# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_mx8179e_sq
_database_code_depnum_ccdc_archive 'CCDC 1960863'
loop_
_audit_author_name
_audit_author_address
'zeng min'
;Institute of chemistry chinese academy of sciences
China
;
_audit_update_record             
;
2019-10-23 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_audit_creation_date             2019-10-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C108 H60 O84 Tb12)'
_chemical_formula_sum            'C27 H15 O21 Tb3'
_chemical_formula_weight         1152.15
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Eu O H C'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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      tetragonal
_space_group_IT_number           95
_space_group_name_H-M_alt        'P 43 2 2'
_space_group_name_Hall           'P 4cw 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+3/4'
'-x, -y, z+1/2'
'y, -x, z+1/4'
'x, -y, -z+1/2'
'y, x, -z+1/4'
'-x, y, -z'
'-y, -x, -z+3/4'

_cell_length_a                   10.2107(2)
_cell_length_b                   10.2107(2)
_cell_length_c                   43.1372(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4497.4(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11665
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      29.6620
_cell_measurement_theta_min      1.8620
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.45i (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            29168
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.355
_diffrn_reflns_theta_min         1.888
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -103.00  12.00   0.50    4.40    --  -14.20  45.00 -14.83  230
  2  ω    -99.00  38.00   0.50    4.40    --  -14.20  45.00 120.00  274
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0531017000
_diffrn_orient_matrix_UB_12      -0.0408797000
_diffrn_orient_matrix_UB_13      -0.0043818000
_diffrn_orient_matrix_UB_21      0.0254723000
_diffrn_orient_matrix_UB_22      -0.0508538000
_diffrn_orient_matrix_UB_23      0.0094455000
_diffrn_orient_matrix_UB_31      -0.0370215000
_diffrn_orient_matrix_UB_32      0.0235784000
_diffrn_orient_matrix_UB_33      0.0127219000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.642
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.862
_reflns_number_gt                5719
_reflns_number_total             6144
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.429
_refine_diff_density_min         -2.326
_refine_diff_density_rms         0.259
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.14(4)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         6144
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0575
_refine_ls_restrained_S_all      1.151
_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)+(0.0304P)²+74.7209P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1285
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.86(4)
 0.14(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: H10A(0.5) H10B(0.5)
 Fixed Z: O10(0.125001)
5.a Riding coordinates:
 O10(H10A,H10B), O11(H11A,H11B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C11(H11), C15(H15)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.16230(5) 0.87350(5) 0.04065(2) 0.01176(13) Uani 1 1 d . . . . .
Tb2 Tb 0.14853(6) 1.14853(6) 0.125000 0.0191(2) Uani 1 2 d S T P . .
O1 O 0.1258(17) 1.0930(13) 0.0494(3) 0.070(4) Uani 1 1 d . . . . .
O2 O 0.0795(12) 1.2542(12) 0.0803(2) 0.038(3) Uani 1 1 d . . . . .
O3 O 0.333(2) 1.062(2) 0.1062(5) 0.114(7) Uani 1 1 d . . . . .
O4 O 0.3474(12) 0.9452(15) 0.0633(3) 0.058(4) Uani 1 1 d . . . . .
O5 O 0.1033(12) 0.9334(10) 0.1065(2) 0.033(2) Uani 1 1 d . . . . .
O6 O 0.1439(11) 0.7404(10) 0.0848(2) 0.031(2) Uani 1 1 d . . . . .
O7 O 0.0812(13) 0.6866(11) 0.0178(2) 0.040(3) Uani 1 1 d . . . . .
O8 O 0.2194(13) 0.9406(12) -0.0079(2) 0.040(3) Uani 1 1 d . . . . .
O9 O -0.0583(14) 0.9126(17) 0.0370(4) 0.073(4) Uani 1 1 d . . . . .
O10 O 0.3114(14) 1.3114(14) 0.125001 0.131(11) Uani 1 2 d S T P . .
H10A H 0.343615 1.350430 0.139770 0.196 Uiso 0.5 1 d R . . . .
H10B H 0.349925 1.344660 0.110290 0.196 Uiso 0.5 1 d R . . . .
O11 O 0.3427(12) 0.7267(12) 0.0290(3) 0.057(4) Uani 1 1 d . U . . .
H11A H 0.421201 0.743649 0.028430 0.085 Uiso 1 1 d R . . . .
H11B H 0.340011 0.648479 0.024790 0.085 Uiso 1 1 d R . . . .
C1 C 0.0865(16) 1.2049(16) 0.0546(3) 0.032(3) Uani 1 1 d . . . . .
C2 C 0.0438(15) 1.2838(13) 0.0263(3) 0.025(3) Uani 1 1 d . . . . .
C3 C 0.000000 1.219(2) 0.000000 0.027(4) Uani 1 2 d S T P . .
H3 H 0.000003 1.128196 -0.000001 0.032 Uiso 1 2 calc RS T P . .
C4 C 0.0448(15) 1.4166(13) 0.0261(3) 0.022(3) Uani 1 1 d . . . . .
H4 H 0.075517 1.461814 0.043305 0.027 Uiso 1 1 calc R . . . .
C5 C 0.000000 1.4871(17) 0.000000 0.019(4) Uani 1 2 d S T P . .
C6 C 0.393(2) 1.018(3) 0.0830(5) 0.071(7) Uani 1 1 d . . . . .
C7 C 0.1070(13) 0.8085(13) 0.1081(3) 0.021(3) Uani 1 1 d . . . . .
C8 C 0.0648(15) 0.7410(14) 0.1369(3) 0.024(3) Uani 1 1 d . . . . .
C9 C 0.0623(15) 0.6078(14) 0.1375(3) 0.026(3) Uani 1 1 d . . . . .
H9 H 0.090145 0.559696 0.120422 0.032 Uiso 1 1 calc R . . . .
C10 C 0.0181(19) 0.5455(17) 0.1636(4) 0.040(4) Uani 1 1 d . . . . .
C11 C 0.0230(14) 0.8097(13) 0.1623(3) 0.024(3) Uani 1 1 d . . . . .
H11 H 0.022141 0.900650 0.161314 0.028 Uiso 1 1 calc R . . . .
C12 C 0.000000 0.632(2) 0.000000 0.034(5) Uani 1 2 d S T P . .
C13 C 0.1708(13) 0.9370(14) -0.0338(3) 0.022(3) Uani 1 1 d . . . . .
C14 C 0.2500(13) 0.9821(13) -0.0609(3) 0.020(3) Uani 1 1 d . . . . .
C15 C 0.3849(15) 0.9806(15) -0.0593(3) 0.027(3) Uani 1 1 d . . . . .
H15 H 0.428390 0.955996 -0.041315 0.033 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.303(14) . ?
Tb1 O4 2.251(12) . ?
Tb1 O6 2.347(9) . ?
Tb1 O7 2.301(10) . ?
Tb1 O8 2.281(10) . ?
Tb1 O9 2.293(14) . ?
Tb1 O11 2.427(10) . ?
Tb2 O2 2.319(10) . ?
Tb2 O2 2.319(10) 6_465 ?
Tb2 O3 2.23(2) 6_465 ?
Tb2 O3 2.23(2) . ?
Tb2 O5 2.383(11) . ?
Tb2 O5 2.383(11) 6_465 ?
Tb2 O10 2.35(2) . ?
O1 C1 1.23(2) . ?
O2 C1 1.222(18) . ?
O3 C6 1.26(3) . ?
O4 C6 1.22(2) . ?
O5 C7 1.278(16) . ?
O6 C7 1.278(15) . ?
O7 C12 1.263(14) . ?
O8 C13 1.222(16) . ?
O9 C13 1.183(18) 7 ?
O10 H10A 0.8204 . ?
O10 H10B 0.8204 . ?
O11 H11A 0.8201 . ?
O11 H11B 0.8201 . ?
C1 C2 1.525(19) . ?
C2 C3 1.386(17) . ?
C2 C4 1.356(18) . ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C4 C5 1.411(16) . ?
C5 C12 1.47(3) 1_565 ?
C6 C10 1.57(3) 6_565 ?
C7 C8 1.485(17) . ?
C8 C9 1.361(19) . ?
C8 C11 1.368(19) . ?
C9 H9 0.9300 . ?
C9 C10 1.37(2) . ?
C10 C15 1.42(2) 4_465 ?
C11 H11 0.9300 . ?
C11 C14 1.374(17) 4_465 ?
C13 C14 1.492(17) . ?
C14 C15 1.38(2) . ?
C15 H15 0.9300 . ?

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 O6 114.7(4) . . ?
O1 Tb1 O11 139.2(5) . . ?
O4 Tb1 O1 75.4(6) . . ?
O4 Tb1 O6 84.4(5) . . ?
O4 Tb1 O7 139.3(5) . . ?
O4 Tb1 O8 95.0(5) . . ?
O4 Tb1 O9 143.0(5) . . ?
O4 Tb1 O11 69.7(5) . . ?
O6 Tb1 O11 82.6(4) . . ?
O7 Tb1 O1 145.0(5) . . ?
O7 Tb1 O6 80.7(4) . . ?
O7 Tb1 O11 70.9(5) . . ?
O8 Tb1 O1 84.3(5) . . ?
O8 Tb1 O6 160.1(4) . . ?
O8 Tb1 O7 87.0(4) . . ?
O8 Tb1 O9 97.8(5) . . ?
O8 Tb1 O11 78.6(5) . . ?
O9 Tb1 O1 71.5(6) . . ?
O9 Tb1 O6 94.5(5) . . ?
O9 Tb1 O7 76.2(5) . . ?
O9 Tb1 O11 147.0(5) . . ?
O2 Tb2 O2 166.9(6) 6_465 . ?
O2 Tb2 O5 95.1(4) 6_465 . ?
O2 Tb2 O5 95.2(4) . . ?
O2 Tb2 O5 95.1(4) . 6_465 ?
O2 Tb2 O5 95.2(4) 6_465 6_465 ?
O2 Tb2 O10 83.4(3) . . ?
O2 Tb2 O10 83.4(3) 6_465 . ?
O3 Tb2 O2 98.0(7) . . ?
O3 Tb2 O2 98.0(7) 6_465 6_465 ?
O3 Tb2 O2 77.8(6) . 6_465 ?
O3 Tb2 O2 77.8(6) 6_465 . ?
O3 Tb2 O3 143.3(12) 6_465 . ?
O3 Tb2 O5 71.0(6) . . ?
O3 Tb2 O5 145.2(7) 6_465 . ?
O3 Tb2 O5 145.2(7) . 6_465 ?
O3 Tb2 O5 71.0(6) 6_465 6_465 ?
O3 Tb2 O10 71.7(6) . . ?
O3 Tb2 O10 71.7(6) 6_465 . ?
O5 Tb2 O5 75.8(6) 6_465 . ?
O10 Tb2 O5 142.1(3) . 6_465 ?
O10 Tb2 O5 142.1(3) . . ?
C1 O1 Tb1 170.2(15) . . ?
C1 O2 Tb2 123.1(11) . . ?
C6 O3 Tb2 147.3(19) . . ?
C6 O4 Tb1 145.1(15) . . ?
C7 O5 Tb2 153.7(10) . . ?
C7 O6 Tb1 110.3(8) . . ?
C12 O7 Tb1 150.0(12) . . ?
C13 O8 Tb1 136.6(10) . . ?
C13 O9 Tb1 176.5(16) 7 . ?
Tb2 O10 H10A 128.8 . . ?
Tb2 O10 H10B 129.2 . . ?
H10A O10 H10B 101.9 . . ?
Tb1 O11 H11A 128.2 . . ?
Tb1 O11 H11B 128.5 . . ?
H11A O11 H11B 103.4 . . ?
O1 C1 C2 116.0(14) . . ?
O2 C1 O1 124.5(16) . . ?
O2 C1 C2 119.5(14) . . ?
C3 C2 C1 119.7(14) . . ?
C4 C2 C1 122.2(13) . . ?
C4 C2 C3 118.1(14) . . ?
C2 C3 C2 123.2(19) 7 . ?
C2 C3 H3 118.4 7 . ?
C2 C3 H3 118.4 . . ?
C2 C4 H4 119.5 . . ?
C2 C4 C5 120.9(13) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C4 118.7(16) . 7 ?
C4 C5 C12 120.7(8) 7 1_565 ?
C4 C5 C12 120.7(8) . 1_565 ?
O3 C6 C10 114(2) . 6_565 ?
O4 C6 O3 126(2) . . ?
O4 C6 C10 116.4(19) . 6_565 ?
O5 C7 C8 120.0(12) . . ?
O6 C7 O5 120.6(11) . . ?
O6 C7 C8 119.4(12) . . ?
C9 C8 C7 119.0(13) . . ?
C9 C8 C11 119.4(13) . . ?
C11 C8 C7 121.5(12) . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.0(14) . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C6 122.6(15) . 6_455 ?
C9 C10 C15 122.2(16) . 4_465 ?
C15 C10 C6 114.9(15) 4_465 6_455 ?
C8 C11 H11 118.6 . . ?
C8 C11 C14 122.8(13) . 4_465 ?
C14 C11 H11 118.6 4_465 . ?
O7 C12 O7 127(2) . 7 ?
O7 C12 C5 116.5(11) 7 1_545 ?
O7 C12 C5 116.5(11) . 1_545 ?
O8 C13 C14 118.9(13) . . ?
O9 C13 O8 120.4(15) 7 . ?
O9 C13 C14 120.1(13) 7 . ?
C11 C14 C13 120.8(12) 2_664 . ?
C11 C14 C15 119.1(12) 2_664 . ?
C15 C14 C13 120.1(12) . . ?
C10 C15 H15 121.4 2_664 . ?
C14 C15 C10 117.3(13) . 2_664 ?
C14 C15 H15 121.4 . . ?

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
Tb1 O4 C6 O3 23(5) . . . . ?
Tb1 O4 C6 C10 -179.7(16) . . . 6_565 ?
Tb1 O6 C7 O5 -9.8(17) . . . . ?
Tb1 O6 C7 C8 168.5(10) . . . . ?
Tb1 O7 C12 O7 7.9(13) . . . 7 ?
Tb1 O7 C12 C5 -172.1(13) . . . 1_545 ?
Tb1 O8 C13 O9 15(3) . . . 7 ?
Tb1 O8 C13 C14 -173.7(10) . . . . ?
Tb2 O2 C1 O1 3(3) . . . . ?
Tb2 O2 C1 C2 -177.5(10) . . . . ?
Tb2 O3 C6 O4 -44(6) . . . . ?
Tb2 O3 C6 C10 159(3) . . . 6_565 ?
Tb2 O5 C7 O6 -131.2(18) . . . . ?
Tb2 O5 C7 C8 50(3) . . . . ?
O1 C1 C2 C3 26(2) . . . . ?
O1 C1 C2 C4 -155.2(17) . . . . ?
O2 C1 C2 C3 -153.6(14) . . . . ?
O2 C1 C2 C4 25(2) . . . . ?
O5 C7 C8 C9 176.2(15) . . . . ?
O5 C7 C8 C11 -1(2) . . . . ?
O6 C7 C8 C9 -2(2) . . . . ?
O6 C7 C8 C11 -179.2(14) . . . . ?
O8 C13 C14 C11 -157.3(14) . . . 2_664 ?
O8 C13 C14 C15 24(2) . . . . ?
O9 C13 C14 C11 14(2) 7 . . 2_664 ?
O9 C13 C14 C15 -164.5(17) 7 . . . ?
C1 C2 C3 C2 178.2(15) . . . 7 ?
C1 C2 C4 C5 -177.5(11) . . . . ?
C2 C4 C5 C4 -0.7(11) . . . 7 ?
C2 C4 C5 C12 179.3(11) . . . 1_565 ?
C3 C2 C4 C5 1(2) . . . . ?
C4 C2 C3 C2 -0.6(11) . . . 7 ?
C7 C8 C9 C10 -177.3(15) . . . . ?
C7 C8 C11 C14 179.3(14) . . . 4_465 ?
C8 C9 C10 C6 -176.9(19) . . . 6_455 ?
C8 C9 C10 C15 -3(3) . . . 4_465 ?
C9 C8 C11 C14 2(2) . . . 4_465 ?
C11 C8 C9 C10 0(3) . . . . ?
C11 C14 C15 C10 -2(2) 2_664 . . 2_664 ?
C13 C14 C15 C10 176.7(14) . . . 2_664 ?

_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 1.963
_oxdiff_exptl_absorpt_empirical_full_min 0.752
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.86(4)
2 0.14(4)

####################################################################### 
# 
# 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_tx648_sq
_database_code_depnum_ccdc_archive 'CCDC 1960864'
loop_
_audit_author_name
_audit_author_address
'zeng min'
;Institute of chemistry chinese academy of sciences
China
;
_audit_update_record             
;
2019-10-23 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_audit_creation_date             2019-04-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C36 H20 O28 Tb4)'
_chemical_formula_sum            'C9 H5 O7 Tb'
_chemical_formula_weight         384.05
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Tb O C H'
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 '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      tetragonal
_space_group_IT_number           91
_space_group_name_H-M_alt        'P 41 2 2'
_space_group_name_Hall           'P 4w 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+3/4'
'-y, -x, -z+1/4'

_cell_length_a                   10.27740(10)
_cell_length_b                   10.27740(10)
_cell_length_c                   14.32360(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1512.93(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    12312
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      75.3520
_cell_measurement_theta_min      3.1880
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14174
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.467
_diffrn_reflns_theta_min         4.302
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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   -168.00 -82.00   0.50    0.10    --  -99.00 -96.00  57.00  172
  2  ω   -168.00 -76.00   0.50    0.10    --  -99.00 -88.00 -46.00  184
  3  ω   -168.00 -85.00   0.50    0.10    --  -99.00 -44.00 160.00  166
  4  ω    -62.00  25.00   0.50    0.05    --  -47.20  57.00  60.00  174
  5  ω   -120.00 -71.00   0.50    0.05    --  -47.20-125.00   0.00   98
  6  ω   -119.00 -34.00   0.50    0.05    --  -47.20 -44.00 160.00  170
  7  ω   -120.00 -71.00   0.50    0.05    --  -47.20-125.00 120.00   98
  8  ω    -24.00  75.00   0.50    0.05    --   47.20 -88.00 -46.00  198
  9  ω   -168.00 -86.00   0.50    0.10    --  -99.00 -30.00-150.00  164
 10  ω   -117.00 -26.00   0.50    0.10    --  -99.00 125.00 -60.00  182
 11  ω     91.00 169.00   0.50    0.10    --  103.25  30.00-150.00  156
 12  ω     91.00 169.00   0.50    0.10    --  103.25  45.00 -30.00  156
 13  ω     28.00 116.00   0.50    0.10    --  103.25 -30.00  30.00  176
 14  ω     31.00 117.00   0.50    0.10    --  103.25-125.00 -30.00  172
 15  ω   -120.00 -41.00   0.50    0.05    --  -47.20 -77.00 -60.00  158
 16  ω   -120.00 -24.00   0.50    0.05    --  -47.20 -77.00  60.00  192
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0520181000
_diffrn_orient_matrix_UB_12      -0.0469482000
_diffrn_orient_matrix_UB_13      -0.0951127000
_diffrn_orient_matrix_UB_21      0.1309744000
_diffrn_orient_matrix_UB_22      -0.0678575000
_diffrn_orient_matrix_UB_23      -0.0196446000
_diffrn_orient_matrix_UB_31      -0.0513698000
_diffrn_orient_matrix_UB_32      -0.1251143000
_diffrn_orient_matrix_UB_33      0.0460880000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.609
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.957
_reflns_number_gt                1522
_reflns_number_total             1537
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.723
_refine_diff_density_min         -1.257
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.027(17)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1537
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0308
_refine_ls_restrained_S_all      2.159
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0355P)²+5.7773P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0766
_refine_ls_wR_factor_ref         0.0769
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.973(17)
 0.027(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Restrained distances
 O4A-H4AA
 0.85 with sigma of 0.01
 O4A-H4AA
 2.22691 with sigma of 0.02
 Tb1-H4AA
 3.234533 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim C1 \\sim C2 \\sim C2A \\sim C1A \\sim O1A: within 1.7A with sigma of
0.02 and sigma for terminal atoms of 0.04
Uanis(O1) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C2A) \\sim
Ueq, Uanis(C1A) \\sim Ueq, Uanis(O1A) \\sim Ueq: with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
5. Others
 Sof(H3B)=1-FVAR(1)
 Sof(O4A)=Sof(H4AA)=Sof(H4AB)=0.5*(1-FVAR(2))
 Sof(O4)=Sof(H4A)=Sof(H4B)=0.5*FVAR(2)
 Sof(H3A)=FVAR(1)
 Sof(O1A)=1-FVAR(2)
 Sof(C2A)=Sof(C1A)=0.5*(1-FVAR(3))
 Sof(C1)=Sof(C2)=0.5*FVAR(3)
 Sof(O1)=FVAR(2)
6.a Riding coordinates:
 O4(H4A,H4B), C3(H3A,H3B), O4A(H4AA,H4AB)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.64065(4) -0.35935(4) 0.375000 0.02020(17) Uani 1 2 d DS T P . .
O1 O 0.532(3) -0.1740(16) 0.4268(16) 0.034(4) Uani 0.45(5) 1 d . U . A 1
O2 O 0.4168(10) 0.2516(8) 0.7396(5) 0.079(3) Uani 1 1 d . . . . .
O3 O 0.4024(8) 0.4230(6) 0.6610(5) 0.064(2) Uani 1 1 d . . . . .
O4 O 0.8137(19) -0.1863(19) 0.375000 0.076(12) Uani 0.42(6) 2 d S TU P A 1
H4A H 0.848905 -0.149490 0.421690 0.115 Uiso 0.21(3) 1 d R . . A 1
H4B H 0.849305 -0.149250 0.328570 0.115 Uiso 0.21(3) 1 d R . . A 1
C1 C 0.500000 -0.113(5) 0.500000 0.024(6) Uani 0.45(5) 2 d S TU P A 1
C2 C 0.500000 0.024(6) 0.500000 0.021(7) Uani 0.45(5) 2 d S TU P A 1
C3 C 0.4645(9) 0.0980(7) 0.5794(5) 0.0369(19) Uani 1 1 d . . . . .
H3A H 0.439477 0.054231 0.633332 0.044 Uiso 0.42(6) 1 d R . . A 1
H3B H 0.419827 0.050431 0.627382 0.044 Uiso 0.58(6) 1 d R . . A 1
C4 C 0.4644(8) 0.2335(7) 0.5798(5) 0.0307(16) Uani 1 1 d . . . . .
C5 C 0.500000 0.2971(10) 0.500000 0.025(2) Uani 1 2 d S T P . .
H5 H 0.500001 0.387613 0.500000 0.031 Uiso 1 2 calc RS T P . .
C6 C 0.4250(9) 0.3069(8) 0.6647(6) 0.0368(17) Uani 1 1 d . . . . .
C2A C 0.524(4) 0.038(4) 0.514(3) 0.017(6) Uani 0.27(2) 1 d . U . A 2
C1A C 0.533(4) -0.119(4) 0.513(3) 0.022(5) Uani 0.27(2) 1 d . U . A 2
O1A O 0.589(3) -0.1709(11) 0.4468(11) 0.030(4) Uani 0.55(5) 1 d . U . A 2
O4A O 0.796(3) -0.197(3) 0.314(3) 0.068(9) Uani 0.29(3) 1 d D U . A 2
H4AA H 0.872353 -0.174377 0.330182 0.103 Uiso 0.29(3) 1 d DR . . A 2
H4AB H 0.802524 -0.208107 0.255762 0.103 Uiso 0.29(3) 1 d R . . 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
Tb1 O1 2.330(17) 7_645 ?
Tb1 O1 2.330(17) . ?
Tb1 O2 2.310(7) 8_656 ?
Tb1 O2 2.310(7) 2_654 ?
Tb1 O3 2.338(7) 4_554 ?
Tb1 O3 2.338(7) 5_646 ?
Tb1 O4 2.52(3) . ?
Tb1 O1A 2.257(12) . ?
Tb1 O1A 2.257(12) 7_645 ?
Tb1 O4A 2.467(19) . ?
Tb1 O4A 2.467(19) 7_645 ?
O1 C1 1.26(3) . ?
O2 C6 1.216(11) . ?
O3 C6 1.216(10) . ?
C1 C2 1.41(8) . ?
C2 C3 1.41(3) 5_656 ?
C2 C3 1.41(3) . ?
C3 C4 1.393(10) . ?
C3 C2A 1.48(4) 5_656 ?
C3 C2A 1.27(4) . ?
C4 C5 1.367(9) . ?
C4 C6 1.487(10) . ?
C2A C2A 0.64(8) 5_656 ?
C2A C1A 1.62(7) . ?
C2A C1A 1.76(6) 5_656 ?
C1A C1A 0.76(8) 5_656 ?
C1A O1A 1.23(4) . ?
C1A O1A 1.47(5) 5_656 ?
O4A O4A 1.74(8) 7_645 ?

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 152.3(14) . 7_645 ?
O1 Tb1 O3 68.0(7) 7_645 5_646 ?
O1 Tb1 O3 139.6(7) . 5_646 ?
O1 Tb1 O3 68.0(7) . 4_554 ?
O1 Tb1 O3 139.6(7) 7_645 4_554 ?
O1 Tb1 O4 76.2(7) 7_645 . ?
O1 Tb1 O4 76.2(7) . . ?
O1 Tb1 O4A 82.5(9) 7_645 7_645 ?
O1 Tb1 O4A 71.6(11) . 7_645 ?
O2 Tb1 O1 99.9(8) 2_654 7_645 ?
O2 Tb1 O1 75.7(6) 2_654 . ?
O2 Tb1 O1 75.7(6) 8_656 7_645 ?
O2 Tb1 O1 99.9(8) 8_656 . ?
O2 Tb1 O2 161.8(5) 8_656 2_654 ?
O2 Tb1 O3 103.0(3) 8_656 4_554 ?
O2 Tb1 O3 91.8(3) 2_654 4_554 ?
O2 Tb1 O3 91.8(3) 8_656 5_646 ?
O2 Tb1 O3 103.0(3) 2_654 5_646 ?
O2 Tb1 O4 80.9(2) 8_656 . ?
O2 Tb1 O4 80.9(2) 2_654 . ?
O2 Tb1 O4A 99.1(9) 8_656 . ?
O2 Tb1 O4A 99.1(9) 2_654 7_645 ?
O2 Tb1 O4A 62.9(9) 8_656 7_645 ?
O2 Tb1 O4A 62.9(9) 2_654 . ?
O3 Tb1 O3 71.7(4) 5_646 4_554 ?
O3 Tb1 O4 144.15(19) 5_646 . ?
O3 Tb1 O4 144.15(19) 4_554 . ?
O3 Tb1 O4A 133.8(8) 4_554 7_645 ?
O3 Tb1 O4A 133.8(8) 5_646 . ?
O3 Tb1 O4A 145.5(8) 5_646 7_645 ?
O3 Tb1 O4A 145.5(8) 4_554 . ?
O1A Tb1 O2 84.9(5) 7_645 8_656 ?
O1A Tb1 O2 87.1(7) 7_645 2_654 ?
O1A Tb1 O2 84.9(5) . 2_654 ?
O1A Tb1 O2 87.1(7) . 8_656 ?
O1A Tb1 O1A 127.9(12) 7_645 . ?
O1A Tb1 O4A 56.3(10) . 7_645 ?
O1A Tb1 O4A 74.5(9) 7_645 7_645 ?
O1A Tb1 O4A 56.3(10) 7_645 . ?
O1A Tb1 O4A 74.5(9) . . ?
O4A Tb1 O4A 41.3(18) . 7_645 ?
C1 O1 Tb1 142(2) . . ?
C6 O2 Tb1 122.3(6) . 2_655 ?
C6 O3 Tb1 169.8(6) . 3 ?
O1 C1 O1 121(4) 5_656 . ?
O1 C1 C2 120(2) . . ?
O1 C1 C2 120(2) 5_656 . ?
C3 C2 C1 122(2) 5_656 . ?
C3 C2 C1 122(2) . . ?
C3 C2 C3 115(4) 5_656 . ?
C2 C3 C2A 14(2) . 5_656 ?
C4 C3 C2 123(2) . . ?
C4 C3 C2A 114.9(17) . 5_656 ?
C2A C3 C4 119.3(19) . . ?
C3 C4 C6 120.8(7) . . ?
C5 C4 C3 118.3(7) . . ?
C5 C4 C6 120.9(7) . . ?
C4 C5 C4 122.9(10) . 5_656 ?
O2 C6 C4 120.2(8) . . ?
O3 C6 O2 118.9(8) . . ?
O3 C6 C4 120.9(8) . . ?
C3 C2A C3 120(3) . 5_656 ?
C3 C2A C1A 117(3) . 5_656 ?
C3 C2A C1A 102(3) 5_656 5_656 ?
C3 C2A C1A 113(3) 5_656 . ?
C3 C2A C1A 121(3) . . ?
C2A C2A C3 96(6) 5_656 . ?
C2A C2A C1A 91.9(16) 5_656 . ?
C1A C1A C2A 87.6(16) 5_656 . ?
C1A C1A O1A 93(5) 5_656 . ?
C1A C1A O1A 56(4) 5_656 5_656 ?
O1A C1A C2A 108(3) 5_656 . ?
O1A C1A C2A 118(3) . . ?
O1A C1A O1A 123(3) . 5_656 ?
C1A O1A Tb1 147(2) . . ?
C1A O1A Tb1 134(2) 5_656 . ?
O4A O4A Tb1 69.4(9) 7_645 . ?

_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 3.842
_oxdiff_exptl_absorpt_empirical_full_min 0.579
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.973(17)
2 0.027(17)

####################################################################### 
# 
# 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_tx1608_sq
_database_code_depnum_ccdc_archive 'CCDC 1966281'
loop_
_audit_author_name
_audit_author_address
'zeng min'
;Institute of chemistry chinese academy of sciences
China
;
_audit_update_record             
;
2019-11-18 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_audit_creation_date             2019-11-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C108 H60 O84 Tb12)'
_chemical_formula_sum            'C27 H15 O21 Tb3'
_chemical_formula_weight         1152.15
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         TbCHO
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 '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      tetragonal
_space_group_IT_number           91
_space_group_name_H-M_alt        'P 41 2 2'
_space_group_name_Hall           'P 4w 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y, x, z+1/4'
'y, -x, z+3/4'
'-x, y, -z'
'x, -y, -z+1/2'
'y, x, -z+3/4'
'-y, -x, -z+1/4'

_cell_length_a                   10.22870(10)
_cell_length_b                   10.22870(10)
_cell_length_c                   43.1650(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4516.20(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    11037
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      74.5790
_cell_measurement_theta_min      4.1000
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.287
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19206
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.695
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            21640
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.437
_diffrn_reflns_theta_min         4.097
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -63.00  26.30   0.38    0.05    --  -47.20  12.00-149.00  235
  2  ω     31.00 118.02   0.38    0.20    --  103.25-128.00-164.00  229
  3  ω     87.00 167.94   0.38    0.20    --  103.25  12.00-149.00  213
  4  ω    -60.00  24.74   0.38    0.05    --  -47.20  38.00 120.00  223
  5  ω     91.00 167.76   0.38    0.20    --  103.25  30.00-150.00  202
  6  ω     91.00 167.76   0.38    0.20    --  103.25  45.00 -60.00  202
  7  ω     31.00 108.14   0.38    0.20    --  103.25 -94.00-150.00  203
  8  ω     35.00  60.08   0.38    0.05    --   47.20  38.00  60.00   66
  9  ω     32.00 119.02   0.38    0.05    --   47.20  57.00 120.00  229
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1186132000
_diffrn_orient_matrix_UB_12      0.0184438000
_diffrn_orient_matrix_UB_13      0.0215505000
_diffrn_orient_matrix_UB_21      0.0883245000
_diffrn_orient_matrix_UB_22      -0.0228202000
_diffrn_orient_matrix_UB_23      0.0284088000
_diffrn_orient_matrix_UB_31      0.0283784000
_diffrn_orient_matrix_UB_32      0.1477208000
_diffrn_orient_matrix_UB_33      0.0016792000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.647
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                4474
_reflns_number_total             4577
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.975
_refine_diff_density_min         -1.732
_refine_diff_density_rms         0.201
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.12(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4577
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0636
_refine_ls_restrained_S_all      1.080
_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)+(0.0612P)²+87.7014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1645
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.88(2)
 0.12(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(O1A)=1-FVAR(1)
 Sof(O1)=FVAR(1)
 Fixed Sof: H11A(0.5) H11B(0.5)
5.a Riding coordinates:
 O11(H11A,H11B)
5.b Rotating group:
 O10(H10A,H10B)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C8(H8), C23(H23), C27(H27)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb -0.14746(7) 0.14746(7) 0.625000 0.0197(3) Uani 1 2 d S T P . .
Tb2 Tb 0.13123(7) 0.15786(7) 0.70908(2) 0.0187(2) Uani 1 1 d . . . . .
O1 O -0.099(4) 0.334(3) 0.6488(7) 0.046(10) Uani 0.52(7) 1 d . U . A 1
O2 O 0.0559(16) 0.3418(12) 0.6870(3) 0.060(4) Uani 1 1 d . U . . .
O3 O 0.0675(14) 0.7749(16) 0.7430(3) 0.058(4) Uani 1 1 d . . . . .
O4 O 0.092(2) 0.9365(14) 0.7153(5) 0.089(6) Uani 1 1 d . . . . .
O5 O -0.1001(14) 0.9294(11) 0.6084(3) 0.045(3) Uani 1 1 d . . . . .
O6 O -0.1299(18) 0.7412(15) 0.5852(3) 0.067(5) Uani 1 1 d . . . . .
O7 O 0.3159(12) 0.0751(16) 0.7310(3) 0.056(4) Uani 1 1 d . . . . .
O8 O 0.7477(14) -0.0823(14) 0.8304(3) 0.053(4) Uani 1 1 d . . . . .
O9 O 0.9129(14) -0.112(2) 0.8004(4) 0.083(6) Uani 1 1 d . . . . .
O10 O 0.2814(16) 0.3341(17) 0.7188(5) 0.091(6) Uani 1 1 d . U . . .
H10A H 0.260349 0.430817 0.726104 0.136 Uiso 1 1 d GR . . . .
H10B H 0.384297 0.332987 0.716817 0.136 Uiso 1 1 d GR . . . .
O11 O -0.314(2) 0.314(2) 0.625000 0.130(12) Uani 1 2 d S TU P A .
H11A H -0.284786 0.390950 0.624530 0.195 Uiso 0.5 1 d R . . . .
H11B H -0.375966 0.337090 0.613160 0.195 Uiso 0.5 1 d R . . . .
C3 C -0.0121(19) 0.5404(19) 0.6651(4) 0.044(5) Uani 1 1 d . . . . .
C4 C -0.0530(19) 0.6057(15) 0.6384(3) 0.035(4) Uani 1 1 d . . . . .
H4 H -0.077437 0.557947 0.621016 0.042 Uiso 1 1 calc R . . . .
C5 C -0.0573(18) 0.7387(15) 0.6376(3) 0.032(4) Uani 1 1 d . . . . .
C6 C -0.0156(15) 0.8062(13) 0.6631(3) 0.026(3) Uani 1 1 d . . . . .
H6 H -0.013922 0.897046 0.662119 0.031 Uiso 1 1 calc R . . . .
C7 C 0.0241(14) 0.7466(15) 0.6903(3) 0.026(3) Uani 1 1 d . . . . .
C8 C 0.0245(15) 0.6101(15) 0.6913(3) 0.028(3) Uani 1 1 d . . . . .
H8 H 0.048958 0.566616 0.709336 0.034 Uiso 1 1 calc R . . . .
C9 C -0.009(2) 0.3901(19) 0.6660(4) 0.054(5) Uani 1 1 d . U . . .
C12 C 0.0689(17) 0.8253(17) 0.7175(4) 0.036(4) Uani 1 1 d . . . . .
C15 C -0.0981(17) 0.8118(17) 0.6091(4) 0.039(4) Uani 1 1 d . . . . .
C20 C 0.8012(18) -0.0802(16) 0.8047(4) 0.040(4) Uani 1 1 d . . . . .
C22 C 0.7202(15) -0.0442(15) 0.7764(3) 0.029(3) Uani 1 1 d . . . . .
C23 C 0.5890(14) -0.0408(16) 0.7763(3) 0.030(3) Uani 1 1 d . . . . .
H23 H 0.543934 -0.066082 0.794038 0.036 Uiso 1 1 calc R . . . .
C24 C 0.517(2) 0.000000 0.750000 0.027(4) Uani 1 2 d S T P . .
C25 C 0.374(2) 0.000000 0.750000 0.035(5) Uani 1 2 d S T P . .
C27 C 0.790(2) 0.000000 0.750000 0.028(4) Uani 1 2 d S T P . .
H27 H 0.881026 0.000002 0.750000 0.033 Uiso 1 2 calc RS T P . .
O1A O -0.029(4) 0.333(3) 0.6395(7) 0.040(10) Uani 0.48(7) 1 d . U . 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
Tb1 O1 2.22(2) . ?
Tb1 O1 2.22(2) 8_556 ?
Tb1 O5 2.393(12) 1_545 ?
Tb1 O5 2.393(12) 8_656 ?
Tb1 O8 2.303(12) 4_564 ?
Tb1 O8 2.303(12) 6_456 ?
Tb1 O11 2.41(3) . ?
Tb1 O1A 2.33(3) 8_556 ?
Tb1 O1A 2.33(3) . ?
Tb2 O2 2.246(13) . ?
Tb2 O3 2.276(12) 6_566 ?
Tb2 O4 2.315(14) 1_545 ?
Tb2 O6 2.332(14) 8_656 ?
Tb2 O7 2.276(12) . ?
Tb2 O9 2.318(14) 6_456 ?
Tb2 O10 2.405(14) . ?
O1 C9 1.32(3) . ?
O2 C9 1.23(2) . ?
O3 C12 1.21(2) . ?
O4 C12 1.17(2) . ?
O5 C15 1.20(2) . ?
O6 C15 1.30(2) . ?
O7 C25 1.273(15) . ?
O8 C20 1.24(2) . ?
O9 C20 1.20(2) . ?
C3 C4 1.40(2) . ?
C3 C8 1.39(2) . ?
C3 C9 1.54(3) . ?
C4 C5 1.36(2) . ?
C5 C6 1.37(2) . ?
C5 C15 1.50(2) . ?
C6 C7 1.38(2) . ?
C7 C8 1.40(2) . ?
C7 C12 1.50(2) . ?
C9 O1A 1.30(3) . ?
C20 C22 1.52(2) . ?
C22 C23 1.34(2) . ?
C22 C27 1.419(19) . ?
C23 C24 1.414(18) . ?
C24 C25 1.46(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O1 127(2) . 8_556 ?
O1 Tb1 O5 80.0(11) 8_556 1_545 ?
O1 Tb1 O5 80.0(11) . 8_656 ?
O1 Tb1 O5 153.2(11) . 1_545 ?
O1 Tb1 O5 153.2(11) 8_556 8_656 ?
O1 Tb1 O8 85.6(10) . 4_564 ?
O1 Tb1 O8 88.0(11) . 6_456 ?
O1 Tb1 O8 85.6(10) 8_556 6_456 ?
O1 Tb1 O8 88.0(11) 8_556 4_564 ?
O1 Tb1 O11 63.4(10) 8_556 . ?
O1 Tb1 O11 63.4(10) . . ?
O1 Tb1 O1A 138.6(16) . 8_556 ?
O1 Tb1 O1A 20.4(8) 8_556 8_556 ?
O5 Tb1 O5 73.3(6) 8_656 1_545 ?
O5 Tb1 O11 143.4(3) 1_545 . ?
O5 Tb1 O11 143.4(3) 8_656 . ?
O8 Tb1 O5 97.1(5) 6_456 8_656 ?
O8 Tb1 O5 97.1(5) 4_564 1_545 ?
O8 Tb1 O5 94.3(5) 4_564 8_656 ?
O8 Tb1 O5 94.3(5) 6_456 1_545 ?
O8 Tb1 O8 165.7(8) 6_456 4_564 ?
O8 Tb1 O11 82.8(4) 6_456 . ?
O8 Tb1 O11 82.8(4) 4_564 . ?
O8 Tb1 O1A 104.6(10) 4_564 8_556 ?
O8 Tb1 O1A 72.3(10) 4_564 . ?
O8 Tb1 O1A 72.3(9) 6_456 8_556 ?
O8 Tb1 O1A 104.6(10) 6_456 . ?
O1A Tb1 O5 137.1(10) 8_556 8_656 ?
O1A Tb1 O5 66.5(8) 8_556 1_545 ?
O1A Tb1 O5 137.1(10) . 1_545 ?
O1A Tb1 O5 66.5(8) . 8_656 ?
O1A Tb1 O11 78.0(8) . . ?
O1A Tb1 O11 78.0(8) 8_556 . ?
O1A Tb1 O1A 155.9(16) 8_556 . ?
O2 Tb2 O3 92.0(5) . 6_566 ?
O2 Tb2 O4 144.0(6) . 1_545 ?
O2 Tb2 O6 87.0(6) . 8_656 ?
O2 Tb2 O7 140.6(6) . . ?
O2 Tb2 O9 76.4(7) . 6_456 ?
O2 Tb2 O10 70.5(6) . . ?
O3 Tb2 O4 98.1(7) 6_566 1_545 ?
O3 Tb2 O6 160.5(6) 6_566 8_656 ?
O3 Tb2 O9 86.8(6) 6_566 6_456 ?
O3 Tb2 O10 78.3(7) 6_566 . ?
O4 Tb2 O6 94.2(7) 1_545 8_656 ?
O4 Tb2 O9 69.8(8) 1_545 6_456 ?
O4 Tb2 O10 145.4(6) 1_545 . ?
O6 Tb2 O10 83.0(7) 8_656 . ?
O7 Tb2 O3 88.4(5) . 6_566 ?
O7 Tb2 O4 74.5(6) . 1_545 ?
O7 Tb2 O6 80.2(5) . 8_656 ?
O7 Tb2 O9 142.9(6) . 6_456 ?
O7 Tb2 O10 71.1(6) . . ?
O9 Tb2 O6 111.7(6) 6_456 8_656 ?
O9 Tb2 O10 142.9(7) 6_456 . ?
C9 O1 Tb1 143(3) . . ?
C9 O2 Tb2 146.7(13) . . ?
C12 O3 Tb2 133.8(13) . 6_566 ?
C12 O4 Tb2 177.4(17) . 1_565 ?
C15 O5 Tb1 157.9(13) . 1_565 ?
C15 O6 Tb2 111.8(11) . 8_566 ?
C25 O7 Tb2 151.9(12) . . ?
C20 O8 Tb1 123.4(12) . 3_655 ?
C20 O9 Tb2 175.8(18) . 6_656 ?
C4 C3 C9 120.2(15) . . ?
C8 C3 C4 120.5(17) . . ?
C8 C3 C9 119.3(16) . . ?
C5 C4 C3 120.6(16) . . ?
C4 C5 C6 118.3(14) . . ?
C4 C5 C15 121.9(15) . . ?
C6 C5 C15 119.7(14) . . ?
C5 C6 C7 123.4(14) . . ?
C6 C7 C8 118.0(13) . . ?
C6 C7 C12 121.3(14) . . ?
C8 C7 C12 120.7(14) . . ?
C3 C8 C7 119.1(15) . . ?
O1 C9 C3 114(2) . . ?
O2 C9 O1 128(2) . . ?
O2 C9 C3 115.5(17) . . ?
O2 C9 O1A 124(2) . . ?
O1A C9 C3 115.3(19) . . ?
O3 C12 C7 118.7(16) . . ?
O4 C12 O3 119.3(18) . . ?
O4 C12 C7 121.5(17) . . ?
O5 C15 O6 121.9(17) . . ?
O5 C15 C5 121.8(16) . . ?
O6 C15 C5 116.3(15) . . ?
O8 C20 C22 118.9(16) . . ?
O9 C20 O8 123.6(18) . . ?
O9 C20 C22 117.4(17) . . ?
C23 C22 C20 123.6(15) . . ?
C23 C22 C27 119.6(14) . . ?
C27 C22 C20 116.6(14) . . ?
C22 C23 C24 121.8(14) . . ?
C23 C24 C23 117.6(19) 6_556 . ?
C23 C24 C25 121.2(9) . . ?
C23 C24 C25 121.2(9) 6_556 . ?
O7 C25 O7 124(2) . 6_556 ?
O7 C25 C24 118.0(10) 6_556 . ?
O7 C25 C24 118.0(10) . . ?
C22 C27 C22 119.5(19) 6_556 . ?
C9 O1A Tb1 133(3) . . ?

_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 2.723
_oxdiff_exptl_absorpt_empirical_full_min 0.616
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.88(2)
2 0.12(2)

####################################################################### 
# 
# 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_tx1606-a_sq
_database_code_depnum_ccdc_archive 'CCDC 1966280'
loop_
_audit_author_name
_audit_author_address
'zeng min'
;Institute of chemistry chinese academy of sciences
China
;
_audit_update_record             
;
2019-11-18 deposited with the CCDC.	2020-08-17 downloaded from the CCDC.
;
_audit_creation_date             2019-11-15
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C36 H20 O28 Tb4)'
_chemical_formula_sum            'C9 H5 O7 Tb'
_chemical_formula_weight         384.05
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         TbCHO
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -9.1472 9.1891 '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      tetragonal
_space_group_IT_number           95
_space_group_name_H-M_alt        'P 43 2 2'
_space_group_name_Hall           'P 4cw 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z+3/4'
'-x, -y, z+1/2'
'y, -x, z+1/4'
'x, -y, -z+1/2'
'-x, y, -z'
'y, x, -z+1/4'
'-y, -x, -z+3/4'

_cell_length_a                   10.2191(2)
_cell_length_b                   10.2191(2)
_cell_length_c                   14.3738(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1501.06(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4119
_cell_measurement_temperature    169.97(10)
_cell_measurement_theta_max      73.6750
_cell_measurement_theta_min      3.0040
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    23.354
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.19424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7117
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.165
_diffrn_reflns_theta_min         4.326
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     11.00  91.00   0.50    0.13    --   46.95-117.00  78.00  160
  2  ω   -168.00 -86.00   0.50    0.53    --  -99.00 -45.00 150.00  164
  3  ω     82.00 169.00   0.50    0.53    --  103.25 117.00 166.00  174
  4  ω     32.00 116.00   0.50    0.53    --  103.25 -45.00 150.00  168
  5  ω   -119.00 -71.00   0.50    0.13    --  -46.95-125.00-120.00   96
  6  ω     34.00 119.00   0.50    0.13    --   46.95  45.00 -59.00  170
  7  ω   -168.00 -86.00   0.50    0.53    --  -99.00 -45.00   0.00  164
  8  ω     91.00 169.00   0.50    0.53    --  103.25  45.00-180.00  156
  9  ω     32.00  92.00   0.50    0.13    --   46.95  57.00  60.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0626153000
_diffrn_orient_matrix_UB_12      0.1118369000
_diffrn_orient_matrix_UB_13      0.0563954000
_diffrn_orient_matrix_UB_21      -0.0564280000
_diffrn_orient_matrix_UB_22      0.0584394000
_diffrn_orient_matrix_UB_23      -0.0902703000
_diffrn_orient_matrix_UB_31      -0.1250730000
_diffrn_orient_matrix_UB_32      -0.0823723000
_diffrn_orient_matrix_UB_33      0.0125045000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_reflns_Friedel_coverage         0.599
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                1446
_reflns_number_total             1490
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.900
_refine_diff_density_rms         0.148
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.11(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1490
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0536
_refine_ls_restrained_S_all      1.176
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0218P)²+15.9645P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1210
_refine_ls_wR_factor_ref         0.1272
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.89(3)
 0.11(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
O3A \\sim O3 \\sim O2 \\sim O2A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O2) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O3)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O2A)=Sof(O3A)=1-FVAR(1)
 Sof(O2)=Sof(O3)=FVAR(1)
 Fixed Sof: O4(0.5) H4A(0.5) H4B(0.5)
5.a Riding coordinates:
 O4(H4A,H4B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4)
;
_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
Tb1 Tb 0.14509(7) 0.85491(7) 0.375000 0.0361(3) Uani 1 2 d S T P . .
O1 O 0.0745(11) 0.8979(17) 0.5909(13) 0.117(7) Uani 1 1 d . . . . .
O2 O 0.233(3) 0.933(3) 0.5154(18) 0.060(7) Uani 0.53(4) 1 d . U . A 1
O3 O 0.331(2) 0.901(3) 0.2997(17) 0.046(6) Uani 0.53(4) 1 d . U . A 1
O4 O 0.323(5) 0.701(4) 0.347(2) 0.123(15) Uani 0.5 1 d . . . A .
H4A H 0.383278 0.663898 0.378441 0.185 Uiso 0.5 1 d R . . . .
H4B H 0.337638 0.684708 0.290291 0.185 Uiso 0.5 1 d R . . . .
C1 C 0.467(2) 1.000000 0.750000 0.063(7) Uani 1 2 d S T P . .
C2 C 0.3985(13) 0.9593(17) 0.6709(9) 0.048(4) Uani 1 1 d . . . . .
H2 H 0.442990 0.931171 0.618114 0.057 Uiso 1 1 calc R . . . .
C3 C 0.2638(14) 0.9617(16) 0.6728(10) 0.047(4) Uani 1 1 d . . . . .
C4 C 0.1974(19) 1.000000 0.750000 0.050(5) Uani 1 2 d S T P . .
H4 H 0.106372 0.999999 0.750001 0.060 Uiso 1 2 calc RS T P . .
C5 C 0.1904(17) 0.915(2) 0.5879(12) 0.063(5) Uani 1 1 d . . . . .
C6 C 0.385(2) 1.000000 0.250000 0.067(7) Uani 1 2 d S T P . .
O2A O 0.270(3) 0.879(4) 0.509(2) 0.063(8) Uani 0.47(4) 1 d . U . A 2
O3A O 0.331(2) 0.965(3) 0.3228(18) 0.039(6) Uani 0.47(4) 1 d . U . 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
Tb1 O1 2.339(13) 6_556 ?
Tb1 O1 2.339(13) 2_664 ?
Tb1 O2 2.35(2) 8_665 ?
Tb1 O2 2.35(2) . ?
Tb1 O3 2.24(2) 8_665 ?
Tb1 O3 2.24(2) . ?
Tb1 O4 2.44(2) . ?
Tb1 O4 2.44(2) 8_665 ?
Tb1 O2A 2.32(3) . ?
Tb1 O2A 2.32(3) 8_665 ?
Tb1 O3A 2.33(2) . ?
Tb1 O3A 2.33(2) 8_665 ?
O1 C5 1.20(2) . ?
O2 C5 1.14(3) . ?
O3 C6 1.36(3) . ?
O4 O4 0.87(5) 8_665 ?
C1 C2 1.399(16) 5_576 ?
C1 C2 1.399(16) . ?
C1 C6 1.52(3) 3_675 ?
C2 C3 1.377(19) . ?
C3 C4 1.358(18) . ?
C3 C5 1.51(2) . ?
C5 O2A 1.44(4) . ?
C6 O3A 1.23(2) . ?
C6 O3A 1.23(2) 5_575 ?

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 71.5(8) 2_664 6_556 ?
O1 Tb1 O2 97.0(10) 6_556 . ?
O1 Tb1 O2 97.0(10) 2_664 8_665 ?
O1 Tb1 O2 85.6(10) 2_664 . ?
O1 Tb1 O2 85.6(10) 6_556 8_665 ?
O1 Tb1 O4 136.5(11) 2_664 . ?
O1 Tb1 O4 150.6(14) 2_664 8_665 ?
O1 Tb1 O4 136.5(11) 6_556 8_665 ?
O1 Tb1 O4 150.6(14) 6_556 . ?
O2 Tb1 O2 176.8(19) . 8_665 ?
O2 Tb1 O4 94.4(16) . . ?
O2 Tb1 O4 94.4(16) 8_665 8_665 ?
O2 Tb1 O4 82.5(16) . 8_665 ?
O2 Tb1 O4 82.5(16) 8_665 . ?
O3 Tb1 O1 81.8(9) . 2_664 ?
O3 Tb1 O1 151.4(8) . 6_556 ?
O3 Tb1 O1 151.4(8) 8_665 2_664 ?
O3 Tb1 O1 81.8(9) 8_665 6_556 ?
O3 Tb1 O2 91.2(11) . . ?
O3 Tb1 O2 87.4(9) . 8_665 ?
O3 Tb1 O2 87.4(9) 8_665 . ?
O3 Tb1 O2 91.2(11) 8_665 8_665 ?
O3 Tb1 O3 126.1(15) . 8_665 ?
O3 Tb1 O4 54.7(13) 8_665 8_665 ?
O3 Tb1 O4 54.7(13) . . ?
O3 Tb1 O4 71.7(12) . 8_665 ?
O3 Tb1 O4 71.7(12) 8_665 . ?
O3 Tb1 O2A 78.7(10) . 8_665 ?
O3 Tb1 O2A 85.0(11) 8_665 8_665 ?
O3 Tb1 O3A 18.4(6) 8_665 8_665 ?
O3 Tb1 O3A 137.3(12) . 8_665 ?
O4 Tb1 O4 20.5(13) . 8_665 ?
O2A Tb1 O1 109.4(10) . 6_556 ?
O2A Tb1 O1 100.0(11) 8_665 6_556 ?
O2A Tb1 O4 65.8(16) 8_665 . ?
O2A Tb1 O4 78.2(16) . . ?
O2A Tb1 O3A 94.9(10) . 8_665 ?
O2A Tb1 O3A 76.6(10) 8_665 8_665 ?
O2A Tb1 O3A 76.6(10) . . ?
O2A Tb1 O3A 94.9(10) 8_665 . ?
O3A Tb1 O1 139.4(8) . 6_556 ?
O3A Tb1 O1 67.9(8) 8_665 6_556 ?
O3A Tb1 O4 83.4(13) 8_665 . ?
O3A Tb1 O4 69.6(14) . . ?
O3A Tb1 O3A 152.8(14) . 8_665 ?
C5 O1 Tb1 169.6(17) . 4_465 ?
C5 O2 Tb1 126(2) . . ?
C6 O3 Tb1 139(2) . . ?
O4 O4 Tb1 79.8(6) 8_665 . ?
C2 C1 C2 119.9(19) 5_576 . ?
C2 C1 C6 120.1(10) 5_576 3_675 ?
C2 C1 C6 120.1(10) . 3_675 ?
C3 C2 C1 118.6(15) . . ?
C2 C3 C5 118.3(15) . . ?
C4 C3 C2 121.4(15) . . ?
C4 C3 C5 120.2(14) . . ?
C3 C4 C3 120.0(19) 5_576 . ?
O1 C5 C3 120.5(18) . . ?
O1 C5 O2A 123(2) . . ?
O2 C5 O1 115(2) . . ?
O2 C5 C3 120(2) . . ?
O2A C5 C3 115.9(17) . . ?
O3 C6 O3 132(3) 5_575 . ?
O3 C6 C1 113.8(13) 5_575 3_674 ?
O3 C6 C1 113.8(13) . 3_674 ?
O3A C6 O3 119.0(19) . 5_575 ?
O3A C6 O3 32.6(12) 5_575 5_575 ?
O3A C6 O3A 127(3) 5_575 . ?
C5 O2A Tb1 111.7(19) . . ?
C6 O3A Tb1 141(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
;
_oxdiff_exptl_absorpt_empirical_full_max 3.653
_oxdiff_exptl_absorpt_empirical_full_min 0.573
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.89(3)
2 0.11(3)

