . ?
C1_3 H1A_3 0.9900 . ?
C1_3 H1B_3 0.9900 . ?
C1_3 C2_3 1.539(13) . ?
C2_3 H2A_3 0.9800 . ?
C2_3 H2B_3 0.9800 . ?
C2_3 H2C_3 0.9800 . ?
C3_3 H3A_3 0.9900 . ?
C3_3 H3B_3 0.9900 . ?
C3_3 C4_3 1.525(13) . ?
C4_3 H4A_3 0.9800 . ?
C4_3 H4B_3 0.9800 . ?
C4_3 H4C_3 0.9800 . ?
C5_3 H5A_3 0.9900 . ?
C5_3 H5B_3 0.9900 . ?
C5_3 C6_3 1.504(13) . ?
C6_3 H6A_3 0.9800 . ?
C6_3 H6B_3 0.9800 . ?
C6_3 H6C_3 0.9800 . ?
C7_3 H7A_3 0.9900 . ?
C7_3 H7B_3 0.9900 . ?
C7_3 C8_3 1.519(11) . ?
C8_3 H8A_3 0.9800 . ?
C8_3 H8B_3 0.9800 . ?
C8_3 H8C_3 0.9800 . ?
C9_3 H9A_3 0.9900 . ?
C9_3 H9B_3 0.9900 . ?
C9_3 C10_3 1.524(13) . ?
C10_3 H10A_3 0.9800 . ?
C10_3 H10B_3 0.9800 . ?
C10_3 H10C_3 0.9800 . ?
C11_3 H11A_3 0.9900 . ?
C11_3 H11B_3 0.9900 . ?
C11_3 C12_3 1.523(12) . ?
C12_3 H12A_3 0.9800 . ?
C12_3 H12B_3 0.9800 . ?
C12_3 H12C_3 0.9800 . ?
Tm1_1 I1_1 2.9380(12) . ?
Tm1_1 I2_1 2.9344(10) . ?
Tm1_1 I3_1 2.9629(11) . ?
Tm1_1 O1_1 2.315(5) . ?
Tm1_1 O2_1 2.288(5) . ?
Tm1_1 O3_1 2.279(5) . ?
O1_1 C1_1 1.456(11) . ?
O1_1 C3_1 1.467(9) . ?
O2_1 C5_1 1.451(9) . ?
O2_1 C7_1 1.474(9) . ?
O3_1 C9_1 1.475(11) . ?
O3_1 C11_1 1.435(10) . ?
C1_1 H1A_1 0.9900 . ?
C1_1 H1B_1 0.9900 . ?
C1_1 C2_1 1.539(13) . ?
C2_1 H2A_1 0.9800 . ?
C2_1 H2B_1 0.9800 . ?
C2_1 H2C_1 0.9800 . ?
C3_1 H3A_1 0.9900 . ?
C3_1 H3B_1 0.9900 . ?
C3_1 C4_1 1.525(13) . ?
C4_1 H4A_1 0.9800 . ?
C4_1 H4B_1 0.9800 . ?
C4_1 H4C_1 0.9800 . ?
C5_1 H5A_1 0.9900 . ?
C5_1 H5B_1 0.9900 . ?
C5_1 C6_1 1.504(13) . ?
C6_1 H6A_1 0.9800 . ?
C6_1 H6B_1 0.9800 . ?
C6_1 H6C_1 0.9800 . ?
C7_1 H7A_1 0.9900 . ?
C7_1 H7B_1 0.9900 . ?
C7_1 C8_1 1.520(11) . ?
C8_1 H8A_1 0.9800 . ?
C8_1 H8B_1 0.9800 . ?
C8_1 H8C_1 0.9800 . ?
C9_1 H9A_1 0.9900 . ?
C9_1 H9B_1 0.9900 . ?
C9_1 C10_1 1.524(13) . ?
C10_1 H10A_1 0.9800 . ?
C10_1 H10B_1 0.9800 . ?
C10_1 H10C_1 0.9800 . ?
C11_1 H11A_1 0.9900 . ?
C11_1 H11B_1 0.9900 . ?
C11_1 C12_1 1.523(12) . ?
C12_1 H12A_1 0.9800 . ?
C12_1 H12B_1 0.9800 . ?
C12_1 H12C_1 0.9800 . ?
Tm1_4 I1_4 2.9359(11) . ?
Tm1_4 I2_4 2.9332(12) . ?
Tm1_4 I3_4 2.9519(12) . ?
Tm1_4 O1_4 2.315(5) . ?
Tm1_4 O2_4 2.289(5) . ?
Tm1_4 O3_4 2.279(5) . ?
O1_4 C1_4 1.456(11) . ?
O1_4 C3_4 1.467(9) . ?
O2_4 C5_4 1.451(9) . ?
O2_4 C7_4 1.475(9) . ?
O3_4 C9_4 1.475(11) . ?
O3_4 C11_4 1.435(10) . ?
C1_4 H1A_4 0.9900 . ?
C1_4 H1B_4 0.9900 . ?
C1_4 C2_4 1.539(13) . ?
C2_4 H2A_4 0.9800 . ?
C2_4 H2B_4 0.9800 . ?
C2_4 H2C_4 0.9800 . ?
C3_4 H3A_4 0.9900 . ?
C3_4 H3B_4 0.9900 . ?
C3_4 C4_4 1.525(13) . ?
C4_4 H4A_4 0.9800 . ?
C4_4 H4B_4 0.9800 . ?
C4_4 H4C_4 0.9800 . ?
C5_4 H5A_4 0.9900 . ?
C5_4 H5B_4 0.9900 . ?
C5_4 C6_4 1.504(13) . ?
C6_4 H6A_4 0.9800 . ?
C6_4 H6B_4 0.9800 . ?
C6_4 H6C_4 0.9800 . ?
C7_4 H7A_4 0.9900 . ?
C7_4 H7B_4 0.9900 . ?
C7_4 C8_4 1.520(11) . ?
C8_4 H8A_4 0.9800 . ?
C8_4 H8B_4 0.9800 . ?
C8_4 H8C_4 0.9800 . ?
C9_4 H9A_4 0.9900 . ?
C9_4 H9B_4 0.9900 . ?
C9_4 C10_4 1.524(13) . ?
C10_4 H10A_4 0.9800 . ?
C10_4 H10B_4 0.9800 . ?
C10_4 H10C_4 0.9800 . ?
C11_4 H11A_4 0.9900 . ?
C11_4 H11B_4 0.9900 . ?
C11_4 C12_4 1.524(12) . ?
C12_4 H12A_4 0.9800 . ?
C12_4 H12B_4 0.9800 . ?
C12_4 H12C_4 0.9800 . ?
Tm1_5 I1_5 2.9400(17) . ?
Tm1_5 I2_5 2.9291(17) . ?
Tm1_5 I3_5 2.9559(17) . ?
Tm1_5 O1_5 2.315(5) . ?
Tm1_5 O2_5 2.289(5) . ?
Tm1_5 O3_5 2.279(5) . ?
O1_5 C1_5 1.456(11) . ?
O1_5 C3_5 1.467(10) . ?
O2_5 C5_5 1.451(9) . ?
O2_5 C7_5 1.475(9) . ?
O3_5 C9_5 1.475(11) . ?
O3_5 C11_5 1.435(10) . ?
C1_5 H1A_5 0.9900 . ?
C1_5 H1B_5 0.9900 . ?
C1_5 C2_5 1.539(13) . ?
C2_5 H2A_5 0.9800 . ?
C2_5 H2B_5 0.9800 . ?
C2_5 H2C_5 0.9800 . ?
C3_5 H3A_5 0.9900 . ?
C3_5 H3B_5 0.9900 . ?
C3_5 C4_5 1.525(13) . ?
C4_5 H4A_5 0.9800 . ?
C4_5 H4B_5 0.9800 . ?
C4_5 H4C_5 0.9800 . ?
C5_5 H5A_5 0.9900 . ?
C5_5 H5B_5 0.9900 . ?
C5_5 C6_5 1.504(13) . ?
C6_5 H6A_5 0.9800 . ?
C6_5 H6B_5 0.9800 . ?
C6_5 H6C_5 0.9800 . ?
C7_5 H7A_5 0.9900 . ?
C7_5 H7B_5 0.9900 . ?
C7_5 C8_5 1.520(11) . ?
C8_5 H8A_5 0.9800 . ?
C8_5 H8B_5 0.9800 . ?
C8_5 H8C_5 0.9800 . ?
C9_5 H9A_5 0.9900 . ?
C9_5 H9B_5 0.9900 . ?
C9_5 C10_5 1.524(13) . ?
C10_5 H10A_5 0.9800 . ?
C10_5 H10B_5 0.9800 . ?
C10_5 H10C_5 0.9800 . ?
C11_5 H11A_5 0.9900 . ?
C11_5 H11B_5 0.9900 . ?
C11_5 C12_5 1.523(12) . ?
C12_5 H12A_5 0.9800 . ?
C12_5 H12B_5 0.9800 . ?
C12_5 H12C_5 0.9800 . ?

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
I1_2 Tm1_2 I3_2 179.19(5) . . ?
I2_2 Tm1_2 I1_2 89.07(5) . . ?
I2_2 Tm1_2 I3_2 91.33(4) . . ?
O1_2 Tm1_2 I1_2 90.7(2) . . ?
O1_2 Tm1_2 I2_2 179.0(3) . . ?
O1_2 Tm1_2 I3_2 88.9(2) . . ?
O2_2 Tm1_2 I1_2 90.08(19) . . ?
O2_2 Tm1_2 I2_2 93.2(2) . . ?
O2_2 Tm1_2 I3_2 89.19(19) . . ?
O2_2 Tm1_2 O1_2 85.9(3) . . ?
O3_2 Tm1_2 I1_2 90.7(3) . . ?
O3_2 Tm1_2 I2_2 95.1(3) . . ?
O3_2 Tm1_2 I3_2 89.9(3) . . ?
O3_2 Tm1_2 O1_2 85.8(4) . . ?
O3_2 Tm1_2 O2_2 171.7(4) . . ?
C1_2 O1_2 Tm1_2 122.1(10) . . ?
C1_2 O1_2 C3_2 117.8(12) . . ?
C3_2 O1_2 Tm1_2 120.0(9) . . ?
C5_2 O2_2 Tm1_2 121.4(8) . . ?
C5_2 O2_2 C7_2 117.2(10) . . ?
C7_2 O2_2 Tm1_2 121.4(7) . . ?
C9_2 O3_2 Tm1_2 122.1(9) . . ?
C11_2 O3_2 Tm1_2 126.1(10) . . ?
C11_2 O3_2 C9_2 111.5(11) . . ?
O1_2 C1_2 H1A_2 109.4 . . ?
O1_2 C1_2 H1B_2 109.4 . . ?
O1_2 C1_2 C2_2 111.2(14) . . ?
H1A_2 C1_2 H1B_2 108.0 . . ?
C2_2 C1_2 H1A_2 109.4 . . ?
C2_2 C1_2 H1B_2 109.4 . . ?
C1_2 C2_2 H2A_2 109.5 . . ?
C1_2 C2_2 H2B_2 109.5 . . ?
C1_2 C2_2 H2C_2 109.5 . . ?
H2A_2 C2_2 H2B_2 109.5 . . ?
H2A_2 C2_2 H2C_2 109.5 . . ?
H2B_2 C2_2 H2C_2 109.5 . . ?
O1_2 C3_2 H3A_2 110.0 . . ?
O1_2 C3_2 H3B_2 110.0 . . ?
O1_2 C3_2 C4_2 108.6(12) . . ?
H3A_2 C3_2 H3B_2 108.4 . . ?
C4_2 C3_2 H3A_2 110.0 . . ?
C4_2 C3_2 H3B_2 110.0 . . ?
C3_2 C4_2 H4A_2 109.5 . . ?
C3_2 C4_2 H4B_2 109.5 . . ?
C3_2 C4_2 H4C_2 109.5 . . ?
H4A_2 C4_2 H4B_2 109.5 . . ?
H4A_2 C4_2 H4C_2 109.5 . . ?
H4B_2 C4_2 H4C_2 109.5 . . ?
O2_2 C5_2 H5A_2 109.3 . . ?
O2_2 C5_2 H5B_2 109.3 . . ?
O2_2 C5_2 C6_2 111.8(11) . . ?
H5A_2 C5_2 H5B_2 107.9 . . ?
C6_2 C5_2 H5A_2 109.3 . . ?
C6_2 C5_2 H5B_2 109.3 . . ?
C5_2 C6_2 H6A_2 109.5 . . ?
C5_2 C6_2 H6B_2 109.5 . . ?
C5_2 C6_2 H6C_2 109.5 . . ?
H6A_2 C6_2 H6B_2 109.5 . . ?
H6A_2 C6_2 H6C_2 109.5 . . ?
H6B_2 C6_2 H6C_2 109.5 . . ?
O2_2 C7_2 H7A_2 109.7 . . ?
O2_2 C7_2 H7B_2 109.7 . . ?
O2_2 C7_2 C8_2 110.0(10) . . ?
H7A_2 C7_2 H7B_2 108.2 . . ?
C8_2 C7_2 H7A_2 109.7 . . ?
C8_2 C7_2 H7B_2 109.7 . . ?
C7_2 C8_2 H8A_2 109.5 . . ?
C7_2 C8_2 H8B_2 109.5 . . ?
C7_2 C8_2 H8C_2 109.5 . . ?
H8A_2 C8_2 H8B_2 109.5 . . ?
H8A_2 C8_2 H8C_2 109.5 . . ?
H8B_2 C8_2 H8C_2 109.5 . . ?
O3_2 C9_2 H9A_2 109.0 . . ?
O3_2 C9_2 H9B_2 109.0 . . ?
O3_2 C9_2 C10_2 113.1(14) . . ?
H9A_2 C9_2 H9B_2 107.8 . . ?
C10_2 C9_2 H9A_2 109.0 . . ?
C10_2 C9_2 H9B_2 109.0 . . ?
C9_2 C10_2 H10A_2 109.5 . . ?
C9_2 C10_2 H10B_2 109.5 . . ?
C9_2 C10_2 H10C_2 109.5 . . ?
H10A_2 C10_2 H10B_2 109.5 . . ?
H10A_2 C10_2 H10C_2 109.5 . . ?
H10B_2 C10_2 H10C_2 109.5 . . ?
O3_2 C11_2 H11A_2 108.3 . . ?
O3_2 C11_2 H11B_2 108.3 . . ?
O3_2 C11_2 C12_2 116.0(13) . . ?
H11A_2 C11_2 H11B_2 107.4 . . ?
C12_2 C11_2 H11A_2 108.3 . . ?
C12_2 C11_2 H11B_2 108.3 . . ?
C11_2 C12_2 H12A_2 109.5 . . ?
C11_2 C12_2 H12B_2 109.5 . . ?
C11_2 C12_2 H12C_2 109.5 . . ?
H12A_2 C12_2 H12B_2 109.5 . . ?
H12A_2 C12_2 H12C_2 109.5 . . ?
H12B_2 C12_2 H12C_2 109.5 . . ?
I1_3 Tm1_3 I3_3 172.06(4) . . ?
I2_3 Tm1_3 I1_3 92.63(4) . . ?
I2_3 Tm1_3 I3_3 93.73(4) . . ?
O1_3 Tm1_3 I1_3 85.9(2) . . ?
O1_3 Tm1_3 I2_3 175.0(2) . . ?
O1_3 Tm1_3 I3_3 88.1(2) . . ?
O2_3 Tm1_3 I1_3 93.4(2) . . ?
O2_3 Tm1_3 I2_3 92.4(2) . . ?
O2_3 Tm1_3 I3_3 91.0(2) . . ?
O2_3 Tm1_3 O1_3 82.9(3) . . ?
O3_3 Tm1_3 I1_3 85.3(2) . . ?
O3_3 Tm1_3 I2_3 98.1(3) . . ?
O3_3 Tm1_3 I3_3 89.1(2) . . ?
O3_3 Tm1_3 O1_3 86.5(3) . . ?
O3_3 Tm1_3 O2_3 169.5(3) . . ?
C1_3 O1_3 Tm1_3 125.0(7) . . ?
C1_3 O1_3 C3_3 111.1(9) . . ?
C3_3 O1_3 Tm1_3 123.9(7) . . ?
C5_3 O2_3 Tm1_3 122.2(9) . . ?
C5_3 O2_3 C7_3 112.4(11) . . ?
C7_3 O2_3 Tm1_3 125.1(8) . . ?
C9_3 O3_3 Tm1_3 122.4(8) . . ?
C11_3 O3_3 Tm1_3 123.5(8) . . ?
C11_3 O3_3 C9_3 114.1(10) . . ?
O1_3 C1_3 H1A_3 109.0 . . ?
O1_3 C1_3 H1B_3 109.0 . . ?
O1_3 C1_3 C2_3 113.1(11) . . ?
H1A_3 C1_3 H1B_3 107.8 . . ?
C2_3 C1_3 H1A_3 109.0 . . ?
C2_3 C1_3 H1B_3 109.0 . . ?
C1_3 C2_3 H2A_3 109.5 . . ?
C1_3 C2_3 H2B_3 109.5 . . ?
C1_3 C2_3 H2C_3 109.5 . . ?
H2A_3 C2_3 H2B_3 109.5 . . ?
H2A_3 C2_3 H2C_3 109.5 . . ?
H2B_3 C2_3 H2C_3 109.5 . . ?
O1_3 C3_3 H3A_3 109.2 . . ?
O1_3 C3_3 H3B_3 109.2 . . ?
O1_3 C3_3 C4_3 112.0(10) . . ?
H3A_3 C3_3 H3B_3 107.9 . . ?
C4_3 C3_3 H3A_3 109.2 . . ?
C4_3 C3_3 H3B_3 109.2 . . ?
C3_3 C4_3 H4A_3 109.5 . . ?
C3_3 C4_3 H4B_3 109.5 . . ?
C3_3 C4_3 H4C_3 109.5 . . ?
H4A_3 C4_3 H4B_3 109.5 . . ?
H4A_3 C4_3 H4C_3 109.5 . . ?
H4B_3 C4_3 H4C_3 109.5 . . ?
O2_3 C5_3 H5A_3 109.2 . . ?
O2_3 C5_3 H5B_3 109.2 . . ?
O2_3 C5_3 C6_3 112.2(12) . . ?
H5A_3 C5_3 H5B_3 107.9 . . ?
C6_3 C5_3 H5A_3 109.2 . . ?
C6_3 C5_3 H5B_3 109.2 . . ?
C5_3 C6_3 H6A_3 109.5 . . ?
C5_3 C6_3 H6B_3 109.5 . . ?
C5_3 C6_3 H6C_3 109.5 . . ?
H6A_3 C6_3 H6B_3 109.5 . . ?
H6A_3 C6_3 H6C_3 109.5 . . ?
H6B_3 C6_3 H6C_3 109.5 . . ?
O2_3 C7_3 H7A_3 108.5 . . ?
O2_3 C7_3 H7B_3 108.5 . . ?
O2_3 C7_3 C8_3 115.0(12) . . ?
H7A_3 C7_3 H7B_3 107.5 . . ?
C8_3 C7_3 H7A_3 108.5 . . ?
C8_3 C7_3 H7B_3 108.5 . . ?
C7_3 C8_3 H8A_3 109.5 . . ?
C7_3 C8_3 H8B_3 109.5 . . ?
C7_3 C8_3 H8C_3 109.5 . . ?
H8A_3 C8_3 H8B_3 109.5 . . ?
H8A_3 C8_3 H8C_3 109.5 . . ?
H8B_3 C8_3 H8C_3 109.5 . . ?
O3_3 C9_3 H9A_3 109.6 . . ?
O3_3 C9_3 H9B_3 109.6 . . ?
O3_3 C9_3 C10_3 110.2(12) . . ?
H9A_3 C9_3 H9B_3 108.1 . . ?
C10_3 C9_3 H9A_3 109.6 . . ?
C10_3 C9_3 H9B_3 109.6 . . ?
C9_3 C10_3 H10A_3 109.5 . . ?
C9_3 C10_3 H10B_3 109.5 . . ?
C9_3 C10_3 H10C_3 109.5 . . ?
H10A_3 C10_3 H10B_3 109.5 . . ?
H10A_3 C10_3 H10C_3 109.5 . . ?
H10B_3 C10_3 H10C_3 109.5 . . ?
O3_3 C11_3 H11A_3 109.0 . . ?
O3_3 C11_3 H11B_3 109.0 . . ?
O3_3 C11_3 C12_3 113.1(11) . . ?
H11A_3 C11_3 H11B_3 107.8 . . ?
C12_3 C11_3 H11A_3 109.0 . . ?
C12_3 C11_3 H11B_3 109.0 . . ?
C11_3 C12_3 H12A_3 109.5 . . ?
C11_3 C12_3 H12B_3 109.5 . . ?
C11_3 C12_3 H12C_3 109.5 . . ?
H12A_3 C12_3 H12B_3 109.5 . . ?
H12A_3 C12_3 H12C_3 109.5 . . ?
H12B_3 C12_3 H12C_3 109.5 . . ?
I1_1 Tm1_1 I3_1 173.76(3) . . ?
I2_1 Tm1_1 I1_1 94.02(4) . . ?
I2_1 Tm1_1 I3_1 91.96(4) . . ?
O1_1 Tm1_1 I1_1 87.9(2) . . ?
O1_1 Tm1_1 I2_1 177.3(2) . . ?
O1_1 Tm1_1 I3_1 86.2(2) . . ?
O2_1 Tm1_1 I1_1 89.5(2) . . ?
O2_1 Tm1_1 I2_1 91.21(19) . . ?
O2_1 Tm1_1 I3_1 92.1(2) . . ?
O2_1 Tm1_1 O1_1 86.9(3) . . ?
O3_1 Tm1_1 I1_1 87.6(2) . . ?
O3_1 Tm1_1 I2_1 94.6(2) . . ?
O3_1 Tm1_1 I3_1 90.2(2) . . ?
O3_1 Tm1_1 O1_1 87.4(3) . . ?
O3_1 Tm1_1 O2_1 173.7(3) . . ?
C1_1 O1_1 Tm1_1 122.0(7) . . ?
C1_1 O1_1 C3_1 114.7(10) . . ?
C3_1 O1_1 Tm1_1 123.3(8) . . ?
C5_1 O2_1 Tm1_1 121.8(7) . . ?
C5_1 O2_1 C7_1 115.2(9) . . ?
C7_1 O2_1 Tm1_1 122.7(7) . . ?
C9_1 O3_1 Tm1_1 120.5(7) . . ?
C11_1 O3_1 Tm1_1 125.9(8) . . ?
C11_1 O3_1 C9_1 113.4(9) . . ?
O1_1 C1_1 H1A_1 109.2 . . ?
O1_1 C1_1 H1B_1 109.2 . . ?
O1_1 C1_1 C2_1 112.0(12) . . ?
H1A_1 C1_1 H1B_1 107.9 . . ?
C2_1 C1_1 H1A_1 109.2 . . ?
C2_1 C1_1 H1B_1 109.2 . . ?
C1_1 C2_1 H2A_1 109.5 . . ?
C1_1 C2_1 H2B_1 109.5 . . ?
C1_1 C2_1 H2C_1 109.5 . . ?
H2A_1 C2_1 H2B_1 109.5 . . ?
H2A_1 C2_1 H2C_1 109.5 . . ?
H2B_1 C2_1 H2C_1 109.5 . . ?
O1_1 C3_1 H3A_1 109.3 . . ?
O1_1 C3_1 H3B_1 109.3 . . ?
O1_1 C3_1 C4_1 111.6(11) . . ?
H3A_1 C3_1 H3B_1 108.0 . . ?
C4_1 C3_1 H3A_1 109.3 . . ?
C4_1 C3_1 H3B_1 109.3 . . ?
C3_1 C4_1 H4A_1 109.5 . . ?
C3_1 C4_1 H4B_1 109.5 . . ?
C3_1 C4_1 H4C_1 109.5 . . ?
H4A_1 C4_1 H4B_1 109.5 . . ?
H4A_1 C4_1 H4C_1 109.5 . . ?
H4B_1 C4_1 H4C_1 109.5 . . ?
O2_1 C5_1 H5A_1 109.2 . . ?
O2_1 C5_1 H5B_1 109.2 . . ?
O2_1 C5_1 C6_1 112.2(10) . . ?
H5A_1 C5_1 H5B_1 107.9 . . ?
C6_1 C5_1 H5A_1 109.2 . . ?
C6_1 C5_1 H5B_1 109.2 . . ?
C5_1 C6_1 H6A_1 109.5 . . ?
C5_1 C6_1 H6B_1 109.5 . . ?
C5_1 C6_1 H6C_1 109.5 . . ?
H6A_1 C6_1 H6B_1 109.5 . . ?
H6A_1 C6_1 H6C_1 109.5 . . ?
H6B_1 C6_1 H6C_1 109.5 . . ?
O2_1 C7_1 H7A_1 109.2 . . ?
O2_1 C7_1 H7B_1 109.2 . . ?
O2_1 C7_1 C8_1 112.2(10) . . ?
H7A_1 C7_1 H7B_1 107.9 . . ?
C8_1 C7_1 H7A_1 109.2 . . ?
C8_1 C7_1 H7B_1 109.2 . . ?
C7_1 C8_1 H8A_1 109.5 . . ?
C7_1 C8_1 H8B_1 109.5 . . ?
C7_1 C8_1 H8C_1 109.5 . . ?
H8A_1 C8_1 H8B_1 109.5 . . ?
H8A_1 C8_1 H8C_1 109.5 . . ?
H8B_1 C8_1 H8C_1 109.5 . . ?
O3_1 C9_1 H9A_1 109.1 . . ?
O3_1 C9_1 H9B_1 109.1 . . ?
O3_1 C9_1 C10_1 112.5(11) . . ?
H9A_1 C9_1 H9B_1 107.8 . . ?
C10_1 C9_1 H9A_1 109.1 . . ?
C10_1 C9_1 H9B_1 109.1 . . ?
C9_1 C10_1 H10A_1 109.5 . . ?
C9_1 C10_1 H10B_1 109.5 . . ?
C9_1 C10_1 H10C_1 109.5 . . ?
H10A_1 C10_1 H10B_1 109.5 . . ?
H10A_1 C10_1 H10C_1 109.5 . . ?
H10B_1 C10_1 H10C_1 109.5 . . ?
O3_1 C11_1 H11A_1 108.9 . . ?
O3_1 C11_1 H11B_1 108.9 . . ?
O3_1 C11_1 C12_1 113.2(12) . . ?
H11A_1 C11_1 H11B_1 107.8 . . ?
C12_1 C11_1 H11A_1 108.9 . . ?
C12_1 C11_1 H11B_1 108.9 . . ?
C11_1 C12_1 H12A_1 109.5 . . ?
C11_1 C12_1 H12B_1 109.5 . . ?
C11_1 C12_1 H12C_1 109.5 . . ?
H12A_1 C12_1 H12B_1 109.5 . . ?
H12A_1 C12_1 H12C_1 109.5 . . ?
H12B_1 C12_1 H12C_1 109.5 . . ?
I1_4 Tm1_4 I3_4 174.80(7) . . ?
I2_4 Tm1_4 I1_4 91.10(10) . . ?
I2_4 Tm1_4 I3_4 90.80(6) . . ?
O1_4 Tm1_4 I1_4 87.9(3) . . ?
O1_4 Tm1_4 I2_4 176.1(4) . . ?
O1_4 Tm1_4 I3_4 90.5(3) . . ?
O2_4 Tm1_4 I1_4 91.7(3) . . ?
O2_4 Tm1_4 I2_4 91.1(3) . . ?
O2_4 Tm1_4 I3_4 93.1(3) . . ?
O2_4 Tm1_4 O1_4 85.2(4) . . ?
O3_4 Tm1_4 I1_4 86.7(3) . . ?
O3_4 Tm1_4 I2_4 97.0(3) . . ?
O3_4 Tm1_4 I3_4 88.3(3) . . ?
O3_4 Tm1_4 O1_4 86.7(4) . . ?
O3_4 Tm1_4 O2_4 171.8(4) . . ?
C1_4 O1_4 Tm1_4 123.6(10) . . ?
C1_4 O1_4 C3_4 113.3(12) . . ?
C3_4 O1_4 Tm1_4 123.0(10) . . ?
C5_4 O2_4 Tm1_4 124.3(8) . . ?
C5_4 O2_4 C7_4 112.3(11) . . ?
C7_4 O2_4 Tm1_4 122.6(9) . . ?
C9_4 O3_4 Tm1_4 119.5(9) . . ?
C11_4 O3_4 Tm1_4 125.3(9) . . ?
C11_4 O3_4 C9_4 115.0(12) . . ?
O1_4 C1_4 H1A_4 108.6 . . ?
O1_4 C1_4 H1B_4 108.6 . . ?
O1_4 C1_4 C2_4 114.6(16) . . ?
H1A_4 C1_4 H1B_4 107.6 . . ?
C2_4 C1_4 H1A_4 108.6 . . ?
C2_4 C1_4 H1B_4 108.6 . . ?
C1_4 C2_4 H2A_4 109.5 . . ?
C1_4 C2_4 H2B_4 109.5 . . ?
C1_4 C2_4 H2C_4 109.5 . . ?
H2A_4 C2_4 H2B_4 109.5 . . ?
H2A_4 C2_4 H2C_4 109.5 . . ?
H2B_4 C2_4 H2C_4 109.5 . . ?
O1_4 C3_4 H3A_4 109.9 . . ?
O1_4 C3_4 H3B_4 109.9 . . ?
O1_4 C3_4 C4_4 109.1(13) . . ?
H3A_4 C3_4 H3B_4 108.3 . . ?
C4_4 C3_4 H3A_4 109.9 . . ?
C4_4 C3_4 H3B_4 109.9 . . ?
C3_4 C4_4 H4A_4 109.5 . . ?
C3_4 C4_4 H4B_4 109.5 . . ?
C3_4 C4_4 H4C_4 109.5 . . ?
H4A_4 C4_4 H4B_4 109.5 . . ?
H4A_4 C4_4 H4C_4 109.5 . . ?
H4B_4 C4_4 H4C_4 109.5 . . ?
O2_4 C5_4 H5A_4 108.6 . . ?
O2_4 C5_4 H5B_4 108.6 . . ?
O2_4 C5_4 C6_4 114.7(14) . . ?
H5A_4 C5_4 H5B_4 107.6 . . ?
C6_4 C5_4 H5A_4 108.6 . . ?
C6_4 C5_4 H5B_4 108.6 . . ?
C5_4 C6_4 H6A_4 109.5 . . ?
C5_4 C6_4 H6B_4 109.5 . . ?
C5_4 C6_4 H6C_4 109.5 . . ?
H6A_4 C6_4 H6B_4 109.5 . . ?
H6A_4 C6_4 H6C_4 109.5 . . ?
H6B_4 C6_4 H6C_4 109.5 . . ?
O2_4 C7_4 H7A_4 109.3 . . ?
O2_4 C7_4 H7B_4 109.3 . . ?
O2_4 C7_4 C8_4 111.8(11) . . ?
H7A_4 C7_4 H7B_4 107.9 . . ?
C8_4 C7_4 H7A_4 109.3 . . ?
C8_4 C7_4 H7B_4 109.3 . . ?
C7_4 C8_4 H8A_4 109.5 . . ?
C7_4 C8_4 H8B_4 109.5 . . ?
C7_4 C8_4 H8C_4 109.5 . . ?
H8A_4 C8_4 H8B_4 109.5 . . ?
H8A_4 C8_4 H8C_4 109.5 . . ?
H8B_4 C8_4 H8C_4 109.5 . . ?
O3_4 C9_4 H9A_4 109.3 . . ?
O3_4 C9_4 H9B_4 109.3 . . ?
O3_4 C9_4 C10_4 111.6(12) . . ?
H9A_4 C9_4 H9B_4 108.0 . . ?
C10_4 C9_4 H9A_4 109.3 . . ?
C10_4 C9_4 H9B_4 109.3 . . ?
C9_4 C10_4 H10A_4 109.5 . . ?
C9_4 C10_4 H10B_4 109.5 . . ?
C9_4 C10_4 H10C_4 109.5 . . ?
H10A_4 C10_4 H10B_4 109.5 . . ?
H10A_4 C10_4 H10C_4 109.5 . . ?
H10B_4 C10_4 H10C_4 109.5 . . ?
O3_4 C11_4 H11A_4 109.6 . . ?
O3_4 C11_4 H11B_4 109.6 . . ?
O3_4 C11_4 C12_4 110.4(13) . . ?
H11A_4 C11_4 H11B_4 108.1 . . ?
C12_4 C11_4 H11A_4 109.6 . . ?
C12_4 C11_4 H11B_4 109.6 . . ?
C11_4 C12_4 H12A_4 109.5 . . ?
C11_4 C12_4 H12B_4 109.5 . . ?
C11_4 C12_4 H12C_4 109.5 . . ?
H12A_4 C12_4 H12B_4 109.5 . . ?
H12A_4 C12_4 H12C_4 109.5 . . ?
H12B_4 C12_4 H12C_4 109.5 . . ?
I1_5 Tm1_5 I3_5 172.0(4) . . ?
I2_5 Tm1_5 I1_5 95.4(4) . . ?
I2_5 Tm1_5 I3_5 91.6(2) . . ?
O1_5 Tm1_5 I1_5 87.1(6) . . ?
O1_5 Tm1_5 I2_5 175.2(7) . . ?
O1_5 Tm1_5 I3_5 86.3(5) . . ?
O2_5 Tm1_5 I1_5 91.6(6) . . ?
O2_5 Tm1_5 I2_5 91.3(6) . . ?
O2_5 Tm1_5 I3_5 92.2(6) . . ?
O2_5 Tm1_5 O1_5 84.5(8) . . ?
O3_5 Tm1_5 I1_5 86.1(6) . . ?
O3_5 Tm1_5 I2_5 97.2(7) . . ?
O3_5 Tm1_5 I3_5 89.1(5) . . ?
O3_5 Tm1_5 O1_5 87.1(8) . . ?
O3_5 Tm1_5 O2_5 171.4(8) . . ?
C1_5 O1_5 Tm1_5 123.4(16) . . ?
C1_5 O1_5 C3_5 113.4(18) . . ?
C3_5 O1_5 Tm1_5 122.9(16) . . ?
C5_5 O2_5 Tm1_5 122.6(15) . . ?
C5_5 O2_5 C7_5 114.1(18) . . ?
C7_5 O2_5 Tm1_5 123.1(16) . . ?
C9_5 O3_5 Tm1_5 121.2(16) . . ?
C11_5 O3_5 Tm1_5 123.7(17) . . ?
C11_5 O3_5 C9_5 112.9(18) . . ?
O1_5 C1_5 H1A_5 108.8 . . ?
O1_5 C1_5 H1B_5 108.8 . . ?
O1_5 C1_5 C2_5 114(2) . . ?
H1A_5 C1_5 H1B_5 107.7 . . ?
C2_5 C1_5 H1A_5 108.8 . . ?
C2_5 C1_5 H1B_5 108.8 . . ?
C1_5 C2_5 H2A_5 109.5 . . ?
C1_5 C2_5 H2B_5 109.5 . . ?
C1_5 C2_5 H2C_5 109.5 . . ?
H2A_5 C2_5 H2B_5 109.5 . . ?
H2A_5 C2_5 H2C_5 109.5 . . ?
H2B_5 C2_5 H2C_5 109.5 . . ?
O1_5 C3_5 H3A_5 109.5 . . ?
O1_5 C3_5 H3B_5 109.5 . . ?
O1_5 C3_5 C4_5 111(2) . . ?
H3A_5 C3_5 H3B_5 108.1 . . ?
C4_5 C3_5 H3A_5 109.5 . . ?
C4_5 C3_5 H3B_5 109.5 . . ?
C3_5 C4_5 H4A_5 109.5 . . ?
C3_5 C4_5 H4B_5 109.5 . . ?
C3_5 C4_5 H4C_5 109.5 . . ?
H4A_5 C4_5 H4B_5 109.5 . . ?
H4A_5 C4_5 H4C_5 109.5 . . ?
H4B_5 C4_5 H4C_5 109.5 . . ?
O2_5 C5_5 H5A_5 109.1 . . ?
O2_5 C5_5 H5B_5 109.1 . . ?
O2_5 C5_5 C6_5 112(2) . . ?
H5A_5 C5_5 H5B_5 107.9 . . ?
C6_5 C5_5 H5A_5 109.1 . . ?
C6_5 C5_5 H5B_5 109.1 . . ?
C5_5 C6_5 H6A_5 109.5 . . ?
C5_5 C6_5 H6B_5 109.5 . . ?
C5_5 C6_5 H6C_5 109.5 . . ?
H6A_5 C6_5 H6B_5 109.5 . . ?
H6A_5 C6_5 H6C_5 109.5 . . ?
H6B_5 C6_5 H6C_5 109.5 . . ?
O2_5 C7_5 H7A_5 109.1 . . ?
O2_5 C7_5 H7B_5 109.1 . . ?
O2_5 C7_5 C8_5 112(2) . . ?
H7A_5 C7_5 H7B_5 107.8 . . ?
C8_5 C7_5 H7A_5 109.1 . . ?
C8_5 C7_5 H7B_5 109.1 . . ?
C7_5 C8_5 H8A_5 109.5 . . ?
C7_5 C8_5 H8B_5 109.5 . . ?
C7_5 C8_5 H8C_5 109.5 . . ?
H8A_5 C8_5 H8B_5 109.5 . . ?
H8A_5 C8_5 H8C_5 109.5 . . ?
H8B_5 C8_5 H8C_5 109.5 . . ?
O3_5 C9_5 H9A_5 109.4 . . ?
O3_5 C9_5 H9B_5 109.4 . . ?
O3_5 C9_5 C10_5 111(2) . . ?
H9A_5 C9_5 H9B_5 108.0 . . ?
C10_5 C9_5 H9A_5 109.4 . . ?
C10_5 C9_5 H9B_5 109.4 . . ?
C9_5 C10_5 H10A_5 109.5 . . ?
C9_5 C10_5 H10B_5 109.5 . . ?
C9_5 C10_5 H10C_5 109.5 . . ?
H10A_5 C10_5 H10B_5 109.5 . . ?
H10A_5 C10_5 H10C_5 109.5 . . ?
H10B_5 C10_5 H10C_5 109.5 . . ?
O3_5 C11_5 H11A_5 108.9 . . ?
O3_5 C11_5 H11B_5 108.9 . . ?
O3_5 C11_5 C12_5 113(2) . . ?
H11A_5 C11_5 H11B_5 107.8 . . ?
C12_5 C11_5 H11A_5 108.9 . . ?
C12_5 C11_5 H11B_5 108.9 . . ?
C11_5 C12_5 H12A_5 109.5 . . ?
C11_5 C12_5 H12B_5 109.5 . . ?
C11_5 C12_5 H12C_5 109.5 . . ?
H12A_5 C12_5 H12B_5 109.5 . . ?
H12A_5 C12_5 H12C_5 109.5 . . ?
H12B_5 C12_5 H12C_5 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id TmI3C4H8O
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_gdiiietheriodide
_database_code_depnum_ccdc_archive 'CCDC 1897956'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
_audit_creation_date             2017-10-24
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2017.10.03 svn.r3461 for OlexSys, GUI svn.r5395)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 Gd I3 O3'
_chemical_formula_sum            'C12 H30 Gd I3 O3'
_chemical_formula_weight         760.31
_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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   10.0525(12)
_cell_length_b                   13.8205(17)
_cell_length_c                   15.8047(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2195.8(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9394
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      44.67
_cell_measurement_theta_min      3.279
_shelx_estimated_absorpt_T_max   0.261
_shelx_estimated_absorpt_T_min   0.218
_exptl_absorpt_coefficient_mu    7.240
_exptl_absorpt_correction_T_max  0.7488
_exptl_absorpt_correction_T_min  0.4218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1158 before and 0.0679 after correction. The Ratio of minimum to maximum transmission is 0.5633. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1396
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.302
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.254
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            114756
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         44.749
_diffrn_reflns_theta_min         2.948
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7570
_reflns_number_total             8912
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2  v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         8912
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0239
_refine_ls_restrained_S_all      1.198
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0120P)²+3.5686P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0545
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.5000 0.62970(2) 0.2500 0.00925(2) Uani 1 2 d S T P . .
I1 I 0.71957(2) 0.62593(2) 0.12012(2) 0.01648(2) Uani 1 1 d . . . . .
I2 I 0.5000 0.41365(2) 0.2500 0.01710(3) Uani 1 2 d S T P . .
O1 O 0.5000 0.80682(11) 0.2500 0.0150(2) Uani 1 2 d S T P . .
O2 O 0.65678(11) 0.64255(8) 0.35988(7) 0.01390(16) Uani 1 1 d . . . . .
C3 C 0.65084(16) 0.57973(11) 0.43421(9) 0.0157(2) Uani 1 1 d . . . . .
H3A H 0.7360 0.5443 0.4396 0.019 Uiso 1 1 calc R . . . .
H3B H 0.5792 0.5314 0.4262 0.019 Uiso 1 1 calc R . . . .
C5 C 0.76777(15) 0.71011(11) 0.35878(10) 0.0160(2) Uani 1 1 d . . . . .
H5A H 0.7623 0.7522 0.4093 0.019 Uiso 1 1 calc R . . . .
H5B H 0.7602 0.7519 0.3081 0.019 Uiso 1 1 calc R . . . .
C1 C 0.41959(18) 0.86705(11) 0.30675(11) 0.0186(2) Uani 1 1 d . . . . .
H1A H 0.3360 0.8328 0.3207 0.022 Uiso 1 1 calc R . . . .
H1B H 0.3961 0.9282 0.2777 0.022 Uiso 1 1 calc R . . . .
C2 C 0.4939(2) 0.88956(14) 0.38709(13) 0.0259(3) Uani 1 1 d . . . . .
H2A H 0.5068 0.8299 0.4195 0.039 Uiso 1 1 calc GR . . . .
H2B H 0.4425 0.9358 0.4209 0.039 Uiso 1 1 calc GR . . . .
H2C H 0.5807 0.9177 0.3731 0.039 Uiso 1 1 calc GR . . . .
C4 C 0.6254(2) 0.63517(14) 0.51432(11) 0.0249(3) Uani 1 1 d . . . . .
H4A H 0.6984 0.6808 0.5241 0.037 Uiso 1 1 calc GR . . . .
H4B H 0.6197 0.5900 0.5620 0.037 Uiso 1 1 calc GR . . . .
H4C H 0.5415 0.6708 0.5092 0.037 Uiso 1 1 calc GR . . . .
C6 C 0.90140(17) 0.66051(15) 0.35773(13) 0.0231(3) Uani 1 1 d . . . . .
H6A H 0.9165 0.6286 0.4122 0.035 Uiso 1 1 calc GR . . . .
H6B H 0.9714 0.7086 0.3479 0.035 Uiso 1 1 calc GR . . . .
H6C H 0.9031 0.6122 0.3124 0.035 Uiso 1 1 calc GR . . . .


_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 I1 3.0147(3) . ?
Gd1 I1 3.0147(3) 3_655 ?
Gd1 I2 2.9859(4) . ?
Gd1 O1 2.4480(15) . ?
Gd1 O2 2.3518(11) 3_655 ?
Gd1 O2 2.3518(11) . ?
O1 C1 1.4665(18) 3_655 ?
O1 C1 1.4665(18) . ?
O2 C3 1.4621(18) . ?
O2 C5 1.4550(18) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.502(2) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.508(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.506(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
I1 Gd1 I1 178.022(5) . 3_655 ?
I2 Gd1 I1 89.011(3) . 3_655 ?
I2 Gd1 I1 89.011(2) . . ?
O1 Gd1 I1 90.989(3) . 3_655 ?
O1 Gd1 I1 90.989(2) . . ?
O1 Gd1 I2 180.0 . . ?
O2 Gd1 I1 89.38(3) . 3_655 ?
O2 Gd1 I1 89.38(3) 3_655 . ?
O2 Gd1 I1 90.77(3) . . ?
O2 Gd1 I1 90.77(3) 3_655 3_655 ?
O2 Gd1 I2 94.33(3) 3_655 . ?
O2 Gd1 I2 94.33(3) . . ?
O2 Gd1 O1 85.67(3) 3_655 . ?
O2 Gd1 O1 85.67(3) . . ?
O2 Gd1 O2 171.34(5) . 3_655 ?
C1 O1 Gd1 124.58(8) . . ?
C1 O1 Gd1 124.58(8) 3_655 . ?
C1 O1 C1 110.83(16) . 3_655 ?
C3 O2 Gd1 121.41(9) . . ?
C5 O2 Gd1 123.61(9) . . ?
C5 O2 C3 114.96(11) . . ?
O2 C3 H3A 109.1 . . ?
O2 C3 H3B 109.1 . . ?
O2 C3 C4 112.42(13) . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
O2 C5 H5A 109.0 . . ?
O2 C5 H5B 109.0 . . ?
O2 C5 C6 113.04(13) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
O1 C1 H1A 109.4 . . ?
O1 C1 H1B 109.4 . . ?
O1 C1 C2 111.08(14) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.4 . . ?
C2 C1 H1B 109.4 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id GdIIIetheriodide
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_bjy-01-081_l
_database_code_depnum_ccdc_archive 'CCDC 1897954'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT342_bjy-01-081_l        
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.025 Ang. 
RESPONSE: In this sample, there was a large degree of peak broadening.
The broadening reflects underlying static disorder from 
partial decomposition of the crystals.  Therefore there is 
short range disorder in the crystal or perhaps alternative 
forms or orientations of the molecule from one part of the structure
to the other.  The effect is large elongated ellipsoids and
low precision on the bond distances and angles.
;
# end Validation Reply Form
_audit_creation_date             2019-01-08
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 I3 Nd O3'
_chemical_formula_sum            'C12 H30 I3 Nd O3'
_chemical_formula_weight         747.30
_chemical_absolute_configuration ad
_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'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   10.3167(5)
_cell_length_b                   16.1003(9)
_cell_length_c                   13.6533(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2267.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.281
_cell_measurement_theta_min      2.94
_shelx_estimated_absorpt_T_max   0.448
_shelx_estimated_absorpt_T_min   0.087
_exptl_absorpt_coefficient_mu    6.375
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.1738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1199 before and 0.0672 after correction. The Ratio of minimum to maximum transmission is 0.2326. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.189
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by ---'
_exptl_crystal_size_max          0.371
_exptl_crystal_size_mid          0.355
_exptl_crystal_size_min          0.233
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39636
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         2.474
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                4964
_reflns_number_total             5126
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2  v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         2.088
_refine_diff_density_min         -1.527
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 
;
 Flack x determined using 2249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(9)
_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     179
_refine_ls_number_reflns         5126
_refine_ls_number_restraints     31
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0381
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0308P)²+20.0269P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0902
_refine_special_details          
;
 Refined as a 2-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.74(4)
 0.26(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Rigid body (RIGU) restrains
 C9, O3
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9, C10
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O3, C11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C11, C12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C3, C4
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O1, C1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1, C2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C7, C8
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2, C5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C5, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C9(H9A,H9B), C11(H11A,H11B), C7(H7A,H7B), C3(H3A,H3B), C1(H1A,H1B)
4.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.29191(5) 0.51363(4) 0.45885(5) 0.02956(13) Uani 1 1 d . . . . .
I1 I 0.50854(7) 0.41460(5) 0.36090(7) 0.04163(19) Uani 1 1 d . . . . .
I2 I 0.20619(9) 0.60206(7) 0.27192(7) 0.0544(3) Uani 1 1 d . . . . .
I3 I 0.12464(11) 0.61259(8) 0.60108(8) 0.0629(3) Uani 1 1 d . . . . .
O1 O 0.3231(7) 0.4177(5) 0.5985(6) 0.0316(15) Uani 1 1 d . U . . .
O2 O 0.1300(8) 0.4101(5) 0.4205(7) 0.0394(18) Uani 1 1 d . U . . .
O3 O 0.4540(10) 0.6158(6) 0.4871(9) 0.056(3) Uani 1 1 d . U . . .
C2 C 0.4693(14) 0.3017(9) 0.6294(12) 0.050(3) Uani 1 1 d . U . . .
H2A H 0.530038 0.290043 0.575912 0.076 Uiso 1 1 calc GR . . . .
H2B H 0.386874 0.273512 0.616610 0.076 Uiso 1 1 calc GR . . . .
H2C H 0.505796 0.281625 0.691258 0.076 Uiso 1 1 calc GR . . . .
C4 C 0.2212(19) 0.4097(12) 0.7598(12) 0.064(4) Uani 1 1 d . U . . .
H4A H 0.225381 0.470390 0.764221 0.097 Uiso 1 1 calc GR . . . .
H4B H 0.299308 0.385625 0.789256 0.097 Uiso 1 1 calc GR . . . .
H4C H 0.144502 0.389686 0.794989 0.097 Uiso 1 1 calc GR . . . .
C6 C 0.1665(18) 0.3029(11) 0.2903(13) 0.064(4) Uani 1 1 d . U . . .
H6A H 0.190985 0.352588 0.253246 0.096 Uiso 1 1 calc GR . . . .
H6B H 0.081059 0.283665 0.268530 0.096 Uiso 1 1 calc GR . . . .
H6C H 0.230690 0.259035 0.279097 0.096 Uiso 1 1 calc GR . . . .
C10 C 0.662(2) 0.5851(14) 0.5603(17) 0.083(5) Uani 1 1 d . U . . .
H10A H 0.712059 0.632248 0.535261 0.124 Uiso 1 1 calc GR . . . .
H10B H 0.661616 0.540426 0.511562 0.124 Uiso 1 1 calc GR . . . .
H10C H 0.701300 0.564938 0.621125 0.124 Uiso 1 1 calc GR . . . .
C5 C 0.1614(18) 0.3232(9) 0.3971(12) 0.058(3) Uani 1 1 d . U . . .
H5A H 0.095940 0.286978 0.428459 0.069 Uiso 1 1 calc R . . . .
H5B H 0.246558 0.309704 0.426510 0.069 Uiso 1 1 calc R . . . .
C9 C 0.5161(19) 0.6141(12) 0.5814(16) 0.073(4) Uani 1 1 d . U . . .
H9A H 0.471963 0.574377 0.625660 0.087 Uiso 1 1 calc R . . . .
H9B H 0.514679 0.669852 0.611980 0.087 Uiso 1 1 calc R . . . .
C11 C 0.4867(16) 0.6921(12) 0.4256(14) 0.066(4) Uani 1 1 d . U . . .
H11A H 0.576073 0.710669 0.440350 0.079 Uiso 1 1 calc R . . . .
H11B H 0.482047 0.677852 0.355167 0.079 Uiso 1 1 calc R . . . .
C12 C 0.397(2) 0.7577(13) 0.447(3) 0.102(8) Uani 1 1 d . U . . .
H12A H 0.387923 0.763579 0.518305 0.153 Uiso 1 1 calc GR . . . .
H12B H 0.312087 0.744434 0.418578 0.153 Uiso 1 1 calc GR . . . .
H12C H 0.428764 0.809932 0.419317 0.153 Uiso 1 1 calc GR . . . .
C8 C -0.1020(17) 0.3914(16) 0.450(2) 0.101(9) Uani 1 1 d . U . . .
H8A H -0.187677 0.404664 0.423032 0.152 Uiso 1 1 calc GR . . . .
H8B H -0.096767 0.410627 0.517744 0.152 Uiso 1 1 calc GR . . . .
H8C H -0.088251 0.331245 0.447498 0.152 Uiso 1 1 calc GR . . . .
C7 C -0.0002(17) 0.4338(14) 0.3903(16) 0.077(6) Uani 1 1 d . U . . .
H7A H -0.012367 0.419397 0.320372 0.092 Uiso 1 1 calc R . . . .
H7B H -0.010210 0.494660 0.396968 0.092 Uiso 1 1 calc R . . . .
C3 C 0.2125(18) 0.3835(12) 0.6514(13) 0.061(4) Uani 1 1 d . U . . .
H3A H 0.212752 0.322211 0.646319 0.074 Uiso 1 1 calc R . . . .
H3B H 0.130824 0.404492 0.622484 0.074 Uiso 1 1 calc R . . . .
C1 C 0.4462(15) 0.3962(9) 0.6362(12) 0.050(3) Uani 1 1 d . U . . .
H1A H 0.452098 0.413940 0.705452 0.060 Uiso 1 1 calc R . . . .
H1B H 0.514282 0.425727 0.598829 0.060 Uiso 1 1 calc R . . . .


_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 I1 3.0537(9) . ?
Nd1 I2 3.0534(10) . ?
Nd1 I3 3.0475(11) . ?
Nd1 O1 2.475(8) . ?
Nd1 O2 2.417(8) . ?
Nd1 O3 2.377(10) . ?
O1 C3 1.458(19) . ?
O1 C1 1.413(16) . ?
O2 C5 1.472(18) . ?
O2 C7 1.456(18) . ?
O3 C9 1.44(2) . ?
O3 C11 1.53(2) . ?
C2 C1 1.54(2) . ?
C4 C3 1.54(2) . ?
C6 C5 1.50(2) . ?
C10 C9 1.60(3) . ?
C11 C12 1.44(3) . ?
C8 C7 1.49(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Nd1 I1 95.13(3) . . ?
I3 Nd1 I1 165.11(4) . . ?
I3 Nd1 I2 97.17(3) . . ?
O1 Nd1 I1 85.21(19) . . ?
O1 Nd1 I2 166.59(17) . . ?
O1 Nd1 I3 84.77(19) . . ?
O2 Nd1 I1 92.9(2) . . ?
O2 Nd1 I2 86.6(2) . . ?
O2 Nd1 I3 96.2(2) . . ?
O2 Nd1 O1 80.0(3) . . ?
O3 Nd1 I1 85.3(2) . . ?
O3 Nd1 I2 91.0(3) . . ?
O3 Nd1 I3 86.2(2) . . ?
O3 Nd1 O1 102.4(3) . . ?
O3 Nd1 O2 176.8(4) . . ?
C3 O1 Nd1 121.0(8) . . ?
C1 O1 Nd1 123.4(8) . . ?
C1 O1 C3 115.5(12) . . ?
C5 O2 Nd1 123.4(9) . . ?
C7 O2 Nd1 121.3(10) . . ?
C7 O2 C5 113.0(13) . . ?
C9 O3 Nd1 116.5(9) . . ?
C9 O3 C11 114.2(12) . . ?
C11 O3 Nd1 128.6(10) . . ?
O2 C5 C6 115.3(12) . . ?
O3 C9 C10 105.2(17) . . ?
C12 C11 O3 109.7(16) . . ?
O2 C7 C8 112.1(14) . . ?
O1 C3 C4 109.1(14) . . ?
O1 C1 C2 111.1(11) . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a None'
_olex2_submission_original_sample_id BJY-01-081
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.74(4)
2 0.26(4)

_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_tbi3thf3
_database_code_depnum_ccdc_archive 'CCDC 1897953'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-19 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
_audit_creation_date             2017-06-28
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2017.06.21 svn.r3421 for OlexSys, GUI svn.r5355)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H40 I2 O5 Tb, C8 H16 I4 O2 Tb'
_chemical_formula_sum            'C28 H56 I6 O7 Tb2'
_chemical_formula_weight         1583.96
_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'
I I -0.4742 1.8119 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   12.742(3)
_cell_length_b                   12.016(3)
_cell_length_c                   28.632(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.442(4)
_cell_angle_gamma                90
_cell_volume                     4336.3(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.823
_cell_measurement_theta_min      2.342
_shelx_estimated_absorpt_T_max   0.494
_shelx_estimated_absorpt_T_min   0.339
_exptl_absorpt_coefficient_mu    7.542
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.3986
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1196 before and 0.0856 after correction. The Ratio of minimum to maximum transmission is 0.5350. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2912
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.109
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            35946
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.139
_diffrn_reflns_theta_min         2.342
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6594
_reflns_number_total             8278
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_refine_diff_density_max         1.908
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         8278
_refine_ls_number_restraints     30
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0283
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0128P)²+18.0819P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0618
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Rigid body (RIGU) restrains
 O4, C12, C11, C10, C9
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C12(H12A,H12B), C8(H8A,H8B), C13(H13A,H13B), C2(H2A,H2B), C3(H3A,
 H3B), C14(H14A,H14B), C1(H1A,H1B), C9(H9A,H9B), C4(H4A,H4B), C7(H7A,H7B),
 C11(H11A,H11B), C6(H6A,H6B), C10(H10A,H10B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Tb2 Tb 0.5000 0.49933(2) 0.2500 0.00873(4) Uani 1 2 d S T P . .
Tb1 Tb 0.0000 0.5000 0.5000 0.01092(4) Uani 1 2 d S T P . .
I2 I 0.08754(2) 0.59783(2) 0.59526(2) 0.01723(5) Uani 1 1 d . . . . .
I1 I 0.02972(2) 0.26697(2) 0.53796(2) 0.01776(5) Uani 1 1 d . . . . .
I3 I 0.28881(2) 0.49786(2) 0.28318(2) 0.01720(5) Uani 1 1 d . . . . .
O3 O 0.5000 0.6985(3) 0.2500 0.0137(6) Uani 1 2 d S T P . .
O2 O 0.45204(19) 0.33912(19) 0.20217(8) 0.0139(4) Uani 1 1 d . . . . .
O1 O 0.1728(2) 0.5042(2) 0.48332(9) 0.0162(5) Uani 1 1 d . . . . .
O4 O 0.5831(2) 0.5622(2) 0.32654(8) 0.0154(5) Uani 1 1 d . U . . .
C5 C 0.5227(3) 0.2517(3) 0.18893(13) 0.0182(7) Uani 1 1 d . . . . .
H5A H 0.5699 0.2238 0.2170 0.022 Uiso 1 1 calc R . . . .
H5B H 0.5668 0.2802 0.1658 0.022 Uiso 1 1 calc R . . . .
C12 C 0.6792(3) 0.6311(3) 0.33495(13) 0.0203(7) Uani 1 1 d . U . . .
H12A H 0.6794 0.6870 0.3096 0.024 Uiso 1 1 calc R . . . .
H12B H 0.7437 0.5845 0.3364 0.024 Uiso 1 1 calc R . . . .
C8 C 0.3422(3) 0.3135(3) 0.18141(12) 0.0162(6) Uani 1 1 d . . . . .
H8A H 0.3064 0.3805 0.1665 0.019 Uiso 1 1 calc R . . . .
H8B H 0.3013 0.2854 0.2058 0.019 Uiso 1 1 calc R . . . .
C13 C 0.4462(3) 0.7690(3) 0.28107(12) 0.0156(6) Uani 1 1 d . . . . .
H13A H 0.4621 0.7435 0.3142 0.019 Uiso 1 1 calc R . . . .
H13B H 0.3684 0.7676 0.2712 0.019 Uiso 1 1 calc R . . . .
C2 C 0.2760(3) 0.4699(3) 0.42367(13) 0.0201(7) Uani 1 1 d . . . . .
H2A H 0.2279 0.5005 0.3964 0.024 Uiso 1 1 calc R . . . .
H2B H 0.3276 0.4189 0.4122 0.024 Uiso 1 1 calc R . . . .
C3 C 0.3318(3) 0.5625(3) 0.45454(15) 0.0237(8) Uani 1 1 d . . . . .
H3A H 0.3512 0.6251 0.4350 0.028 Uiso 1 1 calc R . . . .
H3B H 0.3966 0.5343 0.4743 0.028 Uiso 1 1 calc R . . . .
C14 C 0.4899(3) 0.8845(3) 0.27572(12) 0.0176(7) Uani 1 1 d . . . . .
H14A H 0.5564 0.8966 0.2977 0.021 Uiso 1 1 calc R . . . .
H14B H 0.4377 0.9424 0.2812 0.021 Uiso 1 1 calc R . . . .
C1 C 0.2154(3) 0.4132(3) 0.45796(13) 0.0175(7) Uani 1 1 d . . . . .
H1A H 0.1574 0.3670 0.4412 0.021 Uiso 1 1 calc R . . . .
H1B H 0.2627 0.3653 0.4799 0.021 Uiso 1 1 calc R . . . .
C9 C 0.5449(4) 0.5423(4) 0.37201(12) 0.0246(8) Uani 1 1 d . U . . .
H9A H 0.5397 0.4615 0.3781 0.030 Uiso 1 1 calc R . . . .
H9B H 0.4742 0.5765 0.3721 0.030 Uiso 1 1 calc R . . . .
C4 C 0.2482(3) 0.5984(3) 0.48509(13) 0.0182(7) Uani 1 1 d . . . . .
H4A H 0.2816 0.6127 0.5180 0.022 Uiso 1 1 calc R . . . .
H4B H 0.2114 0.6668 0.4723 0.022 Uiso 1 1 calc R . . . .
C7 C 0.3521(3) 0.2249(3) 0.14485(13) 0.0198(7) Uani 1 1 d . . . . .
H7A H 0.3634 0.2582 0.1143 0.024 Uiso 1 1 calc R . . . .
H7B H 0.2885 0.1767 0.1398 0.024 Uiso 1 1 calc R . . . .
C11 C 0.6745(4) 0.6865(4) 0.38151(15) 0.0314(9) Uani 1 1 d . U . . .
H11A H 0.6288 0.7534 0.3777 0.038 Uiso 1 1 calc R . . . .
H11B H 0.7462 0.7077 0.3972 0.038 Uiso 1 1 calc R . . . .
C6 C 0.4491(3) 0.1609(3) 0.16728(14) 0.0220(8) Uani 1 1 d . . . . .
H6A H 0.4312 0.1088 0.1917 0.026 Uiso 1 1 calc R . . . .
H6B H 0.4813 0.1186 0.1433 0.026 Uiso 1 1 calc R . . . .
C10 C 0.6268(4) 0.5964(4) 0.40893(15) 0.0336(9) Uani 1 1 d . U . . .
H10A H 0.5931 0.6287 0.4349 0.040 Uiso 1 1 calc R . . . .
H10B H 0.6814 0.5420 0.4223 0.040 Uiso 1 1 calc R . . . .


_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
Tb2 I3 2.9824(6) 2_655 ?
Tb2 I3 2.9824(6) . ?
Tb2 O3 2.393(3) . ?
Tb2 O2 2.389(2) 2_655 ?
Tb2 O2 2.389(2) . ?
Tb2 O4 2.411(2) 2_655 ?
Tb2 O4 2.411(2) . ?
Tb1 I2 3.0284(5) . ?
Tb1 I2 3.0285(5) 5_566 ?
Tb1 I1 3.0074(6) 5_566 ?
Tb1 I1 3.0073(6) . ?
Tb1 O1 2.321(2) . ?
Tb1 O1 2.321(2) 5_566 ?
O3 C13 1.469(4) . ?
O3 C13 1.469(4) 2_655 ?
O2 C5 1.469(4) . ?
O2 C8 1.470(4) . ?
O1 C1 1.460(4) . ?
O1 C4 1.480(4) . ?
O4 C12 1.468(4) . ?
O4 C9 1.475(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.511(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C11 1.499(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C7 1.511(5) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.512(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.530(6) . ?
C2 C1 1.499(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.536(5) . ?
C14 C14 1.532(7) 2_655 ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.519(6) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C6 1.516(6) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.516(7) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?

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
I3 Tb2 I3 179.322(12) 2_655 . ?
O3 Tb2 I3 90.340(6) . . ?
O3 Tb2 I3 90.339(6) . 2_655 ?
O3 Tb2 O4 71.75(6) . 2_655 ?
O3 Tb2 O4 71.75(6) . . ?
O2 Tb2 I3 88.83(6) 2_655 . ?
O2 Tb2 I3 90.63(6) 2_655 2_655 ?
O2 Tb2 I3 90.63(6) . . ?
O2 Tb2 I3 88.83(6) . 2_655 ?
O2 Tb2 O3 143.68(6) 2_655 . ?
O2 Tb2 O3 143.68(6) . . ?
O2 Tb2 O2 72.64(11) 2_655 . ?
O2 Tb2 O4 71.95(8) . 2_655 ?
O2 Tb2 O4 144.54(8) . . ?
O2 Tb2 O4 144.54(8) 2_655 2_655 ?
O2 Tb2 O4 71.95(8) 2_655 . ?
O4 Tb2 I3 90.50(6) 2_655 2_655 ?
O4 Tb2 I3 89.71(6) . 2_655 ?
O4 Tb2 I3 90.50(6) . . ?
O4 Tb2 I3 89.71(6) 2_655 . ?
O4 Tb2 O4 143.50(12) 2_655 . ?
I2 Tb1 I2 180.0 . 5_566 ?
I1 Tb1 I2 88.523(13) 5_566 . ?
I1 Tb1 I2 91.476(13) 5_566 5_566 ?
I1 Tb1 I2 91.478(13) . . ?
I1 Tb1 I2 88.522(13) . 5_566 ?
I1 Tb1 I1 180.0 . 5_566 ?
O1 Tb1 I2 93.34(6) . 5_566 ?
O1 Tb1 I2 86.66(6) . . ?
O1 Tb1 I2 93.34(6) 5_566 . ?
O1 Tb1 I2 86.66(6) 5_566 5_566 ?
O1 Tb1 I1 88.76(6) 5_566 . ?
O1 Tb1 I1 91.24(6) . . ?
O1 Tb1 I1 88.75(6) . 5_566 ?
O1 Tb1 I1 91.25(6) 5_566 5_566 ?
O1 Tb1 O1 180.00(11) 5_566 . ?
C13 O3 Tb2 125.21(17) 2_655 . ?
C13 O3 Tb2 125.21(17) . . ?
C13 O3 C13 109.6(3) 2_655 . ?
C5 O2 Tb2 127.5(2) . . ?
C5 O2 C8 109.2(2) . . ?
C8 O2 Tb2 123.28(18) . . ?
C1 O1 Tb1 121.3(2) . . ?
C1 O1 C4 107.6(3) . . ?
C4 O1 Tb1 129.8(2) . . ?
C12 O4 Tb2 124.7(2) . . ?
C12 O4 C9 108.8(3) . . ?
C9 O4 Tb2 126.4(2) . . ?
O2 C5 H5A 110.8 . . ?
O2 C5 H5B 110.8 . . ?
O2 C5 C6 104.8(3) . . ?
H5A C5 H5B 108.9 . . ?
C6 C5 H5A 110.8 . . ?
C6 C5 H5B 110.8 . . ?
O4 C12 H12A 110.8 . . ?
O4 C12 H12B 110.8 . . ?
O4 C12 C11 104.8(3) . . ?
H12A C12 H12B 108.9 . . ?
C11 C12 H12A 110.8 . . ?
C11 C12 H12B 110.8 . . ?
O2 C8 H8A 110.8 . . ?
O2 C8 H8B 110.8 . . ?
O2 C8 C7 104.9(3) . . ?
H8A C8 H8B 108.8 . . ?
C7 C8 H8A 110.8 . . ?
C7 C8 H8B 110.8 . . ?
O3 C13 H13A 110.8 . . ?
O3 C13 H13B 110.8 . . ?
O3 C13 C14 104.9(3) . . ?
H13A C13 H13B 108.8 . . ?
C14 C13 H13A 110.8 . . ?
C14 C13 H13B 110.8 . . ?
H2A C2 H2B 109.4 . . ?
C3 C2 H2A 111.6 . . ?
C3 C2 H2B 111.6 . . ?
C1 C2 H2A 111.6 . . ?
C1 C2 H2B 111.6 . . ?
C1 C2 C3 101.1(3) . . ?
C2 C3 H3A 111.1 . . ?
C2 C3 H3B 111.1 . . ?
C2 C3 C4 103.3(3) . . ?
H3A C3 H3B 109.1 . . ?
C4 C3 H3A 111.1 . . ?
C4 C3 H3B 111.1 . . ?
C13 C14 C14 102.3(2) . 2_655 ?
C13 C14 H14A 111.3 . . ?
C13 C14 H14B 111.3 . . ?
C14 C14 H14A 111.3 2_655 . ?
C14 C14 H14B 111.3 2_655 . ?
H14A C14 H14B 109.2 . . ?
O1 C1 C2 104.5(3) . . ?
O1 C1 H1A 110.9 . . ?
O1 C1 H1B 110.9 . . ?
C2 C1 H1A 110.9 . . ?
C2 C1 H1B 110.9 . . ?
H1A C1 H1B 108.9 . . ?
O4 C9 H9A 110.7 . . ?
O4 C9 H9B 110.7 . . ?
O4 C9 C10 105.2(3) . . ?
H9A C9 H9B 108.8 . . ?
C10 C9 H9A 110.7 . . ?
C10 C9 H9B 110.7 . . ?
O1 C4 C3 105.5(3) . . ?
O1 C4 H4A 110.6 . . ?
O1 C4 H4B 110.6 . . ?
C3 C4 H4A 110.6 . . ?
C3 C4 H4B 110.6 . . ?
H4A C4 H4B 108.8 . . ?
C8 C7 H7A 111.4 . . ?
C8 C7 H7B 111.4 . . ?
C8 C7 C6 102.1(3) . . ?
H7A C7 H7B 109.2 . . ?
C6 C7 H7A 111.4 . . ?
C6 C7 H7B 111.4 . . ?
C12 C11 H11A 111.3 . . ?
C12 C11 H11B 111.3 . . ?
C12 C11 C10 102.4(3) . . ?
H11A C11 H11B 109.2 . . ?
C10 C11 H11A 111.3 . . ?
C10 C11 H11B 111.3 . . ?
C5 C6 C7 103.0(3) . . ?
C5 C6 H6A 111.2 . . ?
C5 C6 H6B 111.2 . . ?
C7 C6 H6A 111.2 . . ?
C7 C6 H6B 111.2 . . ?
H6A C6 H6B 109.1 . . ?
C9 C10 H10A 111.1 . . ?
C9 C10 H10B 111.1 . . ?
C11 C10 C9 103.4(3) . . ?
C11 C10 H10A 111.1 . . ?
C11 C10 H10B 111.1 . . ?
H10A C10 H10B 109.0 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id TbI3THF3
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_lp-230517_01
_database_code_depnum_ccdc_archive 'CCDC 1897952'
loop_
_audit_author_name
_audit_author_address
'John Bacsa'
;Emory University
United States of America
;
_audit_update_record             
;
2019-02-18 deposited with the CCDC.	2019-04-29 downloaded from the CCDC.
;
_audit_creation_date             2017-06-02
_audit_creation_method           
;
Olex2 1.2-dev
(compiled 2017.05.11 svn.r3410 for OlexSys, GUI svn.r5338)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H30 I3 O3 Pr'
_chemical_formula_sum            'C12 H30 I3 O3 Pr'
_chemical_formula_weight         743.97
_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'
I I -0.4742 1.8119 '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      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, z-1/2'

_cell_length_a                   10.1152(4)
_cell_length_b                   13.9216(7)
_cell_length_c                   15.8716(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2235.04(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.459
_cell_measurement_theta_min      2.567
_shelx_estimated_absorpt_T_max   0.484
_shelx_estimated_absorpt_T_min   0.224
_exptl_absorpt_coefficient_mu    6.325
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1307 before and 0.0784 after correction. The Ratio of minimum to maximum transmission is 0.4993. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.211
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.332
_exptl_crystal_size_min          0.134
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40923
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.513
_diffrn_reflns_theta_min         2.489
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_voltage           50
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2762
_reflns_number_total             3418
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.100
_refine_diff_density_min         -1.047
_refine_diff_density_rms         0.188
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         3418
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0255
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0337P)²+5.8540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0653
_refine_ls_wR_factor_ref         0.0747
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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 0.5000 0.62877(2) 0.2500 0.01242(7) Uani 1 2 d S T P . .
I1 I 0.72167(2) 0.62538(2) 0.11688(2) 0.02093(7) Uani 1 1 d . . . . .
I2 I 0.5000 0.41011(2) 0.2500 0.02237(9) Uani 1 2 d S T P . .
O1 O 0.5000 0.8099(3) 0.2500 0.0186(7) Uani 1 2 d S T P . .
O2 O 0.6596(2) 0.64166(17) 0.36179(16) 0.0180(5) Uani 1 1 d . . . . .
C3 C 0.6535(4) 0.5797(2) 0.4360(2) 0.0204(7) Uani 1 1 d . . . . .
H3A H 0.7388 0.5455 0.4421 0.024 Uiso 1 1 calc R . . . .
H3B H 0.5836 0.5309 0.4275 0.024 Uiso 1 1 calc R . . . .
C5 C 0.7707(3) 0.7093(3) 0.3607(2) 0.0193(7) Uani 1 1 d . . . . .
H5A H 0.7661 0.7504 0.4116 0.023 Uiso 1 1 calc R . . . .
H5B H 0.7625 0.7515 0.3108 0.023 Uiso 1 1 calc R . . . .
C1 C 0.4201(4) 0.8685(3) 0.3068(3) 0.0231(7) Uani 1 1 d . . . . .
H1A H 0.3373 0.8340 0.3206 0.028 Uiso 1 1 calc R . . . .
H1B H 0.3963 0.9294 0.2784 0.028 Uiso 1 1 calc R . . . .
C2 C 0.4945(5) 0.8903(3) 0.3869(3) 0.0309(9) Uani 1 1 d . . . . .
H2A H 0.5097 0.8306 0.4181 0.046 Uiso 1 1 calc GR . . . .
H2B H 0.4425 0.9346 0.4216 0.046 Uiso 1 1 calc GR . . . .
H2C H 0.5796 0.9200 0.3730 0.046 Uiso 1 1 calc GR . . . .
C4 C 0.6252(5) 0.6344(3) 0.5158(3) 0.0296(9) Uani 1 1 d . . . . .
H4A H 0.6965 0.6806 0.5262 0.044 Uiso 1 1 calc GR . . . .
H4B H 0.6194 0.5895 0.5632 0.044 Uiso 1 1 calc GR . . . .
H4C H 0.5412 0.6689 0.5100 0.044 Uiso 1 1 calc GR . . . .
C6 C 0.9025(4) 0.6600(3) 0.3584(3) 0.0287(8) Uani 1 1 d . . . . .
H6A H 0.9180 0.6273 0.4122 0.043 Uiso 1 1 calc GR . . . .
H6B H 0.9722 0.7076 0.3488 0.043 Uiso 1 1 calc GR . . . .
H6C H 0.9033 0.6127 0.3126 0.043 Uiso 1 1 calc GR . . . .


_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 I1 3.0812(2) 4_655 ?
Pr1 I1 3.0812(2) . ?
Pr1 I2 3.0441(4) . ?
Pr1 O1 2.521(4) . ?
Pr1 O2 2.406(2) 4_655 ?
Pr1 O2 2.406(2) . ?
O1 C1 1.460(4) . ?
O1 C1 1.460(4) 4_655 ?
O2 C3 1.461(4) . ?
O2 C5 1.466(4) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.506(5) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C5 C6 1.501(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.509(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?

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
I1 Pr1 I1 178.248(12) 4_655 . ?
I2 Pr1 I1 89.124(6) . . ?
I2 Pr1 I1 89.124(6) . 4_655 ?
O1 Pr1 I1 90.876(6) . . ?
O1 Pr1 I1 90.876(6) . 4_655 ?
O1 Pr1 I2 180.0 . . ?
O2 Pr1 I1 91.06(6) . . ?
O2 Pr1 I1 91.06(6) 4_655 4_655 ?
O2 Pr1 I1 89.08(6) . 4_655 ?
O2 Pr1 I1 89.07(6) 4_655 . ?
O2 Pr1 I2 94.28(6) 4_655 . ?
O2 Pr1 I2 94.28(6) . . ?
O2 Pr1 O1 85.72(6) 4_655 . ?
O2 Pr1 O1 85.72(6) . . ?
O2 Pr1 O2 171.45(12) . 4_655 ?
C1 O1 Pr1 124.01(19) . . ?
C1 O1 Pr1 124.01(19) 4_655 . ?
C1 O1 C1 112.0(4) 4_655 . ?
C3 O2 Pr1 121.5(2) . . ?
C3 O2 C5 114.9(3) . . ?
C5 O2 Pr1 123.6(2) . . ?
O2 C3 H3A 109.0 . . ?
O2 C3 H3B 109.0 . . ?
O2 C3 C4 112.8(3) . . ?
H3A C3 H3B 107.8 . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
O2 C5 H5A 109.0 . . ?
O2 C5 H5B 109.0 . . ?
O2 C5 C6 112.7(3) . . ?
H5A C5 H5B 107.8 . . ?
C6 C5 H5A 109.0 . . ?
C6 C5 H5B 109.0 . . ?
O1 C1 H1A 109.5 . . ?
O1 C1 H1B 109.5 . . ?
O1 C1 C2 110.9(3) . . ?
H1A C1 H1B 108.0 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?

_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id LP-230517
_olex2_submission_special_instructions 'No special instructions were received'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
