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

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

data_1-Tb
_database_code_depnum_ccdc_archive 'CCDC 1844350'
_audit_update_record             
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;

_manchester_internal_coll_name   rdpm80
_manchester_internal_coll_client CAPG/FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 2s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   18/11/17
_manchester_internal_process_user CAPG/FO
_manchester_internal_process_date 20/11/17
_manchester_internal_solution_user CAPG/FO
_manchester_internal_solution_date 20/11/17
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 20/11/17
_manchester_internal_validation_user FO
_manchester_internal_validation_date 20/11/17
_manchester_internal_archive_date 20/11/17

_refine_special_details          
;
The site occupied by one of the BH4 groups was found to be partially occupied
by iodine. THerefore, the BH4 and I groups were refined competitively,
converging at a ratio of 0.818(2):0.182(2). Similarity restraints were
applied to the atoms within the disorder components. Additionally, all the
BH distances were constrained to 1.1A and the displacement parameters of the
hydrogen atoms fixed to 1.5x their parent atom (B).

Finally, enhanced rigid bond restraints were applied globally.
;


_audit_creation_date             2017-11-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        '[Tb(BH4)3(THF)3]'
_chemical_formula_moiety         'C12 H34.54 B2.64 I0.36 O3 Tb'
_chemical_formula_sum            'C12 H34.54 B2.63 I0.37 O3 Tb'
_chemical_formula_weight         460.66
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     FO/CAPG
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'
B B 0.0013 0.0007 '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                   9.1844(2)
_cell_length_b                   14.3006(3)
_cell_length_c                   14.7076(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1931.72(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8710
_cell_measurement_temperature    149.95(10)
_cell_measurement_theta_max      29.8080
_cell_measurement_theta_min      2.1950
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.244
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 -8 0 0.1820
-7 -16 1 0.1753
5 -18 1 0.1673
-2 20 -1 0.1735
-13 5 0 0.2017
11 2 -10 0.1237
10 -6 -10 0.1136
-11 5 11 0.1458
-6 -17 4 0.1681
4 13 15 0.1912
-1 4 -20 0.2021
3 19 -7 0.1481
4 19 1 0.1537
-3 -19 4 0.1382
-6 -11 -14 0.1985
-8 10 -13 0.2296
-11 10 -2 0.2065
-9 10 12 0.1310
-10 2 12 0.1489
-3 5 20 0.1215
5 -14 13 0.1760
9 10 11 0.2171
8 -6 15 0.2104
8 14 8 0.2013
9 3 -15 0.1053
8 -5 -15 0.0991
5 -14 -12 0.1523
6 6 -18 0.1280
4 -6 -19 0.1255
-5 9 17 0.1202
1 -4 20 0.1603
3 12 16 0.1847

_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.493
_exptl_crystal_size_mid          0.293
_exptl_crystal_size_min          0.242
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
12.0000 -8.0000 -0.0000 -0.3487 -0.9371 -0.1287
-7.0000 -16.0000 1.0000 0.1045 0.2856 -0.9123
5.0000 -18.0000 1.0000 -0.2286 -0.5708 -0.7550
-2.0000 20.0000 -1.0000 0.1518 0.3903 0.9135
-13.0000 5.0000 0.0000 0.3682 0.9658 -0.0354
11.0000 2.0000 -10.0000 0.1550 -0.9041 0.3503
10.0000 -6.0000 -10.0000 0.1615 -0.9426 -0.0521
-11.0000 5.0000 11.0000 -0.1818 1.0153 -0.0190
-6.0000 -17.0000 4.0000 -0.0605 0.2542 -0.9459
4.0000 13.0000 15.0000 -0.7510 0.1545 0.6687
-1.0000 4.0000 -20.0000 0.9385 -0.2184 0.2164
3.0000 19.0000 -7.0000 0.2828 -0.0711 0.9851
4.0000 19.0000 1.0000 -0.1048 -0.0037 0.9875
-3.0000 -19.0000 4.0000 -0.1477 0.0199 -0.9781
-6.0000 -11.0000 -14.0000 0.7658 0.0278 -0.6178
-8.0000 10.0000 -13.0000 0.8301 0.4657 0.3386
-11.0000 10.0000 -2.0000 0.4167 0.8607 0.2497
-9.0000 10.0000 12.0000 -0.2685 0.9614 0.2591
-10.0000 2.0000 12.0000 -0.2620 0.9229 -0.1433
-3.0000 5.0000 20.0000 -0.8058 0.6160 0.1283
5.0000 -14.0000 13.0000 -0.7586 -0.3121 -0.5925
9.0000 10.0000 11.0000 -0.7153 -0.2998 0.6403
8.0000 -6.0000 15.0000 -0.9098 -0.3777 -0.1527
8.0000 14.0000 8.0000 -0.5424 -0.2280 0.8170
9.0000 3.0000 -15.0000 0.4375 -0.8377 0.3676
8.0000 -5.0000 -15.0000 0.4440 -0.8762 -0.0348
5.0000 -14.0000 -12.0000 0.3674 -0.7388 -0.5339
6.0000 6.0000 -18.0000 0.6624 -0.6412 0.4544
4.0000 -6.0000 -19.0000 0.7308 -0.6815 -0.1573
-5.0000 9.0000 17.0000 -0.6056 0.7568 0.2839
1.0000 -4.0000 20.0000 -0.9385 0.2184 -0.2164
3.0000 12.0000 16.0000 -0.7713 0.2272 0.5977

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12868
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.849
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.95(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -6.00  21.00   0.50    2.00    --   -7.80  21.00 -15.00   54
  2  ω    -43.00 -18.00   0.50    2.00    --   -7.80 -21.00 178.00   50
  3  ω    -94.00  31.00   0.50    2.00    --   -7.80 -38.00  30.00  250
  4  ω    -39.00  58.00   0.50    2.00    --   -7.80  57.00-150.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0273237000
_diffrn_orient_matrix_UB_12      0.0026061000
_diffrn_orient_matrix_UB_13      -0.0450381000
_diffrn_orient_matrix_UB_21      -0.0691189000
_diffrn_orient_matrix_UB_22      0.0134569000
_diffrn_orient_matrix_UB_23      0.0170663000
_diffrn_orient_matrix_UB_31      0.0210514000
_diffrn_orient_matrix_UB_32      0.0476628000
_diffrn_orient_matrix_UB_33      -0.0023407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1731
_reflns_number_total             1762
_reflns_odcompleteness_completeness 99.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.276
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1762
_refine_ls_number_restraints     113
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0267
_refine_ls_restrained_S_all      1.307
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+6.1771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0537
_refine_ls_wR_factor_ref         0.0539

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All I(H) groups
2. Restrained distances
 B2-H2A = B2-H2B
 1.1 with sigma of 0.02
 B1-H1D = B1-H1A = B1-H1B = B1-H1C
 1.1 with sigma of 0.02
 H1D-H1A
 1.5 with sigma of 0.02
 H1D-H1C
 1.5 with sigma of 0.02
 H1A-H1B
 1.5 with sigma of 0.02
 H1D-H1B
 1.5 with sigma of 0.02
 Tb1-B1 \\sim Tb1-B2
 with sigma of 0.02
 Tb1-H1B \\sim Tb1-H1A \\sim Tb1-H1D
 with sigma of 0.02
 H1C-H1A \\sim H1C-H1B \\sim H1C-H1D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B1 \\sim I2A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(I2A)=1-FVAR(1)
 Sof(H1A)=Sof(H1B)=Sof(H1D)=Sof(B1)=Sof(H1C)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1E,H1F), C2(H2C,H2D), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.500000 0.15286(2) 0.750000 0.02606(10) Uani 1 2 d DS TU P . .
H1A H 0.405(3) 0.176(3) 0.6016(17) 0.059(19) Uiso 0.8179(16) 1 d D . . A 1
H1B H 0.320(4) 0.0959(15) 0.648(3) 0.07(2) Uiso 0.8179(16) 1 d D . . A 1
H1D H 0.285(3) 0.197(3) 0.671(2) 0.07(2) Uiso 0.8179(16) 1 d D . . A 1
O1 O 0.6918(3) 0.11988(18) 0.64833(17) 0.0299(6) Uani 1 1 d . U . . .
O2 O 0.500000 -0.0174(2) 0.750000 0.0351(9) Uani 1 2 d S TU P A .
C1 C 0.7105(5) 0.1570(4) 0.5560(3) 0.0458(12) Uani 1 1 d . U . . .
H1E H 0.703374 0.224711 0.556230 0.055 Uiso 1 1 calc R . . . .
H1F H 0.636392 0.132170 0.515722 0.055 Uiso 1 1 calc R . . . .
C2 C 0.8593(5) 0.1267(4) 0.5257(3) 0.0490(12) Uani 1 1 d . U . . .
H2C H 0.859073 0.110137 0.461717 0.059 Uiso 1 1 calc R . . . .
H2D H 0.930261 0.175822 0.535668 0.059 Uiso 1 1 calc R . . . .
C3 C 0.8920(6) 0.0431(4) 0.5836(3) 0.0524(13) Uani 1 1 d . U . . .
H3A H 0.852487 -0.013425 0.556700 0.063 Uiso 1 1 calc R . . . .
H3B H 0.996175 0.035409 0.591646 0.063 Uiso 1 1 calc R . . . .
C4 C 0.8201(5) 0.0642(3) 0.6710(3) 0.0437(11) Uani 1 1 d . U . . .
H4A H 0.791929 0.006908 0.701657 0.052 Uiso 1 1 calc R . . . .
H4B H 0.884972 0.099112 0.710455 0.052 Uiso 1 1 calc R . . . .
C5 C 0.5178(6) -0.0774(3) 0.8293(3) 0.0514(12) Uani 1 1 d . U . . .
H5A H 0.455217 -0.056898 0.878525 0.062 Uiso 1 1 calc R . . A .
H5B H 0.617970 -0.076582 0.850179 0.062 Uiso 1 1 calc R . . . .
C6 C 0.4758(7) -0.1731(3) 0.7982(4) 0.0683(17) Uani 1 1 d . U . . .
H6A H 0.525729 -0.220985 0.833017 0.082 Uiso 1 1 calc R . . . .
H6B H 0.371571 -0.182752 0.802877 0.082 Uiso 1 1 calc R . . . .
B2 B 0.500000 0.3440(4) 0.750000 0.0320(13) Uani 1 2 d DS TU P A .
H2B H 0.567(6) 0.392(3) 0.788(4) 0.10(2) Uiso 1 1 d D . . . .
B1 B 0.302(2) 0.1566(10) 0.6157(11) 0.036(4) Uani 0.8179(16) 1 d D U . A 1
H1C H 0.225(3) 0.163(2) 0.571(2) 0.08(2) Uiso 0.8179(16) 1 d D . . A 1
I2A I 0.3051(5) 0.1324(3) 0.5984(3) 0.0401(10) Uani 0.1821(16) 1 d . U . A 2
H2A H 0.440(5) 0.298(3) 0.794(3) 0.060 Uiso 1 1 d DR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.358(3) 4_656 ?
Tb1 O1 2.358(2) . ?
Tb1 O2 2.434(3) . ?
Tb1 B2 2.733(6) . ?
Tb1 B1 2.686(14) . ?
Tb1 B1 2.686(14) 4_656 ?
Tb1 I2A 2.874(4) . ?
Tb1 I2A 2.874(4) 4_656 ?
O1 C1 1.468(4) . ?
O1 C4 1.461(5) . ?
O2 C5 1.457(5) . ?
O2 C5 1.457(5) 4_656 ?
C1 C2 1.502(6) . ?
C2 C3 1.498(7) . ?
C3 C4 1.477(6) . ?
C5 C6 1.494(7) . ?
C6 C6 1.485(12) 4_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 156.93(13) 4_656 . ?
O1 Tb1 O2 78.47(6) . . ?
O1 Tb1 O2 78.47(6) 4_656 . ?
O1 Tb1 B2 101.53(6) 4_656 . ?
O1 Tb1 B2 101.53(6) . . ?
O1 Tb1 B1 92.5(4) 4_656 4_656 ?
O1 Tb1 B1 88.0(5) 4_656 . ?
O1 Tb1 B1 88.0(5) . 4_656 ?
O1 Tb1 B1 92.5(4) . . ?
O1 Tb1 I2A 90.36(12) 4_656 . ?
O1 Tb1 I2A 90.36(12) . 4_656 ?
O1 Tb1 I2A 87.31(12) 4_656 4_656 ?
O1 Tb1 I2A 87.31(12) . . ?
O2 Tb1 B2 180.0 . . ?
O2 Tb1 B1 91.1(3) . . ?
O2 Tb1 B1 91.1(3) . 4_656 ?
O2 Tb1 I2A 84.17(8) . 4_656 ?
O2 Tb1 I2A 84.17(8) . . ?
B2 Tb1 I2A 95.83(8) . 4_656 ?
B2 Tb1 I2A 95.83(8) . . ?
B1 Tb1 B2 88.9(3) 4_656 . ?
B1 Tb1 B2 88.9(3) . . ?
B1 Tb1 B1 177.7(6) . 4_656 ?
B1 Tb1 I2A 8.0(3) 4_656 4_656 ?
B1 Tb1 I2A 173.9(5) . 4_656 ?
I2A Tb1 I2A 168.34(17) . 4_656 ?
C1 O1 Tb1 127.0(2) . . ?
C4 O1 Tb1 124.5(2) . . ?
C4 O1 C1 108.3(3) . . ?
C5 O2 Tb1 126.1(2) . . ?
C5 O2 Tb1 126.1(2) 4_656 . ?
C5 O2 C5 107.8(4) . 4_656 ?
O1 C1 C2 106.1(3) . . ?
C3 C2 C1 104.2(4) . . ?
C4 C3 C2 104.0(4) . . ?
O1 C4 C3 105.9(3) . . ?
O2 C5 C6 105.4(4) . . ?
C6 C6 C5 102.4(4) 4_656 . ?

_olex2_exptl_crystal_mounting_method 'in fomblin oil on micromount'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.132
_oxdiff_exptl_absorpt_empirical_full_min 0.646
_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_1-Y
_database_code_depnum_ccdc_archive 'CCDC 1844351'
_audit_update_record             
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;

_manchester_internal_coll_name   xdpm42
_manchester_internal_coll_client FO/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 5s
_manchester_internal_coll_frame_width 1
_manchester_internal_coll_frame_method '\w and \p scans'
_manchester_internal_coll_user   FO
_manchester_internal_coll_date   12/08/2015
_manchester_internal_process_user FO
_manchester_internal_process_date 13/08/2015
_manchester_internal_solution_user FO
_manchester_internal_solution_date 13/08/2015
_manchester_internal_refinement_user FO
_manchester_internal_refinement_date 18/05/2018
_manchester_internal_validation_user FO
_manchester_internal_validation_date 18/05/2018
_manchester_internal_archive_date 18/05/2018

# start Validation Reply Form
_vrf_PLAT973_1-Y                 
;
PROBLEM: Check Calcd Positive Residual Density on      Y1       1.76 eA-3  
RESPONSE: The model does not show any inconsistencies and the presence of
          twinning component has been checked. Therefore, the residual
          density is likely to be due to imperfections in the absorption
          corrections.
;
# end Validation Reply Form



_refine_special_details          
;
The positions of the hydrogen atoms of the BH4 fragments were identified in 
the difmap. The B-H distances were restrained and their displacement 
parameters fixed at 1.2 with respect to B.

Disorder was identified around two of the B centres. These were found to be
partially occupied by iodine, due to the employment of YI3 as a starting 
material.The occupancies of the boron and iodine atoms were refined 
competitively, converging at a ratio of 0.816(3):0.184(3) and 
0.790(3):0.210(3) respectively. Additionally the Y-I and Y-B distances were 
restrained to be approximately
equal.

Furthermore, positional disorder was identified around atom C2 of one of the
coordinated THF molecules. This was modelled over two positions and the two
components refined competitively, converging at a ratio of 0.51(2):0.49(2).
Chemically equivalent bonds of the disordered THF molecule were restrianed
to be approximately equal.

Finally restraints were applied to the anisotropic displacement parameters.
;

_audit_creation_date             2018-05-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_shelx_SHELXL_version_number     2018/1
loop_
_audit_author_email
david.mills@manchester.ac.uk
fabrizio.ortu@manchester.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        '[Y(BH4)3(THF)3]'
_chemical_formula_moiety         'C12 H34.42 B2.61 I0.39 O3 Y'
_chemical_formula_sum            'C12 H34.42 B2.61 I0.40 O3 Y'
_chemical_formula_weight         394.01
_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 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -0.2670 2.0244 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.9188(2)
_cell_length_b                   12.5674(3)
_cell_length_c                   16.2017(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.122(2)
_cell_angle_gamma                90
_cell_volume                     1815.64(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11904
_cell_measurement_temperature    150.11(2)
_cell_measurement_theta_max      74.5737
_cell_measurement_theta_min      2.7256
_shelx_estimated_absorpt_T_max   0.909
_shelx_estimated_absorpt_T_min   0.828
_exptl_absorpt_coefficient_mu    9.781
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1426
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27112
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         4.453
_diffrn_ambient_temperature      150.11(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   60.71  247.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.8669  249.2094 187

#__ type_ start__ end____ width___ exp.time_
  2 omega   50.71  237.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       80.0000   73.8669  114.2094 187

#__ type_ start__ end____ width___ exp.time_
  3 phi   -205.79  153.43   1.0006    5.0000
omega____ theta____ kappa____ phi______ frames
 128.8997  110.5000   73.8669     -     359

#__ type_ start__ end____ width___ exp.time_
  4 omega   81.21  268.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8669    4.2094 187

#__ type_ start__ end____ width___ exp.time_
  5 omega  -13.14  161.86   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       15.0000   73.8669   19.2094 175

#__ type_ start__ end____ width___ exp.time_
  6 phi     51.88  326.22   1.0012    5.0000
omega____ theta____ kappa____ phi______ frames
 224.2097  111.0000   73.8669     -     274

#__ type_ start__ end____ width___ exp.time_
  7 omega   80.71  267.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8669  314.2094 187

#__ type_ start__ end____ width___ exp.time_
  8 omega   30.71  217.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       60.0000   73.8669  -20.7900 187

#__ type_ start__ end____ width___ exp.time_
  9 omega   80.71  267.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8669   54.2081 187

#__ type_ start__ end____ width___ exp.time_
 10 omega   81.83  192.80   0.9997    5.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   73.8669  254.2100 111

#__ type_ start__ end____ width___ exp.time_
 11 omega   60.71  247.71   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       90.0000   73.8669   29.2100 187

#__ type_ start__ end____ width___ exp.time_
 12 omega   83.21  268.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  194.2088 185

#__ type_ start__ end____ width___ exp.time_
 13 omega   68.21  153.21   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   73.8669  279.2081 85

#__ type_ start__ end____ width___ exp.time_
 14 omega  106.91  183.91   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  319.2094 77

#__ type_ start__ end____ width___ exp.time_
 15 omega   83.30  172.30   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      113.0000   73.8669  169.2088 89

#__ type_ start__ end____ width___ exp.time_
 16 omega  110.03  232.03   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   73.8669  184.2094 122

#__ type_ start__ end____ width___ exp.time_
 17 omega  -91.38   84.62   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -70.0000   73.8669  104.2088 176

#__ type_ start__ end____ width___ exp.time_
 18 omega   71.24  254.24   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      100.0000   73.8669  234.2081 183

#__ type_ start__ end____ width___ exp.time_
 19 omega  -58.78  119.22   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -30.0000   73.8669  124.2088 178
;
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and π scans'
_diffrn_orient_matrix_UB_11      -0.0852507000
_diffrn_orient_matrix_UB_12      0.0207515000
_diffrn_orient_matrix_UB_13      -0.0819751000
_diffrn_orient_matrix_UB_21      0.1273353000
_diffrn_orient_matrix_UB_22      -0.0536174000
_diffrn_orient_matrix_UB_23      -0.0474988000
_diffrn_orient_matrix_UB_31      -0.0796743000
_diffrn_orient_matrix_UB_32      -0.1083621000
_diffrn_orient_matrix_UB_33      0.0078451000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2578
_reflns_number_total             3328
_reflns_odcompleteness_completeness 97.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.57
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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    ?
_refine_diff_density_max         2.009
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.226
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         3328
_refine_ls_number_restraints     277
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0715
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0872P)²+10.0720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1690
_refine_ls_wR_factor_ref         0.1882

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All C(H,H,H,H,H,H,H,H,H,H) groups,
   All I(H,H,H,H) groups
2. Restrained distances
 B2-H2D = B2-H2C = B2-H2E = B2-H2F
 1 with sigma of 0.008
 B3-H3A = B3-H3C = B3-H3D = B3-H3B
 1 with sigma of 0.02
 Y1-B2 \\sim Y1-B3 \\sim Y1-B1
 with sigma of 0.02
 H1D-H1A \\sim H1D-H1B \\sim H1D-H1C
 with sigma of 0.02
 H1A-H1B \\sim H1A-H1C \\sim H1B-H1C
 with sigma of 0.02
 C2-C1 \\sim C2A-C1 \\sim C4-C3 \\sim C6-C5 \\sim C8-C7 \\sim C12-C11 \\sim
C9-C10
 with sigma of 0.02
 C3-C2A \\sim C3-C2 \\sim C7-C6 \\sim C11-C10
 with sigma of 0.02
 H2C-H2D \\sim H2C-H2E \\sim H2C-H2F \\sim H2D-H2E \\sim H2D-H2F \\sim H2E-H2F
 with sigma of 0.02
 I3-Y1 \\sim I2-Y1
 with sigma of 0.02
 H3A-H3B \\sim H3A-H3C \\sim H3A-H3D \\sim H3B-H3C \\sim H3B-H3D \\sim H3C-H3D
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
B3 \\sim I3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(I2)=1-FVAR(1)
 Sof(B2)=Sof(H2C)=Sof(H2D)=Sof(H2E)=Sof(H2F)=FVAR(1)
 Sof(I3)=1-FVAR(2)
 Sof(B3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(H3D)=FVAR(2)
 Sof(H1BC)=Sof(H1BD)=Sof(H3BC)=Sof(H3BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(3)
 Sof(H1AA)=Sof(H1AB)=Sof(H3AA)=Sof(H3AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=FVAR(3)
 Fixed U11: Y1(0.025014)
 Fixed U12: Y1(-0.002091)
 Fixed U13: Y1(-0.001939)
 Fixed U22: Y1(0.02856)
 Fixed U23: Y1(0.00514)
 Fixed U33: Y1(0.02905)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4A,H4B),
 C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,
 H10B), C11(H11A,H11B), C12(H12A,H12B), C2(H2A,H2B), C2A(H2AA,H2AB)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.73908(7) 0.23265(5) 0.24004(4) 0.028 Uani 1 1 d D U . . .
O1 O 0.9166(6) 0.3196(5) 0.1637(3) 0.0398(13) Uani 1 1 d . U . . .
O2 O 0.7432(6) 0.3957(4) 0.3146(3) 0.0371(12) Uani 1 1 d . U . . .
O3 O 0.5515(6) 0.1996(4) 0.3344(3) 0.0342(11) Uani 1 1 d . U . . .
C1 C 0.9138(9) 0.3240(8) 0.0749(5) 0.044(2) Uani 1 1 d D U . . .
H1AA H 0.814878 0.344091 0.054316 0.053 Uiso 0.51(2) 1 calc R . P A 1
H1AB H 0.939693 0.255376 0.051799 0.053 Uiso 0.51(2) 1 calc R . P A 1
H1BC H 0.863543 0.387799 0.055018 0.053 Uiso 0.49(2) 1 calc R . P A 2
H1BD H 0.864172 0.262102 0.051266 0.053 Uiso 0.49(2) 1 calc R . P A 2
C3 C 1.1439(8) 0.3948(7) 0.1209(5) 0.0392(17) Uani 1 1 d D U . . .
H3AA H 1.213696 0.337917 0.108869 0.047 Uiso 0.51(2) 1 calc R . P A 1
H3AB H 1.199455 0.460510 0.128439 0.047 Uiso 0.51(2) 1 calc R . P A 1
H3BC H 1.248840 0.376701 0.129092 0.047 Uiso 0.49(2) 1 calc R . P A 2
H3BD H 1.135624 0.469521 0.106557 0.047 Uiso 0.49(2) 1 calc R . P A 2
C4 C 1.0554(8) 0.3693(7) 0.1957(5) 0.0415(18) Uani 1 1 d D U . . .
H4A H 1.110173 0.320691 0.231625 0.050 Uiso 1 1 calc R . . . .
H4B H 1.033096 0.433544 0.226315 0.050 Uiso 1 1 calc R . . . .
C5 C 0.7139(9) 0.5013(6) 0.2803(5) 0.0366(16) Uani 1 1 d D U . . .
H5A H 0.608858 0.508657 0.264564 0.044 Uiso 1 1 calc R . . . .
H5B H 0.774117 0.513352 0.231970 0.044 Uiso 1 1 calc R . . . .
C6 C 0.7550(11) 0.5785(7) 0.3471(5) 0.051(2) Uani 1 1 d D U . . .
H6A H 0.692941 0.641758 0.344102 0.061 Uiso 1 1 calc R . . . .
H6B H 0.859720 0.598923 0.344499 0.061 Uiso 1 1 calc R . . . .
C7 C 0.7247(18) 0.5147(8) 0.4239(6) 0.078(4) Uani 1 1 d D U . . .
H7A H 0.781470 0.542281 0.470863 0.094 Uiso 1 1 calc R . . . .
H7B H 0.618803 0.515797 0.436531 0.094 Uiso 1 1 calc R . . . .
C8 C 0.7741(14) 0.4059(7) 0.4029(5) 0.057(3) Uani 1 1 d D U . . .
H8A H 0.880228 0.396915 0.415106 0.068 Uiso 1 1 calc R . . . .
H8B H 0.718448 0.353259 0.433629 0.068 Uiso 1 1 calc R . . . .
C9 C 0.4213(10) 0.2688(8) 0.3449(5) 0.047(2) Uani 1 1 d D U . . .
H9A H 0.345430 0.254878 0.302616 0.056 Uiso 1 1 calc R . . . .
H9B H 0.450182 0.343093 0.342216 0.056 Uiso 1 1 calc R . . . .
C10 C 0.3638(11) 0.2415(7) 0.4295(5) 0.046(2) Uani 1 1 d D U . . .
H10A H 0.257198 0.255670 0.433135 0.055 Uiso 1 1 calc R . . . .
H10B H 0.417076 0.280708 0.472436 0.055 Uiso 1 1 calc R . . . .
C11 C 0.3968(8) 0.1225(6) 0.4350(5) 0.0365(16) Uani 1 1 d D U . . .
H11A H 0.400642 0.098670 0.491904 0.044 Uiso 1 1 calc R . . . .
H11B H 0.321866 0.081448 0.404681 0.044 Uiso 1 1 calc R . . . .
C12 C 0.5487(8) 0.1137(6) 0.3957(4) 0.0320(15) Uani 1 1 d D U . . .
H12A H 0.628471 0.122762 0.436653 0.038 Uiso 1 1 calc R . . . .
H12B H 0.560288 0.044929 0.369356 0.038 Uiso 1 1 calc R . . . .
B1 B 0.7372(11) 0.0546(8) 0.1624(6) 0.040(2) Uani 1 1 d D U . . .
C2 C 1.0270(15) 0.4059(14) 0.0523(8) 0.041(5) Uani 0.51(2) 1 d D U P A 1
H2A H 0.983502 0.476691 0.051544 0.050 Uiso 0.51(2) 1 calc R . P A 1
H2B H 1.069309 0.391045 -0.001200 0.050 Uiso 0.51(2) 1 calc R . P A 1
B2 B 0.951(3) 0.182(2) 0.3426(14) 0.033(7) Uani 0.816(3) 1 d D U P B 1
B3 B 0.552(3) 0.331(3) 0.1459(15) 0.030(5) Uani 0.790(3) 1 d D U P B 1
C2A C 1.0711(14) 0.3255(13) 0.0556(9) 0.038(4) Uani 0.49(2) 1 d D U P A 2
H2AA H 1.086025 0.354971 0.001024 0.046 Uiso 0.49(2) 1 calc R . P A 2
H2AB H 1.112583 0.254137 0.057421 0.046 Uiso 0.49(2) 1 calc R . P A 2
H1A H 0.840(8) 0.101(6) 0.157(5) 0.046 Uiso 1 1 d DR . . . .
H1B H 0.668(8) 0.113(6) 0.127(5) 0.046 Uiso 1 1 d DR . . . .
H1C H 0.706(9) 0.063(6) 0.216(4) 0.046 Uiso 1 1 d DR . . . .
H2C H 0.949(4) 0.230(5) 0.294(3) 0.046 Uiso 0.816(3) 1 d DR . P B 1
H2D H 0.848(4) 0.153(5) 0.351(3) 0.046 Uiso 0.816(3) 1 d DR . P B 1
H1D H 0.744(9) -0.012(8) 0.131(5) 0.046 Uiso 1 1 d DR . . . .
H2E H 1.022(7) 0.122(5) 0.333(5) 0.046 Uiso 0.816(3) 1 d DR . P B 1
H2F H 0.985(8) 0.223(6) 0.392(3) 0.046 Uiso 0.816(3) 1 d DR . P B 1
I3 I 0.5406(7) 0.3272(6) 0.1478(4) 0.0383(17) Uani 0.210(3) 1 d D U P B 2
I2 I 0.9449(7) 0.1785(7) 0.3458(4) 0.042(2) Uani 0.184(3) 1 d D U P B 2
H3A H 0.498(8) 0.281(6) 0.108(4) 0.051 Uiso 0.790(3) 1 d DR . P B 1
H3B H 0.617(8) 0.290(6) 0.185(4) 0.051 Uiso 0.790(3) 1 d DR . P B 1
H3C H 0.478(7) 0.373(4) 0.177(4) 0.051 Uiso 0.790(3) 1 d DR . P B 1
H3D H 0.615(5) 0.380(4) 0.113(4) 0.051 Uiso 0.790(3) 1 d DR . P B 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O1 2.304(5) . ?
Y1 O2 2.378(5) . ?
Y1 O3 2.325(5) . ?
Y1 B1 2.566(10) . ?
Y1 B2 2.572(18) . ?
Y1 B3 2.559(19) . ?
Y1 H1A 2.32(8) . ?
Y1 H1B 2.45(8) . ?
Y1 H1C 2.18(8) . ?
Y1 H2C 2.05(4) . ?
Y1 H2D 2.26(5) . ?
Y1 I3 2.583(4) . ?
Y1 I2 2.578(4) . ?
Y1 H3B 1.57(3) . ?
O1 C1 1.440(9) . ?
O1 C4 1.472(9) . ?
O2 C5 1.461(9) . ?
O2 C8 1.458(10) . ?
O3 C9 1.463(9) . ?
O3 C12 1.467(9) . ?
C1 H1AA 0.9700 . ?
C1 H1AB 0.9700 . ?
C1 H1BC 0.9700 . ?
C1 H1BD 0.9700 . ?
C1 C2 1.493(12) . ?
C1 C2A 1.444(13) . ?
C3 H3AA 0.9700 . ?
C3 H3AB 0.9700 . ?
C3 H3BC 0.9700 . ?
C3 H3BD 0.9700 . ?
C3 C4 1.494(9) . ?
C3 C2 1.515(13) . ?
C3 C2A 1.507(14) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.493(10) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C7 1.510(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.478(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.511(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.526(10) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.513(9) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
B1 H1A 1.09(7) . ?
B1 H1B 1.11(7) . ?
B1 H1C 0.92(7) . ?
B1 H1D 0.99(10) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
B2 H2C 0.999(8) . ?
B2 H2D 0.999(8) . ?
B2 H2E 1.000(8) . ?
B2 H2F 1.000(8) . ?
B3 H3A 0.99(2) . ?
B3 H3B 1.00(2) . ?
B3 H3C 0.99(2) . ?
B3 H3D 0.99(2) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Y1 O2 82.0(2) . . ?
O1 Y1 O3 161.5(2) . . ?
O1 Y1 B1 98.5(3) . . ?
O1 Y1 B2 87.7(7) . . ?
O1 Y1 B3 84.1(8) . . ?
O1 Y1 H1A 75.5(17) . . ?
O1 Y1 H1B 93.4(18) . . ?
O1 Y1 H1C 117.3(19) . . ?
O1 Y1 H2C 66.5(6) . . ?
O1 Y1 H2D 110.3(7) . . ?
O1 Y1 I3 86.7(2) . . ?
O1 Y1 I2 89.7(2) . . ?
O1 Y1 H3B 87(3) . . ?
O2 Y1 B1 178.7(3) . . ?
O2 Y1 B2 83.2(6) . . ?
O2 Y1 B3 83.6(8) . . ?
O2 Y1 H1A 154.8(16) . . ?
O2 Y1 H1B 155.7(15) . . ?
O2 Y1 H1C 158.6(18) . . ?
O2 Y1 H2C 78(2) . . ?
O2 Y1 H2D 88.4(19) . . ?
O2 Y1 I3 84.3(2) . . ?
O2 Y1 I2 83.5(2) . . ?
O2 Y1 H3B 84(3) . . ?
O3 Y1 O2 79.9(2) . . ?
O3 Y1 B1 99.7(3) . . ?
O3 Y1 B2 93.5(6) . . ?
O3 Y1 B3 90.5(7) . . ?
O3 Y1 H1A 123.0(17) . . ?
O3 Y1 H1B 101.8(18) . . ?
O3 Y1 H1C 81.2(19) . . ?
O3 Y1 H2C 112.5(10) . . ?
O3 Y1 H2D 72.6(10) . . ?
O3 Y1 I3 88.2(2) . . ?
O3 Y1 I2 91.6(2) . . ?
O3 Y1 H3B 87(3) . . ?
B1 Y1 B2 95.7(7) . . ?
B1 Y1 H1A 25.1(17) . . ?
B1 Y1 H1B 25.5(16) . . ?
B1 Y1 H1C 20.4(18) . . ?
B1 Y1 H2C 101(2) . . ?
B1 Y1 H2D 90.3(19) . . ?
B1 Y1 I3 96.9(3) . . ?
B1 Y1 I2 95.3(3) . . ?
B1 Y1 H3B 97(3) . . ?
B2 Y1 H1A 84.8(19) . . ?
B2 Y1 H1B 120.6(17) . . ?
B2 Y1 H1C 88(2) . . ?
B2 Y1 H2C 21.4(4) . . ?
B2 Y1 H2D 22.7(3) . . ?
B2 Y1 H3B 167(3) . . ?
B3 Y1 B1 97.6(8) . . ?
B3 Y1 B2 165.3(11) . . ?
B3 Y1 H1A 105(2) . . ?
B3 Y1 H1B 72.2(17) . . ?
B3 Y1 H1C 106(2) . . ?
B3 Y1 H2C 147.1(12) . . ?
B3 Y1 H2D 162.4(15) . . ?
B3 Y1 H3B 3(3) . . ?
H1A Y1 H1B 39(2) . . ?
H1A Y1 H1C 42(2) . . ?
H1A Y1 H2C 83(3) . . ?
H1A Y1 H2D 89(3) . . ?
H1A Y1 H3B 106(3) . . ?
H1B Y1 H1C 40(2) . . ?
H1B Y1 H2C 122(3) . . ?
H1B Y1 H2D 115(2) . . ?
H1B Y1 H3B 72(3) . . ?
H1C Y1 H2C 100(3) . . ?
H1C Y1 H2D 77(3) . . ?
H1C Y1 H3B 105(4) . . ?
H2C Y1 H2D 44.1(5) . . ?
H2C Y1 H3B 150(3) . . ?
H2D Y1 H3B 160(3) . . ?
I3 Y1 H1A 105.1(19) . . ?
I3 Y1 H1B 71.6(15) . . ?
I3 Y1 H1C 105(2) . . ?
I2 Y1 H1A 85.3(18) . . ?
I2 Y1 H1B 120.5(15) . . ?
I2 Y1 H1C 87(2) . . ?
I2 Y1 I3 167.7(3) . . ?
C1 O1 Y1 123.8(4) . . ?
C1 O1 C4 109.5(6) . . ?
C4 O1 Y1 126.5(4) . . ?
C5 O2 Y1 126.1(4) . . ?
C8 O2 Y1 125.1(5) . . ?
C8 O2 C5 108.8(6) . . ?
C9 O3 Y1 123.6(4) . . ?
C9 O3 C12 109.5(5) . . ?
C12 O3 Y1 126.8(4) . . ?
O1 C1 H1AA 110.6 . . ?
O1 C1 H1AB 110.6 . . ?
O1 C1 H1BC 111.2 . . ?
O1 C1 H1BD 111.2 . . ?
O1 C1 C2 105.8(8) . . ?
O1 C1 C2A 102.6(8) . . ?
H1AA C1 H1AB 108.7 . . ?
H1BC C1 H1BD 109.2 . . ?
C2 C1 H1AA 110.6 . . ?
C2 C1 H1AB 110.6 . . ?
C2A C1 H1BC 111.2 . . ?
C2A C1 H1BD 111.2 . . ?
H3AA C3 H3AB 108.9 . . ?
H3BC C3 H3BD 109.2 . . ?
C4 C3 H3AA 110.9 . . ?
C4 C3 H3AB 110.9 . . ?
C4 C3 H3BC 111.2 . . ?
C4 C3 H3BD 111.2 . . ?
C4 C3 C2 104.4(7) . . ?
C4 C3 C2A 102.6(8) . . ?
C2 C3 H3AA 110.9 . . ?
C2 C3 H3AB 110.9 . . ?
C2A C3 H3BC 111.2 . . ?
C2A C3 H3BD 111.2 . . ?
O1 C4 C3 105.0(6) . . ?
O1 C4 H4A 110.7 . . ?
O1 C4 H4B 110.7 . . ?
C3 C4 H4A 110.7 . . ?
C3 C4 H4B 110.7 . . ?
H4A C4 H4B 108.8 . . ?
O2 C5 H5A 110.5 . . ?
O2 C5 H5B 110.5 . . ?
O2 C5 C6 105.9(6) . . ?
H5A C5 H5B 108.7 . . ?
C6 C5 H5A 110.5 . . ?
C6 C5 H5B 110.5 . . ?
C5 C6 H6A 111.4 . . ?
C5 C6 H6B 111.4 . . ?
C5 C6 C7 102.0(7) . . ?
H6A C6 H6B 109.2 . . ?
C7 C6 H6A 111.4 . . ?
C7 C6 H6B 111.4 . . ?
C6 C7 H7A 111.0 . . ?
C6 C7 H7B 111.0 . . ?
H7A C7 H7B 109.0 . . ?
C8 C7 C6 104.0(8) . . ?
C8 C7 H7A 111.0 . . ?
C8 C7 H7B 111.0 . . ?
O2 C8 C7 104.8(7) . . ?
O2 C8 H8A 110.8 . . ?
O2 C8 H8B 110.8 . . ?
C7 C8 H8A 110.8 . . ?
C7 C8 H8B 110.8 . . ?
H8A C8 H8B 108.9 . . ?
O3 C9 H9A 110.8 . . ?
O3 C9 H9B 110.8 . . ?
O3 C9 C10 104.8(6) . . ?
H9A C9 H9B 108.9 . . ?
C10 C9 H9A 110.8 . . ?
C10 C9 H9B 110.8 . . ?
C9 C10 H10A 111.4 . . ?
C9 C10 H10B 111.4 . . ?
C9 C10 C11 101.9(6) . . ?
H10A C10 H10B 109.2 . . ?
C11 C10 H10A 111.4 . . ?
C11 C10 H10B 111.4 . . ?
C10 C11 H11A 111.2 . . ?
C10 C11 H11B 111.2 . . ?
H11A C11 H11B 109.1 . . ?
C12 C11 C10 102.8(6) . . ?
C12 C11 H11A 111.2 . . ?
C12 C11 H11B 111.2 . . ?
O3 C12 C11 104.9(6) . . ?
O3 C12 H12A 110.8 . . ?
O3 C12 H12B 110.8 . . ?
C11 C12 H12A 110.8 . . ?
C11 C12 H12B 110.8 . . ?
H12A C12 H12B 108.8 . . ?
Y1 B1 H1A 65(4) . . ?
Y1 B1 H1B 71(4) . . ?
Y1 B1 H1C 56(5) . . ?
Y1 B1 H1D 176(5) . . ?
H1A B1 H1B 94(4) . . ?
H1A B1 H1C 106(5) . . ?
H1A B1 H1D 111(5) . . ?
H1B B1 H1C 104(5) . . ?
H1B B1 H1D 109(5) . . ?
H1C B1 H1D 128(6) . . ?
C1 C2 C3 102.4(9) . . ?
C1 C2 H2A 111.3 . . ?
C1 C2 H2B 111.3 . . ?
C3 C2 H2A 111.3 . . ?
C3 C2 H2B 111.3 . . ?
H2A C2 H2B 109.2 . . ?
Y1 B2 H2C 49(2) . . ?
Y1 B2 H2D 61(2) . . ?
Y1 B2 H2E 123(4) . . ?
Y1 B2 H2F 127(4) . . ?
H2C B2 H2D 109.5(15) . . ?
H2C B2 H2E 109.6(15) . . ?
H2C B2 H2F 109.4(15) . . ?
H2D B2 H2E 109.6(15) . . ?
H2D B2 H2F 109.7(15) . . ?
H2E B2 H2F 109.1(15) . . ?
Y1 B3 H3A 111(5) . . ?
Y1 B3 H3C 112(4) . . ?
Y1 B3 H3D 104(4) . . ?
H3A B3 H3B 109(2) . . ?
H3A B3 H3C 110(2) . . ?
H3A B3 H3D 110(2) . . ?
H3B B3 H3C 109(2) . . ?
H3B B3 H3D 110(2) . . ?
H3C B3 H3D 109(2) . . ?
C1 C2A C3 105.2(9) . . ?
C1 C2A H2AA 110.7 . . ?
C1 C2A H2AB 110.7 . . ?
C3 C2A H2AA 110.7 . . ?
C3 C2A H2AB 110.7 . . ?
H2AA C2A H2AB 108.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Y1 O1 C1 C2 168.1(8) . . . . ?
Y1 O1 C1 C2A -147.2(8) . . . . ?
Y1 O1 C4 C3 169.1(5) . . . . ?
Y1 O2 C5 C6 -170.5(5) . . . . ?
Y1 O2 C8 C7 -165.3(7) . . . . ?
Y1 O3 C9 C10 -159.9(5) . . . . ?
Y1 O3 C12 C11 -174.9(5) . . . . ?
O1 C1 C2 C3 32.3(13) . . . . ?
O1 C1 C2A C3 -38.6(12) . . . . ?
O2 C5 C6 C7 -29.4(10) . . . . ?
O3 C9 C10 C11 -34.4(9) . . . . ?
C1 O1 C4 C3 -5.4(9) . . . . ?
C4 O1 C1 C2 -17.3(11) . . . . ?
C4 O1 C1 C2A 27.4(10) . . . . ?
C4 C3 C2 C1 -35.4(13) . . . . ?
C4 C3 C2A C1 35.5(12) . . . . ?
C5 O2 C8 C7 14.1(12) . . . . ?
C5 C6 C7 C8 38.1(12) . . . . ?
C6 C7 C8 O2 -32.5(13) . . . . ?
C8 O2 C5 C6 10.1(10) . . . . ?
C9 O3 C12 C11 9.3(8) . . . . ?
C9 C10 C11 C12 39.8(9) . . . . ?
C10 C11 C12 O3 -30.5(8) . . . . ?
C12 O3 C9 C10 16.0(9) . . . . ?
C2 C3 C4 O1 25.4(11) . . . . ?
C2A C3 C4 O1 -17.9(10) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_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_3-Tb
_database_code_depnum_ccdc_archive 'CCDC 1844354'
_audit_update_record             
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;

_manchester_internal_coll_name   rdpm83
_manchester_internal_coll_client CAPG/DPM
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 3.75s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w & \f scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   20/11/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 20/11/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 20/11/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 26/11/17
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 29/4/18
_manchester_internal_archive_date 29/4/18

_refine_special_details          
;
2 large Q peaks can be seen near the metal centre, these are attributed to 
unresolved twinning which we have found to be a common problem in these 
systems. Treatment of the original data with Platon or CrysAlisPro did not
yield a satisfactory solution however we believe the model to be correct.

Rotational disorder was identified at tBu group C31-C34. This was modelled over 
two positions, with equivalent C-C distances restrained to be approximately 
equivalent (SADI) and restraints were applied to the ADPs (SIMU). The two 
components were then refined competetively, converging at a ratio of
0.66(2):0.34(2) (FVAR2). 

Additionally a badly disordered dicholoromethane (DCM) molecule was identified 
in the lattice, in a void relatively distant from the metal coordination 
sphere. This could not be modelled sensibly, so it was removed using SQUEEZE 
(Platon). The resulting solvent void accounts for approximately one molecule of 
DCM, in terms of electron density, to give one molecule of solvent per complex.
Hence, one molecule of DCM should be taken into account in the formula and 
other derived parameters (Mr, density, etc.). 

Finally, global rigid bond restraints (RIGU) were applied.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 217 40 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?


_audit_creation_date             2017-11-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        '[Tb(Cpttt)2][BArF20]'
_chemical_formula_moiety         'C34 H58 Tb, B C24 F20'
_chemical_formula_sum            'C58 H58 B F20 Tb'
_chemical_formula_weight         1304.77
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      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                   11.7358(4)
_cell_length_b                   12.4581(4)
_cell_length_c                   19.9710(9)
_cell_angle_alpha                82.810(3)
_cell_angle_beta                 89.321(3)
_cell_angle_gamma                79.728(3)
_cell_volume                     2850.33(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3620
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      23.7890
_cell_measurement_theta_min      2.1940
_shelx_estimated_absorpt_T_max   0.987
_shelx_estimated_absorpt_T_min   0.877
_exptl_absorpt_coefficient_mu    1.343
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72224
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1312
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/hexane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_av_unetI/netI     0.1128
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35372
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.051
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  φ      0.00  72.00   0.25    3.75  -8.00   0.00   0.00    --   288
  2  φ     72.00 144.00   0.25    3.75  -8.00   0.00  40.00    --   288
  3  ω    -12.00  23.00   0.25    3.75    --    5.00  57.00-120.00  140
  4  ω     49.00  75.00   0.25    3.75    --    5.00  57.00-180.00  104
  5  ω     -7.00  19.00   0.25    3.75    --    5.00  54.00 -49.16  104
  6  ω    -35.00  74.00   0.25    3.75    --   -7.70  57.00  30.00  436
  7  ω      1.00  82.00   0.25    3.75    --   -7.70  38.00 -30.00  324
  8  ω    -96.00  25.00   0.25    3.75    --   -7.70 -57.00-150.00  484
  9  ω    -84.00 -26.00   0.25    3.75    --   -7.70 -38.00  90.00  232
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7152
_reflns_number_total             10291
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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    ?
_refine_diff_density_max         4.327
_refine_diff_density_min         -1.227
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         10291
_refine_ls_number_restraints     922
_refine_ls_R_factor_all          0.1249
_refine_ls_R_factor_gt           0.0852
_refine_ls_restrained_S_all      0.983
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0948P)²+20.8484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1912
_refine_ls_wR_factor_ref         0.2105

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C33A-C31 \\sim C31-C33B \\sim C32A-C31 \\sim C31-C32B \\sim C34A-C31 \\sim
C31-C34B
 with sigma of 0.008
 C32A-C33A \\sim C34A-C32A \\sim C32B-C33B \\sim C33B-C34B \\sim C34B-C32B
 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C32A \\sim C33A \\sim C34A \\sim C32B \\sim C33B \\sim C34B: within 2A with
sigma of 0.008 and sigma for terminal atoms of 0.016
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Others
 Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(H33D)=Sof(H33E)=
 Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=Sof(H33A)=Sof(H33B)=
 Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
6.a Me refined with riding coordinates:
 C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C), C32B(H32D,
 H32E,H32F), C33B(H33D,H33E,H33F), C34B(H34D,H34E,H34F)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
6.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.87491(4) 0.68541(4) 0.71558(3) 0.03264(18) Uani 1 1 d . U . . .
C1 C 0.9940(7) 0.8391(8) 0.7078(5) 0.034(2) Uani 1 1 d . U . . .
C2 C 1.0623(8) 0.7496(7) 0.7514(5) 0.035(2) Uani 1 1 d . U . . .
C3 C 1.1031(7) 0.6687(8) 0.7067(6) 0.036(2) Uani 1 1 d . U . . .
H3 H 1.150750 0.599752 0.720743 0.043 Uiso 1 1 calc R . . . .
C4 C 1.0648(8) 0.7033(8) 0.6409(6) 0.039(2) Uani 1 1 d . U . . .
C5 C 0.9970(7) 0.8082(8) 0.6427(5) 0.036(2) Uani 1 1 d . U . . .
H5 H 0.958320 0.852394 0.604575 0.043 Uiso 1 1 calc R . . . .
C6 C 0.9142(8) 0.9454(8) 0.7235(6) 0.040(2) Uani 1 1 d . U . . .
C7 C 0.8021(8) 0.9100(8) 0.7542(6) 0.046(3) Uani 1 1 d . U . . .
H7A H 0.762891 0.878287 0.720470 0.070 Uiso 1 1 calc GR . . . .
H7B H 0.750345 0.974332 0.767737 0.070 Uiso 1 1 calc GR . . . .
H7C H 0.822308 0.855071 0.793804 0.070 Uiso 1 1 calc GR . . . .
C8 C 0.8781(10) 1.0253(8) 0.6597(6) 0.050(3) Uani 1 1 d . U . . .
H8A H 0.836824 0.989840 0.628912 0.075 Uiso 1 1 calc GR . . . .
H8B H 0.947189 1.046265 0.637474 0.075 Uiso 1 1 calc GR . . . .
H8C H 0.827182 1.091178 0.671883 0.075 Uiso 1 1 calc GR . . . .
C9 C 0.9662(9) 1.0116(8) 0.7722(7) 0.052(3) Uani 1 1 d . U . . .
H9A H 0.914719 1.082260 0.774076 0.077 Uiso 1 1 calc GR . . . .
H9B H 1.042344 1.024448 0.755934 0.077 Uiso 1 1 calc GR . . . .
H9C H 0.974587 0.969934 0.817397 0.077 Uiso 1 1 calc GR . . . .
C10 C 1.1021(9) 0.7327(8) 0.8249(6) 0.042(2) Uani 1 1 d . U . . .
C11 C 1.0037(10) 0.7558(10) 0.8753(7) 0.055(3) Uani 1 1 d . U . . .
H11A H 0.967247 0.833482 0.867172 0.083 Uiso 1 1 calc GR . . . .
H11B H 1.035208 0.739023 0.921415 0.083 Uiso 1 1 calc GR . . . .
H11C H 0.945921 0.709724 0.869546 0.083 Uiso 1 1 calc GR . . . .
C12 C 1.1646(11) 0.6134(8) 0.8466(6) 0.050(3) Uani 1 1 d . U . . .
H12A H 1.112739 0.562144 0.839648 0.076 Uiso 1 1 calc GR . . . .
H12B H 1.186336 0.604837 0.894502 0.076 Uiso 1 1 calc GR . . . .
H12C H 1.234415 0.597549 0.819582 0.076 Uiso 1 1 calc GR . . . .
C13 C 1.1931(9) 0.8055(9) 0.8338(7) 0.050(3) Uani 1 1 d . U . . .
H13A H 1.263917 0.778765 0.809941 0.075 Uiso 1 1 calc GR . . . .
H13B H 1.210835 0.802316 0.881943 0.075 Uiso 1 1 calc GR . . . .
H13C H 1.162364 0.881652 0.815278 0.075 Uiso 1 1 calc GR . . . .
C14 C 1.1117(8) 0.6490(9) 0.5815(6) 0.042(2) Uani 1 1 d . U . . .
C15 C 1.0230(13) 0.6610(16) 0.5265(7) 0.095(6) Uani 1 1 d . U . . .
H15A H 0.964816 0.615511 0.540653 0.143 Uiso 1 1 calc GR . . . .
H15B H 1.060781 0.637229 0.485463 0.143 Uiso 1 1 calc GR . . . .
H15C H 0.985215 0.738205 0.517264 0.143 Uiso 1 1 calc GR . . . .
C16 C 1.1564(12) 0.5222(10) 0.5989(7) 0.063(3) Uani 1 1 d . U . . .
H16A H 1.215680 0.509510 0.634561 0.095 Uiso 1 1 calc GR . . . .
H16B H 1.189913 0.492100 0.558525 0.095 Uiso 1 1 calc GR . . . .
H16C H 1.091700 0.485903 0.614439 0.095 Uiso 1 1 calc GR . . . .
C17 C 1.2161(12) 0.6973(11) 0.5573(8) 0.070(4) Uani 1 1 d . U . . .
H17A H 1.190803 0.771698 0.534144 0.105 Uiso 1 1 calc GR . . . .
H17B H 1.260001 0.651206 0.526101 0.105 Uiso 1 1 calc GR . . . .
H17C H 1.265363 0.700251 0.596099 0.105 Uiso 1 1 calc GR . . . .
C18 C 0.7543(8) 0.5339(8) 0.7052(5) 0.033(2) Uani 1 1 d . U . . .
C19 C 0.6861(8) 0.6114(7) 0.7454(5) 0.033(2) Uani 1 1 d . U . . .
C20 C 0.6475(8) 0.7065(8) 0.6994(6) 0.038(2) Uani 1 1 d . U . . .
H20 H 0.599247 0.770656 0.711589 0.045 Uiso 1 1 calc R . . . .
C21 C 0.6875(8) 0.6957(8) 0.6351(6) 0.039(2) Uani 1 1 d . U . . .
C22 C 0.7552(8) 0.5903(8) 0.6387(5) 0.037(2) Uani 1 1 d . U . . .
H22 H 0.795900 0.560629 0.601847 0.044 Uiso 1 1 calc R . . . .
C23 C 0.8368(8) 0.4224(8) 0.7261(6) 0.039(2) Uani 1 1 d . U . . .
C24 C 0.9476(8) 0.4450(8) 0.7568(6) 0.042(3) Uani 1 1 d . U . . .
H24A H 0.984871 0.491953 0.723652 0.064 Uiso 1 1 calc GR . . . .
H24B H 1.000496 0.375320 0.769562 0.064 Uiso 1 1 calc GR . . . .
H24C H 0.928292 0.482242 0.796974 0.064 Uiso 1 1 calc GR . . . .
C25 C 0.7819(9) 0.3422(8) 0.7740(7) 0.050(3) Uani 1 1 d . U . . .
H25A H 0.761109 0.373953 0.815961 0.076 Uiso 1 1 calc GR . . . .
H25B H 0.837122 0.273216 0.784157 0.076 Uiso 1 1 calc GR . . . .
H25C H 0.712162 0.327761 0.752949 0.076 Uiso 1 1 calc GR . . . .
C26 C 0.8711(9) 0.3652(8) 0.6637(6) 0.048(3) Uani 1 1 d . U . . .
H26A H 0.801113 0.357324 0.639811 0.072 Uiso 1 1 calc GR . . . .
H26B H 0.917454 0.292360 0.677409 0.072 Uiso 1 1 calc GR . . . .
H26C H 0.916633 0.409277 0.633683 0.072 Uiso 1 1 calc GR . . . .
C27 C 0.6479(9) 0.6013(8) 0.8181(6) 0.041(2) Uani 1 1 d . U . . .
C28 C 0.7481(10) 0.5638(12) 0.8696(6) 0.058(3) Uani 1 1 d . U . . .
H28A H 0.782547 0.487068 0.866170 0.087 Uiso 1 1 calc GR . . . .
H28B H 0.718461 0.570353 0.915234 0.087 Uiso 1 1 calc GR . . . .
H28C H 0.807028 0.610225 0.860065 0.087 Uiso 1 1 calc GR . . . .
C29 C 0.5848(11) 0.7147(9) 0.8366(7) 0.061(4) Uani 1 1 d . U . . .
H29A H 0.638283 0.767246 0.831481 0.092 Uiso 1 1 calc GR . . . .
H29B H 0.558837 0.706093 0.883495 0.092 Uiso 1 1 calc GR . . . .
H29C H 0.517762 0.742021 0.806574 0.092 Uiso 1 1 calc GR . . . .
C30 C 0.5565(10) 0.5257(9) 0.8296(6) 0.051(3) Uani 1 1 d . U . . .
H30A H 0.488881 0.556217 0.800499 0.076 Uiso 1 1 calc GR . . . .
H30B H 0.532777 0.520971 0.876978 0.076 Uiso 1 1 calc GR . . . .
H30C H 0.589840 0.452176 0.818761 0.076 Uiso 1 1 calc GR . . . .
C31 C 0.6417(7) 0.7703(8) 0.5723(6) 0.049(3) Uani 1 1 d D U . . .
C32A C 0.6039(14) 0.8885(11) 0.5887(10) 0.063(5) Uani 0.662(16) 1 d D U P A 1
H32A H 0.574271 0.936434 0.547578 0.095 Uiso 0.662(16) 1 calc R . P A 1
H32B H 0.542868 0.890277 0.622652 0.095 Uiso 0.662(16) 1 calc R . P A 1
H32C H 0.670382 0.914390 0.606253 0.095 Uiso 0.662(16) 1 calc R . P A 1
C33A C 0.5293(12) 0.7355(14) 0.5530(11) 0.051(5) Uani 0.662(16) 1 d D U P A 1
H33A H 0.496192 0.782018 0.512149 0.076 Uiso 0.662(16) 1 calc R . P A 1
H33B H 0.545530 0.658499 0.544402 0.076 Uiso 0.662(16) 1 calc R . P A 1
H33C H 0.474060 0.743558 0.589973 0.076 Uiso 0.662(16) 1 calc R . P A 1
C34A C 0.7246(15) 0.7787(16) 0.5137(9) 0.070(5) Uani 0.662(16) 1 d D U P A 1
H34A H 0.685507 0.829176 0.475960 0.105 Uiso 0.662(16) 1 calc R . P A 1
H34B H 0.792352 0.806436 0.527949 0.105 Uiso 0.662(16) 1 calc R . P A 1
H34C H 0.749576 0.705826 0.499304 0.105 Uiso 0.662(16) 1 calc R . P A 1
C32B C 0.680(3) 0.8815(15) 0.5591(18) 0.069(6) Uani 0.338(16) 1 d D U P A 2
H32D H 0.644230 0.921606 0.516967 0.103 Uiso 0.338(16) 1 calc R . P A 2
H32E H 0.655665 0.923962 0.596519 0.103 Uiso 0.338(16) 1 calc R . P A 2
H32F H 0.764388 0.870515 0.555224 0.103 Uiso 0.338(16) 1 calc R . P A 2
C33B C 0.5109(11) 0.793(3) 0.5629(19) 0.057(6) Uani 0.338(16) 1 d D U P A 2
H33D H 0.490140 0.841974 0.520855 0.086 Uiso 0.338(16) 1 calc R . P A 2
H33E H 0.483677 0.723532 0.560709 0.086 Uiso 0.338(16) 1 calc R . P A 2
H33F H 0.474657 0.827907 0.601020 0.086 Uiso 0.338(16) 1 calc R . P A 2
C34B C 0.689(2) 0.709(2) 0.5132(12) 0.061(7) Uani 0.338(16) 1 d D U P A 2
H34D H 0.662140 0.753755 0.470531 0.092 Uiso 0.338(16) 1 calc R . P A 2
H34E H 0.773949 0.695372 0.514877 0.092 Uiso 0.338(16) 1 calc R . P A 2
H34F H 0.661597 0.638825 0.516297 0.092 Uiso 0.338(16) 1 calc R . P A 2
F1 F 0.8063(5) 0.7145(4) 0.2999(3) 0.0444(15) Uani 1 1 d . U . . .
F2 F 0.9078(5) 0.7914(6) 0.3980(3) 0.0547(17) Uani 1 1 d . U . . .
F3 F 0.8485(5) 1.0051(6) 0.4195(3) 0.0564(17) Uani 1 1 d . U . . .
F4 F 0.6876(6) 1.1438(5) 0.3370(4) 0.0560(17) Uani 1 1 d . U . . .
F5 F 0.5812(5) 1.0701(4) 0.2423(3) 0.0432(14) Uani 1 1 d . U . . .
F6 F 0.4433(5) 0.9100(4) 0.3047(3) 0.0443(14) Uani 1 1 d . U . . .
F7 F 0.3505(5) 0.7966(5) 0.4062(3) 0.0500(16) Uani 1 1 d . U . . .
F8 F 0.4045(5) 0.5728(5) 0.4271(3) 0.0530(16) Uani 1 1 d . U . . .
F9 F 0.5555(5) 0.4661(5) 0.3421(3) 0.0538(17) Uani 1 1 d . U . . .
F10 F 0.6565(5) 0.5753(4) 0.2451(3) 0.0444(14) Uani 1 1 d . U . . .
F11 F 0.3572(5) 0.8473(5) 0.1862(3) 0.0499(16) Uani 1 1 d . U . . .
F12 F 0.2310(6) 0.9929(7) 0.0969(4) 0.074(2) Uani 1 1 d . U . . .
F13 F 0.3275(7) 1.1439(6) 0.0172(4) 0.080(2) Uani 1 1 d . U . . .
F14 F 0.5572(7) 1.1458(5) 0.0290(4) 0.069(2) Uani 1 1 d . U . . .
F15 F 0.6882(5) 1.0000(5) 0.1212(3) 0.0529(16) Uani 1 1 d . U . . .
F16 F 0.5395(5) 0.6917(5) 0.1264(3) 0.0449(14) Uani 1 1 d . U . . .
F17 F 0.6552(6) 0.5795(5) 0.0349(3) 0.0597(18) Uani 1 1 d . U . . .
F18 F 0.8845(6) 0.5858(6) 0.0143(3) 0.0637(19) Uani 1 1 d . U . . .
F19 F 0.9919(5) 0.7067(6) 0.0880(4) 0.069(2) Uani 1 1 d . U . . .
F20 F 0.8788(5) 0.8199(5) 0.1789(3) 0.0511(16) Uani 1 1 d . U . . .
C35 C 0.6885(7) 0.8858(9) 0.2651(5) 0.039(2) Uani 1 1 d . U . . .
C36 C 0.7744(8) 0.8233(7) 0.3074(5) 0.037(2) Uani 1 1 d . U . . .
C37 C 0.8264(8) 0.8607(9) 0.3585(6) 0.042(2) Uani 1 1 d . U . . .
C38 C 0.7984(9) 0.9672(10) 0.3691(6) 0.045(3) Uani 1 1 d . U . . .
C39 C 0.7173(10) 1.0363(8) 0.3275(6) 0.044(2) Uani 1 1 d . U . . .
C40 C 0.6657(9) 0.9966(8) 0.2780(6) 0.041(2) Uani 1 1 d . U . . .
C41 C 0.5535(8) 0.7506(8) 0.2675(5) 0.033(2) Uani 1 1 d . U . . .
C42 C 0.4729(9) 0.7996(7) 0.3115(6) 0.039(2) Uani 1 1 d . U . . .
C43 C 0.4250(8) 0.7422(8) 0.3646(5) 0.039(2) Uani 1 1 d . U . . .
C44 C 0.4524(9) 0.6296(9) 0.3752(5) 0.042(2) Uani 1 1 d . U . . .
C45 C 0.5276(8) 0.5770(8) 0.3331(6) 0.038(2) Uani 1 1 d . U . . .
C46 C 0.5779(8) 0.6366(8) 0.2816(5) 0.033(2) Uani 1 1 d . U . . .
C47 C 0.5299(8) 0.9173(7) 0.1597(5) 0.033(2) Uani 1 1 d . U . . .
C48 C 0.4126(9) 0.9198(8) 0.1495(6) 0.040(2) Uani 1 1 d . U . . .
C49 C 0.3458(10) 0.9957(10) 0.1022(6) 0.053(3) Uani 1 1 d . U . . .
C50 C 0.3923(11) 1.0711(10) 0.0618(6) 0.056(3) Uani 1 1 d . U . . .
C51 C 0.5090(11) 1.0705(8) 0.0682(6) 0.049(3) Uani 1 1 d . U . . .
C52 C 0.5754(10) 0.9957(8) 0.1164(6) 0.042(2) Uani 1 1 d . U . . .
C53 C 0.7020(8) 0.7583(7) 0.1595(5) 0.033(2) Uani 1 1 d . U . . .
C54 C 0.6522(9) 0.6971(8) 0.1190(6) 0.041(2) Uani 1 1 d . U . . .
C55 C 0.7109(10) 0.6391(8) 0.0709(5) 0.043(2) Uani 1 1 d . U . . .
C56 C 0.8247(10) 0.6435(9) 0.0605(6) 0.051(3) Uani 1 1 d . U . . .
C57 C 0.8789(9) 0.7025(9) 0.0972(6) 0.048(3) Uani 1 1 d . U . . .
C58 C 0.8172(8) 0.7608(8) 0.1454(6) 0.040(2) Uani 1 1 d . U . . .
B1 B 0.6207(8) 0.8281(9) 0.2132(6) 0.034(2) Uani 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 C1 2.554(9) . ?
Tb1 C2 2.606(9) . ?
Tb1 C3 2.654(8) . ?
Tb1 C4 2.693(10) . ?
Tb1 C5 2.586(9) . ?
Tb1 C7 2.971(10) . ?
Tb1 C18 2.582(8) . ?
Tb1 C19 2.583(9) . ?
Tb1 C20 2.655(9) . ?
Tb1 C21 2.715(10) . ?
Tb1 C22 2.615(10) . ?
Tb1 C24 2.977(10) . ?
C1 C2 1.449(13) . ?
C1 C5 1.400(15) . ?
C1 C6 1.543(13) . ?
C2 C3 1.444(14) . ?
C2 C10 1.522(15) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(15) . ?
C4 C5 1.408(14) . ?
C4 C14 1.491(15) . ?
C5 H5 0.9500 . ?
C6 C7 1.556(13) . ?
C6 C8 1.530(16) . ?
C6 C9 1.547(15) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.535(15) . ?
C10 C12 1.547(14) . ?
C10 C13 1.546(14) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.498(18) . ?
C14 C16 1.569(16) . ?
C14 C17 1.508(15) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.456(13) . ?
C18 C22 1.424(15) . ?
C18 C23 1.557(13) . ?
C19 C20 1.413(13) . ?
C19 C27 1.511(15) . ?
C20 H20 0.9500 . ?
C20 C21 1.377(15) . ?
C21 C22 1.402(14) . ?
C21 C31 1.508(15) . ?
C22 H22 0.9500 . ?
C23 C24 1.529(14) . ?
C23 C25 1.518(14) . ?
C23 C26 1.527(15) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.539(16) . ?
C27 C29 1.560(14) . ?
C27 C30 1.547(14) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32A 1.535(10) . ?
C31 C33A 1.528(10) . ?
C31 C34A 1.519(10) . ?
C31 C32B 1.522(11) . ?
C31 C33B 1.519(11) . ?
C31 C34B 1.531(11) . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C34A H34A 0.9800 . ?
C34A H34B 0.9800 . ?
C34A H34C 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 0.9800 . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C34B H34D 0.9800 . ?
C34B H34E 0.9800 . ?
C34B H34F 0.9800 . ?
F1 C36 1.367(10) . ?
F2 C37 1.354(12) . ?
F3 C38 1.346(13) . ?
F4 C39 1.359(12) . ?
F5 C40 1.363(11) . ?
F6 C42 1.347(10) . ?
F7 C43 1.351(11) . ?
F8 C44 1.356(12) . ?
F9 C45 1.351(11) . ?
F10 C46 1.356(11) . ?
F11 C48 1.346(12) . ?
F12 C49 1.360(13) . ?
F13 C50 1.327(13) . ?
F14 C51 1.344(13) . ?
F15 C52 1.340(13) . ?
F16 C54 1.342(12) . ?
F17 C55 1.347(13) . ?
F18 C56 1.352(12) . ?
F19 C57 1.346(12) . ?
F20 C58 1.356(12) . ?
C35 C36 1.382(14) . ?
C35 C40 1.414(14) . ?
C35 B1 1.624(15) . ?
C36 C37 1.368(15) . ?
C37 C38 1.351(15) . ?
C38 C39 1.372(16) . ?
C39 C40 1.354(16) . ?
C41 C42 1.396(14) . ?
C41 C46 1.391(13) . ?
C41 B1 1.649(14) . ?
C42 C43 1.375(14) . ?
C43 C44 1.371(15) . ?
C44 C45 1.353(15) . ?
C45 C46 1.382(14) . ?
C47 C48 1.388(14) . ?
C47 C52 1.397(14) . ?
C47 B1 1.679(15) . ?
C48 C49 1.390(15) . ?
C49 C50 1.347(18) . ?
C50 C51 1.375(18) . ?
C51 C52 1.391(15) . ?
C53 C54 1.379(14) . ?
C53 C58 1.383(13) . ?
C53 B1 1.652(15) . ?
C54 C55 1.378(15) . ?
C55 C56 1.359(16) . ?
C56 C57 1.340(17) . ?
C57 C58 1.396(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Tb1 C2 32.6(3) . . ?
C1 Tb1 C3 51.8(3) . . ?
C1 Tb1 C4 52.4(3) . . ?
C1 Tb1 C5 31.6(3) . . ?
C1 Tb1 C7 52.7(3) . . ?
C1 Tb1 C18 172.0(3) . . ?
C1 Tb1 C19 151.0(3) . . ?
C1 Tb1 C20 127.3(3) . . ?
C1 Tb1 C21 122.4(3) . . ?
C1 Tb1 C22 140.3(3) . . ?
C1 Tb1 C24 129.7(3) . . ?
C2 Tb1 C3 31.9(3) . . ?
C2 Tb1 C4 52.6(3) . . ?
C2 Tb1 C7 73.3(3) . . ?
C2 Tb1 C20 153.8(3) . . ?
C2 Tb1 C21 154.0(3) . . ?
C2 Tb1 C22 153.8(3) . . ?
C2 Tb1 C24 98.4(3) . . ?
C3 Tb1 C4 30.0(3) . . ?
C3 Tb1 C7 102.4(3) . . ?
C3 Tb1 C20 169.3(3) . . ?
C3 Tb1 C21 139.7(3) . . ?
C3 Tb1 C24 80.0(3) . . ?
C4 Tb1 C7 103.2(3) . . ?
C4 Tb1 C21 110.7(3) . . ?
C4 Tb1 C24 94.0(3) . . ?
C5 Tb1 C2 52.5(3) . . ?
C5 Tb1 C3 50.0(3) . . ?
C5 Tb1 C4 30.9(3) . . ?
C5 Tb1 C7 74.3(3) . . ?
C5 Tb1 C20 122.5(3) . . ?
C5 Tb1 C21 102.4(3) . . ?
C5 Tb1 C22 110.4(3) . . ?
C5 Tb1 C24 124.8(3) . . ?
C7 Tb1 C24 149.1(3) . . ?
C18 Tb1 C2 151.6(3) . . ?
C18 Tb1 C3 127.4(3) . . ?
C18 Tb1 C4 122.2(3) . . ?
C18 Tb1 C5 140.6(3) . . ?
C18 Tb1 C7 129.9(3) . . ?
C18 Tb1 C19 32.8(3) . . ?
C18 Tb1 C20 51.6(3) . . ?
C18 Tb1 C21 51.9(3) . . ?
C18 Tb1 C22 31.8(3) . . ?
C18 Tb1 C24 53.1(3) . . ?
C19 Tb1 C2 151.0(3) . . ?
C19 Tb1 C3 154.3(3) . . ?
C19 Tb1 C4 153.8(3) . . ?
C19 Tb1 C5 153.2(3) . . ?
C19 Tb1 C7 98.2(3) . . ?
C19 Tb1 C20 31.3(3) . . ?
C19 Tb1 C21 51.8(3) . . ?
C19 Tb1 C22 52.5(3) . . ?
C19 Tb1 C24 74.4(3) . . ?
C20 Tb1 C4 139.4(3) . . ?
C20 Tb1 C7 80.6(3) . . ?
C20 Tb1 C21 29.7(3) . . ?
C20 Tb1 C24 102.7(3) . . ?
C21 Tb1 C7 94.8(3) . . ?
C21 Tb1 C24 102.9(3) . . ?
C22 Tb1 C3 122.6(3) . . ?
C22 Tb1 C4 102.0(3) . . ?
C22 Tb1 C7 125.1(3) . . ?
C22 Tb1 C20 49.8(3) . . ?
C22 Tb1 C21 30.4(3) . . ?
C22 Tb1 C24 74.5(3) . . ?
C2 C1 Tb1 75.7(5) . . ?
C2 C1 C6 131.6(10) . . ?
C5 C1 Tb1 75.5(6) . . ?
C5 C1 C2 107.5(8) . . ?
C5 C1 C6 120.4(9) . . ?
C6 C1 Tb1 108.4(5) . . ?
C1 C2 Tb1 71.7(5) . . ?
C1 C2 C10 134.8(9) . . ?
C3 C2 Tb1 75.9(5) . . ?
C3 C2 C1 103.8(9) . . ?
C3 C2 C10 121.1(8) . . ?
C10 C2 Tb1 121.3(6) . . ?
Tb1 C3 H3 118.8 . . ?
C2 C3 Tb1 72.2(5) . . ?
C2 C3 H3 123.9 . . ?
C4 C3 Tb1 76.6(5) . . ?
C4 C3 C2 112.3(9) . . ?
C4 C3 H3 123.9 . . ?
C3 C4 Tb1 73.4(5) . . ?
C3 C4 C5 105.1(9) . . ?
C3 C4 C14 124.3(9) . . ?
C5 C4 Tb1 70.4(5) . . ?
C5 C4 C14 129.2(10) . . ?
C14 C4 Tb1 131.3(7) . . ?
Tb1 C5 H5 115.7 . . ?
C1 C5 Tb1 72.9(5) . . ?
C1 C5 C4 111.3(9) . . ?
C1 C5 H5 124.3 . . ?
C4 C5 Tb1 78.8(6) . . ?
C4 C5 H5 124.3 . . ?
C1 C6 C7 106.4(7) . . ?
C1 C6 C9 115.2(8) . . ?
C8 C6 C1 112.1(9) . . ?
C8 C6 C7 107.1(9) . . ?
C8 C6 C9 106.0(8) . . ?
C9 C6 C7 109.8(9) . . ?
Tb1 C7 H7A 54.9 . . ?
Tb1 C7 H7B 158.5 . . ?
Tb1 C7 H7C 68.2 . . ?
C6 C7 Tb1 90.9(5) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C2 C10 C11 114.2(9) . . ?
C2 C10 C12 111.8(9) . . ?
C2 C10 C13 109.6(9) . . ?
C11 C10 C12 106.2(9) . . ?
C11 C10 C13 109.5(9) . . ?
C13 C10 C12 105.2(9) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C4 C14 C15 112.3(9) . . ?
C4 C14 C16 113.3(10) . . ?
C4 C14 C17 107.7(9) . . ?
C15 C14 C16 106.0(12) . . ?
C15 C14 C17 111.8(12) . . ?
C17 C14 C16 105.7(9) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 Tb1 73.7(5) . . ?
C19 C18 C23 131.4(9) . . ?
C22 C18 Tb1 75.4(5) . . ?
C22 C18 C19 106.0(9) . . ?
C22 C18 C23 121.2(9) . . ?
C23 C18 Tb1 106.2(6) . . ?
C18 C19 Tb1 73.6(5) . . ?
C18 C19 C27 132.5(9) . . ?
C20 C19 Tb1 77.2(5) . . ?
C20 C19 C18 105.1(9) . . ?
C20 C19 C27 122.1(9) . . ?
C27 C19 Tb1 118.8(6) . . ?
Tb1 C20 H20 118.5 . . ?
C19 C20 Tb1 71.6(5) . . ?
C19 C20 H20 123.8 . . ?
C21 C20 Tb1 77.6(6) . . ?
C21 C20 C19 112.5(9) . . ?
C21 C20 H20 123.8 . . ?
C20 C21 Tb1 72.7(6) . . ?
C20 C21 C22 105.9(9) . . ?
C20 C21 C31 125.2(9) . . ?
C22 C21 Tb1 70.9(6) . . ?
C22 C21 C31 127.2(10) . . ?
C31 C21 Tb1 132.7(6) . . ?
Tb1 C22 H22 115.5 . . ?
C18 C22 Tb1 72.8(5) . . ?
C18 C22 H22 124.7 . . ?
C21 C22 Tb1 78.7(6) . . ?
C21 C22 C18 110.5(9) . . ?
C21 C22 H22 124.7 . . ?
C24 C23 C18 108.9(7) . . ?
C25 C23 C18 113.4(8) . . ?
C25 C23 C24 110.9(10) . . ?
C25 C23 C26 106.2(9) . . ?
C26 C23 C18 109.7(9) . . ?
C26 C23 C24 107.5(8) . . ?
Tb1 C24 H24A 52.8 . . ?
Tb1 C24 H24B 157.7 . . ?
Tb1 C24 H24C 70.4 . . ?
C23 C24 Tb1 90.8(6) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C19 C27 C28 114.1(8) . . ?
C19 C27 C29 110.7(9) . . ?
C19 C27 C30 111.1(9) . . ?
C28 C27 C29 105.3(10) . . ?
C28 C27 C30 110.6(10) . . ?
C30 C27 C29 104.5(8) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C21 C31 C32A 110.1(10) . . ?
C21 C31 C33A 106.6(10) . . ?
C21 C31 C34A 116.8(10) . . ?
C21 C31 C32B 117.7(14) . . ?
C21 C31 C33B 115.8(16) . . ?
C21 C31 C34B 105.5(14) . . ?
C33A C31 C32A 104.4(8) . . ?
C34A C31 C32A 105.3(8) . . ?
C34A C31 C33A 113.0(14) . . ?
C32B C31 C34B 105.1(9) . . ?
C33B C31 C32B 106.2(9) . . ?
C33B C31 C34B 105.3(9) . . ?
C31 C32A H32A 109.5 . . ?
C31 C32A H32B 109.5 . . ?
C31 C32A H32C 109.5 . . ?
H32A C32A H32B 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C31 C33A H33A 109.5 . . ?
C31 C33A H33B 109.5 . . ?
C31 C33A H33C 109.5 . . ?
H33A C33A H33B 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C31 C34A H34A 109.5 . . ?
C31 C34A H34B 109.5 . . ?
C31 C34A H34C 109.5 . . ?
H34A C34A H34B 109.5 . . ?
H34A C34A H34C 109.5 . . ?
H34B C34A H34C 109.5 . . ?
C31 C32B H32D 109.5 . . ?
C31 C32B H32E 109.5 . . ?
C31 C32B H32F 109.5 . . ?
H32D C32B H32E 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C31 C33B H33D 109.5 . . ?
C31 C33B H33E 109.5 . . ?
C31 C33B H33F 109.5 . . ?
H33D C33B H33E 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C31 C34B H34D 109.5 . . ?
C31 C34B H34E 109.5 . . ?
C31 C34B H34F 109.5 . . ?
H34D C34B H34E 109.5 . . ?
H34D C34B H34F 109.5 . . ?
H34E C34B H34F 109.5 . . ?
C36 C35 C40 111.6(9) . . ?
C36 C35 B1 120.3(9) . . ?
C40 C35 B1 127.9(9) . . ?
F1 C36 C35 117.9(9) . . ?
F1 C36 C37 117.1(9) . . ?
C37 C36 C35 124.9(9) . . ?
F2 C37 C36 119.9(9) . . ?
C38 C37 F2 119.8(10) . . ?
C38 C37 C36 120.2(10) . . ?
F3 C38 C37 120.8(10) . . ?
F3 C38 C39 120.5(10) . . ?
C37 C38 C39 118.7(10) . . ?
F4 C39 C38 119.9(10) . . ?
C40 C39 F4 120.2(10) . . ?
C40 C39 C38 119.9(10) . . ?
F5 C40 C35 120.0(9) . . ?
C39 C40 F5 115.3(9) . . ?
C39 C40 C35 124.5(10) . . ?
C42 C41 B1 119.8(8) . . ?
C46 C41 C42 112.9(9) . . ?
C46 C41 B1 126.8(8) . . ?
F6 C42 C41 119.2(8) . . ?
F6 C42 C43 116.9(8) . . ?
C43 C42 C41 123.9(9) . . ?
F7 C43 C42 120.0(9) . . ?
F7 C43 C44 120.0(9) . . ?
C44 C43 C42 120.0(9) . . ?
F8 C44 C43 120.1(10) . . ?
C45 C44 F8 121.0(9) . . ?
C45 C44 C43 118.9(10) . . ?
F9 C45 C44 120.1(9) . . ?
F9 C45 C46 119.8(9) . . ?
C44 C45 C46 120.1(9) . . ?
F10 C46 C41 121.2(8) . . ?
F10 C46 C45 114.7(8) . . ?
C45 C46 C41 124.1(9) . . ?
C48 C47 C52 113.7(9) . . ?
C48 C47 B1 127.8(8) . . ?
C52 C47 B1 118.4(8) . . ?
F11 C48 C47 120.7(9) . . ?
F11 C48 C49 116.2(9) . . ?
C47 C48 C49 123.2(10) . . ?
F12 C49 C48 118.8(11) . . ?
C50 C49 F12 119.7(10) . . ?
C50 C49 C48 121.5(11) . . ?
F13 C50 C49 121.0(12) . . ?
F13 C50 C51 121.0(12) . . ?
C49 C50 C51 118.0(11) . . ?
F14 C51 C50 119.2(10) . . ?
F14 C51 C52 120.3(11) . . ?
C50 C51 C52 120.4(11) . . ?
F15 C52 C47 118.9(9) . . ?
F15 C52 C51 117.9(10) . . ?
C51 C52 C47 123.2(11) . . ?
C54 C53 C58 113.5(9) . . ?
C54 C53 B1 119.5(8) . . ?
C58 C53 B1 126.8(9) . . ?
F16 C54 C53 119.0(9) . . ?
F16 C54 C55 116.7(10) . . ?
C55 C54 C53 124.3(10) . . ?
F17 C55 C54 119.9(10) . . ?
F17 C55 C56 121.0(10) . . ?
C56 C55 C54 119.1(11) . . ?
F18 C56 C55 120.1(11) . . ?
C57 C56 F18 119.8(11) . . ?
C57 C56 C55 120.1(10) . . ?
F19 C57 C58 119.6(11) . . ?
C56 C57 F19 120.8(10) . . ?
C56 C57 C58 119.6(10) . . ?
F20 C58 C53 121.4(9) . . ?
F20 C58 C57 115.3(9) . . ?
C53 C58 C57 123.3(10) . . ?
C35 B1 C41 99.9(9) . . ?
C35 B1 C47 114.1(8) . . ?
C35 B1 C53 116.3(7) . . ?
C41 B1 C47 113.2(7) . . ?
C41 B1 C53 113.5(8) . . ?
C53 B1 C47 100.7(8) . . ?

_olex2_date_sample_completion    2017-11-20
_olex2_date_sample_data_collection 2017-11-20
_olex2_date_sample_submission    2017-11-20
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id rdpm83
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-Tb
_database_code_depnum_ccdc_archive 'CCDC 1844352'
_audit_update_record             
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;

_manchester_internal_coll_name   rdpm82
_manchester_internal_coll_client CAPG/FO
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 2s
_manchester_internal_coll_frame_width 0.5
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG/FO
_manchester_internal_coll_date   20/11/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 20/11/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 20/11/17
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 20/11/17
_manchester_internal_validation_user FO
_manchester_internal_validation_date 19/5/18
_manchester_internal_archive_date 19/5/18

_refine_special_details          
;
One peak was identified in the density map on the same axis of the Tb-B bond 
which was assigned as a second Tb atom with an occupancy of ca. 8%. Following
this, two disordered cyclopentadienyl rings and a second B atom were modelled 
around the disordered metal centre and their parameters restrained using SAME. 

The two disordered components were refined competitively, converging at a ratio 
of 0.9234(5):0.0766(5). 

Atoms Tb1A/Tb1B and B1A/B1B were constrained in order to have similar
anisotropic displacement parameters (EADP). Additionally, similarity restraints
were applied globally. 

The BH4 unit at B1A/B was assembled using DFIX and SADI commands, with H atoms 
refined using a riding model (UISO 1.5 parent).
;


_audit_creation_date             2018-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
conrad.goowin@manchester.ac.uk
fabrizio.ortu@manchester.ac.uk
david.manchester.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        '[Tb(Cpttt)29BH4)]'
_chemical_formula_moiety         '1(C34 H62 B1 Tb1)'
_chemical_formula_sum            'C34 H62 B Tb'
_chemical_formula_weight         640.56
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C11 H10 N O'
_chemical_oxdiff_usercomment     CAPG/FO
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'
B B 0.0013 0.0007 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3320(2)
_cell_length_b                   15.6294(3)
_cell_length_c                   20.5234(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.173(2)
_cell_angle_gamma                90
_cell_volume                     3271.78(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11602
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      30.0820
_cell_measurement_theta_min      2.4510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.541
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -20 7 0.0764
12 -6 -17 0.1429
-12 12 12 0.0993
2 -19 13 0.0924
10 -6 15 0.1044
1 3 -29 0.0574
-9 14 16 0.0870
4 -21 2 0.0669
-9 16 -4 0.0793
-13 9 2 0.1296
14 4 -11 0.1310
-3 3 -27 0.0364
3 8 25 0.0722
0 21 -9 0.0869
-5 13 22 0.0760
8 6 20 0.0885
5 20 6 0.1006

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.142
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
4.0000 -20.0000 7.0000 0.1228 0.2442 -0.9528
12.0000 -6.0000 -17.0000 0.3160 0.9278 -0.0775
-12.0000 12.0000 12.0000 -0.3369 -0.8865 0.3979
2.0000 -19.0000 13.0000 0.1314 0.0096 -0.9861
10.0000 -6.0000 15.0000 0.8149 0.0508 -0.5316
1.0000 3.0000 -29.0000 -0.4630 0.7243 0.5405
-9.0000 14.0000 16.0000 -0.0541 -0.9124 0.4023
4.0000 -21.0000 2.0000 0.0135 0.3846 -0.9210
-9.0000 16.0000 -4.0000 -0.4157 -0.4357 0.7767
-13.0000 9.0000 2.0000 -0.6283 -0.6260 0.4267
14.0000 4.0000 -11.0000 0.6786 0.7037 0.2341
-3.0000 3.0000 -27.0000 -0.6646 0.5359 0.5374
3.0000 8.0000 25.0000 0.7649 -0.6411 -0.0547
-0.0000 21.0000 -9.0000 0.0914 -0.0700 0.9971
-5.0000 13.0000 22.0000 0.2896 -0.9118 0.2474
8.0000 6.0000 20.0000 0.9432 -0.3142 -0.0968
5.0000 20.0000 6.0000 0.6692 -0.2622 0.7042

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24081
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         2.384
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00 -28.00   0.50    2.00    --   -7.70 -33.00  52.00   54
  2  ω     -3.00  23.00   0.50    2.00    --   -7.70  33.00-148.00   52
  3  ω     38.00  65.00   0.50    2.00    --   -7.70  38.00  90.00   54
  4  ω    -97.00 -50.00   0.50    2.00    --   -7.70 -38.00-120.00   94
  5  ω    -42.00  32.00   0.50    2.00    --   -7.70 -38.00-120.00  148
  6  ω    -47.00  29.00   0.50    2.00    --   -7.70  38.00  90.00  152
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0600611000
_diffrn_orient_matrix_UB_12      0.0126407000
_diffrn_orient_matrix_UB_13      0.0193441000
_diffrn_orient_matrix_UB_21      0.0344672000
_diffrn_orient_matrix_UB_22      -0.0141535000
_diffrn_orient_matrix_UB_23      -0.0252503000
_diffrn_orient_matrix_UB_31      -0.0065299000
_diffrn_orient_matrix_UB_32      0.0412241000
_diffrn_orient_matrix_UB_33      -0.0145976000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5231
_reflns_number_total             5942
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.036
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         5942
_refine_ls_number_restraints     1880
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_gt           0.0357
_refine_ls_restrained_S_all      0.949
_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)+(0.0724P)²+2.8169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1022

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H,H,H,H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 B1A-H1AA = B1A-H1AB = B1A-H1AC = B1A-H1AD
 1.1 with sigma of 0.02
 B1B-H1BB = B1B-H1BD = B1B-H1BA = B1B-H1BC
 1.1 with sigma of 0.02
 Tb1B-H1BD
 1.66 with sigma of 0.02
 Tb1A-H1AA \\sim Tb1A-H1AB
 with sigma of 0.02
 H1BA-H1BB \\sim H1BA-H1BC \\sim H1BA-H1BD \\sim H1BB-H1BC \\sim H1BB-H1BD
\\sim H1BC-H1BD
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(Tb1B) = Uanis(Tb1A)
Uanis(B1B) = Uanis(B1A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{Tb1A, C1A, C2A, C3A, C4A, C5A, C6A, C7A, C8A, C9A, C10A, C11A, C12A, C13A,
C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A,
C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, B1A} sigma for 1-2: 0.02, 1-3:
0.04
as
{Tb1B, C0AA, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B, C11B, C12B, C13B,
C14B, C15B, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B, C25B, C26B,
C27B, C28B, C29B, C30B, C31B, C32B, C33B, C34B, B1B}
6. Others
 Sof(Tb1B)=Sof(C0AA)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(H5B)=
 Sof(C6B)=Sof(C7B)=Sof(H7BC)=Sof(H7BA)=Sof(H7BB)=Sof(C8B)=Sof(H8BB)=Sof(H8BC)=
 Sof(H8BA)=Sof(C9B)=Sof(H9BB)=Sof(H9BA)=Sof(H9BC)=Sof(C10B)=Sof(C11B)=Sof(H11D)=
 Sof(H11F)=Sof(H11E)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13B)=
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14B)=Sof(C15B)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17B)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(C21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(C24B)=Sof(H24E)=Sof(H24D)=Sof(H24F)=
 Sof(C25B)=Sof(H25E)=Sof(H25F)=Sof(H25D)=Sof(C26B)=Sof(H26E)=Sof(H26F)=
 Sof(H26D)=Sof(C27B)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=
 Sof(C31B)=Sof(C32B)=Sof(H32F)=Sof(H32D)=Sof(H32E)=Sof(C33B)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(B1B)=Sof(H1BD)=
 Sof(H1BA)=Sof(H1BB)=Sof(H1BC)=1-FVAR(1)
 Sof(Tb1A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AC)=Sof(H8AA)=
 Sof(H8AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13A)=
 Sof(H13B)=Sof(H13A)=Sof(H13C)=Sof(C14A)=Sof(C15A)=Sof(H15C)=Sof(H15A)=
 Sof(H15B)=Sof(C16A)=Sof(H16B)=Sof(H16A)=Sof(H16C)=Sof(C17A)=Sof(H17C)=
 Sof(H17A)=Sof(H17B)=Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(C21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25A)=Sof(H25B)=Sof(H25A)=Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30C)=Sof(H30A)=Sof(H30B)=
 Sof(C31A)=Sof(C32A)=Sof(H32C)=Sof(H32A)=Sof(H32B)=Sof(C33A)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(B1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(H1AC)=Sof(H1AD)=FVAR(1)
7.a Me refined with riding coordinates:
 C7A(H7AA,H7AB,H7AC), C8A(H8AC,H8AA,H8AB), C9A(H9AA,H9AB,H9AC), C11A(H11A,H11B,
 H11C), C12A(H12A,H12B,H12C), C13A(H13B,H13A,H13C), C15A(H15C,H15A,H15B),
 C16A(H16B,H16A,H16C), C17A(H17C,H17A,H17B), C24A(H24A,H24B,H24C), C25A(H25B,
 H25A,H25C), C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C),
 C30A(H30C,H30A,H30B), C32A(H32C,H32A,H32B), C33A(H33A,H33B,H33C), C34A(H34A,
 H34B,H34C), C7B(H7BC,H7BA,H7BB), C8B(H8BB,H8BC,H8BA), C9B(H9BB,H9BA,H9BC),
 C11B(H11D,H11F,H11E), C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F), C15B(H15D,
 H15E,H15F), C16B(H16D,H16E,H16F), C17B(H17D,H17E,H17F), C24B(H24E,H24D,H24F),
 C25B(H25E,H25F,H25D), C26B(H26E,H26F,H26D), C28B(H28D,H28E,H28F), C29B(H29D,
 H29E,H29F), C30B(H30D,H30E,H30F), C32B(H32F,H32D,H32E), C33B(H33D,H33E,H33F),
 C34B(H34D,H34E,H34F)
7.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C5A(H5A), C19A(H19A), C22A(H22A), C2B(H2B), C5B(H5B), C19B(H19B),
 C22B(H22B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1A Tb 0.49831(2) 0.20481(2) 0.62072(2) 0.01435(10) Uani 0.9234(5) 1 d D U P A
1
C1A C 0.4708(3) 0.2437(2) 0.74469(16) 0.0132(7) Uani 0.9234(5) 1 d D U P A 1
C2A C 0.5313(4) 0.3135(2) 0.72166(18) 0.0174(7) Uani 0.9234(5) 1 d D U P A 1
H2A H 0.490709 0.366008 0.711417 0.021 Uiso 0.9234(5) 1 calc R . P A 1
C3A C 0.6648(4) 0.2949(2) 0.71552(19) 0.0167(7) Uani 0.9234(5) 1 d D U P A 1
C4A C 0.6843(4) 0.2058(2) 0.73320(19) 0.0137(7) Uani 0.9234(5) 1 d D U P A 1
C5A C 0.5629(4) 0.1759(2) 0.74833(17) 0.0149(7) Uani 0.9234(5) 1 d D U P A 1
H5A H 0.546078 0.119596 0.759128 0.018 Uiso 0.9234(5) 1 calc R . P A 1
C6A C 0.3336(4) 0.2385(3) 0.76260(17) 0.0166(7) Uani 0.9234(5) 1 d D U P A 1
C7A C 0.2462(4) 0.1841(3) 0.7104(2) 0.0333(10) Uani 0.9234(5) 1 d D U P A 1
H7AA H 0.284748 0.128567 0.707960 0.050 Uiso 0.9234(5) 1 calc R . P A 1
H7AB H 0.160711 0.178241 0.722572 0.050 Uiso 0.9234(5) 1 calc R . P A 1
H7AC H 0.238795 0.211732 0.668190 0.050 Uiso 0.9234(5) 1 calc R . P A 1
C8A C 0.2736(4) 0.3263(3) 0.7668(2) 0.0278(9) Uani 0.9234(5) 1 d D U P A 1
H8AC H 0.187389 0.320595 0.778197 0.042 Uiso 0.9234(5) 1 calc R . P A 1
H8AA H 0.327468 0.359440 0.800070 0.042 Uiso 0.9234(5) 1 calc R . P A 1
H8AB H 0.267895 0.354619 0.724971 0.042 Uiso 0.9234(5) 1 calc R . P A 1
C9A C 0.3385(5) 0.1930(3) 0.8295(2) 0.0285(9) Uani 0.9234(5) 1 d D U P A 1
H9AA H 0.376374 0.137245 0.827349 0.043 Uiso 0.9234(5) 1 calc R . P A 1
H9AB H 0.390898 0.225971 0.863400 0.043 Uiso 0.9234(5) 1 calc R . P A 1
H9AC H 0.251197 0.187597 0.839531 0.043 Uiso 0.9234(5) 1 calc R . P A 1
C10A C 0.7570(4) 0.3706(2) 0.70867(18) 0.0212(8) Uani 0.9234(5) 1 d D U P A 1
C11A C 0.8805(4) 0.3514(3) 0.6792(2) 0.0263(8) Uani 0.9234(5) 1 d D U P A 1
H11A H 0.929917 0.403126 0.677384 0.039 Uiso 0.9234(5) 1 calc R . P A 1
H11B H 0.932888 0.310134 0.706211 0.039 Uiso 0.9234(5) 1 calc R . P A 1
H11C H 0.856236 0.328917 0.635416 0.039 Uiso 0.9234(5) 1 calc R . P A 1
C12A C 0.6854(4) 0.4417(2) 0.6646(2) 0.0293(9) Uani 0.9234(5) 1 d D U P A 1
H12A H 0.606097 0.456979 0.680561 0.044 Uiso 0.9234(5) 1 calc R . P A 1
H12B H 0.741141 0.491053 0.665769 0.044 Uiso 0.9234(5) 1 calc R . P A 1
H12C H 0.664521 0.421376 0.620009 0.044 Uiso 0.9234(5) 1 calc R . P A 1
C13A C 0.7966(4) 0.4103(3) 0.77804(19) 0.0292(9) Uani 0.9234(5) 1 d D U P A 1
H13B H 0.719193 0.422482 0.796775 0.044 Uiso 0.9234(5) 1 calc R . P A 1
H13A H 0.850791 0.370699 0.805903 0.044 Uiso 0.9234(5) 1 calc R . P A 1
H13C H 0.844337 0.462332 0.774485 0.044 Uiso 0.9234(5) 1 calc R . P A 1
C14A C 0.8081(4) 0.1491(3) 0.74788(19) 0.0224(8) Uani 0.9234(5) 1 d D U P A 1
C15A C 0.8764(5) 0.1294(3) 0.6889(2) 0.0246(10) Uani 0.9234(5) 1 d D U P A 1
H15C H 0.900643 0.181933 0.669873 0.037 Uiso 0.9234(5) 1 calc R . P A 1
H15A H 0.953622 0.095898 0.703255 0.037 Uiso 0.9234(5) 1 calc R . P A 1
H15B H 0.817944 0.097850 0.656511 0.037 Uiso 0.9234(5) 1 calc R . P A 1
C16A C 0.7727(4) 0.0621(3) 0.7754(2) 0.0305(9) Uani 0.9234(5) 1 d D U P A 1
H16B H 0.729256 0.071077 0.812804 0.046 Uiso 0.9234(5) 1 calc R . P A 1
H16A H 0.715587 0.031445 0.741868 0.046 Uiso 0.9234(5) 1 calc R . P A 1
H16C H 0.851266 0.029493 0.788611 0.046 Uiso 0.9234(5) 1 calc R . P A 1
C17A C 0.9069(4) 0.1878(3) 0.8046(2) 0.0298(9) Uani 0.9234(5) 1 d D U P A 1
H17C H 0.863142 0.200025 0.841427 0.045 Uiso 0.9234(5) 1 calc R . P A 1
H17A H 0.976655 0.147813 0.817809 0.045 Uiso 0.9234(5) 1 calc R . P A 1
H17B H 0.942441 0.239794 0.789789 0.045 Uiso 0.9234(5) 1 calc R . P A 1
C18A C 0.5204(3) 0.2473(2) 0.49797(16) 0.0122(7) Uani 0.9234(5) 1 d D U P A 1
C19A C 0.4550(4) 0.3161(2) 0.52116(17) 0.0153(7) Uani 0.9234(5) 1 d D U P A 1
H19A H 0.491574 0.369920 0.530793 0.018 Uiso 0.9234(5) 1 calc R . P A 1
C20A C 0.3233(4) 0.2928(2) 0.52818(19) 0.0130(7) Uani 0.9234(5) 1 d D U P A 1
C21A C 0.3081(4) 0.2040(2) 0.5085(2) 0.0174(7) Uani 0.9234(5) 1 d D U P A 1
C22A C 0.4311(4) 0.1782(2) 0.49176(17) 0.0170(7) Uani 0.9234(5) 1 d D U P A 1
H22A H 0.449967 0.123306 0.478539 0.020 Uiso 0.9234(5) 1 calc R . P A 1
C23A C 0.6600(4) 0.2451(2) 0.48251(17) 0.0155(7) Uani 0.9234(5) 1 d D U P A 1
C24A C 0.7458(4) 0.1964(3) 0.5375(2) 0.0265(9) Uani 0.9234(5) 1 d D U P A 1
H24A H 0.710862 0.139944 0.540962 0.040 Uiso 0.9234(5) 1 calc R . P A 1
H24B H 0.833350 0.192320 0.527599 0.040 Uiso 0.9234(5) 1 calc R . P A 1
H24C H 0.747275 0.226145 0.578494 0.040 Uiso 0.9234(5) 1 calc R . P A 1
C25A C 0.7134(4) 0.3347(3) 0.4760(2) 0.0266(9) Uani 0.9234(5) 1 d D U P A 1
H25B H 0.658368 0.364555 0.441216 0.040 Uiso 0.9234(5) 1 calc R . P A 1
H25A H 0.714755 0.365002 0.516799 0.040 Uiso 0.9234(5) 1 calc R . P A 1
H25C H 0.800830 0.331177 0.465903 0.040 Uiso 0.9234(5) 1 calc R . P A 1
C26A C 0.6640(4) 0.1959(3) 0.4172(2) 0.0266(9) Uani 0.9234(5) 1 d D U P A 1
H26A H 0.630427 0.139112 0.420719 0.040 Uiso 0.9234(5) 1 calc R . P A 1
H26B H 0.611122 0.225387 0.381409 0.040 Uiso 0.9234(5) 1 calc R . P A 1
H26C H 0.752781 0.192831 0.409009 0.040 Uiso 0.9234(5) 1 calc R . P A 1
C27A C 0.2284(4) 0.3655(2) 0.53636(18) 0.0207(8) Uani 0.9234(5) 1 d D U P A 1
C28A C 0.2966(4) 0.4368(2) 0.5815(2) 0.0286(9) Uani 0.9234(5) 1 d D U P A 1
H28A H 0.234752 0.481566 0.585720 0.043 Uiso 0.9234(5) 1 calc R . P A 1
H28B H 0.328988 0.413543 0.624229 0.043 Uiso 0.9234(5) 1 calc R . P A 1
H28C H 0.368281 0.459745 0.562457 0.043 Uiso 0.9234(5) 1 calc R . P A 1
C29A C 0.1072(4) 0.3426(3) 0.56697(18) 0.0252(8) Uani 0.9234(5) 1 d D U P A 1
H29A H 0.055162 0.393004 0.569607 0.038 Uiso 0.9234(5) 1 calc R . P A 1
H29B H 0.056246 0.300569 0.540043 0.038 Uiso 0.9234(5) 1 calc R . P A 1
H29C H 0.134169 0.319883 0.610473 0.038 Uiso 0.9234(5) 1 calc R . P A 1
C30A C 0.1852(5) 0.4079(3) 0.46828(19) 0.0326(10) Uani 0.9234(5) 1 d D U P A 1
H30C H 0.125384 0.453784 0.472617 0.049 Uiso 0.9234(5) 1 calc R . P A 1
H30A H 0.260746 0.430069 0.452130 0.049 Uiso 0.9234(5) 1 calc R . P A 1
H30B H 0.142677 0.366168 0.437827 0.049 Uiso 0.9234(5) 1 calc R . P A 1
C31A C 0.1875(4) 0.1454(3) 0.49176(19) 0.0225(8) Uani 0.9234(5) 1 d D U P A 1
C32A C 0.1212(4) 0.1213(3) 0.5515(2) 0.0249(9) Uani 0.9234(5) 1 d D U P A 1
H32C H 0.094332 0.172395 0.571601 0.037 Uiso 0.9234(5) 1 calc R . P A 1
H32A H 0.045857 0.086207 0.536950 0.037 Uiso 0.9234(5) 1 calc R . P A 1
H32B H 0.182122 0.090271 0.583082 0.037 Uiso 0.9234(5) 1 calc R . P A 1
C33A C 0.2266(4) 0.0610(3) 0.4632(2) 0.0286(9) Uani 0.9234(5) 1 d D U P A 1
H33A H 0.150686 0.025121 0.452974 0.043 Uiso 0.9234(5) 1 calc R . P A 1
H33B H 0.262731 0.071952 0.423731 0.043 Uiso 0.9234(5) 1 calc R . P A 1
H33C H 0.290916 0.032874 0.494933 0.043 Uiso 0.9234(5) 1 calc R . P A 1
C34A C 0.0858(4) 0.1856(3) 0.4369(2) 0.0295(9) Uani 0.9234(5) 1 d D U P A 1
H34A H 0.056886 0.239525 0.451821 0.044 Uiso 0.9234(5) 1 calc R . P A 1
H34B H 0.125218 0.194502 0.398095 0.044 Uiso 0.9234(5) 1 calc R . P A 1
H34C H 0.012076 0.147880 0.426594 0.044 Uiso 0.9234(5) 1 calc R . P A 1
B1A B 0.4958(4) 0.0312(3) 0.62175(19) 0.0237(10) Uani 0.9234(5) 1 d D U P A 1
Tb1B Tb 0.4993(2) 0.29414(12) 0.63118(11) 0.01435(10) Uani 0.0766(5) 1 d D U P
A -2
C0AA C 0.7125(16) 0.2487(17) 0.7160(9) 0.023(2) Uani 0.0766(5) 1 d D U P A -2
C2B C 0.626(2) 0.1822(14) 0.7169(10) 0.021(2) Uani 0.0766(5) 1 d D U P A -2
H2B H 0.638759 0.128615 0.699235 0.025 Uiso 0.0766(5) 1 calc R . P A -2
C3B C 0.514(2) 0.2023(13) 0.7475(8) 0.020(2) Uani 0.0766(5) 1 d D U P A -2
C4B C 0.532(2) 0.2913(14) 0.7658(7) 0.023(2) Uani 0.0766(5) 1 d D U P A -2
C5B C 0.652(2) 0.3169(16) 0.7445(9) 0.023(2) Uani 0.0766(5) 1 d D U P A -2
H5B H 0.686013 0.372050 0.748929 0.027 Uiso 0.0766(5) 1 calc R . P A -2
C6B C 0.835(2) 0.2459(19) 0.6824(15) 0.030(3) Uani 0.0766(5) 1 d D U P A -2
C7B C 0.808(5) 0.287(3) 0.6135(16) 0.036(6) Uani 0.0766(5) 1 d D U P A -2
H7BC H 0.779965 0.345486 0.617481 0.054 Uiso 0.0766(5) 1 calc R . P A -2
H7BA H 0.886578 0.286641 0.594114 0.054 Uiso 0.0766(5) 1 calc R . P A -2
H7BB H 0.740406 0.255999 0.585951 0.054 Uiso 0.0766(5) 1 calc R . P A -2
C8B C 0.880(6) 0.153(2) 0.678(3) 0.028(6) Uani 0.0766(5) 1 d D U P A -2
H8BB H 0.956307 0.151550 0.657032 0.043 Uiso 0.0766(5) 1 calc R . P A -2
H8BC H 0.900141 0.129764 0.721663 0.043 Uiso 0.0766(5) 1 calc R . P A -2
H8BA H 0.810906 0.120509 0.652711 0.043 Uiso 0.0766(5) 1 calc R . P A -2
C9B C 0.948(4) 0.295(3) 0.724(2) 0.042(7) Uani 0.0766(5) 1 d D U P A -2
H9BB H 0.923378 0.353870 0.727594 0.063 Uiso 0.0766(5) 1 calc R . P A -2
H9BA H 0.967381 0.270113 0.767013 0.063 Uiso 0.0766(5) 1 calc R . P A -2
H9BC H 1.024619 0.292083 0.702719 0.063 Uiso 0.0766(5) 1 calc R . P A -2
C10B C 0.407(3) 0.1327(16) 0.7526(13) 0.024(3) Uani 0.0766(5) 1 d D U P A -2
C11B C 0.282(3) 0.163(3) 0.777(2) 0.027(5) Uani 0.0766(5) 1 d D U P A -2
H11D H 0.244359 0.209404 0.749130 0.040 Uiso 0.0766(5) 1 calc R . P A -2
H11F H 0.221046 0.116912 0.774446 0.040 Uiso 0.0766(5) 1 calc R . P A -2
H11E H 0.303731 0.182851 0.821386 0.040 Uiso 0.0766(5) 1 calc R . P A -2
C12B C 0.360(4) 0.093(3) 0.6832(16) 0.040(6) Uani 0.0766(5) 1 d D U P A -2
H12D H 0.434477 0.072729 0.665197 0.060 Uiso 0.0766(5) 1 calc R . P A -2
H12E H 0.301213 0.046789 0.687028 0.060 Uiso 0.0766(5) 1 calc R . P A -2
H12F H 0.315654 0.136331 0.654523 0.060 Uiso 0.0766(5) 1 calc R . P A -2
C13B C 0.465(4) 0.059(2) 0.797(2) 0.039(7) Uani 0.0766(5) 1 d D U P A -2
H13D H 0.544001 0.038875 0.783144 0.059 Uiso 0.0766(5) 1 calc R . P A -2
H13E H 0.485742 0.079162 0.842148 0.059 Uiso 0.0766(5) 1 calc R . P A -2
H13F H 0.403057 0.013223 0.795208 0.059 Uiso 0.0766(5) 1 calc R . P A -2
C14B C 0.454(3) 0.3527(18) 0.8047(13) 0.035(4) Uani 0.0766(5) 1 d D U P A -2
C15B C 0.402(5) 0.432(3) 0.764(2) 0.052(8) Uani 0.0766(5) 1 d D U P A -2
H15D H 0.345978 0.413985 0.724829 0.078 Uiso 0.0766(5) 1 calc R . P A -2
H15E H 0.353023 0.466948 0.790168 0.078 Uiso 0.0766(5) 1 calc R . P A -2
H15F H 0.474223 0.464049 0.752974 0.078 Uiso 0.0766(5) 1 calc R . P A -2
C16B C 0.542(5) 0.383(3) 0.8669(19) 0.051(8) Uani 0.0766(5) 1 d D U P A -2
H16D H 0.576041 0.334802 0.892913 0.077 Uiso 0.0766(5) 1 calc R . P A -2
H16E H 0.613824 0.415784 0.854974 0.077 Uiso 0.0766(5) 1 calc R . P A -2
H16F H 0.492623 0.418683 0.892167 0.077 Uiso 0.0766(5) 1 calc R . P A -2
C17B C 0.339(4) 0.308(3) 0.831(2) 0.033(5) Uani 0.0766(5) 1 d D U P A -2
H17D H 0.278013 0.286164 0.794296 0.050 Uiso 0.0766(5) 1 calc R . P A -2
H17E H 0.372304 0.261027 0.859066 0.050 Uiso 0.0766(5) 1 calc R . P A -2
H17F H 0.295470 0.347839 0.855306 0.050 Uiso 0.0766(5) 1 calc R . P A -2
C18B C 0.2951(16) 0.2514(16) 0.5412(9) 0.023(2) Uani 0.0766(5) 1 d D U P A -2
C19B C 0.381(2) 0.1828(13) 0.5404(10) 0.021(2) Uani 0.0766(5) 1 d D U P A -2
H19B H 0.367590 0.128556 0.556667 0.026 Uiso 0.0766(5) 1 calc R . P A -2
C20B C 0.493(2) 0.2060(13) 0.5116(8) 0.022(2) Uani 0.0766(5) 1 d D U P A -2
C21B C 0.475(2) 0.2945(14) 0.4938(7) 0.021(2) Uani 0.0766(5) 1 d D U P A -2
C22B C 0.354(2) 0.3199(16) 0.5138(8) 0.021(2) Uani 0.0766(5) 1 d D U P A -2
H22B H 0.319890 0.374940 0.509277 0.025 Uiso 0.0766(5) 1 calc R . P A -2
C23B C 0.164(2) 0.2463(19) 0.5663(15) 0.031(4) Uani 0.0766(5) 1 d D U P A -2
C24B C 0.181(5) 0.291(3) 0.6334(17) 0.040(6) Uani 0.0766(5) 1 d D U P A -2
H24E H 0.099336 0.288920 0.650402 0.059 Uiso 0.0766(5) 1 calc R . P A -2
H24D H 0.247800 0.263016 0.663472 0.059 Uiso 0.0766(5) 1 calc R . P A -2
H24F H 0.204806 0.349817 0.628265 0.059 Uiso 0.0766(5) 1 calc R . P A -2
C25B C 0.123(4) 0.153(2) 0.574(3) 0.030(6) Uani 0.0766(5) 1 d D U P A -2
H25E H 0.040691 0.151675 0.589368 0.045 Uiso 0.0766(5) 1 calc R . P A -2
H25F H 0.114582 0.125372 0.531385 0.045 Uiso 0.0766(5) 1 calc R . P A -2
H25D H 0.188500 0.124473 0.604285 0.045 Uiso 0.0766(5) 1 calc R . P A -2
C26B C 0.052(4) 0.293(3) 0.521(2) 0.042(7) Uani 0.0766(5) 1 d D U P A -2
H26E H -0.027603 0.287696 0.539468 0.063 Uiso 0.0766(5) 1 calc R . P A -2
H26F H 0.073878 0.352475 0.518332 0.063 Uiso 0.0766(5) 1 calc R . P A -2
H26D H 0.040173 0.267993 0.478013 0.063 Uiso 0.0766(5) 1 calc R . P A -2
C27B C 0.596(3) 0.1398(16) 0.4981(13) 0.024(3) Uani 0.0766(5) 1 d D U P A -2
C28B C 0.641(5) 0.094(3) 0.5654(18) 0.046(8) Uani 0.0766(5) 1 d D U P A -2
H28D H 0.566531 0.069972 0.581085 0.069 Uiso 0.0766(5) 1 calc R . P A -2
H28E H 0.702151 0.049318 0.559653 0.069 Uiso 0.0766(5) 1 calc R . P A -2
H28F H 0.683128 0.134749 0.597018 0.069 Uiso 0.0766(5) 1 calc R . P A -2
C29B C 0.726(3) 0.173(3) 0.482(2) 0.027(5) Uani 0.0766(5) 1 d D U P A -2
H29D H 0.760159 0.216637 0.512956 0.041 Uiso 0.0766(5) 1 calc R . P A -2
H29E H 0.788133 0.126936 0.483977 0.041 Uiso 0.0766(5) 1 calc R . P A -2
H29F H 0.712809 0.196948 0.438050 0.041 Uiso 0.0766(5) 1 calc R . P A -2
C30B C 0.539(4) 0.070(2) 0.449(2) 0.038(8) Uani 0.0766(5) 1 d D U P A -2
H30D H 0.457512 0.049970 0.460169 0.057 Uiso 0.0766(5) 1 calc R . P A -2
H30E H 0.524348 0.093070 0.405085 0.057 Uiso 0.0766(5) 1 calc R . P A -2
H30F H 0.599672 0.023058 0.451012 0.057 Uiso 0.0766(5) 1 calc R . P A -2
C31B C 0.541(3) 0.3499(17) 0.4469(12) 0.026(3) Uani 0.0766(5) 1 d D U P A -2
C32B C 0.670(4) 0.311(3) 0.431(2) 0.028(5) Uani 0.0766(5) 1 d D U P A -2
H32F H 0.651802 0.256994 0.408704 0.042 Uiso 0.0766(5) 1 calc R . P A -2
H32D H 0.707939 0.349226 0.402125 0.042 Uiso 0.0766(5) 1 calc R . P A -2
H32E H 0.730823 0.302566 0.470614 0.042 Uiso 0.0766(5) 1 calc R . P A -2
C33B C 0.577(5) 0.435(2) 0.481(2) 0.046(8) Uani 0.0766(5) 1 d D U P A -2
H33D H 0.619476 0.471267 0.453176 0.068 Uiso 0.0766(5) 1 calc R . P A -2
H33E H 0.499433 0.462732 0.490798 0.068 Uiso 0.0766(5) 1 calc R . P A -2
H33F H 0.636139 0.425269 0.521885 0.068 Uiso 0.0766(5) 1 calc R . P A -2
C34B C 0.452(5) 0.372(3) 0.3811(16) 0.046(8) Uani 0.0766(5) 1 d D U P A -2
H34D H 0.426346 0.320483 0.357309 0.068 Uiso 0.0766(5) 1 calc R . P A -2
H34E H 0.375472 0.401689 0.390252 0.068 Uiso 0.0766(5) 1 calc R . P A -2
H34F H 0.499138 0.408187 0.355090 0.068 Uiso 0.0766(5) 1 calc R . P A -2
B1B B 0.504(4) 0.4665(10) 0.6313(13) 0.0237(10) Uani 0.0766(5) 1 d D U P A -2
H1AA H 0.586(3) 0.072(2) 0.620(2) 0.036 Uiso 0.9234(5) 1 d DR . P A 1
H1AB H 0.407(3) 0.073(2) 0.623(2) 0.036 Uiso 0.9234(5) 1 d DR . P A 1
H1AC H 0.526(4) -0.010(3) 0.6650(16) 0.036 Uiso 0.9234(5) 1 d DR . P A 1
H1AD H 0.471(5) -0.002(3) 0.5740(14) 0.036 Uiso 0.9234(5) 1 d DR . P A 1
H1BD H 0.475(12) 0.3990(11) 0.634(13) 0.036 Uiso 0.0766(5) 1 d DR . P A -2
H1BA H 0.419(9) 0.508(4) 0.633(12) 0.036 Uiso 0.0766(5) 1 d DR . P A -2
H1BB H 0.54(2) 0.477(13) 0.585(6) 0.036 Uiso 0.0766(5) 1 d DR . P A -2
H1BC H 0.581(16) 0.482(16) 0.673(8) 0.036 Uiso 0.0766(5) 1 d DR . 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
Tb1A C1A 2.675(3) . ?
Tb1A C2A 2.659(4) . ?
Tb1A C3A 2.768(4) . ?
Tb1A C4A 2.758(4) . ?
Tb1A C5A 2.637(3) . ?
Tb1A C18A 2.650(3) . ?
Tb1A C19A 2.667(4) . ?
Tb1A C20A 2.770(4) . ?
Tb1A C21A 2.779(4) . ?
Tb1A C22A 2.660(4) . ?
C1A C2A 1.378(5) . ?
C1A C5A 1.418(5) . ?
C1A C6A 1.523(5) . ?
C2A C3A 1.435(5) . ?
C3A C4A 1.445(5) . ?
C3A C10A 1.540(5) . ?
C4A C5A 1.419(5) . ?
C4A C14A 1.547(5) . ?
C6A C7A 1.541(6) . ?
C6A C8A 1.514(6) . ?
C6A C9A 1.540(5) . ?
C10A C11A 1.526(5) . ?
C10A C12A 1.545(6) . ?
C10A C13A 1.547(5) . ?
C14A C15A 1.526(6) . ?
C14A C16A 1.538(6) . ?
C14A C17A 1.544(6) . ?
C18A C19A 1.394(5) . ?
C18A C22A 1.413(5) . ?
C18A C23A 1.526(5) . ?
C19A C20A 1.437(5) . ?
C20A C21A 1.448(5) . ?
C20A C27A 1.528(5) . ?
C21A C22A 1.426(5) . ?
C21A C31A 1.540(5) . ?
C23A C24A 1.523(5) . ?
C23A C25A 1.519(5) . ?
C23A C26A 1.551(5) . ?
C27A C28A 1.545(6) . ?
C27A C29A 1.530(5) . ?
C27A C30A 1.546(5) . ?
C31A C32A 1.544(5) . ?
C31A C33A 1.524(6) . ?
C31A C34A 1.547(6) . ?
Tb1B C0AA 2.676(14) . ?
Tb1B C2B 2.672(15) . ?
Tb1B C3B 2.770(14) . ?
Tb1B C4B 2.730(14) . ?
Tb1B C5B 2.618(15) . ?
Tb1B C18B 2.658(14) . ?
Tb1B C19B 2.695(15) . ?
Tb1B C20B 2.806(14) . ?
Tb1B C21B 2.790(14) . ?
Tb1B C22B 2.656(14) . ?
Tb1B B1B 2.695(15) . ?
C0AA C2B 1.374(18) . ?
C0AA C5B 1.407(18) . ?
C0AA C6B 1.535(18) . ?
C2B C3B 1.437(19) . ?
C3B C4B 1.446(17) . ?
C3B C10B 1.565(17) . ?
C4B C5B 1.434(19) . ?
C4B C14B 1.555(17) . ?
C6B C7B 1.54(2) . ?
C6B C8B 1.52(2) . ?
C6B C9B 1.54(2) . ?
C10B C11B 1.526(19) . ?
C10B C12B 1.56(2) . ?
C10B C13B 1.536(19) . ?
C14B C15B 1.54(2) . ?
C14B C16B 1.52(2) . ?
C14B C17B 1.55(2) . ?
C18B C19B 1.397(18) . ?
C18B C22B 1.394(18) . ?
C18B C23B 1.525(17) . ?
C19B C20B 1.428(19) . ?
C20B C21B 1.436(17) . ?
C20B C27B 1.540(17) . ?
C21B C22B 1.426(19) . ?
C21B C31B 1.537(17) . ?
C23B C24B 1.53(2) . ?
C23B C25B 1.53(2) . ?
C23B C26B 1.547(19) . ?
C27B C28B 1.56(2) . ?
C27B C29B 1.529(19) . ?
C27B C30B 1.539(19) . ?
C31B C32B 1.549(19) . ?
C31B C33B 1.53(2) . ?
C31B C34B 1.548(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1A Tb1A C3A 50.51(11) . . ?
C1A Tb1A C4A 50.79(11) . . ?
C1A Tb1A C20A 112.51(11) . . ?
C1A Tb1A C21A 128.40(11) . . ?
C2A Tb1A C1A 29.95(11) . . ?
C2A Tb1A C3A 30.58(11) . . ?
C2A Tb1A C4A 50.10(11) . . ?
C2A Tb1A C19A 99.50(13) . . ?
C2A Tb1A C20A 101.85(11) . . ?
C2A Tb1A C21A 129.38(11) . . ?
C2A Tb1A C22A 148.87(12) . . ?
C3A Tb1A C20A 119.59(12) . . ?
C3A Tb1A C21A 149.66(10) . . ?
C4A Tb1A C3A 30.31(10) . . ?
C4A Tb1A C20A 149.58(10) . . ?
C4A Tb1A C21A 179.17(9) . . ?
C5A Tb1A C1A 30.96(11) . . ?
C5A Tb1A C2A 49.84(12) . . ?
C5A Tb1A C3A 50.10(11) . . ?
C5A Tb1A C4A 30.39(11) . . ?
C5A Tb1A C18A 160.18(11) . . ?
C5A Tb1A C19A 149.10(10) . . ?
C5A Tb1A C20A 143.17(11) . . ?
C5A Tb1A C21A 148.86(11) . . ?
C5A Tb1A C22A 161.12(13) . . ?
C18A Tb1A C1A 152.34(11) . . ?
C18A Tb1A C2A 124.11(11) . . ?
C18A Tb1A C3A 113.75(11) . . ?
C18A Tb1A C4A 129.80(11) . . ?
C18A Tb1A C19A 30.40(10) . . ?
C18A Tb1A C20A 50.91(11) . . ?
C18A Tb1A C21A 50.95(11) . . ?
C18A Tb1A C22A 30.86(11) . . ?
C19A Tb1A C1A 123.40(11) . . ?
C19A Tb1A C3A 102.50(11) . . ?
C19A Tb1A C4A 130.32(11) . . ?
C19A Tb1A C20A 30.58(11) . . ?
C19A Tb1A C21A 50.04(11) . . ?
C20A Tb1A C21A 30.24(10) . . ?
C22A Tb1A C1A 158.70(11) . . ?
C22A Tb1A C3A 144.44(11) . . ?
C22A Tb1A C4A 150.50(11) . . ?
C22A Tb1A C19A 49.78(11) . . ?
C22A Tb1A C20A 49.99(11) . . ?
C22A Tb1A C21A 30.31(11) . . ?
C2A C1A Tb1A 74.4(2) . . ?
C2A C1A C5A 105.9(3) . . ?
C2A C1A C6A 128.0(3) . . ?
C5A C1A Tb1A 73.05(19) . . ?
C5A C1A C6A 126.2(3) . . ?
C6A C1A Tb1A 117.5(2) . . ?
C1A C2A Tb1A 75.7(2) . . ?
C1A C2A C3A 111.3(3) . . ?
C3A C2A Tb1A 78.9(2) . . ?
C2A C3A Tb1A 70.5(2) . . ?
C2A C3A C4A 105.7(3) . . ?
C2A C3A C10A 118.0(3) . . ?
C4A C3A Tb1A 74.5(2) . . ?
C4A C3A C10A 134.4(4) . . ?
C10A C3A Tb1A 130.6(2) . . ?
C3A C4A Tb1A 75.2(2) . . ?
C3A C4A C14A 132.8(3) . . ?
C5A C4A Tb1A 70.1(2) . . ?
C5A C4A C3A 106.3(3) . . ?
C5A C4A C14A 120.0(3) . . ?
C14A C4A Tb1A 127.2(2) . . ?
C1A C5A Tb1A 75.99(19) . . ?
C1A C5A C4A 110.5(3) . . ?
C4A C5A Tb1A 79.5(2) . . ?
C1A C6A C7A 109.0(3) . . ?
C1A C6A C9A 109.9(3) . . ?
C8A C6A C1A 111.8(3) . . ?
C8A C6A C7A 109.9(3) . . ?
C8A C6A C9A 108.8(3) . . ?
C9A C6A C7A 107.3(3) . . ?
C3A C10A C12A 111.2(3) . . ?
C3A C10A C13A 107.5(3) . . ?
C11A C10A C3A 117.0(3) . . ?
C11A C10A C12A 105.2(3) . . ?
C11A C10A C13A 109.2(3) . . ?
C12A C10A C13A 106.4(3) . . ?
C15A C14A C4A 115.7(3) . . ?
C15A C14A C16A 106.2(3) . . ?
C15A C14A C17A 110.1(4) . . ?
C16A C14A C4A 109.9(3) . . ?
C16A C14A C17A 103.7(3) . . ?
C17A C14A C4A 110.4(3) . . ?
C19A C18A Tb1A 75.5(2) . . ?
C19A C18A C22A 106.0(3) . . ?
C19A C18A C23A 127.9(3) . . ?
C22A C18A Tb1A 74.94(19) . . ?
C22A C18A C23A 126.1(3) . . ?
C23A C18A Tb1A 114.8(2) . . ?
C18A C19A Tb1A 74.1(2) . . ?
C18A C19A C20A 110.9(3) . . ?
C20A C19A Tb1A 78.7(2) . . ?
C19A C20A Tb1A 70.7(2) . . ?
C19A C20A C21A 106.1(3) . . ?
C19A C20A C27A 117.2(3) . . ?
C21A C20A Tb1A 75.2(2) . . ?
C21A C20A C27A 134.5(4) . . ?
C27A C20A Tb1A 130.9(2) . . ?
C20A C21A Tb1A 74.5(2) . . ?
C20A C21A C31A 132.9(3) . . ?
C22A C21A Tb1A 70.2(2) . . ?
C22A C21A C20A 106.1(3) . . ?
C22A C21A C31A 119.9(3) . . ?
C31A C21A Tb1A 128.9(2) . . ?
C18A C22A Tb1A 74.2(2) . . ?
C18A C22A C21A 110.9(3) . . ?
C21A C22A Tb1A 79.5(2) . . ?
C18A C23A C26A 110.3(3) . . ?
C24A C23A C18A 108.4(3) . . ?
C24A C23A C26A 107.5(3) . . ?
C25A C23A C18A 111.4(3) . . ?
C25A C23A C24A 110.5(3) . . ?
C25A C23A C26A 108.7(3) . . ?
C20A C27A C28A 111.3(3) . . ?
C20A C27A C29A 116.9(3) . . ?
C20A C27A C30A 108.5(3) . . ?
C28A C27A C30A 105.7(3) . . ?
C29A C27A C28A 104.3(3) . . ?
C29A C27A C30A 109.5(3) . . ?
C21A C31A C32A 114.4(3) . . ?
C21A C31A C34A 110.7(3) . . ?
C32A C31A C34A 110.0(3) . . ?
C33A C31A C21A 110.2(3) . . ?
C33A C31A C32A 105.8(3) . . ?
C33A C31A C34A 105.2(3) . . ?
C0AA Tb1B C3B 51.4(5) . . ?
C0AA Tb1B C4B 51.7(5) . . ?
C0AA Tb1B C19B 120.8(7) . . ?
C0AA Tb1B C20B 109.8(6) . . ?
C0AA Tb1B C21B 126.2(6) . . ?
C0AA Tb1B B1B 104.6(7) . . ?
C2B Tb1B C0AA 29.8(4) . . ?
C2B Tb1B C3B 30.6(4) . . ?
C2B Tb1B C4B 49.7(6) . . ?
C2B Tb1B C19B 98.7(7) . . ?
C2B Tb1B C20B 101.2(6) . . ?
C2B Tb1B C21B 128.6(7) . . ?
C2B Tb1B B1B 130.3(7) . . ?
C3B Tb1B C20B 119.3(6) . . ?
C3B Tb1B C21B 148.9(6) . . ?
C4B Tb1B C3B 30.5(4) . . ?
C4B Tb1B C20B 149.2(6) . . ?
C4B Tb1B C21B 177.9(7) . . ?
C5B Tb1B C0AA 30.8(4) . . ?
C5B Tb1B C2B 48.8(6) . . ?
C5B Tb1B C3B 50.4(6) . . ?
C5B Tb1B C4B 31.0(4) . . ?
C5B Tb1B C18B 161.9(7) . . ?
C5B Tb1B C19B 147.5(7) . . ?
C5B Tb1B C20B 140.3(6) . . ?
C5B Tb1B C21B 147.4(7) . . ?
C5B Tb1B C22B 163.3(8) . . ?
C5B Tb1B B1B 81.7(7) . . ?
C18B Tb1B C0AA 149.9(7) . . ?
C18B Tb1B C2B 123.0(7) . . ?
C18B Tb1B C3B 113.4(6) . . ?
C18B Tb1B C4B 131.0(6) . . ?
C18B Tb1B C19B 30.2(4) . . ?
C18B Tb1B C20B 50.6(5) . . ?
C18B Tb1B C21B 50.5(5) . . ?
C18B Tb1B B1B 105.3(7) . . ?
C19B Tb1B C3B 102.6(6) . . ?
C19B Tb1B C4B 131.2(7) . . ?
C19B Tb1B C20B 30.0(4) . . ?
C19B Tb1B C21B 49.0(5) . . ?
C19B Tb1B B1B 130.8(7) . . ?
C21B Tb1B C20B 29.7(4) . . ?
C22B Tb1B C0AA 156.4(7) . . ?
C22B Tb1B C2B 147.4(7) . . ?
C22B Tb1B C3B 143.7(7) . . ?
C22B Tb1B C4B 151.8(7) . . ?
C22B Tb1B C18B 30.4(4) . . ?
C22B Tb1B C19B 49.0(6) . . ?
C22B Tb1B C20B 49.5(6) . . ?
C22B Tb1B C21B 30.2(4) . . ?
C22B Tb1B B1B 81.8(7) . . ?
B1B Tb1B C3B 121.2(7) . . ?
B1B Tb1B C4B 90.9(6) . . ?
B1B Tb1B C20B 119.3(7) . . ?
B1B Tb1B C21B 89.9(6) . . ?
C2B C0AA Tb1B 74.9(8) . . ?
C2B C0AA C5B 103.6(15) . . ?
C2B C0AA C6B 124.7(19) . . ?
C5B C0AA Tb1B 72.3(8) . . ?
C5B C0AA C6B 131.3(19) . . ?
C6B C0AA Tb1B 111.6(13) . . ?
C0AA C2B Tb1B 75.3(8) . . ?
C0AA C2B C3B 114.3(16) . . ?
C3B C2B Tb1B 78.5(8) . . ?
C2B C3B Tb1B 70.9(8) . . ?
C2B C3B C4B 104.0(14) . . ?
C2B C3B C10B 120.2(17) . . ?
C4B C3B Tb1B 73.2(8) . . ?
C4B C3B C10B 135.8(19) . . ?
C10B C3B Tb1B 118.4(13) . . ?
C3B C4B Tb1B 76.3(8) . . ?
C3B C4B C14B 132.0(18) . . ?
C5B C4B Tb1B 70.2(8) . . ?
C5B C4B C3B 105.9(14) . . ?
C5B C4B C14B 122.0(17) . . ?
C14B C4B Tb1B 121.2(14) . . ?
C0AA C5B Tb1B 76.9(8) . . ?
C0AA C5B C4B 112.2(16) . . ?
C4B C5B Tb1B 78.8(8) . . ?
C0AA C6B C7B 111(2) . . ?
C0AA C6B C9B 110(2) . . ?
C8B C6B C0AA 109(2) . . ?
C8B C6B C7B 111(2) . . ?
C8B C6B C9B 107(2) . . ?
C9B C6B C7B 108(2) . . ?
C11B C10B C3B 116(2) . . ?
C11B C10B C12B 105(2) . . ?
C11B C10B C13B 108(2) . . ?
C12B C10B C3B 110(2) . . ?
C13B C10B C3B 110(2) . . ?
C13B C10B C12B 107(2) . . ?
C15B C14B C4B 113(2) . . ?
C15B C14B C17B 109(2) . . ?
C16B C14B C4B 110(2) . . ?
C16B C14B C15B 108(2) . . ?
C16B C14B C17B 104(2) . . ?
C17B C14B C4B 113(2) . . ?
C19B C18B Tb1B 76.3(8) . . ?
C19B C18B C23B 124.5(18) . . ?
C22B C18B Tb1B 74.7(8) . . ?
C22B C18B C19B 105.3(15) . . ?
C22B C18B C23B 130.3(19) . . ?
C23B C18B Tb1B 115.3(14) . . ?
C18B C19B Tb1B 73.4(8) . . ?
C18B C19B C20B 111.7(16) . . ?
C20B C19B Tb1B 79.3(8) . . ?
C19B C20B Tb1B 70.7(8) . . ?
C19B C20B C21B 105.4(14) . . ?
C19B C20B C27B 122.1(17) . . ?
C21B C20B Tb1B 74.5(8) . . ?
C21B C20B C27B 132.1(19) . . ?
C27B C20B Tb1B 124.6(13) . . ?
C20B C21B Tb1B 75.8(8) . . ?
C20B C21B C31B 130.2(18) . . ?
C22B C21B Tb1B 69.7(8) . . ?
C22B C21B C20B 106.4(15) . . ?
C22B C21B C31B 121.5(17) . . ?
C31B C21B Tb1B 131.0(15) . . ?
C18B C22B Tb1B 74.9(8) . . ?
C18B C22B C21B 111.2(16) . . ?
C21B C22B Tb1B 80.1(8) . . ?
C18B C23B C24B 108(2) . . ?
C18B C23B C25B 111(2) . . ?
C18B C23B C26B 113(2) . . ?
C24B C23B C26B 107(2) . . ?
C25B C23B C24B 110(2) . . ?
C25B C23B C26B 108(2) . . ?
C20B C27B C28B 105(2) . . ?
C29B C27B C20B 118(2) . . ?
C29B C27B C28B 102(2) . . ?
C29B C27B C30B 111(2) . . ?
C30B C27B C20B 113(2) . . ?
C30B C27B C28B 107(2) . . ?
C21B C31B C32B 114(2) . . ?
C21B C31B C34B 114(2) . . ?
C33B C31B C21B 108(2) . . ?
C33B C31B C32B 107(2) . . ?
C33B C31B C34B 106(2) . . ?
C34B C31B C32B 108(2) . . ?

_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id rdpm82
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.413
_oxdiff_exptl_absorpt_empirical_full_min 0.636
_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_2-Y
_database_code_depnum_ccdc_archive 'CCDC 1844353'
_audit_update_record             
;
2018-05-21 deposited with the CCDC.
2018-07-24 downloaded from the CCDC.
;

_manchester_internal_coll_name   adpm454
_manchester_internal_coll_client CAPG/FO
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 15s
_manchester_internal_coll_frame_width 0.8
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   8/12/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 8/12/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 8/12/17
_manchester_internal_refinement_user CAPG/FO
_manchester_internal_refinement_date 9/12/17
_manchester_internal_validation_user FO
_manchester_internal_validation_date 19/5/18
_manchester_internal_archive_date 19/5/18

# start Validation Reply Form
_vrf_PLAT973_2-Y                 
;
PROBLEM: Check Calcd Positive Resid. Density on       Y1B       3.06 eA-3  
RESPONSE: 
Large residual density is located at the positions of unresolved modulation on 
the positions where additioinal cyclopentadienyl rings would be located. This 
is a feature we have observed with numerous ML2X-type complexes. See 
_refine_special_details for details on how one component was modelled. 
;
# end Validation Reply Form

_refine_special_details          
;
Large residual density is located at the positions of unresolved modulation on 
the positions where additioinal cyclopentadienyl rings would be located. This 
is a feature we have observed with numerous ML2X-type complexes. See below for 
details on how one component was modelled. 

One peak was identified in the density map on the same axis of the Y-B bond 
which was assigned as a second Y atom with an occupancy of ca. 10%. Following
this, two disordered cyclopentadienyl rings and a second B atom were modelled 
around the disordered metal centre and their parameters restrained using SAME. 

The two disordered components were refined competitively, converging at a ratio 
of 0.899(1):0.101(1). 

Atoms Y1A/Y1B and B1A/B1B were constrained in order to have similar
anisotropic displacement parameters (EADP), and both B atoms had to be 
restrained to be approximately isotropic (ISOR) Additionally, similarity 
restraints were applied globally. 

The BH4 unit at B1A/B was assembled using DFIX commands, with H atoms refined 
using a riding model (UISO 1.5 parent).
;


_audit_creation_date             2018-05-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2017/1
loop_
_audit_author_email
conrad.goodwin@manchester.ac.uk
david.mills@manchester.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        '[Y(Cpttt)2(BH4)]'
_chemical_formula_moiety         'C34 H62 B1 Y1'
_chemical_formula_sum            'C34 H62 B Y'
_chemical_formula_weight         570.55
_chemical_melting_point          ?
_chemical_oxdiff_formula         Y(C5H2(C4H9)3)2BH4
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.3453(5)
_cell_length_b                   15.6331(9)
_cell_length_c                   20.5613(11)
_cell_angle_alpha                90
_cell_angle_beta                 99.312(5)
_cell_angle_gamma                90
_cell_volume                     3281.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2170
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      26.3010
_cell_measurement_theta_min      3.2930
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 5 -26 0.0694
-15 0 2 0.1188
1 -5 28 0.0894
11 -3 15 0.0773
3 -20 10 0.0925
0 -22 2 0.0997
-7 11 -19 0.0715
5 18 12 0.0561
-1 22 -5 0.0512
6 -20 -7 0.0848
8 -13 -19 0.0843
-11 11 -8 0.0618
-6 12 22 0.1161
-11 -13 -2 0.1232

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.151
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
7.0000 5.0000 -26.0000 -0.3737 -0.7744 -0.4813
-15.0000 0.0000 2.0000 0.3629 0.7423 -0.6198
1.0000 -5.0000 28.0000 0.2275 0.4154 0.9006
11.0000 -3.0000 15.0000 -0.1215 -0.2704 0.9581
3.0000 -20.0000 10.0000 -0.6434 0.4833 0.6038
-0.0000 -22.0000 2.0000 -0.7737 0.5815 0.2545
-7.0000 11.0000 -19.0000 0.2638 -0.1719 -0.9647
5.0000 18.0000 12.0000 0.7330 -0.5512 0.4125
-1.0000 22.0000 -5.0000 0.7495 -0.5696 -0.3866
6.0000 -20.0000 -7.0000 -0.9724 0.1353 0.2471
8.0000 -13.0000 -19.0000 -0.9460 -0.2821 -0.0725
-11.0000 11.0000 -8.0000 0.5222 0.1518 -0.8269
-6.0000 12.0000 22.0000 0.9115 0.2477 0.2587
-11.0000 -13.0000 -2.0000 -0.2629 0.8321 -0.4387

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0956
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            10183
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.708
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -51.00  47.40   0.80   15.00    --  -20.55  77.00-150.00  123
  2  ω    -50.00  48.40   0.80   15.00    --   21.65 -77.00   0.00  123
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0221344000
_diffrn_orient_matrix_UB_12      0.0365743000
_diffrn_orient_matrix_UB_13      0.0154455000
_diffrn_orient_matrix_UB_21      -0.0478832000
_diffrn_orient_matrix_UB_22      -0.0253374000
_diffrn_orient_matrix_UB_23      0.0120210000
_diffrn_orient_matrix_UB_31      0.0451809000
_diffrn_orient_matrix_UB_32      -0.0089364000
_diffrn_orient_matrix_UB_33      0.0289556000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3635
_reflns_number_total             5931
_reflns_odcompleteness_completeness 98.50
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_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    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         2.943
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     664
_refine_ls_number_reflns         5931
_refine_ls_number_restraints     1402
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0876
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1635P)²+1.2014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2304
_refine_ls_wR_factor_ref         0.2756

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All B(H,H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 H1AA-H1AC
 1.9 with sigma of 0.02
 H1AA-H1AB
 1.9 with sigma of 0.02
 H1AC-H1AB
 1.9 with sigma of 0.02
 H1AC-H1AD
 1.9 with sigma of 0.02
 H1AB-H1AD
 1.9 with sigma of 0.02
 H1AD-H1AA
 1.9 with sigma of 0.02
 B1A-H1AA = B1A-H1AC = B1A-H1AB
 1.1 with sigma of 0.001
 B1A-H1AD
 1.1 with sigma of 0.001
 B1B-H1BA = B1B-H1BB = B1B-H1BC = B1B-H1BD
 1.1 with sigma of 0.02
 H1BA-H1BB \\sim H1BA-H1BC \\sim H1BA-H1BD \\sim H1BB-H1BC \\sim H1BB-H1BD
\\sim H1BC-H1BD
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(C19A) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(Y1A) = Uanis(Y1B)
Uanis(B1A) = Uanis(B1B)
5. Same fragment restrains
{Y1A, C6A, C2A, C3A, C4A, C5A, C1A, C7A, C8A, C9A, C10A, C11A, C12A, C13A,
C14A, C15A, C16A, C17A, C18A, C19A, C20A, C21A, C22A, C23A, C24A, C25A, C26A,
C27A, C28A, C29A, C30A, C31A, C32A, C33A, C34A, B1A} sigma for 1-2: 0.02, 1-3:
0.04
as
{Y1B, C0AA, C2B, C3B, C4B, C5B, C6B, C7B, C8B, C9B, C10B, C11B, C12B, C13B,
C14B, C15B, C16B, C17B, C18B, C19B, C20B, C21B, C22B, C23B, C24B, C25B, C26B,
C27B, C28B, C29B, C30B, C31B, C32B, C33B, C34B, B1B}
6. Others
 Sof(Y1B)=Sof(C0AA)=Sof(C2B)=Sof(H2B)=Sof(C3B)=Sof(C4B)=Sof(C5B)=Sof(H5B)=
 Sof(C6B)=Sof(C7B)=Sof(H7BA)=Sof(H7BB)=Sof(H7BC)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=
 Sof(H8BC)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C10B)=Sof(C11B)=Sof(H11D)=
 Sof(H11E)=Sof(H11F)=Sof(C12B)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C13B)=
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14B)=Sof(C15B)=Sof(H15D)=Sof(H15E)=
 Sof(H15F)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17B)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C18B)=Sof(C19B)=Sof(H19B)=Sof(C20B)=Sof(C21B)=
 Sof(C22B)=Sof(H22B)=Sof(C23B)=Sof(C24B)=Sof(H24D)=Sof(H24E)=Sof(H24F)=
 Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26B)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C27B)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=
 Sof(C31B)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=Sof(H33D)=
 Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(B1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(H1BC)=Sof(H1BD)=1-FVAR(1)
 Sof(Y1A)=Sof(C1A)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=
 Sof(C6A)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(C11A)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=Sof(C12A)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(C13A)=
 Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C17A)=Sof(H17A)=
 Sof(H17B)=Sof(H17C)=Sof(C18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(C21A)=
 Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C27A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=
 Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(B1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(H1AC)=Sof(H1AD)=FVAR(1)
7.a Me refined with riding coordinates:
 C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C11A(H11A,H11B,
 H11C), C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C15A(H15A,H15B,H15C),
 C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C24A(H24A,H24B,H24C), C25A(H25A,
 H25B,H25C), C26A(H26A,H26B,H26C), C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C),
 C30A(H30A,H30B,H30C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34A(H34A,
 H34B,H34C), C7B(H7BA,H7BB,H7BC), C8B(H8BA,H8BB,H8BC), C9B(H9BA,H9BB,H9BC),
 C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F), C16B(H16D,H16E,H16F), C17B(H17D,
 H17E,H17F), C24B(H24D,H24E,H24F), C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F),
 C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F), C30B(H30D,H30E,H30F), C32B(H32D,
 H32E,H32F), C33B(H33D,H33E,H33F), C34B(H34D,H34E,H34F)
7.b Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C5A(H5A), C19A(H19A), C22A(H22A), C2B(H2B), C5B(H5B), C19B(H19B),
 C22B(H22B)
7.c Idealised Me refined as rotating group:
 C11B(H11D,H11E,H11F), C15B(H15D,H15E,H15F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1A Y 0.50076(6) 0.70435(4) 0.87834(3) 0.0189(3) Uani 0.8996(14) 1 d D U P A 1
C1A C 0.4768(7) 0.7457(4) 0.9999(3) 0.0179(10) Uani 0.8996(14) 1 d D U P A 1
C2A C 0.5660(6) 0.6775(5) 1.0063(3) 0.0206(10) Uani 0.8996(14) 1 d D U P A 1
H2A H 0.547547 0.622454 1.019382 0.025 Uiso 0.8996(14) 1 calc R . P A 1
C3A C 0.6884(6) 0.7038(4) 0.9901(3) 0.0204(10) Uani 0.8996(14) 1 d D U P A 1
C4A C 0.6737(6) 0.7933(4) 0.9709(3) 0.0187(10) Uani 0.8996(14) 1 d D U P A 1
C5A C 0.5401(6) 0.8146(4) 0.9771(3) 0.0189(10) Uani 0.8996(14) 1 d D U P A 1
H5A H 0.501864 0.867855 0.967090 0.023 Uiso 0.8996(14) 1 calc R . P A 1
C6A C 0.3396(7) 0.7441(4) 1.0165(3) 0.0204(11) Uani 0.8996(14) 1 d D U P A 1
C7A C 0.2531(7) 0.6953(5) 0.9624(3) 0.0286(15) Uani 0.8996(14) 1 d D U P A 1
H7AA H 0.165208 0.693361 0.971792 0.043 Uiso 0.8996(14) 1 calc R . P A 1
H7AB H 0.253434 0.723615 0.920965 0.043 Uiso 0.8996(14) 1 calc R . P A 1
H7AC H 0.285833 0.638141 0.960086 0.043 Uiso 0.8996(14) 1 calc R . P A 1
C8A C 0.2847(7) 0.8339(5) 1.0230(4) 0.0285(15) Uani 0.8996(14) 1 d D U P A 1
H8AA H 0.197877 0.829898 1.033577 0.043 Uiso 0.8996(14) 1 calc R . P A 1
H8AB H 0.339980 0.864291 1.057436 0.043 Uiso 0.8996(14) 1 calc R . P A 1
H8AC H 0.281915 0.864046 0.982127 0.043 Uiso 0.8996(14) 1 calc R . P A 1
C9A C 0.3353(7) 0.6951(5) 1.0820(3) 0.0294(15) Uani 0.8996(14) 1 d D U P A 1
H9AA H 0.247322 0.695093 1.091353 0.044 Uiso 0.8996(14) 1 calc R . P A 1
H9AB H 0.363850 0.637240 1.077800 0.044 Uiso 0.8996(14) 1 calc R . P A 1
H9AC H 0.392115 0.722767 1.117352 0.044 Uiso 0.8996(14) 1 calc R . P A 1
C10A C 0.8106(7) 0.6450(5) 1.0065(3) 0.0269(12) Uani 0.8996(14) 1 d D U P A 1
C11A C 0.8760(7) 0.6196(5) 0.9457(4) 0.0302(16) Uani 0.8996(14) 1 d D U P A 1
H11A H 0.903247 0.670322 0.925340 0.045 Uiso 0.8996(14) 1 calc R . P A 1
H11B H 0.950792 0.583973 0.959962 0.045 Uiso 0.8996(14) 1 calc R . P A 1
H11C H 0.813967 0.588875 0.914415 0.045 Uiso 0.8996(14) 1 calc R . P A 1
C12A C 0.7709(7) 0.5606(5) 1.0352(4) 0.0328(16) Uani 0.8996(14) 1 d D U P A 1
H12A H 0.707854 0.531943 1.003218 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H12B H 0.846844 0.525015 1.046516 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H12C H 0.733167 0.571962 1.074049 0.049 Uiso 0.8996(14) 1 calc R . P A 1
C13A C 0.9108(7) 0.6846(5) 1.0618(3) 0.0334(16) Uani 0.8996(14) 1 d D U P A 1
H13A H 0.940591 0.738354 1.047191 0.050 Uiso 0.8996(14) 1 calc R . P A 1
H13B H 0.870354 0.693494 1.100070 0.050 Uiso 0.8996(14) 1 calc R . P A 1
H13C H 0.984031 0.646548 1.072537 0.050 Uiso 0.8996(14) 1 calc R . P A 1
C14A C 0.7708(7) 0.8649(5) 0.9635(3) 0.0244(11) Uani 0.8996(14) 1 d D U P A 1
C15A C 0.8907(8) 0.8451(5) 0.9333(3) 0.0305(17) Uani 0.8996(14) 1 d D U P A 1
H15A H 0.941716 0.896191 0.932007 0.046 Uiso 0.8996(14) 1 calc R . P A 1
H15B H 0.942309 0.802515 0.959264 0.046 Uiso 0.8996(14) 1 calc R . P A 1
H15C H 0.864500 0.823987 0.889258 0.046 Uiso 0.8996(14) 1 calc R . P A 1
C16A C 0.8112(8) 0.9073(5) 1.0309(3) 0.0352(18) Uani 0.8996(14) 1 d D U P A 1
H16A H 0.734432 0.919698 1.049914 0.053 Uiso 0.8996(14) 1 calc R . P A 1
H16B H 0.867089 0.869218 1.059398 0.053 Uiso 0.8996(14) 1 calc R . P A 1
H16C H 0.857374 0.959420 1.025646 0.053 Uiso 0.8996(14) 1 calc R . P A 1
C17A C 0.7026(7) 0.9380(5) 0.9187(3) 0.0325(16) Uani 0.8996(14) 1 d D U P A 1
H17A H 0.623939 0.955152 0.934358 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H17B H 0.760796 0.986036 0.920117 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H17C H 0.681096 0.917790 0.874198 0.049 Uiso 0.8996(14) 1 calc R . P A 1
C18A C 0.5276(6) 0.7444(4) 0.7560(3) 0.0179(10) Uani 0.8996(14) 1 d D U P A 1
C19A C 0.4372(6) 0.6773(4) 0.7513(3) 0.0181(10) Uani 0.8996(14) 1 d D U P A 1
H19A H 0.454065 0.621515 0.739509 0.022 Uiso 0.8996(14) 1 calc R . P A 1
C20A C 0.3150(6) 0.7067(4) 0.7672(3) 0.0190(10) Uani 0.8996(14) 1 d D U P A 1
C21A C 0.3351(6) 0.7952(4) 0.7849(3) 0.0201(10) Uani 0.8996(14) 1 d D U P A 1
C22A C 0.4683(6) 0.8139(4) 0.7791(3) 0.0201(10) Uani 0.8996(14) 1 d D U P A 1
H22A H 0.509186 0.866185 0.789687 0.024 Uiso 0.8996(14) 1 calc R . P A 1
C23A C 0.6643(6) 0.7392(5) 0.7365(3) 0.0209(11) Uani 0.8996(14) 1 d D U P A 1
C24A C 0.7531(7) 0.6846(5) 0.7882(4) 0.0331(16) Uani 0.8996(14) 1 d D U P A 1
H24A H 0.714968 0.628914 0.790733 0.050 Uiso 0.8996(14) 1 calc R . P A 1
H24B H 0.838096 0.678890 0.775621 0.050 Uiso 0.8996(14) 1 calc R . P A 1
H24C H 0.761484 0.711949 0.830493 0.050 Uiso 0.8996(14) 1 calc R . P A 1
C25A C 0.6588(7) 0.6945(5) 0.6697(4) 0.0315(16) Uani 0.8996(14) 1 d D U P A 1
H25A H 0.620268 0.638901 0.671486 0.047 Uiso 0.8996(14) 1 calc R . P A 1
H25B H 0.606867 0.727982 0.636021 0.047 Uiso 0.8996(14) 1 calc R . P A 1
H25C H 0.745957 0.688764 0.659780 0.047 Uiso 0.8996(14) 1 calc R . P A 1
C26A C 0.7258(7) 0.8275(5) 0.7329(4) 0.0310(15) Uani 0.8996(14) 1 d D U P A 1
H26A H 0.729676 0.855997 0.774504 0.046 Uiso 0.8996(14) 1 calc R . P A 1
H26B H 0.812804 0.821446 0.722795 0.046 Uiso 0.8996(14) 1 calc R . P A 1
H26C H 0.673714 0.860665 0.699037 0.046 Uiso 0.8996(14) 1 calc R . P A 1
C27A C 0.1915(6) 0.6481(5) 0.7507(3) 0.0243(12) Uani 0.8996(14) 1 d D U P A 1
C28A C 0.1231(7) 0.6285(5) 0.8099(3) 0.0272(15) Uani 0.8996(14) 1 d D U P A 1
H28A H 0.098876 0.681135 0.828749 0.041 Uiso 0.8996(14) 1 calc R . P A 1
H28B H 0.046074 0.594922 0.795656 0.041 Uiso 0.8996(14) 1 calc R . P A 1
H28C H 0.181731 0.597193 0.842384 0.041 Uiso 0.8996(14) 1 calc R . P A 1
C29A C 0.2270(7) 0.5617(5) 0.7235(4) 0.0376(18) Uani 0.8996(14) 1 d D U P A 1
H29A H 0.270224 0.570685 0.686175 0.056 Uiso 0.8996(14) 1 calc R . P A 1
H29B H 0.284273 0.531206 0.757057 0.056 Uiso 0.8996(14) 1 calc R . P A 1
H29C H 0.148616 0.528934 0.710329 0.056 Uiso 0.8996(14) 1 calc R . P A 1
C30A C 0.0934(7) 0.6877(5) 0.6947(3) 0.0318(15) Uani 0.8996(14) 1 d D U P A 1
H30A H 0.066257 0.742754 0.708137 0.048 Uiso 0.8996(14) 1 calc R . P A 1
H30B H 0.134275 0.694062 0.656211 0.048 Uiso 0.8996(14) 1 calc R . P A 1
H30C H 0.018382 0.651035 0.684615 0.048 Uiso 0.8996(14) 1 calc R . P A 1
C31A C 0.2416(7) 0.8710(5) 0.7906(3) 0.0252(12) Uani 0.8996(14) 1 d D U P A 1
C32A C 0.3110(7) 0.9429(5) 0.8351(4) 0.0336(16) Uani 0.8996(14) 1 d D U P A 1
H32A H 0.390734 0.958592 0.819884 0.050 Uiso 0.8996(14) 1 calc R . P A 1
H32B H 0.254494 0.991864 0.833232 0.050 Uiso 0.8996(14) 1 calc R . P A 1
H32C H 0.330767 0.922787 0.879698 0.050 Uiso 0.8996(14) 1 calc R . P A 1
C33A C 0.1168(7) 0.8528(5) 0.8205(4) 0.0324(16) Uani 0.8996(14) 1 d D U P A 1
H33A H 0.140869 0.827897 0.863491 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H33B H 0.070440 0.905282 0.824164 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H33C H 0.061640 0.813745 0.792622 0.049 Uiso 0.8996(14) 1 calc R . P A 1
C34A C 0.2028(7) 0.9110(5) 0.7215(3) 0.0326(17) Uani 0.8996(14) 1 d D U P A 1
H34A H 0.280333 0.922366 0.702865 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H34B H 0.147614 0.871968 0.693624 0.049 Uiso 0.8996(14) 1 calc R . P A 1
H34C H 0.156414 0.963506 0.725167 0.049 Uiso 0.8996(14) 1 calc R . P A 1
B1A B 0.5019(6) 0.5351(4) 0.8773(3) 0.0097(12) Uani 0.8996(14) 1 d D U P A 1
H1AA H 0.5897(19) 0.5738(17) 0.8746(19) 0.014 Uiso 0.8996(14) 1 d DR . P A 1
H1AB H 0.417(2) 0.5770(17) 0.8799(19) 0.014 Uiso 0.8996(14) 1 d DR . P A 1
H1AC H 0.521(4) 0.4949(17) 0.9217(9) 0.014 Uiso 0.8996(14) 1 d DR . P A 1
H1AD H 0.482(4) 0.4947(17) 0.8330(9) 0.014 Uiso 0.8996(14) 1 d DR . P A 1
Y1B Y 0.5019(5) 0.7944(4) 0.8697(3) 0.0189(3) Uani 0.1004(14) 1 d D U P A -2
C0AA C 0.177(2) 0.762(2) 0.7644(16) 0.0239(14) Uani 0.1004(14) 1 d D U P A -2
C2B C 0.401(2) 0.8258(18) 0.7458(9) 0.0200(14) Uani 0.1004(14) 1 d D U P A -2
H2B H 0.373937 0.882134 0.738292 0.024 Uiso 0.1004(14) 1 calc R . P A -2
C3B C 0.524(2) 0.7950(16) 0.7372(8) 0.0211(13) Uani 0.1004(14) 1 d D U P A -2
C4B C 0.526(3) 0.7055(15) 0.7557(9) 0.0207(13) Uani 0.1004(14) 1 d D U P A -2
C5B C 0.400(2) 0.6876(15) 0.7748(11) 0.0199(13) Uani 0.1004(14) 1 d D U P A -2
H5B H 0.374951 0.635111 0.789860 0.024 Uiso 0.1004(14) 1 calc R . P A -2
C6B C 0.3233(19) 0.7606(18) 0.7673(10) 0.0202(13) Uani 0.1004(14) 1 d D U P A
-2
C7B C 0.136(5) 0.816(4) 0.819(2) 0.029(3) Uani 0.1004(14) 1 d D U P A -2
H7BA H 0.042152 0.815497 0.814634 0.043 Uiso 0.1004(14) 1 calc R . P A -2
H7BB H 0.174116 0.793728 0.860676 0.043 Uiso 0.1004(14) 1 calc R . P A -2
H7BC H 0.165054 0.874154 0.814621 0.043 Uiso 0.1004(14) 1 calc R . P A -2
C8B C 0.120(5) 0.671(3) 0.764(3) 0.029(3) Uani 0.1004(14) 1 d D U P A -2
H8BA H 0.027257 0.674431 0.762350 0.043 Uiso 0.1004(14) 1 calc R . P A -2
H8BB H 0.139916 0.640535 0.726577 0.043 Uiso 0.1004(14) 1 calc R . P A -2
H8BC H 0.158741 0.642007 0.803770 0.043 Uiso 0.1004(14) 1 calc R . P A -2
C9B C 0.106(4) 0.806(3) 0.699(2) 0.030(3) Uani 0.1004(14) 1 d D U P A -2
H9BA H 0.013532 0.806090 0.698066 0.045 Uiso 0.1004(14) 1 calc R . P A -2
H9BB H 0.136956 0.863737 0.696429 0.045 Uiso 0.1004(14) 1 calc R . P A -2
H9BC H 0.126004 0.774482 0.661211 0.045 Uiso 0.1004(14) 1 calc R . P A -2
C10B C 0.643(3) 0.849(2) 0.7198(15) 0.0251(19) Uani 0.1004(14) 1 d D U P A -2
C11B C 0.763(4) 0.828(4) 0.776(2) 0.028(3) Uani 0.1004(14) 1 d D U P A -2
H11D H 0.739870 0.781842 0.802607 0.043 Uiso 0.1004(14) 1 calc GR . P A -2
H11E H 0.786000 0.877336 0.802250 0.043 Uiso 0.1004(14) 1 calc GR . P A -2
H11F H 0.836950 0.810402 0.755572 0.043 Uiso 0.1004(14) 1 calc GR . P A -2
C12B C 0.617(5) 0.944(2) 0.725(3) 0.030(5) Uani 0.1004(14) 1 d D U P A -2
H12D H 0.599097 0.956410 0.768243 0.045 Uiso 0.1004(14) 1 calc R . P A -2
H12E H 0.692692 0.975139 0.717120 0.045 Uiso 0.1004(14) 1 calc R . P A -2
H12F H 0.543091 0.959222 0.692724 0.045 Uiso 0.1004(14) 1 calc R . P A -2
C13B C 0.672(5) 0.828(4) 0.6517(18) 0.029(4) Uani 0.1004(14) 1 d D U P A -2
H13D H 0.688121 0.768020 0.648625 0.044 Uiso 0.1004(14) 1 calc R . P A -2
H13E H 0.597647 0.843779 0.619412 0.044 Uiso 0.1004(14) 1 calc R . P A -2
H13F H 0.747249 0.859696 0.643807 0.044 Uiso 0.1004(14) 1 calc R . P A -2
C14B C 0.621(3) 0.6295(18) 0.7564(15) 0.0251(19) Uani 0.1004(14) 1 d D U P A -2
C15B C 0.748(3) 0.653(3) 0.736(3) 0.029(3) Uani 0.1004(14) 1 d D U P A -2
H15D H 0.733848 0.666856 0.689689 0.044 Uiso 0.1004(14) 1 calc GR . P A -2
H15E H 0.807269 0.604796 0.743182 0.044 Uiso 0.1004(14) 1 calc GR . P A -2
H15F H 0.785799 0.700739 0.760882 0.044 Uiso 0.1004(14) 1 calc GR . P A -2
C16B C 0.550(5) 0.559(3) 0.714(2) 0.031(5) Uani 0.1004(14) 1 d D U P A -2
H16D H 0.468945 0.546155 0.728825 0.047 Uiso 0.1004(14) 1 calc R . P A -2
H16E H 0.532375 0.577562 0.668789 0.047 Uiso 0.1004(14) 1 calc R . P A -2
H16F H 0.603758 0.508568 0.717087 0.047 Uiso 0.1004(14) 1 calc R . P A -2
C17B C 0.655(5) 0.589(3) 0.8271(18) 0.030(5) Uani 0.1004(14) 1 d D U P A -2
H17D H 0.575534 0.572775 0.842453 0.046 Uiso 0.1004(14) 1 calc R . P A -2
H17E H 0.708413 0.538744 0.825151 0.046 Uiso 0.1004(14) 1 calc R . P A -2
H17F H 0.701914 0.629467 0.856944 0.046 Uiso 0.1004(14) 1 calc R . P A -2
C18B C 0.686(2) 0.7574(18) 0.9703(11) 0.0210(12) Uani 0.1004(14) 1 d D U P A -2
C19B C 0.607(2) 0.8187(18) 0.9927(9) 0.0200(13) Uani 0.1004(14) 1 d D U P A -2
H19B H 0.629886 0.875620 1.001111 0.024 Uiso 0.1004(14) 1 calc R . P A -2
C20B C 0.484(3) 0.7820(16) 1.0011(8) 0.0203(12) Uani 0.1004(14) 1 d D U P A -2
C21B C 0.490(3) 0.6951(14) 0.9796(10) 0.0208(12) Uani 0.1004(14) 1 d D U P A -2
C22B C 0.614(2) 0.6837(15) 0.9594(11) 0.0207(13) Uani 0.1004(14) 1 d D U P A -2
H22B H 0.641288 0.633665 0.941344 0.025 Uiso 0.1004(14) 1 calc R . P A -2
C23B C 0.835(2) 0.756(2) 0.9753(16) 0.0238(14) Uani 0.1004(14) 1 d D U P A -2
C24B C 0.881(6) 0.817(4) 0.925(3) 0.027(3) Uani 0.1004(14) 1 d D U P A -2
H24D H 0.974860 0.814828 0.929155 0.040 Uiso 0.1004(14) 1 calc R . P A -2
H24E H 0.842797 0.800151 0.881135 0.040 Uiso 0.1004(14) 1 calc R . P A -2
H24F H 0.854423 0.874386 0.933013 0.040 Uiso 0.1004(14) 1 calc R . P A -2
C25B C 0.901(4) 0.789(4) 1.0434(19) 0.029(4) Uani 0.1004(14) 1 d D U P A -2
H25D H 0.994871 0.787115 1.045683 0.044 Uiso 0.1004(14) 1 calc R . P A -2
H25E H 0.873897 0.846143 1.049657 0.044 Uiso 0.1004(14) 1 calc R . P A -2
H25F H 0.876979 0.752570 1.077279 0.044 Uiso 0.1004(14) 1 calc R . P A -2
C26B C 0.882(5) 0.664(3) 0.965(3) 0.029(3) Uani 0.1004(14) 1 d D U P A -2
H26D H 0.975863 0.663867 0.967845 0.044 Uiso 0.1004(14) 1 calc R . P A -2
H26E H 0.857153 0.626996 0.997591 0.044 Uiso 0.1004(14) 1 calc R . P A -2
H26F H 0.843088 0.644454 0.921692 0.044 Uiso 0.1004(14) 1 calc R . P A -2
C27B C 0.381(3) 0.842(2) 1.0277(14) 0.0227(17) Uani 0.1004(14) 1 d D U P A -2
C28B C 0.251(3) 0.835(3) 0.979(2) 0.025(3) Uani 0.1004(14) 1 d D U P A -2
H28D H 0.265394 0.852435 0.936007 0.038 Uiso 0.1004(14) 1 calc R . P A -2
H28E H 0.221208 0.776642 0.977255 0.038 Uiso 0.1004(14) 1 calc R . P A -2
H28F H 0.186904 0.871093 0.993595 0.038 Uiso 0.1004(14) 1 calc R . P A -2
C29B C 0.422(5) 0.936(2) 1.027(3) 0.030(5) Uani 0.1004(14) 1 d D U P A -2
H29D H 0.432846 0.952167 0.983614 0.045 Uiso 0.1004(14) 1 calc R . P A -2
H29E H 0.356137 0.970739 1.041892 0.045 Uiso 0.1004(14) 1 calc R . P A -2
H29F H 0.503750 0.943348 1.056682 0.045 Uiso 0.1004(14) 1 calc R . P A -2
C30B C 0.364(5) 0.814(3) 1.0961(17) 0.027(3) Uani 0.1004(14) 1 d D U P A -2
H30D H 0.338100 0.755378 1.095546 0.040 Uiso 0.1004(14) 1 calc R . P A -2
H30E H 0.445148 0.821573 1.125594 0.040 Uiso 0.1004(14) 1 calc R . P A -2
H30F H 0.297535 0.848964 1.110803 0.040 Uiso 0.1004(14) 1 calc R . P A -2
C31B C 0.397(3) 0.6169(17) 0.9807(15) 0.0238(19) Uani 0.1004(14) 1 d D U P A -2
C32B C 0.365(5) 0.574(3) 0.9119(18) 0.023(4) Uani 0.1004(14) 1 d D U P A -2
H32D H 0.323679 0.614464 0.880265 0.035 Uiso 0.1004(14) 1 calc R . P A -2
H32E H 0.445182 0.554180 0.898688 0.035 Uiso 0.1004(14) 1 calc R . P A -2
H32F H 0.307855 0.526054 0.914090 0.035 Uiso 0.1004(14) 1 calc R . P A -2
C33B C 0.261(3) 0.643(3) 0.996(3) 0.027(3) Uani 0.1004(14) 1 d D U P A -2
H33D H 0.222873 0.685380 0.965498 0.041 Uiso 0.1004(14) 1 calc R . P A -2
H33E H 0.205123 0.593470 0.993245 0.041 Uiso 0.1004(14) 1 calc R . P A -2
H33F H 0.270791 0.665665 1.040268 0.041 Uiso 0.1004(14) 1 calc R . P A -2
C34B C 0.463(5) 0.549(3) 1.029(2) 0.031(5) Uani 0.1004(14) 1 d D U P A -2
H34D H 0.546789 0.534201 1.017434 0.046 Uiso 0.1004(14) 1 calc R . P A -2
H34E H 0.474602 0.570585 1.072903 0.046 Uiso 0.1004(14) 1 calc R . P A -2
H34F H 0.408934 0.498390 1.025879 0.046 Uiso 0.1004(14) 1 calc R . P A -2
B1B B 0.502(4) 0.9633(10) 0.8740(13) 0.0097(12) Uani 0.1004(14) 1 d D U P A -2
H1BA H 0.50(3) 0.894(4) 0.864(13) 0.014 Uiso 0.1004(14) 1 d DR . P A -2
H1BB H 0.47(2) 0.975(18) 0.922(6) 0.014 Uiso 0.1004(14) 1 d DR . P A -2
H1BC H 0.603(11) 0.987(16) 0.876(12) 0.014 Uiso 0.1004(14) 1 d DR . P A -2
H1BD H 0.436(19) 0.996(15) 0.835(9) 0.014 Uiso 0.1004(14) 1 d DR . 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
Y1A C1A 2.632(6) . ?
Y1A C2A 2.642(6) . ?
Y1A C3A 2.758(7) . ?
Y1A C4A 2.766(7) . ?
Y1A C5A 2.645(6) . ?
Y1A C18A 2.650(6) . ?
Y1A C19A 2.623(6) . ?
Y1A C20A 2.738(7) . ?
Y1A C21A 2.754(7) . ?
Y1A C22A 2.643(6) . ?
C1A C2A 1.403(9) . ?
C1A C5A 1.381(9) . ?
C1A C6A 1.514(9) . ?
C2A C3A 1.422(9) . ?
C3A C4A 1.455(10) . ?
C3A C10A 1.556(9) . ?
C4A C5A 1.447(9) . ?
C4A C14A 1.527(9) . ?
C6A C7A 1.517(9) . ?
C6A C8A 1.528(10) . ?
C6A C9A 1.556(9) . ?
C10A C11A 1.566(9) . ?
C10A C12A 1.528(10) . ?
C10A C13A 1.539(10) . ?
C14A C15A 1.507(10) . ?
C14A C16A 1.533(9) . ?
C14A C17A 1.563(10) . ?
C18A C19A 1.398(9) . ?
C18A C22A 1.369(9) . ?
C18A C23A 1.533(9) . ?
C19A C20A 1.431(9) . ?
C20A C21A 1.438(10) . ?
C20A C27A 1.564(9) . ?
C21A C22A 1.433(9) . ?
C21A C31A 1.546(9) . ?
C23A C24A 1.546(10) . ?
C23A C25A 1.533(9) . ?
C23A C26A 1.528(10) . ?
C27A C28A 1.535(9) . ?
C27A C29A 1.528(10) . ?
C27A C30A 1.537(10) . ?
C31A C32A 1.551(10) . ?
C31A C33A 1.544(10) . ?
C31A C34A 1.543(9) . ?
Y1B C2B 2.637(16) . ?
Y1B C3B 2.770(15) . ?
Y1B C4B 2.769(16) . ?
Y1B C5B 2.651(16) . ?
Y1B C6B 2.619(16) . ?
Y1B C18B 2.643(15) . ?
Y1B C19B 2.615(16) . ?
Y1B C20B 2.744(16) . ?
Y1B C21B 2.761(16) . ?
Y1B C22B 2.654(16) . ?
Y1B B1B 2.642(16) . ?
C0AA C6B 1.501(19) . ?
C0AA C7B 1.51(2) . ?
C0AA C8B 1.54(2) . ?
C0AA C9B 1.59(2) . ?
C2B C3B 1.40(2) . ?
C2B C6B 1.41(2) . ?
C3B C4B 1.449(19) . ?
C3B C10B 1.578(19) . ?
C4B C5B 1.44(2) . ?
C4B C14B 1.543(19) . ?
C5B C6B 1.39(2) . ?
C10B C11B 1.58(2) . ?
C10B C12B 1.51(2) . ?
C10B C13B 1.51(2) . ?
C14B C15B 1.49(2) . ?
C14B C16B 1.52(2) . ?
C14B C17B 1.58(2) . ?
C18B C19B 1.39(2) . ?
C18B C22B 1.37(2) . ?
C18B C23B 1.525(19) . ?
C19B C20B 1.43(2) . ?
C20B C21B 1.432(19) . ?
C20B C27B 1.580(19) . ?
C21B C22B 1.42(2) . ?
C21B C31B 1.561(19) . ?
C23B C24B 1.54(2) . ?
C23B C25B 1.54(2) . ?
C23B C26B 1.54(2) . ?
C27B C28B 1.54(2) . ?
C27B C29B 1.53(2) . ?
C27B C30B 1.51(2) . ?
C31B C32B 1.55(2) . ?
C31B C33B 1.54(2) . ?
C31B C34B 1.54(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1A Y1A C2A 30.9(2) . . ?
C1A Y1A C3A 51.0(2) . . ?
C1A Y1A C4A 51.2(2) . . ?
C1A Y1A C5A 30.34(19) . . ?
C1A Y1A C18A 152.1(2) . . ?
C1A Y1A C20A 128.9(2) . . ?
C1A Y1A C21A 113.1(2) . . ?
C1A Y1A C22A 123.6(2) . . ?
C2A Y1A C3A 30.43(19) . . ?
C2A Y1A C4A 50.4(2) . . ?
C2A Y1A C5A 49.9(2) . . ?
C2A Y1A C18A 159.0(2) . . ?
C2A Y1A C20A 149.9(2) . . ?
C2A Y1A C21A 143.8(2) . . ?
C2A Y1A C22A 148.4(2) . . ?
C3A Y1A C4A 30.5(2) . . ?
C5A Y1A C3A 50.4(2) . . ?
C5A Y1A C4A 30.92(19) . . ?
C5A Y1A C18A 123.2(2) . . ?
C5A Y1A C20A 129.2(2) . . ?
C5A Y1A C21A 101.6(2) . . ?
C5A Y1A C22A 98.9(2) . . ?
C18A Y1A C3A 128.6(2) . . ?
C18A Y1A C4A 112.25(19) . . ?
C18A Y1A C20A 51.1(2) . . ?
C18A Y1A C21A 50.5(2) . . ?
C19A Y1A C1A 159.8(2) . . ?
C19A Y1A C2A 161.6(2) . . ?
C19A Y1A C3A 149.2(2) . . ?
C19A Y1A C4A 142.8(2) . . ?
C19A Y1A C5A 148.5(2) . . ?
C19A Y1A C18A 30.7(2) . . ?
C19A Y1A C20A 30.87(19) . . ?
C19A Y1A C21A 50.2(2) . . ?
C19A Y1A C22A 49.9(2) . . ?
C20A Y1A C3A 179.4(2) . . ?
C20A Y1A C4A 148.9(2) . . ?
C20A Y1A C21A 30.4(2) . . ?
C21A Y1A C3A 149.1(2) . . ?
C21A Y1A C4A 118.7(2) . . ?
C22A Y1A C3A 129.0(2) . . ?
C22A Y1A C4A 101.1(2) . . ?
C22A Y1A C18A 29.98(19) . . ?
C22A Y1A C20A 50.4(2) . . ?
C22A Y1A C21A 30.70(19) . . ?
C2A C1A Y1A 75.0(4) . . ?
C2A C1A C6A 126.3(6) . . ?
C5A C1A Y1A 75.4(4) . . ?
C5A C1A C2A 106.5(6) . . ?
C5A C1A C6A 127.1(6) . . ?
C6A C1A Y1A 116.5(4) . . ?
C1A C2A Y1A 74.2(4) . . ?
C1A C2A C3A 110.8(6) . . ?
C3A C2A Y1A 79.3(4) . . ?
C2A C3A Y1A 70.3(4) . . ?
C2A C3A C4A 106.5(5) . . ?
C2A C3A C10A 120.1(6) . . ?
C4A C3A Y1A 75.1(4) . . ?
C4A C3A C10A 132.3(6) . . ?
C10A C3A Y1A 128.3(4) . . ?
C3A C4A Y1A 74.4(4) . . ?
C3A C4A C14A 133.6(6) . . ?
C5A C4A Y1A 69.9(4) . . ?
C5A C4A C3A 104.9(5) . . ?
C5A C4A C14A 119.5(6) . . ?
C14A C4A Y1A 131.5(4) . . ?
C1A C5A Y1A 74.3(4) . . ?
C1A C5A C4A 111.2(6) . . ?
C4A C5A Y1A 79.2(4) . . ?
C1A C6A C7A 107.8(5) . . ?
C1A C6A C8A 112.3(6) . . ?
C1A C6A C9A 111.3(5) . . ?
C7A C6A C8A 110.1(6) . . ?
C7A C6A C9A 107.0(6) . . ?
C8A C6A C9A 108.3(6) . . ?
C3A C10A C11A 114.7(6) . . ?
C12A C10A C3A 109.5(5) . . ?
C12A C10A C11A 105.5(6) . . ?
C12A C10A C13A 104.6(6) . . ?
C13A C10A C3A 110.4(6) . . ?
C13A C10A C11A 111.5(6) . . ?
C4A C14A C16A 108.3(5) . . ?
C4A C14A C17A 110.7(5) . . ?
C15A C14A C4A 119.3(6) . . ?
C15A C14A C16A 109.8(6) . . ?
C15A C14A C17A 103.3(6) . . ?
C16A C14A C17A 104.3(6) . . ?
C19A C18A Y1A 73.5(4) . . ?
C19A C18A C23A 125.2(6) . . ?
C22A C18A Y1A 74.7(4) . . ?
C22A C18A C19A 106.7(6) . . ?
C22A C18A C23A 128.1(6) . . ?
C23A C18A Y1A 118.6(4) . . ?
C18A C19A Y1A 75.7(4) . . ?
C18A C19A C20A 110.5(6) . . ?
C20A C19A Y1A 79.0(4) . . ?
C19A C20A Y1A 70.1(4) . . ?
C19A C20A C21A 105.6(5) . . ?
C19A C20A C27A 118.9(6) . . ?
C21A C20A Y1A 75.5(4) . . ?
C21A C20A C27A 134.3(6) . . ?
C27A C20A Y1A 127.7(4) . . ?
C20A C21A Y1A 74.2(4) . . ?
C20A C21A C31A 133.7(6) . . ?
C22A C21A Y1A 70.4(4) . . ?
C22A C21A C20A 106.0(5) . . ?
C22A C21A C31A 118.2(6) . . ?
C31A C21A Y1A 132.0(4) . . ?
C18A C22A Y1A 75.3(4) . . ?
C18A C22A C21A 111.0(6) . . ?
C21A C22A Y1A 78.9(4) . . ?
C18A C23A C24A 108.7(6) . . ?
C25A C23A C18A 110.9(5) . . ?
C25A C23A C24A 107.3(6) . . ?
C26A C23A C18A 111.9(6) . . ?
C26A C23A C24A 109.1(6) . . ?
C26A C23A C25A 108.9(6) . . ?
C28A C27A C20A 114.2(5) . . ?
C28A C27A C30A 110.0(6) . . ?
C29A C27A C20A 111.2(6) . . ?
C29A C27A C28A 106.4(6) . . ?
C29A C27A C30A 104.5(6) . . ?
C30A C27A C20A 110.1(6) . . ?
C32A C31A C21A 111.4(5) . . ?
C33A C31A C21A 117.5(6) . . ?
C33A C31A C32A 103.6(6) . . ?
C33A C31A C34A 109.4(6) . . ?
C34A C31A C21A 108.2(5) . . ?
C34A C31A C32A 106.0(6) . . ?
C2B Y1B C3B 29.9(4) . . ?
C2B Y1B C4B 49.6(6) . . ?
C2B Y1B C5B 50.2(6) . . ?
C2B Y1B C18B 156.9(8) . . ?
C2B Y1B C20B 152.3(8) . . ?
C2B Y1B C21B 146.4(7) . . ?
C2B Y1B C22B 148.5(8) . . ?
C2B Y1B B1B 81.1(7) . . ?
C4B Y1B C3B 30.3(4) . . ?
C5B Y1B C3B 50.6(6) . . ?
C5B Y1B C4B 30.8(5) . . ?
C5B Y1B C20B 126.8(8) . . ?
C5B Y1B C21B 100.6(7) . . ?
C5B Y1B C22B 100.2(7) . . ?
C6B Y1B C2B 31.2(5) . . ?
C6B Y1B C3B 51.1(6) . . ?
C6B Y1B C4B 50.7(6) . . ?
C6B Y1B C5B 30.5(5) . . ?
C6B Y1B C18B 155.7(8) . . ?
C6B Y1B C20B 128.8(7) . . ?
C6B Y1B C21B 115.2(7) . . ?
C6B Y1B C22B 126.7(8) . . ?
C6B Y1B B1B 103.1(8) . . ?
C18B Y1B C3B 127.3(7) . . ?
C18B Y1B C4B 113.6(7) . . ?
C18B Y1B C5B 126.0(8) . . ?
C18B Y1B C20B 50.8(6) . . ?
C18B Y1B C21B 50.0(6) . . ?
C18B Y1B C22B 30.1(5) . . ?
C19B Y1B C2B 160.9(8) . . ?
C19B Y1B C3B 149.7(8) . . ?
C19B Y1B C4B 144.3(7) . . ?
C19B Y1B C5B 148.9(8) . . ?
C19B Y1B C6B 159.2(8) . . ?
C19B Y1B C18B 30.7(5) . . ?
C19B Y1B C20B 30.7(5) . . ?
C19B Y1B C21B 49.9(6) . . ?
C19B Y1B C22B 49.9(6) . . ?
C19B Y1B B1B 79.8(7) . . ?
C20B Y1B C3B 176.0(7) . . ?
C20B Y1B C4B 145.8(7) . . ?
C20B Y1B C21B 30.2(4) . . ?
C21B Y1B C3B 146.0(7) . . ?
C21B Y1B C4B 115.6(7) . . ?
C22B Y1B C3B 126.1(7) . . ?
C22B Y1B C4B 99.9(7) . . ?
C22B Y1B C20B 50.2(6) . . ?
C22B Y1B C21B 30.3(5) . . ?
B1B Y1B C3B 91.7(7) . . ?
B1B Y1B C4B 122.1(7) . . ?
B1B Y1B C5B 130.7(7) . . ?
B1B Y1B C18B 101.3(8) . . ?
B1B Y1B C20B 92.1(7) . . ?
B1B Y1B C21B 122.3(7) . . ?
B1B Y1B C22B 129.0(7) . . ?
C6B C0AA C7B 113(2) . . ?
C6B C0AA C8B 111(2) . . ?
C6B C0AA C9B 111(2) . . ?
C7B C0AA C8B 111(3) . . ?
C7B C0AA C9B 104(2) . . ?
C8B C0AA C9B 106(2) . . ?
C3B C2B Y1B 80.3(9) . . ?
C3B C2B C6B 111.6(18) . . ?
C6B C2B Y1B 73.7(9) . . ?
C2B C3B Y1B 69.8(8) . . ?
C2B C3B C4B 105.6(16) . . ?
C2B C3B C10B 127.1(19) . . ?
C4B C3B Y1B 74.8(8) . . ?
C4B C3B C10B 126.9(19) . . ?
C10B C3B Y1B 114.7(14) . . ?
C3B C4B Y1B 74.9(8) . . ?
C3B C4B C14B 136(2) . . ?
C5B C4B Y1B 70.1(8) . . ?
C5B C4B C3B 106.7(15) . . ?
C5B C4B C14B 116.8(18) . . ?
C14B C4B Y1B 121.5(15) . . ?
C4B C5B Y1B 79.1(9) . . ?
C6B C5B Y1B 73.5(9) . . ?
C6B C5B C4B 109.7(17) . . ?
C0AA C6B Y1B 127.1(16) . . ?
C2B C6B Y1B 75.1(9) . . ?
C2B C6B C0AA 126(2) . . ?
C5B C6B Y1B 76.0(9) . . ?
C5B C6B C0AA 125(2) . . ?
C5B C6B C2B 106.4(17) . . ?
C3B C10B C11B 106(2) . . ?
C12B C10B C3B 111(2) . . ?
C12B C10B C11B 106(2) . . ?
C12B C10B C13B 110(2) . . ?
C13B C10B C3B 112(2) . . ?
C13B C10B C11B 112(2) . . ?
C4B C14B C17B 112(2) . . ?
C15B C14B C4B 114(2) . . ?
C15B C14B C16B 112(2) . . ?
C15B C14B C17B 107(2) . . ?
C16B C14B C4B 108(2) . . ?
C16B C14B C17B 105(2) . . ?
C19B C18B Y1B 73.5(9) . . ?
C19B C18B C23B 129(2) . . ?
C22B C18B Y1B 75.4(9) . . ?
C22B C18B C19B 107.1(17) . . ?
C22B C18B C23B 121(2) . . ?
C23B C18B Y1B 130.5(17) . . ?
C18B C19B Y1B 75.8(9) . . ?
C18B C19B C20B 110.4(18) . . ?
C20B C19B Y1B 79.6(9) . . ?
C19B C20B Y1B 69.6(8) . . ?
C19B C20B C21B 105.2(16) . . ?
C19B C20B C27B 117.9(19) . . ?
C21B C20B Y1B 75.6(8) . . ?
C21B C20B C27B 137(2) . . ?
C27B C20B Y1B 117.1(14) . . ?
C20B C21B Y1B 74.3(8) . . ?
C20B C21B C31B 133(2) . . ?
C22B C21B Y1B 70.7(8) . . ?
C22B C21B C20B 107.2(16) . . ?
C22B C21B C31B 119.7(18) . . ?
C31B C21B Y1B 124.1(15) . . ?
C18B C22B Y1B 74.5(9) . . ?
C18B C22B C21B 110.0(17) . . ?
C21B C22B Y1B 79.0(9) . . ?
C18B C23B C24B 111(2) . . ?
C18B C23B C25B 111(2) . . ?
C18B C23B C26B 110(2) . . ?
C24B C23B C25B 105(2) . . ?
C26B C23B C24B 110(2) . . ?
C26B C23B C25B 109(2) . . ?
C28B C27B C20B 108(2) . . ?
C29B C27B C20B 111(2) . . ?
C29B C27B C28B 106(2) . . ?
C30B C27B C20B 110(2) . . ?
C30B C27B C28B 111(2) . . ?
C30B C27B C29B 110(2) . . ?
C32B C31B C21B 111(2) . . ?
C33B C31B C21B 113(2) . . ?
C33B C31B C32B 104(2) . . ?
C34B C31B C21B 110(2) . . ?
C34B C31B C32B 107(2) . . ?
C34B C31B C33B 112(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.922
_oxdiff_exptl_absorpt_empirical_full_min 0.691
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
