# Electronic Supplementary Material (ESI) for CrystEngComm.
# 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_cpdc-Eu
_database_code_depnum_ccdc_archive 'CCDC 1963199'
loop_
_audit_author_name
_audit_author_address
'Qi-Bing Bo'
;university of Jinan
China
;
_audit_update_record             
;
2019-11-02 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_audit_creation_date             2019-11-02
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C30 H36 Eu4 O30)'
_chemical_formula_sum            'C15 H18 Eu2 O15'
_chemical_formula_weight         742.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Eu'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   9.7632(18)
_cell_length_b                   7.9567(15)
_cell_length_c                   12.920(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.11(2)
_cell_angle_gamma                90
_cell_volume                     964.3(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2287
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1350
_cell_measurement_theta_min      4.8300
_shelx_estimated_absorpt_T_max   0.849
_shelx_estimated_absorpt_T_min   0.166
_exptl_absorpt_coefficient_mu    6.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39542
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.556
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             708
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.026
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6352
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.064
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -52.00   43.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -77.0000    0.0000 95

#__ type_ start__ end____ width___ exp.time_
  2 omega  -51.00   33.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -57.0000   60.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   55.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -99.0000  -90.0000 80

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00   62.00   1.0000    1.1400
omega____ theta____ kappa____ phi______ frames
    -       15.8569   57.0000   30.0000 63
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0104606000
_diffrn_orient_matrix_UB_12      -0.0088061000
_diffrn_orient_matrix_UB_13      -0.0562754000
_diffrn_orient_matrix_UB_21      0.0712282000
_diffrn_orient_matrix_UB_22      -0.0286182000
_diffrn_orient_matrix_UB_23      0.0094598000
_diffrn_orient_matrix_UB_31      -0.0231996000
_diffrn_orient_matrix_UB_32      -0.0840308000
_diffrn_orient_matrix_UB_33      0.0027095000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1808
_reflns_number_total             2103
_reflns_odcompleteness_completeness 99.57
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.835
_refine_diff_density_rms         0.155
_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     160
_refine_ls_number_reflns         2103
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0251
_refine_ls_restrained_S_all      1.071
_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)+(0.0232P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0595
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. 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
2. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H8A(0.5) H8B(0.5) H9A(0.5) H9B(0.5)
3.a Rotating group:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B)
3.b Ternary CH refined with riding coordinates:
 C5(H5), C2(H2), C8(H8)
3.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C3(H3A,H3B), C9(H9C,H9D)
;
_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
Eu1 Eu 0.49096(3) 0.7500 0.13280(2) 0.01269(10) Uani 1 2 d S T P . .
Eu2 Eu 0.89865(3) 0.2500 0.50740(2) 0.01497(10) Uani 1 2 d S T P . .
O1 O 0.5840(4) 0.5625(4) 0.2764(3) 0.0332(9) Uani 1 1 d . . . . .
O2 O 0.7199(4) 0.4253(5) 0.4112(3) 0.0443(11) Uani 1 1 d . . . . .
O3 O 0.6592(3) 0.5695(4) 0.0876(2) 0.0198(7) Uani 1 1 d . . . . .
O4 O 0.6845(3) 0.4608(4) -0.0653(2) 0.0257(8) Uani 1 1 d . . . . .
O5 O 0.9898(4) 0.5735(4) 0.5945(3) 0.0313(8) Uani 1 1 d . . . . .
O6 O 0.8377(4) 0.4210(4) 0.6472(3) 0.0319(9) Uani 1 1 d . . . . .
O7 O 0.4483(5) 0.7500 -0.0676(3) 0.0253(11) Uani 1 2 d S T P . .
H7A H 0.4103 0.6425 -0.1065 0.038 Uiso 0.5 1 d GR . . . .
H7B H 0.5320 0.7769 -0.0950 0.038 Uiso 0.5 1 d GR . . . .
O8 O 0.3212(5) 0.7500 0.2426(4) 0.0286(11) Uani 1 2 d S T P . .
H8A H 0.3168 0.8339 0.2970 0.043 Uiso 0.5 1 d GR . . . .
H8B H 0.2496 0.6577 0.2447 0.043 Uiso 0.5 1 d GR . . . .
O9 O 1.1381(5) 0.2500 0.6231(4) 0.0300(12) Uani 1 2 d S T P . .
H9A H 1.1837 0.3570 0.6306 0.045 Uiso 0.5 1 d GR . . . .
H9B H 1.2026 0.1844 0.5970 0.045 Uiso 0.5 1 d GR . . . .
C5 C 0.8557(4) 0.6529(5) 0.0237(3) 0.0175(10) Uani 1 1 d . . . . .
H5 H 0.9198 0.6019 -0.0138 0.021 Uiso 1 1 calc R . . . .
C6 C 0.9291(7) 0.7500 0.1217(5) 0.0255(16) Uani 1 2 d S T P . .
H6A H 1.0325 0.7500 0.1433 0.031 Uiso 1 2 calc RS T P . .
H6B H 0.8862 0.7500 0.1811 0.031 Uiso 1 2 calc RS T P . .
C4 C 0.7231(5) 0.5565(5) 0.0151(3) 0.0176(10) Uani 1 1 d . . . . .
C2 C 0.4768(5) 0.3465(6) 0.3467(5) 0.0358(14) Uani 1 1 d . . . . .
H2 H 0.3859 0.3957 0.3058 0.043 Uiso 1 1 calc R . . . .
C3 C 0.4673(10) 0.2500 0.4434(8) 0.051(2) Uani 1 2 d S T P . .
H3A H 0.5502 0.2500 0.5056 0.061 Uiso 1 2 calc RS T P . .
H3B H 0.3766 0.2500 0.4604 0.061 Uiso 1 2 calc RS T P . .
C1 C 0.6016(5) 0.4486(6) 0.3441(4) 0.0208(10) Uani 1 1 d . . . . .
C8 C 0.9269(5) 0.6542(5) 0.7545(3) 0.0210(11) Uani 1 1 d . . . . .
H8 H 0.8812 0.6051 0.8061 0.025 Uiso 1 1 calc R . . . .
C9 C 1.0590(8) 0.7500 0.8064(6) 0.0315(18) Uani 1 2 d S T P . .
H9C H 1.1344 0.7500 0.7709 0.038 Uiso 1 2 calc RS T P . .
H9D H 1.0918 0.7500 0.8845 0.038 Uiso 1 2 calc RS T P . .
C7 C 0.9171(5) 0.5461(6) 0.6585(3) 0.0185(10) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.357(3) 4_575 ?
Eu1 O1 2.357(3) . ?
Eu1 O3 2.374(3) 4_575 ?
Eu1 O3 2.374(3) . ?
Eu1 O4 2.383(3) 3_665 ?
Eu1 O4 2.383(3) 2_655 ?
Eu1 O7 2.506(4) . ?
Eu1 O8 2.463(5) . ?
Eu2 Eu2 4.4711(7) 3_766 ?
Eu2 O2 2.309(3) 4_565 ?
Eu2 O2 2.309(3) . ?
Eu2 O5 2.851(3) . ?
Eu2 O5 2.385(3) 3_766 ?
Eu2 O5 2.851(3) 4_565 ?
Eu2 O5 2.385(3) 2_746 ?
Eu2 O6 2.463(3) 4_565 ?
Eu2 O6 2.463(3) . ?
Eu2 O9 2.400(4) . ?
Eu2 C7 3.033(5) . ?
Eu2 C7 3.033(5) 4_565 ?
O1 C1 1.238(5) . ?
O2 C1 1.250(5) . ?
O3 C4 1.266(5) . ?
O4 Eu1 2.383(3) 3_665 ?
O4 C4 1.259(5) . ?
O5 Eu2 2.385(3) 3_766 ?
O5 C7 1.249(5) . ?
O6 C7 1.246(5) . ?
O7 H7A 1.0090 . ?
O7 H7B 1.0000 . ?
O8 H8A 0.9787 . ?
O8 H8B 1.0192 . ?
O9 H9A 0.9529 . ?
O9 H9B 0.9479 . ?
C5 C5 1.545(8) 4_575 ?
C5 H5 0.9800 . ?
C5 C6 1.487(6) . ?
C5 C4 1.482(6) . ?
C6 C5 1.487(6) 4_575 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C2 C2 1.536(9) 4_565 ?
C2 H2 0.9800 . ?
C2 C3 1.491(9) . ?
C2 C1 1.472(6) . ?
C3 C2 1.491(9) 4_565 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C8 C8 1.524(8) 4_575 ?
C8 H8 0.9800 . ?
C8 C9 1.488(7) . ?
C8 C7 1.491(6) . ?
C9 C8 1.488(7) 4_575 ?
C9 H9C 0.9700 . ?
C9 H9D 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 Eu1 O1 78.53(17) 4_575 . ?
O1 Eu1 O3 70.66(12) . . ?
O1 Eu1 O3 70.66(12) 4_575 4_575 ?
O1 Eu1 O3 115.76(11) . 4_575 ?
O1 Eu1 O3 115.76(11) 4_575 . ?
O1 Eu1 O4 144.51(12) 4_575 3_665 ?
O1 Eu1 O4 85.61(12) 4_575 2_655 ?
O1 Eu1 O4 144.51(12) . 2_655 ?
O1 Eu1 O4 85.61(12) . 3_665 ?
O1 Eu1 O7 136.92(10) . . ?
O1 Eu1 O7 136.92(10) 4_575 . ?
O1 Eu1 O8 73.78(12) . . ?
O1 Eu1 O8 73.78(12) 4_575 . ?
O3 Eu1 O3 74.45(15) 4_575 . ?
O3 Eu1 O4 87.74(11) . 3_665 ?
O3 Eu1 O4 87.74(11) 4_575 2_655 ?
O3 Eu1 O4 144.30(11) 4_575 3_665 ?
O3 Eu1 O4 144.30(11) . 2_655 ?
O3 Eu1 O7 70.96(11) 4_575 . ?
O3 Eu1 O7 70.96(11) . . ?
O3 Eu1 O8 139.83(8) . . ?
O3 Eu1 O8 139.83(8) 4_575 . ?
O4 Eu1 O4 89.46(16) 3_665 2_655 ?
O4 Eu1 O7 74.06(11) 3_665 . ?
O4 Eu1 O7 74.06(11) 2_655 . ?
O4 Eu1 O8 71.35(11) 3_665 . ?
O4 Eu1 O8 71.35(11) 2_655 . ?
O8 Eu1 O7 130.52(15) . . ?
O2 Eu2 Eu2 73.56(9) . 3_766 ?
O2 Eu2 Eu2 142.34(10) 4_565 3_766 ?
O2 Eu2 O2 74.30(18) 4_565 . ?
O2 Eu2 O5 76.93(12) . . ?
O2 Eu2 O5 74.91(13) 4_565 2_746 ?
O2 Eu2 O5 116.81(14) 4_565 3_766 ?
O2 Eu2 O5 149.80(11) 4_565 . ?
O2 Eu2 O5 76.93(12) 4_565 4_565 ?
O2 Eu2 O5 116.81(14) . 2_746 ?
O2 Eu2 O5 149.80(11) . 4_565 ?
O2 Eu2 O5 74.92(13) . 3_766 ?
O2 Eu2 O6 115.36(13) 4_565 . ?
O2 Eu2 O6 76.18(14) . . ?
O2 Eu2 O6 115.36(13) . 4_565 ?
O2 Eu2 O6 76.18(14) 4_565 4_565 ?
O2 Eu2 O9 142.69(9) 4_565 . ?
O2 Eu2 O9 142.69(9) . . ?
O2 Eu2 C7 77.20(13) . . ?
O2 Eu2 C7 135.79(13) . 4_565 ?
O2 Eu2 C7 135.79(13) 4_565 . ?
O2 Eu2 C7 77.20(13) 4_565 4_565 ?
O5 Eu2 Eu2 34.62(8) 3_766 3_766 ?
O5 Eu2 Eu2 136.62(7) 4_565 3_766 ?
O5 Eu2 Eu2 28.37(7) . 3_766 ?
O5 Eu2 Eu2 103.01(9) 2_746 3_766 ?
O5 Eu2 O5 62.99(12) 3_766 . ?
O5 Eu2 O5 62.99(12) 2_746 4_565 ?
O5 Eu2 O5 72.16(17) 2_746 3_766 ?
O5 Eu2 O5 129.06(14) . 4_565 ?
O5 Eu2 O5 127.54(6) 2_746 . ?
O5 Eu2 O5 127.54(6) 3_766 4_565 ?
O5 Eu2 O6 166.06(11) 2_746 . ?
O5 Eu2 O6 108.66(11) 3_766 . ?
O5 Eu2 O6 108.66(11) 2_746 4_565 ?
O5 Eu2 O6 166.06(11) 3_766 4_565 ?
O5 Eu2 O9 80.13(13) 3_766 . ?
O5 Eu2 O9 80.13(13) 2_746 . ?
O5 Eu2 C7 149.11(12) 2_746 . ?
O5 Eu2 C7 24.26(10) . . ?
O5 Eu2 C7 24.26(10) 4_565 4_565 ?
O5 Eu2 C7 119.40(11) 4_565 . ?
O5 Eu2 C7 86.74(12) 2_746 4_565 ?
O5 Eu2 C7 119.40(11) . 4_565 ?
O5 Eu2 C7 149.11(12) 3_766 4_565 ?
O5 Eu2 C7 86.74(12) 3_766 . ?
O6 Eu2 Eu2 136.28(8) 4_565 3_766 ?
O6 Eu2 Eu2 74.92(8) . 3_766 ?
O6 Eu2 O5 47.48(10) 4_565 4_565 ?
O6 Eu2 O5 108.75(10) . 4_565 ?
O6 Eu2 O5 108.76(10) 4_565 . ?
O6 Eu2 O5 47.49(10) . . ?
O6 Eu2 O6 67.05(15) . 4_565 ?
O6 Eu2 C7 23.37(11) . . ?
O6 Eu2 C7 86.57(12) . 4_565 ?
O6 Eu2 C7 23.37(11) 4_565 4_565 ?
O6 Eu2 C7 86.57(12) 4_565 . ?
O9 Eu2 Eu2 70.15(4) . 3_766 ?
O9 Eu2 O5 67.09(7) . 4_565 ?
O9 Eu2 O5 67.09(7) . . ?
O9 Eu2 O6 86.27(13) . 4_565 ?
O9 Eu2 O6 86.27(13) . . ?
O9 Eu2 C7 74.07(11) . . ?
O9 Eu2 C7 74.07(11) . 4_565 ?
C7 Eu2 Eu2 52.29(9) . 3_766 ?
C7 Eu2 Eu2 140.42(8) 4_565 3_766 ?
C7 Eu2 C7 101.94(16) . 4_565 ?
C1 O1 Eu1 165.2(3) . . ?
C1 O2 Eu2 151.3(3) . . ?
C4 O3 Eu1 138.5(3) . . ?
C4 O4 Eu1 138.4(3) . 3_665 ?
Eu2 O5 Eu2 117.01(12) 3_766 . ?
C7 O5 Eu2 86.1(3) . . ?
C7 O5 Eu2 153.9(3) . 3_766 ?
C7 O6 Eu2 105.0(3) . . ?
Eu1 O7 H7A 116.6 . . ?
Eu1 O7 H7B 116.7 . . ?
H7A O7 H7B 103.2 . . ?
Eu1 O8 H8A 125.8 . . ?
Eu1 O8 H8B 126.3 . . ?
H8A O8 H8B 107.8 . . ?
Eu2 O9 H9A 114.2 . . ?
Eu2 O9 H9B 114.0 . . ?
H9A O9 H9B 101.0 . . ?
C5 C5 H5 114.4 4_575 . ?
C6 C5 C5 58.7(2) . 4_575 ?
C6 C5 H5 114.4 . . ?
C4 C5 C5 121.2(2) . 4_575 ?
C4 C5 H5 114.4 . . ?
C4 C5 C6 122.5(4) . . ?
C5 C6 C5 62.6(4) . 4_575 ?
C5 C6 H6A 117.5 4_575 . ?
C5 C6 H6A 117.5 . . ?
C5 C6 H6B 117.5 . . ?
C5 C6 H6B 117.5 4_575 . ?
H6A C6 H6B 114.6 . . ?
O3 C4 C5 120.1(4) . . ?
O4 C4 O3 124.4(4) . . ?
O4 C4 C5 115.5(4) . . ?
C2 C2 H2 113.5 4_565 . ?
C3 C2 C2 59.0(3) . 4_565 ?
C3 C2 H2 113.5 . . ?
C1 C2 C2 123.5(3) . 4_565 ?
C1 C2 H2 113.5 . . ?
C1 C2 C3 123.2(5) . . ?
C2 C3 C2 62.0(5) 4_565 . ?
C2 C3 H3A 117.6 4_565 . ?
C2 C3 H3A 117.6 . . ?
C2 C3 H3B 117.6 4_565 . ?
C2 C3 H3B 117.6 . . ?
H3A C3 H3B 114.7 . . ?
O1 C1 O2 121.2(4) . . ?
O1 C1 C2 117.8(4) . . ?
O2 C1 C2 120.9(4) . . ?
C8 C8 H8 113.5 4_575 . ?
C9 C8 C8 59.2(2) . 4_575 ?
C9 C8 H8 113.5 . . ?
C9 C8 C7 121.2(5) . . ?
C7 C8 C8 125.2(2) . 4_575 ?
C7 C8 H8 113.5 . . ?
C8 C9 C8 61.6(4) . 4_575 ?
C8 C9 H9C 117.6 . . ?
C8 C9 H9C 117.6 4_575 . ?
C8 C9 H9D 117.6 . . ?
C8 C9 H9D 117.6 4_575 . ?
H9C C9 H9D 114.7 . . ?
O5 C7 Eu2 69.7(3) . . ?
O5 C7 C8 122.2(4) . . ?
O6 C7 Eu2 51.7(2) . . ?
O6 C7 O5 120.8(4) . . ?
O6 C7 C8 116.9(4) . . ?
C8 C7 Eu2 164.3(3) . . ?

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
Eu1 O1 C1 O2 177.9(10) . . . . ?
Eu1 O1 C1 C2 -5.0(16) . . . . ?
Eu1 O3 C4 O4 -98.1(5) . . . . ?
Eu1 O3 C4 C5 84.3(5) . . . . ?
Eu1 O4 C4 O3 -5.1(7) 3_665 . . . ?
Eu1 O4 C4 C5 172.6(3) 3_665 . . . ?
Eu2 O2 C1 O1 -137.7(6) . . . . ?
Eu2 O2 C1 C2 45.3(10) . . . . ?
Eu2 O5 C7 Eu2 153.6(7) 3_766 . . . ?
Eu2 O5 C7 O6 -8.0(4) . . . . ?
Eu2 O5 C7 O6 145.7(5) 3_766 . . . ?
Eu2 O5 C7 C8 168.5(4) . . . . ?
Eu2 O5 C7 C8 -37.9(9) 3_766 . . . ?
Eu2 O6 C7 O5 9.5(5) . . . . ?
Eu2 O6 C7 C8 -167.1(3) . . . . ?
C5 C5 C4 O3 -62.5(4) 4_575 . . . ?
C5 C5 C4 O4 119.7(3) 4_575 . . . ?
C6 C5 C4 O3 7.9(6) . . . . ?
C6 C5 C4 O4 -169.9(4) . . . . ?
C4 C5 C6 C5 -109.3(4) . . . 4_575 ?
C2 C2 C1 O1 130.0(3) 4_565 . . . ?
C2 C2 C1 O2 -52.9(6) 4_565 . . . ?
C3 C2 C1 O1 -157.8(5) . . . . ?
C3 C2 C1 O2 19.3(8) . . . . ?
C1 C2 C3 C2 -112.1(4) . . . 4_565 ?
C8 C8 C7 Eu2 -177.9(10) 4_575 . . . ?
C8 C8 C7 O5 45.8(5) 4_575 . . . ?
C8 C8 C7 O6 -137.7(3) 4_575 . . . ?
C9 C8 C7 Eu2 109.9(11) . . . . ?
C9 C8 C7 O5 -26.5(6) . . . . ?
C9 C8 C7 O6 150.1(4) . . . . ?
C7 C8 C9 C8 115.1(4) . . . 4_575 ?

_olex2_date_sample_data_collection 2015-06-15
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cpdc-bc-Eu
_database_code_depnum_ccdc_archive 'CCDC 1963202'
loop_
_audit_author_name
_audit_author_address
'Qi-Bing Bo'
;university of Jinan
China
;
_audit_update_record             
;
2019-11-02 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_audit_creation_date             2019-11-02
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H11 Eu O7'
_chemical_formula_sum            'C12 H11 Eu O7'
_chemical_formula_weight         419.17
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O Eu Ba'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 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                   13.802(3)
_cell_length_b                   7.5145(3)
_cell_length_c                   23.844(6)
_cell_angle_alpha                90
_cell_angle_beta                 148.00(6)
_cell_angle_gamma                90
_cell_volume                     1310.7(12)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4053
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9250
_cell_measurement_theta_min      4.2090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.124
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9623
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.154
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     35.00  88.00   1.00    5.78    --   15.86 178.00 -30.00   53
  2  ω     -1.00  83.00   1.00    5.78    --   15.86  57.00  90.00   84
  3  ω     -3.00  85.00   1.00    5.78    --   15.86  37.00 -30.00   88
  4  ω     -1.00  83.00   1.00    5.78    --   15.86  57.00  30.00   84
  5  ω    -51.00  19.00   1.00    5.78    --   15.86 -57.00   0.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0585106000
_diffrn_orient_matrix_UB_12      0.0054795000
_diffrn_orient_matrix_UB_13      0.0523618000
_diffrn_orient_matrix_UB_21      -0.0659178000
_diffrn_orient_matrix_UB_22      -0.0459589000
_diffrn_orient_matrix_UB_23      -0.0160263000
_diffrn_orient_matrix_UB_31      0.0405648000
_diffrn_orient_matrix_UB_32      -0.0823155000
_diffrn_orient_matrix_UB_33      0.0123276000
_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                2327
_reflns_number_total             2678
_reflns_odcompleteness_completeness 99.69
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2678
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0213
_refine_ls_restrained_S_all      1.062
_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)+(0.0169P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0443
_refine_ls_wR_factor_ref         0.0470
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. 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
2.a Rotating group:
 O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 C4(H4), C3(H3)
2.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C9(H9), C10(H10), C11(H11)
;
_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
Eu1 Eu 0.39557(2) 0.55881(2) 0.20379(2) 0.01602(6) Uani 1 1 d . . . . .
O3 O 0.5997(3) 0.3513(3) 0.34842(17) 0.0205(5) Uani 1 1 d . . . . .
O1 O 0.6657(3) 0.7240(3) 0.35902(17) 0.0211(5) Uani 1 1 d . . . . .
O2 O 0.8066(3) 0.9410(3) 0.47134(19) 0.0280(6) Uani 1 1 d . . . . .
O7 O 0.1582(3) 0.4156(3) 0.1409(2) 0.0276(6) Uani 1 1 d . . . . .
H7A H 0.2012 0.3838 0.1940 0.041 Uiso 1 1 d GR . . . .
H7B H 0.1197 0.3232 0.1046 0.041 Uiso 1 1 d GR . . . .
O5 O 0.5941(4) 0.4979(3) 0.2277(2) 0.0303(6) Uani 1 1 d . . . . .
O4 O 0.8687(3) 0.2668(3) 0.45035(17) 0.0242(6) Uani 1 1 d . . . . .
O6 O 0.6615(3) 0.2165(3) 0.23933(19) 0.0273(6) Uani 1 1 d . . . . .
C1 C 0.7738(4) 0.7772(4) 0.4498(3) 0.0200(7) Uani 1 1 d . . . . .
C2 C 0.7741(5) 0.3556(4) 0.4371(3) 0.0196(7) Uani 1 1 d . . . . .
C4 C 0.8675(5) 0.4533(4) 0.5294(3) 0.0258(8) Uani 1 1 d . . . . .
H4 H 0.9802 0.3967 0.5980 0.031 Uiso 1 1 calc R . . . .
C3 C 0.8655(5) 0.6552(4) 0.5342(3) 0.0248(8) Uani 1 1 d . . . . .
H3 H 0.9771 0.7043 0.6057 0.030 Uiso 1 1 calc R . . . .
C6 C 0.6463(5) 0.3798(5) 0.2197(3) 0.0215(8) Uani 1 1 d . . . . .
C5 C 0.7569(6) 0.5390(4) 0.5202(3) 0.0352(10) Uani 1 1 d . . . . .
H5A H 0.8001 0.5277 0.5797 0.042 Uiso 1 1 calc R . . . .
H5B H 0.6250 0.5384 0.4514 0.042 Uiso 1 1 calc R . . . .
C7 C 0.6948(5) 0.4354(5) 0.1855(3) 0.0255(8) Uani 1 1 d . . . . .
C8 C 0.7571(6) 0.3163(6) 0.1770(3) 0.0421(11) Uani 1 1 d . . . . .
H8 H 0.7716 0.1976 0.1941 0.050 Uiso 1 1 calc R . . . .
C12 C 0.6764(7) 0.6123(6) 0.1611(4) 0.0485(12) Uani 1 1 d . . . . .
H12 H 0.6366 0.6958 0.1677 0.058 Uiso 1 1 calc R . . . .
C9 C 0.7988(8) 0.3692(7) 0.1434(4) 0.0626(14) Uani 1 1 d . . . . .
H9 H 0.8416 0.2870 0.1383 0.075 Uiso 1 1 calc R . . . .
C10 C 0.7764(9) 0.5440(8) 0.1177(5) 0.0747(18) Uani 1 1 d . . . . .
H10 H 0.8019 0.5804 0.0937 0.090 Uiso 1 1 calc R . . . .
C11 C 0.7171(8) 0.6644(7) 0.1270(5) 0.0748(17) Uani 1 1 d . . . . .
H11 H 0.7037 0.7831 0.1102 0.090 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
Eu1 Eu1 4.0631(9) 2_655 ?
Eu1 O3 2.405(3) . ?
Eu1 O3 2.554(2) 2_655 ?
Eu1 O1 2.395(4) . ?
Eu1 O1 2.672(2) 2_645 ?
Eu1 O2 2.499(4) 2_645 ?
Eu1 O7 2.411(3) . ?
Eu1 H7A 2.8140 . ?
Eu1 O5 2.323(3) . ?
Eu1 O4 2.553(4) 2_655 ?
Eu1 O6 2.383(2) 2_655 ?
Eu1 C1 2.973(4) 2_645 ?
Eu1 C2 2.899(4) 2_655 ?
O3 Eu1 2.554(2) 2_645 ?
O3 C2 1.278(4) . ?
O1 Eu1 2.672(2) 2_655 ?
O1 C1 1.263(4) . ?
O2 Eu1 2.499(4) 2_655 ?
O2 C1 1.261(4) . ?
O7 H7A 0.8577 . ?
O7 H7B 0.8567 . ?
O5 C6 1.255(4) . ?
O4 Eu1 2.553(4) 2_645 ?
O4 C2 1.246(4) . ?
O6 Eu1 2.383(2) 2_645 ?
O6 C6 1.266(4) . ?
C1 Eu1 2.973(4) 2_655 ?
C1 C3 1.474(5) . ?
C2 Eu1 2.899(4) 2_645 ?
C2 C4 1.493(5) . ?
C4 H4 0.9800 . ?
C4 C3 1.523(5) . ?
C4 C5 1.492(5) . ?
C3 H3 0.9800 . ?
C3 C5 1.508(5) . ?
C6 C7 1.488(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C7 C8 1.370(5) . ?
C7 C12 1.386(5) . ?
C8 H8 0.9300 . ?
C8 C9 1.384(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.381(6) . ?
C9 H9 0.9300 . ?
C9 C10 1.369(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.360(7) . ?
C11 H11 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
Eu1 Eu1 H7A 131.7 2_655 . ?
O3 Eu1 Eu1 33.79(6) 2_655 2_655 ?
O3 Eu1 Eu1 113.10(10) . 2_655 ?
O3 Eu1 O3 140.70(5) . 2_655 ?
O3 Eu1 O1 67.81(9) . 2_645 ?
O3 Eu1 O1 131.59(7) 2_655 2_645 ?
O3 Eu1 O2 117.18(10) . 2_645 ?
O3 Eu1 O7 85.63(12) . . ?
O3 Eu1 H7A 72.0 . . ?
O3 Eu1 H7A 141.1 2_655 . ?
O3 Eu1 O4 165.34(8) . 2_655 ?
O3 Eu1 C1 109.30(9) 2_655 2_645 ?
O3 Eu1 C1 92.65(11) . 2_645 ?
O3 Eu1 C2 26.14(9) 2_655 2_655 ?
O3 Eu1 C2 166.79(8) . 2_655 ?
O1 Eu1 Eu1 156.41(5) 2_645 2_655 ?
O1 Eu1 Eu1 39.09(5) . 2_655 ?
O1 Eu1 O3 69.96(9) . 2_655 ?
O1 Eu1 O3 74.02(12) . . ?
O1 Eu1 O1 133.81(6) . 2_645 ?
O1 Eu1 O2 146.60(9) . 2_645 ?
O1 Eu1 O7 134.92(9) . . ?
O1 Eu1 H7A 71.8 2_645 . ?
O1 Eu1 H7A 119.7 . . ?
O1 Eu1 O4 111.02(12) . 2_655 ?
O1 Eu1 C1 147.15(9) . 2_645 ?
O1 Eu1 C1 25.13(8) 2_645 2_645 ?
O1 Eu1 C2 93.50(12) . 2_655 ?
O1 Eu1 C2 120.94(9) 2_645 2_655 ?
O2 Eu1 Eu1 120.47(6) 2_645 2_655 ?
O2 Eu1 O3 86.80(7) 2_645 2_655 ?
O2 Eu1 O1 49.89(7) 2_645 2_645 ?
O2 Eu1 H7A 93.5 2_645 . ?
O2 Eu1 O4 66.64(11) 2_645 2_655 ?
O2 Eu1 C1 24.76(8) 2_645 2_645 ?
O2 Eu1 C2 71.09(10) 2_645 2_655 ?
O7 Eu1 Eu1 135.66(6) . 2_655 ?
O7 Eu1 O3 131.63(9) . 2_655 ?
O7 Eu1 O1 67.29(8) . 2_645 ?
O7 Eu1 O2 78.47(12) . 2_645 ?
O7 Eu1 H7A 16.7 . . ?
O7 Eu1 O4 81.32(11) . 2_655 ?
O7 Eu1 C1 71.47(10) . 2_645 ?
O7 Eu1 C2 106.67(12) . 2_655 ?
O5 Eu1 Eu1 84.39(7) . 2_655 ?
O5 Eu1 O3 77.08(8) . 2_655 ?
O5 Eu1 O3 79.44(10) . . ?
O5 Eu1 O1 75.89(10) . . ?
O5 Eu1 O1 72.48(8) . 2_645 ?
O5 Eu1 O2 75.73(13) . 2_645 ?
O5 Eu1 O7 139.76(8) . . ?
O5 Eu1 H7A 140.5 . . ?
O5 Eu1 O4 114.95(9) . 2_655 ?
O5 Eu1 O6 148.11(10) . 2_655 ?
O5 Eu1 C1 72.15(11) . 2_645 ?
O5 Eu1 C2 93.51(11) . 2_655 ?
O4 Eu1 Eu1 72.85(10) 2_655 2_655 ?
O4 Eu1 O3 50.76(8) 2_655 2_655 ?
O4 Eu1 O1 112.50(10) 2_655 2_645 ?
O4 Eu1 H7A 93.9 2_655 . ?
O4 Eu1 C1 89.50(12) 2_655 2_645 ?
O4 Eu1 C2 25.42(8) 2_655 2_655 ?
O6 Eu1 Eu1 69.90(6) 2_655 2_655 ?
O6 Eu1 O3 90.40(7) 2_655 2_655 ?
O6 Eu1 O3 93.26(8) 2_655 . ?
O6 Eu1 O1 133.40(7) 2_655 2_645 ?
O6 Eu1 O1 72.27(8) 2_655 . ?
O6 Eu1 O2 133.45(10) 2_655 2_645 ?
O6 Eu1 O7 69.19(9) 2_655 . ?
O6 Eu1 H7A 61.8 2_655 . ?
O6 Eu1 O4 75.92(9) 2_655 2_655 ?
O6 Eu1 C1 139.59(9) 2_655 2_645 ?
O6 Eu1 C2 86.85(9) 2_655 2_655 ?
C1 Eu1 Eu1 141.40(7) 2_645 2_655 ?
C1 Eu1 H7A 82.3 2_645 . ?
C2 Eu1 Eu1 54.64(10) 2_655 2_655 ?
C2 Eu1 H7A 119.2 2_655 . ?
C2 Eu1 C1 95.82(11) 2_655 2_645 ?
Eu1 O3 Eu1 110.00(9) . 2_645 ?
C2 O3 Eu1 92.16(19) . 2_645 ?
C2 O3 Eu1 128.9(2) . . ?
Eu1 O1 Eu1 106.49(10) . 2_655 ?
C1 O1 Eu1 147.2(2) . . ?
C1 O1 Eu1 90.88(19) . 2_655 ?
C1 O2 Eu1 99.1(2) . 2_655 ?
Eu1 O7 H7A 109.4 . . ?
Eu1 O7 H7B 109.9 . . ?
H7A O7 H7B 109.0 . . ?
C6 O5 Eu1 144.2(2) . . ?
C2 O4 Eu1 93.0(2) . 2_645 ?
C6 O6 Eu1 131.4(2) . 2_645 ?
O1 C1 Eu1 63.98(18) . 2_655 ?
O1 C1 C3 122.9(3) . . ?
O2 C1 Eu1 56.10(18) . 2_655 ?
O2 C1 O1 120.1(3) . . ?
O2 C1 C3 117.1(3) . . ?
C3 C1 Eu1 173.0(2) . 2_655 ?
O3 C2 Eu1 61.70(17) . 2_645 ?
O3 C2 C4 120.8(3) . . ?
O4 C2 Eu1 61.58(18) . 2_645 ?
O4 C2 O3 120.3(3) . . ?
O4 C2 C4 118.7(3) . . ?
C4 C2 Eu1 157.7(2) . 2_645 ?
C2 C4 H4 114.3 . . ?
C2 C4 C3 123.5(3) . . ?
C3 C4 H4 114.3 . . ?
C5 C4 C2 119.9(3) . . ?
C5 C4 H4 114.3 . . ?
C5 C4 C3 60.0(2) . . ?
C1 C3 C4 124.4(3) . . ?
C1 C3 H3 113.8 . . ?
C1 C3 C5 121.1(3) . . ?
C4 C3 H3 113.8 . . ?
C5 C3 C4 59.0(2) . . ?
C5 C3 H3 113.8 . . ?
O5 C6 O6 124.5(3) . . ?
O5 C6 C7 117.9(3) . . ?
O6 C6 C7 117.6(3) . . ?
C4 C5 C3 61.0(2) . . ?
C4 C5 H5A 117.7 . . ?
C4 C5 H5B 117.7 . . ?
C3 C5 H5A 117.7 . . ?
C3 C5 H5B 117.7 . . ?
H5A C5 H5B 114.8 . . ?
C8 C7 C6 121.9(3) . . ?
C8 C7 C12 118.7(4) . . ?
C12 C7 C6 119.4(3) . . ?
C7 C8 H8 119.3 . . ?
C7 C8 C9 121.3(4) . . ?
C9 C8 H8 119.3 . . ?
C7 C12 H12 120.1 . . ?
C11 C12 C7 119.9(4) . . ?
C11 C12 H12 120.1 . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.3(5) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 H10 119.9 . . ?
C12 C11 H11 119.7 . . ?
C10 C11 C12 120.7(5) . . ?
C10 C11 H11 119.7 . . ?

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
Eu1 O3 C2 Eu1 -118.1(2) . . . 2_645 ?
Eu1 O3 C2 O4 -98.2(3) . . . . ?
Eu1 O3 C2 O4 19.9(3) 2_645 . . . ?
Eu1 O3 C2 C4 -154.5(3) 2_645 . . . ?
Eu1 O3 C2 C4 87.4(3) . . . . ?
Eu1 O1 C1 Eu1 -123.3(4) . . . 2_655 ?
Eu1 O1 C1 O2 -1.2(3) 2_655 . . . ?
Eu1 O1 C1 O2 -124.5(4) . . . . ?
Eu1 O1 C1 C3 178.5(3) 2_655 . . . ?
Eu1 O1 C1 C3 55.2(6) . . . . ?
Eu1 O2 C1 O1 1.3(3) 2_655 . . . ?
Eu1 O2 C1 C3 -178.4(3) 2_655 . . . ?
Eu1 O5 C6 O6 -36.7(6) . . . . ?
Eu1 O5 C6 C7 143.7(3) . . . . ?
Eu1 O4 C2 O3 -19.9(3) 2_645 . . . ?
Eu1 O4 C2 C4 154.6(3) 2_645 . . . ?
Eu1 O6 C6 O5 0.2(5) 2_645 . . . ?
Eu1 O6 C6 C7 179.7(2) 2_645 . . . ?
Eu1 C2 C4 C3 -158.5(5) 2_645 . . . ?
Eu1 C2 C4 C5 -86.7(7) 2_645 . . . ?
O3 C2 C4 C3 -68.6(5) . . . . ?
O3 C2 C4 C5 3.3(5) . . . . ?
O1 C1 C3 C4 10.7(5) . . . . ?
O1 C1 C3 C5 -60.9(5) . . . . ?
O2 C1 C3 C4 -169.6(3) . . . . ?
O2 C1 C3 C5 118.8(4) . . . . ?
O5 C6 C7 C8 178.4(4) . . . . ?
O5 C6 C7 C12 -1.8(5) . . . . ?
O4 C2 C4 C3 117.0(4) . . . . ?
O4 C2 C4 C5 -171.2(3) . . . . ?
O6 C6 C7 C8 -1.1(5) . . . . ?
O6 C6 C7 C12 178.7(4) . . . . ?
C1 C3 C5 C4 114.1(3) . . . . ?
C2 C4 C3 C1 -0.7(6) . . . . ?
C2 C4 C3 C5 107.9(4) . . . . ?
C2 C4 C5 C3 -113.8(3) . . . . ?
C6 C7 C8 C9 178.9(4) . . . . ?
C6 C7 C12 C11 -178.5(4) . . . . ?
C5 C4 C3 C1 -108.6(4) . . . . ?
C7 C8 C9 C10 -0.3(8) . . . . ?
C7 C12 C11 C10 -0.4(8) . . . . ?
C8 C7 C12 C11 1.3(7) . . . . ?
C8 C9 C10 C11 1.2(9) . . . . ?
C12 C7 C8 C9 -0.9(7) . . . . ?
C9 C10 C11 C12 -0.8(9) . . . . ?

_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 1.370
_oxdiff_exptl_absorpt_empirical_full_min 0.893
####################################################################### 
# 
# 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_cpdc-Tb
_database_code_depnum_ccdc_archive 'CCDC 1963200'
loop_
_audit_author_name
_audit_author_address
'Qi-Bing Bo'
;university of Jinan
China
;
_audit_update_record             
;
2019-11-02 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_audit_creation_date             2019-11-02
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C30 H36 O30 Tb4)'
_chemical_formula_sum            'C15 H18 O15 Tb2'
_chemical_formula_weight         756.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H N O Tb'
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      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   9.7575(9)
_cell_length_b                   7.9696(7)
_cell_length_c                   12.8428(15)
_cell_angle_alpha                90
_cell_angle_beta                 106.131(11)
_cell_angle_gamma                90
_cell_volume                     959.37(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1947
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.4310
_cell_measurement_theta_min      4.1780
_shelx_estimated_absorpt_T_max   0.777
_shelx_estimated_absorpt_T_min   0.147
_exptl_absorpt_coefficient_mu    7.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.036
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6009
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.342
_diffrn_reflns_theta_min         3.299
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   35.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000 -150.0000 53

#__ type_ start__ end____ width___ exp.time_
  2 omega   32.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569 -178.0000    0.0000 56

#__ type_ start__ end____ width___ exp.time_
  3 omega  -25.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -99.0000  -30.0000 80

#__ type_ start__ end____ width___ exp.time_
  4 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569   57.0000   60.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega   35.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000  -90.0000 53
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0699517000
_diffrn_orient_matrix_UB_12      -0.0284866000
_diffrn_orient_matrix_UB_13      -0.0260865000
_diffrn_orient_matrix_UB_21      -0.0284136000
_diffrn_orient_matrix_UB_22      0.0759157000
_diffrn_orient_matrix_UB_23      0.0139123000
_diffrn_orient_matrix_UB_31      0.0044624000
_diffrn_orient_matrix_UB_32      0.0365710000
_diffrn_orient_matrix_UB_33      -0.0493804000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1783
_reflns_number_total             2081
_reflns_odcompleteness_completeness 99.62
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         3.150
_refine_diff_density_min         -2.629
_refine_diff_density_rms         0.339
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         2081
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0613
_refine_ls_restrained_S_all      1.087
_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)+(0.0560P)²+25.4418P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1534
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(O2) = Uanis(O1) = Uanis(C1) = Uanis(C2) = Uanis(C3)
Uanis(O6) = Uanis(C7) = Uanis(C8) = Uanis(C9)
Uanis(O8) = Uanis(O7) = Uanis(O9)
3. Others
 Fixed Sof: H8A(0.5) H8B(0.5) H7A(0.5) H7B(0.5) H9A(0.5) H9B(0.5)
4.a Riding coordinates:
 O8(H8A,H8B), O7(H7A,H7B), O9(H9A,H9B)
4.b Ternary CH refined with riding coordinates:
 C8(H8), C2(H2), C5(H5)
4.c Secondary CH2 refined with riding coordinates:
 C9(H9C,H9D), C3(H3A,H3B), 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 0.49055(7) 0.7500 0.13311(6) 0.0145(2) Uani 1 2 d S T P . .
Tb2 Tb 0.89686(8) 0.2500 0.50595(6) 0.0185(2) Uani 1 2 d S T P . .
O3 O 0.6573(8) 0.5711(11) 0.0878(7) 0.0225(18) Uani 1 1 d . . . . .
O2 O 0.7192(9) 0.4229(13) 0.4127(8) 0.0352(13) Uani 1 1 d . . . . .
O6 O 0.8409(10) 0.0783(12) 0.6456(7) 0.0303(14) Uani 1 1 d . . . . .
O1 O 0.5839(9) 0.5655(13) 0.2755(8) 0.0352(13) Uani 1 1 d . . . . .
O8 O 0.3224(13) 0.7500 0.2402(10) 0.0255(15) Uani 1 2 d S T P . .
H8A H 0.3166 0.6769 0.2881 0.038 Uiso 0.5 1 d R . . . .
H8B H 0.2541 0.8204 0.2351 0.038 Uiso 0.5 1 d R . . . .
O7 O 0.4516(13) 0.7500 -0.0651(10) 0.0255(15) Uani 1 2 d S T P . .
H7A H 0.3912 0.8225 -0.1005 0.038 Uiso 0.5 1 d R . . . .
H7B H 0.4201 0.6572 -0.0971 0.038 Uiso 0.5 1 d R . . . .
O9 O 1.1352(13) 0.2500 0.6189(10) 0.0255(15) Uani 1 2 d S T P . .
H9A H 1.2007 0.1779 0.6189 0.038 Uiso 0.5 1 d R . . . .
H9B H 1.1875 0.3118 0.6694 0.038 Uiso 0.5 1 d R . . . .
O4 O 0.6814(9) 0.4572(12) -0.0648(7) 0.029(2) Uani 1 1 d . . . . .
O5 O 0.9931(10) -0.0752(13) 0.5944(8) 0.037(2) Uani 1 1 d . . . . .
C1 C 0.5996(14) 0.4500(19) 0.3433(12) 0.0352(13) Uani 1 1 d . . . . .
C4 C 0.7203(11) 0.5582(14) 0.0149(9) 0.019(2) Uani 1 1 d . . . . .
C9 C 1.060(2) -0.2500 0.8086(15) 0.0303(14) Uani 1 2 d S T P . .
H9C H 1.0934 -0.2500 0.8871 0.036 Uiso 1 2 calc RS T P . .
H9D H 1.1345 -0.2500 0.7722 0.036 Uiso 1 2 calc RS T P . .
C8 C 0.9267(15) -0.1540(16) 0.7570(10) 0.0303(14) Uani 1 1 d . . . . .
H8 H 0.8814 -0.1037 0.8087 0.036 Uiso 1 1 calc R . . . .
C2 C 0.4745(14) 0.3457(18) 0.3453(12) 0.0352(13) Uani 1 1 d . . . . .
H2 H 0.3834 0.3945 0.3041 0.042 Uiso 1 1 calc R . . . .
C3 C 0.465(2) 0.2500 0.4417(17) 0.0352(13) Uani 1 2 d S T P . .
H3A H 0.5474 0.2500 0.5045 0.042 Uiso 1 2 calc RS T P . .
H3B H 0.3737 0.2500 0.4585 0.042 Uiso 1 2 calc RS T P . .
C7 C 0.9214(15) -0.0475(17) 0.6617(10) 0.0303(14) Uani 1 1 d . . . . .
C6 C 0.9256(18) 0.7500 0.1211(14) 0.025(4) Uani 1 2 d S T P . .
H6A H 1.0291 0.7500 0.1437 0.030 Uiso 1 2 calc RS T P . .
H6B H 0.8817 0.7500 0.1802 0.030 Uiso 1 2 calc RS T P . .
C5 C 0.8533(11) 0.6523(14) 0.0219(9) 0.018(2) Uani 1 1 d . . . . .
H5 H 0.9174 0.6002 -0.0154 0.021 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 O3 2.354(8) 4_575 ?
Tb1 O3 2.354(8) . ?
Tb1 O1 2.326(9) . ?
Tb1 O1 2.326(9) 4_575 ?
Tb1 O8 2.416(12) . ?
Tb1 O7 2.467(12) . ?
Tb1 O4 2.344(9) 2_655 ?
Tb1 O4 2.344(9) 3_665 ?
Tb2 O2 2.277(9) 4_565 ?
Tb2 O2 2.277(9) . ?
Tb2 O6 2.435(9) . ?
Tb2 O6 2.435(9) 4_565 ?
Tb2 O9 2.374(12) . ?
Tb2 O5 2.350(9) 3_756 ?
Tb2 O5 2.880(11) 4_565 ?
Tb2 O5 2.880(11) . ?
Tb2 O5 2.350(9) 2_756 ?
O3 C4 1.259(14) . ?
O2 C1 1.275(16) . ?
O6 C7 1.255(16) . ?
O1 C1 1.247(17) . ?
O8 H8A 0.8600 . ?
O8 H8B 0.8600 . ?
O7 H7A 0.8600 . ?
O7 H7B 0.8601 . ?
O9 H9A 0.8599 . ?
O9 H9B 0.8600 . ?
O4 Tb1 2.344(9) 3_665 ?
O4 C4 1.274(14) . ?
O5 Tb2 2.350(9) 3_756 ?
O5 C7 1.273(15) . ?
C1 C2 1.483(19) . ?
C4 C5 1.480(15) . ?
C9 H9C 0.9700 . ?
C9 H9D 0.9700 . ?
C9 C8 1.49(2) . ?
C9 C8 1.49(2) 4 ?
C8 C8 1.53(3) 4 ?
C8 H8 0.9800 . ?
C8 C7 1.478(17) . ?
C2 C2 1.53(3) 4_565 ?
C2 H2 0.9800 . ?
C2 C3 1.48(2) . ?
C3 C2 1.48(2) 4_565 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 C5 1.493(17) . ?
C6 C5 1.493(17) 4_575 ?
C5 C5 1.56(2) 4_575 ?
C5 H5 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Tb1 O3 74.5(4) 4_575 . ?
O3 Tb1 O8 140.0(2) 4_575 . ?
O3 Tb1 O8 140.0(2) . . ?
O3 Tb1 O7 70.4(3) . . ?
O3 Tb1 O7 70.4(3) 4_575 . ?
O1 Tb1 O3 115.5(3) 4_575 . ?
O1 Tb1 O3 70.4(3) 4_575 4_575 ?
O1 Tb1 O3 115.5(3) . 4_575 ?
O1 Tb1 O3 70.4(3) . . ?
O1 Tb1 O1 78.4(5) 4_575 . ?
O1 Tb1 O8 74.5(3) . . ?
O1 Tb1 O8 74.5(3) 4_575 . ?
O1 Tb1 O7 136.5(3) 4_575 . ?
O1 Tb1 O7 136.5(3) . . ?
O1 Tb1 O4 145.4(3) . 2_655 ?
O1 Tb1 O4 86.1(3) 4_575 2_655 ?
O1 Tb1 O4 145.4(3) 4_575 3_665 ?
O1 Tb1 O4 86.1(3) . 3_665 ?
O8 Tb1 O7 130.8(4) . . ?
O4 Tb1 O3 87.3(3) 3_665 . ?
O4 Tb1 O3 143.7(3) 2_655 . ?
O4 Tb1 O3 143.7(3) 3_665 4_575 ?
O4 Tb1 O3 87.3(3) 2_655 4_575 ?
O4 Tb1 O8 71.6(3) 3_665 . ?
O4 Tb1 O8 71.6(3) 2_655 . ?
O4 Tb1 O7 74.0(3) 2_655 . ?
O4 Tb1 O7 74.0(3) 3_665 . ?
O4 Tb1 O4 89.6(5) 3_665 2_655 ?
O2 Tb2 O2 74.5(5) 4_565 . ?
O2 Tb2 O6 115.7(3) 4_565 4_565 ?
O2 Tb2 O6 115.7(3) . . ?
O2 Tb2 O6 75.7(3) 4_565 . ?
O2 Tb2 O6 75.7(3) . 4_565 ?
O2 Tb2 O9 142.6(3) 4_565 . ?
O2 Tb2 O9 142.6(3) . . ?
O2 Tb2 O5 117.9(4) 4_565 2_756 ?
O2 Tb2 O5 117.9(4) . 3_756 ?
O2 Tb2 O5 75.5(3) 4_565 3_756 ?
O2 Tb2 O5 77.3(3) 4_565 . ?
O2 Tb2 O5 150.4(3) . . ?
O2 Tb2 O5 150.4(3) 4_565 4_565 ?
O2 Tb2 O5 75.5(3) . 2_756 ?
O2 Tb2 O5 77.3(3) . 4_565 ?
O6 Tb2 O6 68.4(4) . 4_565 ?
O6 Tb2 O5 47.1(3) 4_565 4_565 ?
O6 Tb2 O5 109.3(3) . 4_565 ?
O6 Tb2 O5 47.1(3) . . ?
O6 Tb2 O5 109.3(3) 4_565 . ?
O9 Tb2 O6 86.1(3) . 4_565 ?
O9 Tb2 O6 86.1(3) . . ?
O9 Tb2 O5 66.6(2) . 4_565 ?
O9 Tb2 O5 66.6(2) . . ?
O5 Tb2 O6 165.2(3) 2_756 . ?
O5 Tb2 O6 107.5(3) 3_756 . ?
O5 Tb2 O6 107.5(3) 2_756 4_565 ?
O5 Tb2 O6 165.2(3) 3_756 4_565 ?
O5 Tb2 O9 79.4(3) 2_756 . ?
O5 Tb2 O9 79.4(3) 3_756 . ?
O5 Tb2 O5 62.2(3) 2_756 4_565 ?
O5 Tb2 O5 126.95(19) 3_756 4_565 ?
O5 Tb2 O5 62.2(3) 3_756 . ?
O5 Tb2 O5 72.7(5) 3_756 2_756 ?
O5 Tb2 O5 128.3(4) 4_565 . ?
O5 Tb2 O5 126.95(19) 2_756 . ?
C4 O3 Tb1 138.3(8) . . ?
C1 O2 Tb2 152.3(10) . . ?
C7 O6 Tb2 108.2(8) . . ?
C1 O1 Tb1 163.9(9) . . ?
Tb1 O8 H8A 126.6 . . ?
Tb1 O8 H8B 126.3 . . ?
H8A O8 H8B 107.0 . . ?
Tb1 O7 H7A 115.6 . . ?
Tb1 O7 H7B 115.1 . . ?
H7A O7 H7B 103.0 . . ?
Tb2 O9 H9A 127.1 . . ?
Tb2 O9 H9B 137.4 . . ?
H9A O9 H9B 95.5 . . ?
C4 O4 Tb1 140.2(8) . 3_665 ?
Tb2 O5 Tb2 117.8(3) 3_756 . ?
C7 O5 Tb2 153.6(9) . 3_756 ?
C7 O5 Tb2 86.1(8) . . ?
O2 C1 C2 119.4(13) . . ?
O1 C1 O2 121.6(13) . . ?
O1 C1 C2 118.9(12) . . ?
O3 C4 O4 123.4(10) . . ?
O3 C4 C5 121.0(10) . . ?
O4 C4 C5 115.5(10) . . ?
H9C C9 H9D 114.7 . . ?
C8 C9 H9C 117.6 4 . ?
C8 C9 H9C 117.6 . . ?
C8 C9 H9D 117.6 4 . ?
C8 C9 H9D 117.6 . . ?
C8 C9 C8 61.6(13) . 4 ?
C9 C8 C8 59.2(6) . 4 ?
C9 C8 H8 114.1 . . ?
C8 C8 H8 114.1 4 . ?
C7 C8 C9 119.2(12) . . ?
C7 C8 C8 125.0(7) . 4 ?
C7 C8 H8 114.1 . . ?
C1 C2 C2 124.1(8) . 4_565 ?
C1 C2 H2 113.3 . . ?
C2 C2 H2 113.3 4_565 . ?
C3 C2 C1 123.3(13) . . ?
C3 C2 C2 59.0(7) . 4_565 ?
C3 C2 H2 113.3 . . ?
C2 C3 C2 62.1(14) 4_565 . ?
C2 C3 H3A 117.6 4_565 . ?
C2 C3 H3A 117.6 . . ?
C2 C3 H3B 117.6 4_565 . ?
C2 C3 H3B 117.6 . . ?
H3A C3 H3B 114.6 . . ?
O6 C7 O5 117.6(12) . . ?
O6 C7 C8 118.1(11) . . ?
O5 C7 C8 124.3(12) . . ?
H6A C6 H6B 114.5 . . ?
C5 C6 H6A 117.5 . . ?
C5 C6 H6A 117.5 4_575 . ?
C5 C6 H6B 117.5 . . ?
C5 C6 H6B 117.5 4_575 . ?
C5 C6 C5 62.9(11) . 4_575 ?
C4 C5 C6 121.0(11) . . ?
C4 C5 C5 120.5(6) . 4_575 ?
C4 C5 H5 115.1 . . ?
C6 C5 C5 58.6(5) . 4_575 ?
C6 C5 H5 115.1 . . ?
C5 C5 H5 115.1 4_575 . ?

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 O3 C4 O4 -100.1(14) . . . . ?
Tb1 O3 C4 C5 84.8(14) . . . . ?
Tb1 O1 C1 O2 178(3) . . . . ?
Tb1 O1 C1 C2 -4(5) . . . . ?
Tb1 O4 C4 O3 -2(2) 3_665 . . . ?
Tb1 O4 C4 C5 173.4(8) 3_665 . . . ?
Tb2 O2 C1 O1 -134.6(17) . . . . ?
Tb2 O2 C1 C2 48(3) . . . . ?
Tb2 O6 C7 O5 -11.5(15) . . . . ?
Tb2 O6 C7 C8 168.7(10) . . . . ?
Tb2 O5 C7 O6 -146.6(16) 3_756 . . . ?
Tb2 O5 C7 O6 9.2(12) . . . . ?
Tb2 O5 C7 C8 -170.9(13) . . . . ?
Tb2 O5 C7 C8 33(3) 3_756 . . . ?
O3 C4 C5 C6 7.0(16) . . . . ?
O3 C4 C5 C5 -62.4(12) . . . 4_575 ?
O2 C1 C2 C2 -52.0(17) . . . 4_565 ?
O2 C1 C2 C3 21(2) . . . . ?
O1 C1 C2 C2 130.1(11) . . . 4_565 ?
O1 C1 C2 C3 -157.4(14) . . . . ?
O4 C4 C5 C6 -168.5(10) . . . . ?
O4 C4 C5 C5 122.1(8) . . . 4_575 ?
C1 C2 C3 C2 -112.8(12) . . . 4_565 ?
C9 C8 C7 O6 -151.9(12) . . . . ?
C9 C8 C7 O5 28(2) . . . . ?
C8 C9 C8 C7 -115.6(11) 4 . . . ?
C8 C8 C7 O6 137.0(9) 4 . . . ?
C8 C8 C7 O5 -42.8(17) 4 . . . ?
C5 C6 C5 C4 -109.0(9) 4_575 . . . ?

_olex2_date_sample_data_collection 2015-06-14
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_cpdc-bc-Dy
_database_code_depnum_ccdc_archive 'CCDC 1963204'
loop_
_audit_author_name
_audit_author_address
'Qi-Bing Bo'
;university of Jinan
China
;
_audit_update_record             
;
2019-11-02 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_audit_creation_date             2019-11-02
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H11 Dy O7'
_chemical_formula_sum            'C12 H11 Dy O7'
_chemical_formula_weight         429.71
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O Dy Ba'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 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                   13.758(3)
_cell_length_b                   7.4103(2)
_cell_length_c                   23.889(5)
_cell_angle_alpha                90
_cell_angle_beta                 148.21(5)
_cell_angle_gamma                90
_cell_volume                     1283.1(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4219
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0140
_cell_measurement_theta_min      3.9120
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.852
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53073
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.224
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8184
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.368
_diffrn_reflns_theta_min         3.413
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -25.00  55.00   1.00    1.00    --   16.01 -99.00 -60.00   80
  2  ω    -25.00  22.00   1.00    1.00    --  -17.11 -99.00  30.00   47
  3  ω    -86.00  52.00   1.00    1.00    --  -17.11   0.00 -90.00  138
  4  ω    -53.00  15.00   1.00    1.00    --   16.01 -37.00  30.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0866963000
_diffrn_orient_matrix_UB_12      -0.0413223000
_diffrn_orient_matrix_UB_13      -0.0475035000
_diffrn_orient_matrix_UB_21      0.0328277000
_diffrn_orient_matrix_UB_22      -0.0326794000
_diffrn_orient_matrix_UB_23      -0.0100121000
_diffrn_orient_matrix_UB_31      0.0313734000
_diffrn_orient_matrix_UB_32      -0.0798737000
_diffrn_orient_matrix_UB_33      0.0286332000
_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                2362
_reflns_number_total             2615
_reflns_odcompleteness_completeness 99.51
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2615
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0182
_refine_ls_restrained_S_all      1.094
_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)+(0.0176P)²+0.8995P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0417
_refine_ls_wR_factor_ref         0.0433
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. 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
2.a Rotating group:
 O7(H7A,H7B)
2.b Ternary CH refined with riding coordinates:
 C3(H3), C4(H4)
2.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
2.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C9(H9), C10(H10), C11(H11)
;
_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
Dy1 Dy 0.39678(2) 0.43996(2) 0.20438(2) 0.01366(6) Uani 1 1 d . . . . .
O1 O 0.5965(3) 0.6493(3) 0.34595(16) 0.0196(5) Uani 1 1 d . . . . .
O3 O 0.6636(3) 0.2742(3) 0.35761(16) 0.0196(5) Uani 1 1 d . . . . .
O5 O 0.5968(3) 0.4989(3) 0.2305(2) 0.0275(5) Uani 1 1 d . . . . .
O7 O 0.1631(3) 0.5867(3) 0.14262(18) 0.0240(5) Uani 1 1 d . . . . .
H7A H 0.0798 0.5093 0.1134 0.036 Uiso 1 1 d GR . . . .
H7B H 0.1073 0.6682 0.0949 0.036 Uiso 1 1 d GR . . . .
O6 O 0.6613(3) 0.7834(3) 0.24060(18) 0.0242(5) Uani 1 1 d . . . . .
O4 O 0.8029(3) 0.0550(3) 0.46918(18) 0.0264(5) Uani 1 1 d . . . . .
O2 O 0.8678(3) 0.7331(3) 0.44880(17) 0.0227(5) Uani 1 1 d . . . . .
C6 C 0.6479(4) 0.6197(4) 0.2220(2) 0.0204(7) Uani 1 1 d . . . . .
C2 C 0.7707(4) 0.2200(4) 0.4483(2) 0.0184(7) Uani 1 1 d . . . . .
C1 C 0.7728(4) 0.6437(4) 0.4356(2) 0.0175(6) Uani 1 1 d . . . . .
C3 C 0.8652(5) 0.5469(4) 0.5273(3) 0.0231(7) Uani 1 1 d . . . . .
H3 H 0.9787 0.6047 0.5961 0.028 Uiso 1 1 calc R . . . .
C7 C 0.6947(5) 0.5620(4) 0.1867(3) 0.0239(7) Uani 1 1 d . . . . .
C4 C 0.8632(5) 0.3436(4) 0.5329(2) 0.0220(7) Uani 1 1 d . . . . .
H4 H 0.9755 0.2941 0.6047 0.026 Uiso 1 1 calc R . . . .
C5 C 0.7530(6) 0.4610(4) 0.5175(3) 0.0316(9) Uani 1 1 d . . . . .
H5A H 0.6200 0.4611 0.4481 0.038 Uiso 1 1 calc R . . . .
H5B H 0.7960 0.4736 0.5768 0.038 Uiso 1 1 calc R . . . .
C8 C 0.6755(6) 0.3836(5) 0.1621(4) 0.0445(10) Uani 1 1 d . . . . .
H8 H 0.6363 0.2990 0.1691 0.053 Uiso 1 1 calc R . . . .
C12 C 0.7570(6) 0.6854(6) 0.1784(3) 0.0382(9) Uani 1 1 d . . . . .
H12 H 0.7713 0.8059 0.1955 0.046 Uiso 1 1 calc R . . . .
C9 C 0.7142(8) 0.3308(7) 0.1272(4) 0.0682(15) Uani 1 1 d . . . . .
H9 H 0.6998 0.2106 0.1098 0.082 Uiso 1 1 calc R . . . .
C10 C 0.7740(9) 0.4545(8) 0.1179(5) 0.0699(16) Uani 1 1 d . . . . .
H10 H 0.7981 0.4185 0.0931 0.084 Uiso 1 1 calc R . . . .
C11 C 0.7983(8) 0.6299(7) 0.1448(4) 0.0594(13) Uani 1 1 d . . . . .
H11 H 0.8428 0.7127 0.1406 0.071 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
Dy1 O1 2.506(2) 2_645 ?
Dy1 O1 2.366(3) . ?
Dy1 O3 2.632(2) 2_655 ?
Dy1 O3 2.354(3) . ?
Dy1 O5 2.288(2) . ?
Dy1 O7 2.373(2) . ?
Dy1 O6 2.345(2) 2_645 ?
Dy1 O4 2.470(3) 2_655 ?
Dy1 O2 2.519(3) 2_645 ?
Dy1 C2 2.938(3) 2_655 ?
Dy1 C1 2.861(3) 2_645 ?
O1 Dy1 2.506(2) 2_655 ?
O1 C1 1.281(4) . ?
O3 Dy1 2.632(2) 2_645 ?
O3 C2 1.264(4) . ?
O5 C6 1.256(4) . ?
O7 H7A 0.8767 . ?
O7 H7B 0.8754 . ?
O6 Dy1 2.345(2) 2_655 ?
O6 C6 1.250(4) . ?
O4 Dy1 2.470(3) 2_645 ?
O4 C2 1.251(4) . ?
O2 Dy1 2.519(3) 2_655 ?
O2 C1 1.243(4) . ?
C6 C7 1.495(4) . ?
C2 Dy1 2.938(3) 2_645 ?
C2 C4 1.473(4) . ?
C1 Dy1 2.861(3) 2_655 ?
C1 C3 1.482(4) . ?
C3 H3 0.9800 . ?
C3 C4 1.514(4) . ?
C3 C5 1.493(5) . ?
C7 C8 1.378(5) . ?
C7 C12 1.377(5) . ?
C4 H4 0.9800 . ?
C4 C5 1.498(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C8 H8 0.9300 . ?
C8 C9 1.374(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.383(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.370(7) . ?
C10 H10 0.9300 . ?
C10 C11 1.360(7) . ?
C11 H11 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 Dy1 O1 141.04(5) . 2_645 ?
O1 Dy1 O3 131.41(6) 2_645 2_655 ?
O1 Dy1 O3 67.35(8) . 2_655 ?
O1 Dy1 O7 84.38(11) . . ?
O1 Dy1 O4 117.16(9) . 2_655 ?
O1 Dy1 O2 51.48(8) 2_645 2_645 ?
O1 Dy1 O2 164.59(8) . 2_645 ?
O1 Dy1 C2 108.75(8) 2_645 2_655 ?
O1 Dy1 C2 92.51(10) . 2_655 ?
O1 Dy1 C1 26.58(8) 2_645 2_645 ?
O1 Dy1 C1 167.58(8) . 2_645 ?
O3 Dy1 O1 74.81(11) . . ?
O3 Dy1 O1 69.68(8) . 2_645 ?
O3 Dy1 O3 134.05(6) . 2_655 ?
O3 Dy1 O7 134.74(8) . . ?
O3 Dy1 O4 146.07(9) . 2_655 ?
O3 Dy1 O2 111.06(11) . 2_645 ?
O3 Dy1 C2 25.48(7) 2_655 2_655 ?
O3 Dy1 C2 147.14(8) . 2_655 ?
O3 Dy1 C1 120.71(8) 2_655 2_645 ?
O3 Dy1 C1 93.54(11) . 2_645 ?
O5 Dy1 O1 79.56(9) . . ?
O5 Dy1 O1 76.61(8) . 2_645 ?
O5 Dy1 O3 72.84(8) . 2_655 ?
O5 Dy1 O3 75.59(9) . . ?
O5 Dy1 O7 139.65(8) . . ?
O5 Dy1 O6 147.74(9) . 2_645 ?
O5 Dy1 O4 75.85(12) . 2_655 ?
O5 Dy1 O2 115.47(9) . 2_645 ?
O5 Dy1 C2 72.31(10) . 2_655 ?
O5 Dy1 C1 93.54(10) . 2_645 ?
O7 Dy1 O1 132.71(9) . 2_645 ?
O7 Dy1 O3 66.81(7) . 2_655 ?
O7 Dy1 O4 79.18(11) . 2_655 ?
O7 Dy1 O2 81.63(10) . 2_645 ?
O7 Dy1 C2 71.70(9) . 2_655 ?
O7 Dy1 C1 107.28(11) . 2_645 ?
O6 Dy1 O1 90.72(7) 2_645 2_645 ?
O6 Dy1 O1 93.35(8) 2_645 . ?
O6 Dy1 O3 72.19(8) 2_645 . ?
O6 Dy1 O3 133.34(7) 2_645 2_655 ?
O6 Dy1 O7 69.40(8) 2_645 . ?
O6 Dy1 O4 133.55(9) 2_645 2_655 ?
O6 Dy1 O2 75.70(8) 2_645 2_645 ?
O6 Dy1 C2 139.82(9) 2_645 2_655 ?
O6 Dy1 C1 87.00(8) 2_645 2_645 ?
O4 Dy1 O1 86.17(7) 2_655 2_645 ?
O4 Dy1 O3 50.35(6) 2_655 2_655 ?
O4 Dy1 O2 66.39(10) 2_655 2_645 ?
O4 Dy1 C2 24.87(7) 2_655 2_655 ?
O4 Dy1 C1 70.38(9) 2_655 2_645 ?
O2 Dy1 O3 112.33(9) 2_645 2_655 ?
O2 Dy1 C2 89.22(11) 2_645 2_655 ?
O2 Dy1 C1 25.73(8) 2_645 2_645 ?
C1 Dy1 C2 95.23(10) 2_645 2_655 ?
Dy1 O1 Dy1 110.45(8) . 2_655 ?
C1 O1 Dy1 128.10(19) . . ?
C1 O1 Dy1 92.32(18) . 2_655 ?
Dy1 O3 Dy1 106.68(10) . 2_645 ?
C2 O3 Dy1 90.93(17) . 2_645 ?
C2 O3 Dy1 146.7(2) . . ?
C6 O5 Dy1 143.1(2) . . ?
Dy1 O7 H7A 111.0 . . ?
Dy1 O7 H7B 110.5 . . ?
H7A O7 H7B 108.0 . . ?
C6 O6 Dy1 131.4(2) . 2_655 ?
C2 O4 Dy1 98.98(19) . 2_645 ?
C1 O2 Dy1 92.65(19) . 2_655 ?
O5 C6 C7 117.1(3) . . ?
O6 C6 O5 124.7(3) . . ?
O6 C6 C7 118.2(3) . . ?
O3 C2 Dy1 63.59(16) . 2_645 ?
O3 C2 C4 122.9(3) . . ?
O4 C2 Dy1 56.14(16) . 2_645 ?
O4 C2 O3 119.7(3) . . ?
O4 C2 C4 117.4(3) . . ?
C4 C2 Dy1 173.5(2) . 2_645 ?
O1 C1 Dy1 61.10(15) . 2_655 ?
O1 C1 C3 120.9(3) . . ?
O2 C1 Dy1 61.61(16) . 2_655 ?
O2 C1 O1 119.7(3) . . ?
O2 C1 C3 119.1(3) . . ?
C3 C1 Dy1 157.3(2) . 2_655 ?
C1 C3 H3 114.2 . . ?
C1 C3 C4 123.7(3) . . ?
C1 C3 C5 120.1(3) . . ?
C4 C3 H3 114.2 . . ?
C5 C3 H3 114.2 . . ?
C5 C3 C4 59.7(2) . . ?
C8 C7 C6 119.7(3) . . ?
C12 C7 C6 120.7(3) . . ?
C12 C7 C8 119.6(3) . . ?
C2 C4 C3 123.8(3) . . ?
C2 C4 H4 114.0 . . ?
C2 C4 C5 120.7(3) . . ?
C3 C4 H4 114.0 . . ?
C5 C4 C3 59.4(2) . . ?
C5 C4 H4 114.0 . . ?
C3 C5 C4 60.8(2) . . ?
C3 C5 H5A 117.7 . . ?
C3 C5 H5B 117.7 . . ?
C4 C5 H5A 117.7 . . ?
C4 C5 H5B 117.7 . . ?
H5A C5 H5B 114.8 . . ?
C7 C8 H8 120.0 . . ?
C9 C8 C7 119.9(4) . . ?
C9 C8 H8 120.0 . . ?
C7 C12 H12 120.1 . . ?
C7 C12 C11 119.9(4) . . ?
C11 C12 H12 120.1 . . ?
C8 C9 H9 119.9 . . ?
C10 C9 C8 120.2(4) . . ?
C10 C9 H9 119.9 . . ?
C9 C10 H10 119.9 . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10 119.9 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 C12 120.1(5) . . ?
C10 C11 H11 120.0 . . ?

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
Dy1 O1 C1 Dy1 118.4(2) . . . 2_655 ?
Dy1 O1 C1 O2 98.4(3) . . . . ?
Dy1 O1 C1 O2 -20.0(3) 2_655 . . . ?
Dy1 O1 C1 C3 -87.7(3) . . . . ?
Dy1 O1 C1 C3 153.8(2) 2_655 . . . ?
Dy1 O3 C2 Dy1 123.2(3) . . . 2_645 ?
Dy1 O3 C2 O4 124.7(3) . . . . ?
Dy1 O3 C2 O4 1.5(3) 2_645 . . . ?
Dy1 O3 C2 C4 -55.9(5) . . . . ?
Dy1 O3 C2 C4 -179.1(3) 2_645 . . . ?
Dy1 O5 C6 O6 37.3(6) . . . . ?
Dy1 O5 C6 C7 -142.4(3) . . . . ?
Dy1 O6 C6 O5 -0.2(5) 2_655 . . . ?
Dy1 O6 C6 C7 179.5(2) 2_655 . . . ?
Dy1 O4 C2 O3 -1.6(3) 2_645 . . . ?
Dy1 O4 C2 C4 179.0(2) 2_645 . . . ?
Dy1 O2 C1 O1 19.9(3) 2_655 . . . ?
Dy1 O2 C1 C3 -154.0(2) 2_655 . . . ?
Dy1 C1 C3 C4 157.3(4) 2_655 . . . ?
Dy1 C1 C3 C5 85.6(6) 2_655 . . . ?
O1 C1 C3 C4 69.0(4) . . . . ?
O1 C1 C3 C5 -2.7(4) . . . . ?
O3 C2 C4 C3 -10.2(5) . . . . ?
O3 C2 C4 C5 61.5(4) . . . . ?
O5 C6 C7 C8 1.9(5) . . . . ?
O5 C6 C7 C12 -178.1(3) . . . . ?
O6 C6 C7 C8 -177.8(3) . . . . ?
O6 C6 C7 C12 2.2(5) . . . . ?
O4 C2 C4 C3 169.2(3) . . . . ?
O4 C2 C4 C5 -119.1(3) . . . . ?
O2 C1 C3 C4 -117.1(4) . . . . ?
O2 C1 C3 C5 171.2(3) . . . . ?
C6 C7 C8 C9 178.5(4) . . . . ?
C6 C7 C12 C11 -179.5(4) . . . . ?
C2 C4 C5 C3 -113.7(3) . . . . ?
C1 C3 C4 C2 0.6(5) . . . . ?
C1 C3 C4 C5 -108.0(4) . . . . ?
C1 C3 C5 C4 113.8(3) . . . . ?
C7 C8 C9 C10 0.8(8) . . . . ?
C7 C12 C11 C10 1.3(7) . . . . ?
C5 C3 C4 C2 108.6(4) . . . . ?
C8 C7 C12 C11 0.5(6) . . . . ?
C8 C9 C10 C11 1.1(9) . . . . ?
C12 C7 C8 C9 -1.6(6) . . . . ?
C9 C10 C11 C12 -2.1(9) . . . . ?

_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 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.751
####################################################################### 
# 
# 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_cpdc-bc-Tb
_database_code_depnum_ccdc_archive 'CCDC 1963203'
loop_
_audit_author_name
_audit_author_address
'Qi-Bing Bo'
;university of Jinan
China
;
_audit_update_record             
;
2019-11-02 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_audit_creation_date             2019-11-02
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C12 H11 O7 Tb'
_chemical_formula_sum            'C12 H11 O7 Tb'
_chemical_formula_weight         426.13
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O Tb Ba'
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      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                   13.790(8)
_cell_length_b                   7.4571(8)
_cell_length_c                   23.894(14)
_cell_angle_alpha                90
_cell_angle_beta                 148.12(15)
_cell_angle_gamma                90
_cell_volume                     1298(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2357
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6480
_cell_measurement_theta_min      3.9540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.478
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.181
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7915
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.229
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  35.00   1.00   28.43    --   15.86 -37.00-180.00   88
  2  ω     -3.00  85.00   1.00   28.43    --   15.86  37.00   0.00   88
  3  ω    -25.00  22.00   1.00   28.43    --  -16.95 -99.00 -30.00   47
  4  ω     32.00  88.00   1.00   28.43    --   15.86-178.00  60.00   56
  5  ω    -85.00 -25.00   1.00   28.43    --  -16.95 -77.00 150.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0784973000
_diffrn_orient_matrix_UB_12      -0.0559732000
_diffrn_orient_matrix_UB_13      -0.0402796000
_diffrn_orient_matrix_UB_21      -0.0569317000
_diffrn_orient_matrix_UB_22      0.0737170000
_diffrn_orient_matrix_UB_23      -0.0206691000
_diffrn_orient_matrix_UB_31      -0.0095007000
_diffrn_orient_matrix_UB_32      0.0221258000
_diffrn_orient_matrix_UB_33      -0.0333761000
_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                2009
_reflns_number_total             2633
_reflns_odcompleteness_completeness 99.51
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         4.709
_refine_diff_density_min         -4.668
_refine_diff_density_rms         0.431
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0759
_refine_ls_restrained_S_all      1.068
_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)+(0.1323P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1850
_refine_ls_wR_factor_ref         0.2067
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(O3) = Uanis(O4) = Uanis(O1) = Uanis(O2)
Uanis(C2) = Uanis(C1)
3.a Rotating group:
 O7(H7A,H7B)
3.b Ternary CH refined with riding coordinates:
 C4(H4), C3(H3)
3.c Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B)
3.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C12(H12), C11(H11), C10(H10), C9(H9)
;
_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 0.39655(7) 0.55937(7) 0.20424(4) 0.0213(3) Uani 1 1 d . . . . .
O3 O 0.5970(11) 0.3491(11) 0.3466(6) 0.0286(10) Uani 1 1 d . . . . .
O4 O 0.8673(11) 0.2661(11) 0.4489(6) 0.0286(10) Uani 1 1 d . . . . .
O5 O 0.5941(14) 0.4966(12) 0.2289(8) 0.035(2) Uani 1 1 d . . . . .
O1 O 0.6623(11) 0.7252(11) 0.3569(6) 0.0286(10) Uani 1 1 d . . . . .
O2 O 0.8047(12) 0.9440(10) 0.4699(7) 0.0286(10) Uani 1 1 d . . . . .
O7 O 0.1598(12) 0.4148(11) 0.1407(7) 0.032(2) Uani 1 1 d . . . . .
H7A H 0.1990 0.3891 0.1930 0.048 Uiso 1 1 d GR . . . .
H7B H 0.1271 0.3171 0.1082 0.048 Uiso 1 1 d GR . . . .
O6 O 0.6611(12) 0.2173(11) 0.2401(7) 0.033(2) Uani 1 1 d . . . . .
C2 C 0.7723(16) 0.3562(15) 0.4359(9) 0.0252(18) Uani 1 1 d . . . . .
C4 C 0.8672(19) 0.4514(15) 0.5292(10) 0.030(3) Uani 1 1 d . . . . .
H4 H 0.9801 0.3939 0.5978 0.036 Uiso 1 1 calc R . . . .
C1 C 0.7735(16) 0.7777(15) 0.4489(8) 0.0252(18) Uani 1 1 d . . . . .
C5 C 0.755(2) 0.5388(17) 0.5185(13) 0.039(3) Uani 1 1 d . . . . .
H5A H 0.7971 0.5289 0.5776 0.047 Uiso 1 1 calc R . . . .
H5B H 0.6223 0.5371 0.4492 0.047 Uiso 1 1 calc R . . . .
C7 C 0.696(2) 0.4367(16) 0.1873(11) 0.034(3) Uani 1 1 d . . . . .
C3 C 0.8644(18) 0.6570(18) 0.5328(10) 0.032(3) Uani 1 1 d . . . . .
H3 H 0.9757 0.7074 0.6042 0.039 Uiso 1 1 calc R . . . .
C6 C 0.6486(17) 0.3818(17) 0.2219(9) 0.028(3) Uani 1 1 d . . . . .
C8 C 0.757(2) 0.314(2) 0.1783(11) 0.043(3) Uani 1 1 d . . . . .
H8 H 0.7711 0.1945 0.1948 0.052 Uiso 1 1 calc R . . . .
C12 C 0.677(2) 0.617(2) 0.1634(14) 0.055(4) Uani 1 1 d . . . . .
H12 H 0.6400 0.7021 0.1713 0.066 Uiso 1 1 calc R . . . .
C11 C 0.716(3) 0.667(3) 0.1272(15) 0.076(6) Uani 1 1 d . . . . .
H11 H 0.7008 0.7860 0.1094 0.091 Uiso 1 1 calc R . . . .
C10 C 0.775(3) 0.545(3) 0.1170(19) 0.080(7) Uani 1 1 d . . . . .
H10 H 0.7977 0.5806 0.0916 0.096 Uiso 1 1 calc R . . . .
C9 C 0.799(3) 0.370(3) 0.1446(15) 0.066(5) Uani 1 1 d . . . . .
H9 H 0.8439 0.2879 0.1408 0.080 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 O3 2.517(8) 2_655 ?
Tb1 O3 2.388(10) . ?
Tb1 O4 2.528(10) 2_655 ?
Tb1 O5 2.294(10) . ?
Tb1 O1 2.644(8) 2_645 ?
Tb1 O1 2.359(11) . ?
Tb1 O2 2.479(11) 2_645 ?
Tb1 O7 2.390(9) . ?
Tb1 O6 2.363(8) 2_655 ?
Tb1 C2 2.880(12) 2_655 ?
Tb1 C1 2.954(12) 2_645 ?
O3 Tb1 2.517(8) 2_645 ?
O3 C2 1.281(15) . ?
O4 Tb1 2.528(10) 2_645 ?
O4 C2 1.256(14) . ?
O5 C6 1.240(15) . ?
O1 Tb1 2.644(8) 2_655 ?
O1 C1 1.270(13) . ?
O2 Tb1 2.479(11) 2_655 ?
O2 C1 1.268(13) . ?
O7 H7A 0.8622 . ?
O7 H7B 0.8621 . ?
O6 Tb1 2.363(8) 2_645 ?
O6 C6 1.263(15) . ?
C2 Tb1 2.880(12) 2_645 ?
C2 C4 1.494(17) . ?
C4 H4 0.9800 . ?
C4 C5 1.49(2) . ?
C4 C3 1.538(18) . ?
C1 Tb1 2.954(12) 2_655 ?
C1 C3 1.460(16) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C3 1.52(2) . ?
C7 C6 1.478(19) . ?
C7 C8 1.383(19) . ?
C7 C12 1.399(19) . ?
C3 H3 0.9800 . ?
C8 H8 0.9300 . ?
C8 C9 1.39(2) . ?
C12 H12 0.9300 . ?
C12 C11 1.39(2) . ?
C11 H11 0.9300 . ?
C11 C10 1.37(3) . ?
C10 H10 0.9300 . ?
C10 C9 1.37(3) . ?
C9 H9 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
O3 Tb1 O3 141.15(17) . 2_655 ?
O3 Tb1 O4 164.6(3) . 2_655 ?
O3 Tb1 O4 51.4(3) 2_655 2_655 ?
O3 Tb1 O1 67.0(3) . 2_645 ?
O3 Tb1 O1 131.5(3) 2_655 2_645 ?
O3 Tb1 O2 117.1(3) . 2_645 ?
O3 Tb1 O7 85.0(4) . . ?
O3 Tb1 C2 26.4(3) 2_655 2_655 ?
O3 Tb1 C2 167.5(3) . 2_655 ?
O3 Tb1 C1 109.2(3) 2_655 2_645 ?
O3 Tb1 C1 92.2(3) . 2_645 ?
O4 Tb1 O1 112.7(3) 2_655 2_645 ?
O4 Tb1 C2 25.8(3) 2_655 2_655 ?
O4 Tb1 C1 89.3(4) 2_655 2_645 ?
O5 Tb1 O3 79.3(4) . . ?
O5 Tb1 O3 77.1(3) . 2_655 ?
O5 Tb1 O4 115.6(3) . 2_655 ?
O5 Tb1 O1 71.9(3) . 2_645 ?
O5 Tb1 O1 76.3(4) . . ?
O5 Tb1 O2 75.7(4) . 2_645 ?
O5 Tb1 O7 139.0(3) . . ?
O5 Tb1 O6 148.3(3) . 2_655 ?
O5 Tb1 C2 93.8(4) . 2_655 ?
O5 Tb1 C1 72.2(4) . 2_645 ?
O1 Tb1 O3 75.1(4) . . ?
O1 Tb1 O3 69.6(3) . 2_655 ?
O1 Tb1 O4 110.8(4) . 2_655 ?
O1 Tb1 O1 133.9(2) . 2_645 ?
O1 Tb1 O2 146.3(3) . 2_645 ?
O1 Tb1 O7 135.2(3) . . ?
O1 Tb1 O6 72.0(3) . 2_655 ?
O1 Tb1 C2 93.2(4) . 2_655 ?
O1 Tb1 C2 121.1(3) 2_645 2_655 ?
O1 Tb1 C1 147.7(3) . 2_645 ?
O1 Tb1 C1 25.4(3) 2_645 2_645 ?
O2 Tb1 O3 86.3(3) 2_645 2_655 ?
O2 Tb1 O4 66.3(3) 2_645 2_655 ?
O2 Tb1 O1 50.5(2) 2_645 2_645 ?
O2 Tb1 C2 70.6(3) 2_645 2_655 ?
O2 Tb1 C1 25.1(3) 2_645 2_645 ?
O7 Tb1 O3 132.1(3) . 2_655 ?
O7 Tb1 O4 81.1(4) . 2_655 ?
O7 Tb1 O1 67.1(3) . 2_645 ?
O7 Tb1 O2 78.4(4) . 2_645 ?
O7 Tb1 C2 106.8(4) . 2_655 ?
O7 Tb1 C1 70.9(4) . 2_645 ?
O6 Tb1 O3 90.6(3) 2_655 2_655 ?
O6 Tb1 O3 93.5(3) 2_655 . ?
O6 Tb1 O4 75.6(3) 2_655 2_655 ?
O6 Tb1 O1 133.5(3) 2_655 2_645 ?
O6 Tb1 O2 133.3(3) 2_655 2_645 ?
O6 Tb1 O7 69.6(3) 2_655 . ?
O6 Tb1 C2 86.9(3) 2_655 2_655 ?
O6 Tb1 C1 139.4(3) 2_655 2_645 ?
C2 Tb1 C1 95.7(4) 2_655 2_645 ?
Tb1 O3 Tb1 110.4(3) . 2_645 ?
C2 O3 Tb1 127.6(7) . . ?
C2 O3 Tb1 92.8(7) . 2_645 ?
C2 O4 Tb1 92.9(7) . 2_645 ?
C6 O5 Tb1 146.0(9) . . ?
Tb1 O1 Tb1 107.1(3) . 2_655 ?
C1 O1 Tb1 91.1(7) . 2_655 ?
C1 O1 Tb1 147.7(8) . . ?
C1 O2 Tb1 98.9(7) . 2_655 ?
Tb1 O7 H7A 110.1 . . ?
Tb1 O7 H7B 109.9 . . ?
H7A O7 H7B 108.9 . . ?
C6 O6 Tb1 131.6(8) . 2_645 ?
O3 C2 Tb1 60.8(6) . 2_645 ?
O3 C2 C4 121.9(11) . . ?
O4 C2 Tb1 61.3(6) . 2_645 ?
O4 C2 O3 119.2(10) . . ?
O4 C2 C4 118.6(11) . . ?
C4 C2 Tb1 156.8(8) . 2_645 ?
C2 C4 H4 115.0 . . ?
C2 C4 C3 121.6(10) . . ?
C5 C4 C2 119.1(12) . . ?
C5 C4 H4 115.0 . . ?
C5 C4 C3 60.1(8) . . ?
C3 C4 H4 115.0 . . ?
O1 C1 Tb1 63.5(6) . 2_655 ?
O1 C1 C3 123.6(11) . . ?
O2 C1 Tb1 56.0(6) . 2_655 ?
O2 C1 O1 119.5(11) . . ?
O2 C1 C3 116.9(10) . . ?
C3 C1 Tb1 172.7(8) . 2_655 ?
C4 C5 H5A 117.6 . . ?
C4 C5 H5B 117.6 . . ?
C4 C5 C3 61.5(9) . . ?
H5A C5 H5B 114.7 . . ?
C3 C5 H5A 117.6 . . ?
C3 C5 H5B 117.6 . . ?
C8 C7 C6 121.7(12) . . ?
C8 C7 C12 119.5(14) . . ?
C12 C7 C6 118.8(13) . . ?
C4 C3 H3 113.8 . . ?
C1 C3 C4 124.9(10) . . ?
C1 C3 C5 121.3(12) . . ?
C1 C3 H3 113.8 . . ?
C5 C3 C4 58.4(9) . . ?
C5 C3 H3 113.8 . . ?
O5 C6 O6 123.1(13) . . ?
O5 C6 C7 119.1(12) . . ?
O6 C6 C7 117.7(11) . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.3(15) . . ?
C9 C8 H8 119.9 . . ?
C7 C12 H12 120.8 . . ?
C11 C12 C7 118.4(17) . . ?
C11 C12 H12 120.8 . . ?
C12 C11 H11 119.0 . . ?
C10 C11 C12 122.0(19) . . ?
C10 C11 H11 119.0 . . ?
C11 C10 H10 120.5 . . ?
C9 C10 C11 119.0(18) . . ?
C9 C10 H10 120.5 . . ?
C8 C9 H9 119.6 . . ?
C10 C9 C8 120.8(18) . . ?
C10 C9 H9 119.6 . . ?

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 O3 C2 Tb1 -118.5(8) . . . 2_645 ?
Tb1 O3 C2 O4 -99.0(11) . . . . ?
Tb1 O3 C2 O4 19.5(11) 2_645 . . . ?
Tb1 O3 C2 C4 88.3(13) . . . . ?
Tb1 O3 C2 C4 -153.2(10) 2_645 . . . ?
Tb1 O4 C2 O3 -19.4(11) 2_645 . . . ?
Tb1 O4 C2 C4 153.5(10) 2_645 . . . ?
Tb1 O5 C6 O6 -36(2) . . . . ?
Tb1 O5 C6 C7 142.2(13) . . . . ?
Tb1 O1 C1 Tb1 -125.6(14) . . . 2_655 ?
Tb1 O1 C1 O2 -125.2(13) . . . . ?
Tb1 O1 C1 O2 0.4(12) 2_655 . . . ?
Tb1 O1 C1 C3 177.8(11) 2_655 . . . ?
Tb1 O1 C1 C3 52(2) . . . . ?
Tb1 O2 C1 O1 -0.4(13) 2_655 . . . ?
Tb1 O2 C1 C3 -178.0(10) 2_655 . . . ?
Tb1 O6 C6 O5 -2(2) 2_645 . . . ?
Tb1 O6 C6 C7 -179.9(8) 2_645 . . . ?
Tb1 C2 C4 C5 -89(2) 2_645 . . . ?
Tb1 C2 C4 C3 -159.9(16) 2_645 . . . ?
O3 C2 C4 C5 0.7(17) . . . . ?
O3 C2 C4 C3 -70.3(17) . . . . ?
O4 C2 C4 C5 -172.1(11) . . . . ?
O4 C2 C4 C3 116.9(13) . . . . ?
O1 C1 C3 C4 12(2) . . . . ?
O1 C1 C3 C5 -59.3(18) . . . . ?
O2 C1 C3 C4 -170.8(12) . . . . ?
O2 C1 C3 C5 118.1(13) . . . . ?
C2 C4 C5 C3 -111.9(12) . . . . ?
C2 C4 C3 C1 -1(2) . . . . ?
C2 C4 C3 C5 107.7(15) . . . . ?
C4 C5 C3 C1 114.3(13) . . . . ?
C5 C4 C3 C1 -108.3(15) . . . . ?
C7 C8 C9 C10 -2(3) . . . . ?
C7 C12 C11 C10 -2(3) . . . . ?
C6 C7 C8 C9 179.4(14) . . . . ?
C6 C7 C12 C11 -177.8(15) . . . . ?
C8 C7 C6 O5 179.9(13) . . . . ?
C8 C7 C6 O6 -2(2) . . . . ?
C8 C7 C12 C11 2(2) . . . . ?
C12 C7 C6 O5 0(2) . . . . ?
C12 C7 C6 O6 177.9(13) . . . . ?
C12 C7 C8 C9 -1(2) . . . . ?
C12 C11 C10 C9 -1(4) . . . . ?
C11 C10 C9 C8 3(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 1.273
_oxdiff_exptl_absorpt_empirical_full_min 0.797
####################################################################### 
# 
# 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_cpdc-Dy
_database_code_depnum_ccdc_archive 'CCDC 1963201'
loop_
_audit_author_name
_audit_author_address
'Qi-Bing Bo'
;university of Jinan
China
;
_audit_update_record             
;
2019-11-02 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_audit_creation_date             2019-11-02
_audit_creation_method           
;
Olex2 1.2-alpha
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         '0.5(C30 H36 Dy4 O30)'
_chemical_formula_sum            'C15 H18 Dy2 O15'
_chemical_formula_weight         763.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C H O Dy'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   9.759(2)
_cell_length_b                   7.9677(16)
_cell_length_c                   12.790(3)
_cell_angle_alpha                90
_cell_angle_beta                 106.22(3)
_cell_angle_gamma                90
_cell_volume                     955.0(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2334
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5400
_cell_measurement_theta_min      4.1860
_shelx_estimated_absorpt_T_max   0.834
_shelx_estimated_absorpt_T_min   0.154
_exptl_absorpt_coefficient_mu    7.848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.29451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.654
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.024
_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1028
_diffrn_reflns_av_unetI/netI     0.0993
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6076
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.339
_diffrn_reflns_theta_min         3.314
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0355
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   35.00   88.00   1.0000    1.9850
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
  2 omega   35.00   88.00   1.0000    1.9850
omega____ theta____ kappa____ phi______ frames
    -       15.8569  178.0000  150.0000 53

#__ type_ start__ end____ width___ exp.time_
  3 omega  -51.00   33.00   1.0000    1.9850
omega____ theta____ kappa____ phi______ frames
    -       15.8569  -57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega  -14.00   87.00   1.0000    1.9850
omega____ theta____ kappa____ phi______ frames
    -       15.8569   19.0000    0.0000 101

#__ type_ start__ end____ width___ exp.time_
  5 omega  -11.00   24.00   1.0000    1.9850
omega____ theta____ kappa____ phi______ frames
    -       15.8569   77.0000   60.0000 35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0261526000
_diffrn_orient_matrix_UB_12      0.0183357000
_diffrn_orient_matrix_UB_13      0.0565472000
_diffrn_orient_matrix_UB_21      -0.0355828000
_diffrn_orient_matrix_UB_22      -0.0720690000
_diffrn_orient_matrix_UB_23      0.0116426000
_diffrn_orient_matrix_UB_31      0.0613910000
_diffrn_orient_matrix_UB_32      -0.0490600000
_diffrn_orient_matrix_UB_33      0.0026529000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_source                   'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1646
_reflns_number_total             2076
_reflns_odcompleteness_completeness 99.38
_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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max         4.777
_refine_diff_density_min         -5.173
_refine_diff_density_rms         0.495
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2076
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0963
_refine_ls_restrained_S_all      1.076
_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)+(0.0366P)²+120.5462P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2124
_refine_ls_wR_factor_ref         0.2233
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. 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
2. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(O2) = Uanis(C1) = Uanis(C2) = Uanis(C3)
Uanis(O3) = Uanis(C4) = Uanis(C5) = Uanis(C6)
Uanis(O6) = Uanis(O5) = Uanis(C7) = Uanis(C8) = Uanis(C9)
Uanis(O7) = Uanis(O8) = Uanis(O9)
3. Others
 Fixed Sof: H7A(0.5) H7B(0.5) H8A(0.5) H8B(0.5) H9A(0.5) H9B(0.5)
4.a Riding coordinates:
 O7(H7A,H7B), O8(H8A,H8B), O9(H9A,H9B)
4.b Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C8(H8)
4.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C6(H6A,H6B), C9(H9C,H9D)
;
_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
Dy1 Dy 0.49022(13) 0.7500 0.13299(11) 0.0159(4) Uani 1 2 d S T P . .
Dy2 Dy 0.89520(13) 0.2500 0.50500(11) 0.0219(4) Uani 1 2 d S T P . .
O1 O 0.5837(16) 0.570(2) 0.2753(15) 0.045(3) Uani 1 1 d . . . . .
O2 O 0.7201(16) 0.426(2) 0.4136(15) 0.045(3) Uani 1 1 d . . . . .
O3 O 0.6564(13) 0.9311(17) 0.0884(12) 0.021(2) Uani 1 1 d . . . . .
O4 O 0.6797(15) 1.041(2) -0.0665(12) 0.028(3) Uani 1 1 d . . . . .
O5 O 0.9976(18) 0.574(2) 0.5980(13) 0.035(2) Uani 1 1 d . . . . .
O6 O 0.8446(18) 0.423(2) 0.6465(13) 0.035(2) Uani 1 1 d . . . . .
O7 O 0.452(2) 0.7500 -0.0636(19) 0.028(3) Uani 1 2 d S T P . .
H7A H 0.4073 0.8288 -0.1054 0.042 Uiso 0.5 1 d R . . . .
H7B H 0.4056 0.6721 -0.1054 0.042 Uiso 0.5 1 d R . . . .
O8 O 0.321(2) 0.7500 0.2389(19) 0.028(3) Uani 1 2 d S T P . .
H8A H 0.3099 0.8225 0.2856 0.042 Uiso 0.5 1 d R . . . .
H8B H 0.2568 0.6773 0.2402 0.042 Uiso 0.5 1 d R . . . .
O9 O 1.134(2) 0.2500 0.6153(19) 0.028(3) Uani 1 2 d S T P . .
H9A H 1.1669 0.1744 0.6639 0.042 Uiso 0.5 1 d R . . . .
H9B H 1.2114 0.2951 0.6087 0.042 Uiso 0.5 1 d R . . . .
C1 C 0.600(2) 0.452(4) 0.341(2) 0.045(3) Uani 1 1 d . . . . .
C2 C 0.474(2) 0.347(3) 0.343(2) 0.045(3) Uani 1 1 d . . . . .
H2 H 0.3824 0.3961 0.3026 0.054 Uiso 1 1 calc R . . . .
C3 C 0.465(4) 0.2500 0.442(3) 0.045(3) Uani 1 2 d S T P . .
H3A H 0.3751 0.2500 0.4594 0.054 Uiso 1 2 calc RS T P . .
H3B H 0.5490 0.2500 0.5042 0.054 Uiso 1 2 calc RS T P . .
C4 C 0.718(2) 0.945(2) 0.0139(17) 0.021(2) Uani 1 1 d . . . . .
C5 C 0.8508(19) 0.846(2) 0.0218(17) 0.021(2) Uani 1 1 d . . . . .
H5 H 0.9149 0.8970 -0.0162 0.025 Uiso 1 1 calc R . . . .
C6 C 0.926(3) 0.7500 0.123(3) 0.021(2) Uani 1 2 d S T P . .
H6A H 1.0296 0.7500 0.1452 0.025 Uiso 1 2 calc RS T P . .
H6B H 0.8830 0.7500 0.1832 0.025 Uiso 1 2 calc RS T P . .
C7 C 0.923(3) 0.551(3) 0.6611(19) 0.035(2) Uani 1 1 d . . . . .
C8 C 0.925(3) 0.656(3) 0.7553(19) 0.035(2) Uani 1 1 d . . . . .
H8 H 0.8773 0.6057 0.8055 0.042 Uiso 1 1 calc R . . . .
C9 C 1.061(4) 0.7500 0.811(3) 0.035(2) Uani 1 2 d S T P . .
H9C H 1.0918 0.7500 0.8902 0.042 Uiso 1 2 calc RS T P . .
H9D H 1.1376 0.7500 0.7766 0.042 Uiso 1 2 calc RS T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O1 2.299(17) . ?
Dy1 O1 2.299(17) 4_575 ?
Dy1 O3 2.356(13) . ?
Dy1 O3 2.356(13) 4_575 ?
Dy1 O4 2.335(15) 3_675 ?
Dy1 O4 2.335(15) 2_645 ?
Dy1 O7 2.44(2) . ?
Dy1 O8 2.41(2) . ?
Dy2 O2 2.267(16) 4_565 ?
Dy2 O2 2.267(16) . ?
Dy2 O5 2.358(16) 2_746 ?
Dy2 O5 2.358(16) 3_766 ?
Dy2 O5 2.904(17) . ?
Dy2 O5 2.904(17) 4_565 ?
Dy2 O6 2.433(17) . ?
Dy2 O6 2.433(17) 4_565 ?
Dy2 O9 2.36(2) . ?
O1 C1 1.24(3) . ?
O2 C1 1.29(3) . ?
O3 C4 1.27(2) . ?
O4 Dy1 2.335(15) 3_675 ?
O4 C4 1.25(2) . ?
O5 Dy2 2.358(16) 3_766 ?
O5 C7 1.24(3) . ?
O6 C7 1.26(3) . ?
O7 H7A 0.8600 . ?
O7 H7B 0.8599 . ?
O8 H8A 0.8600 . ?
O8 H8B 0.8600 . ?
O9 H9A 0.8600 . ?
O9 H9B 0.8602 . ?
C1 C2 1.49(3) . ?
C2 C2 1.55(5) 4_565 ?
C2 H2 0.9800 . ?
C2 C3 1.50(4) . ?
C3 C2 1.50(4) 4_565 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.49(2) . ?
C5 C5 1.54(4) 4_575 ?
C5 H5 0.9800 . ?
C5 C6 1.51(3) . ?
C6 C5 1.51(3) 4_575 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.46(3) . ?
C8 C8 1.50(4) 4_575 ?
C8 H8 0.9800 . ?
C8 C9 1.52(4) . ?
C9 C8 1.52(4) 4_575 ?
C9 H9C 0.9700 . ?
C9 H9D 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 Dy1 O1 77.4(10) . 4_575 ?
O1 Dy1 O3 115.2(5) . . ?
O1 Dy1 O3 70.2(6) 4_575 . ?
O1 Dy1 O3 115.2(5) 4_575 4_575 ?
O1 Dy1 O3 70.2(6) . 4_575 ?
O1 Dy1 O4 85.8(6) . 2_645 ?
O1 Dy1 O4 144.9(6) 4_575 2_645 ?
O1 Dy1 O4 144.9(6) . 3_675 ?
O1 Dy1 O4 85.8(6) 4_575 3_675 ?
O1 Dy1 O7 136.9(5) . . ?
O1 Dy1 O7 136.9(5) 4_575 . ?
O1 Dy1 O8 74.8(6) . . ?
O1 Dy1 O8 74.7(6) 4_575 . ?
O3 Dy1 O3 75.5(6) 4_575 . ?
O3 Dy1 O7 70.6(5) 4_575 . ?
O3 Dy1 O7 70.6(5) . . ?
O3 Dy1 O8 139.6(4) 4_575 . ?
O3 Dy1 O8 139.6(4) . . ?
O4 Dy1 O3 144.6(5) 3_675 4_575 ?
O4 Dy1 O3 144.6(5) 2_645 . ?
O4 Dy1 O3 86.7(5) 2_645 4_575 ?
O4 Dy1 O3 86.7(5) 3_675 . ?
O4 Dy1 O4 90.9(8) 2_645 3_675 ?
O4 Dy1 O7 74.7(5) 3_675 . ?
O4 Dy1 O7 74.7(5) 2_645 . ?
O4 Dy1 O8 71.1(5) 2_645 . ?
O4 Dy1 O8 71.1(5) 3_675 . ?
O8 Dy1 O7 130.4(7) . . ?
O2 Dy2 O2 76.5(9) 4_565 . ?
O2 Dy2 O5 77.5(6) 4_565 4_565 ?
O2 Dy2 O5 117.9(7) 4_565 3_766 ?
O2 Dy2 O5 152.4(6) . 4_565 ?
O2 Dy2 O5 74.5(6) 4_565 2_746 ?
O2 Dy2 O5 74.5(6) . 3_766 ?
O2 Dy2 O5 77.5(6) . . ?
O2 Dy2 O5 117.9(7) . 2_746 ?
O2 Dy2 O5 152.4(6) 4_565 . ?
O2 Dy2 O6 75.7(6) 4_565 4_565 ?
O2 Dy2 O6 117.0(6) . 4_565 ?
O2 Dy2 O6 117.0(6) 4_565 . ?
O2 Dy2 O6 75.7(6) . . ?
O2 Dy2 O9 141.5(5) . . ?
O2 Dy2 O9 141.5(5) 4_565 . ?
O5 Dy2 O5 127.0(3) 3_766 4_565 ?
O5 Dy2 O5 63.0(6) 3_766 . ?
O5 Dy2 O5 72.8(8) 2_746 3_766 ?
O5 Dy2 O5 63.0(6) 2_746 4_565 ?
O5 Dy2 O5 127.0(3) 2_746 . ?
O5 Dy2 O5 125.8(6) . 4_565 ?
O5 Dy2 O6 107.1(5) 3_766 . ?
O5 Dy2 O6 165.0(6) 3_766 4_565 ?
O5 Dy2 O6 107.1(5) 2_746 4_565 ?
O5 Dy2 O6 165.0(6) 2_746 . ?
O5 Dy2 O9 79.4(6) 2_746 . ?
O5 Dy2 O9 79.4(6) 3_766 . ?
O6 Dy2 O5 46.3(5) 4_565 4_565 ?
O6 Dy2 O5 108.5(5) 4_565 . ?
O6 Dy2 O5 46.3(5) . . ?
O6 Dy2 O5 108.5(5) . 4_565 ?
O6 Dy2 O6 69.0(7) . 4_565 ?
O9 Dy2 O5 65.6(3) . 4_565 ?
O9 Dy2 O5 65.6(4) . . ?
O9 Dy2 O6 85.8(6) . . ?
O9 Dy2 O6 85.8(6) . 4_565 ?
C1 O1 Dy1 163.1(16) . . ?
C1 O2 Dy2 150.5(19) . . ?
C4 O3 Dy1 137.7(13) . . ?
C4 O4 Dy1 138.9(13) . 3_675 ?
Dy2 O5 Dy2 117.0(6) 3_766 . ?
C7 O5 Dy2 86.3(15) . . ?
C7 O5 Dy2 152.2(16) . 3_766 ?
C7 O6 Dy2 109.0(15) . . ?
Dy1 O7 H7A 123.2 . . ?
Dy1 O7 H7B 122.9 . . ?
H7A O7 H7B 93.1 . . ?
Dy1 O8 H8A 129.2 . . ?
Dy1 O8 H8B 129.2 . . ?
H8A O8 H8B 101.6 . . ?
Dy2 O9 H9A 122.4 . . ?
Dy2 O9 H9B 133.4 . . ?
H9A O9 H9B 101.9 . . ?
O1 C1 O2 122(2) . . ?
O1 C1 C2 119(2) . . ?
O2 C1 C2 119(2) . . ?
C1 C2 C2 124.0(14) . 4_565 ?
C1 C2 H2 113.5 . . ?
C1 C2 C3 123(2) . . ?
C2 C2 H2 113.5 4_565 . ?
C3 C2 C2 58.9(14) . 4_565 ?
C3 C2 H2 113.5 . . ?
C2 C3 C2 62(3) . 4_565 ?
C2 C3 H3A 117.5 . . ?
C2 C3 H3A 117.5 4_565 . ?
C2 C3 H3B 117.5 . . ?
C2 C3 H3B 117.5 4_565 . ?
H3A C3 H3B 114.6 . . ?
O3 C4 C5 119.2(17) . . ?
O4 C4 O3 125.1(18) . . ?
O4 C4 C5 115.6(17) . . ?
C4 C5 C5 121.7(10) . 4_575 ?
C4 C5 H5 114.3 . . ?
C4 C5 C6 122.0(19) . . ?
C5 C5 H5 114.3 4_575 . ?
C6 C5 C5 59.5(9) . 4_575 ?
C6 C5 H5 114.3 . . ?
C5 C6 C5 61.1(18) 4_575 . ?
C5 C6 H6A 117.7 . . ?
C5 C6 H6A 117.7 4_575 . ?
C5 C6 H6B 117.7 4_575 . ?
C5 C6 H6B 117.7 . . ?
H6A C6 H6B 114.8 . . ?
O5 C7 O6 118(2) . . ?
O5 C7 C8 125(2) . . ?
O6 C7 C8 117(2) . . ?
C7 C8 C8 124.9(12) . 4_575 ?
C7 C8 H8 114.1 . . ?
C7 C8 C9 119(2) . . ?
C8 C8 H8 114.1 4_575 . ?
C8 C8 C9 60.4(11) 4_575 . ?
C9 C8 H8 114.1 . . ?
C8 C9 C8 59(2) 4_575 . ?
C8 C9 H9C 117.8 4_575 . ?
C8 C9 H9C 117.8 . . ?
C8 C9 H9D 117.8 . . ?
C8 C9 H9D 117.8 4_575 . ?
H9C C9 H9D 115.0 . . ?

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
Dy1 O1 C1 O2 174(5) . . . . ?
Dy1 O1 C1 C2 -12(9) . . . . ?
Dy1 O3 C4 O4 98(2) . . . . ?
Dy1 O3 C4 C5 -84(2) . . . . ?
Dy1 O4 C4 O3 5(4) 3_675 . . . ?
Dy1 O4 C4 C5 -172.6(14) 3_675 . . . ?
Dy2 O2 C1 O1 -135(3) . . . . ?
Dy2 O2 C1 C2 51(5) . . . . ?
Dy2 O5 C7 O6 143(3) 3_766 . . . ?
Dy2 O5 C7 O6 -5(2) . . . . ?
Dy2 O5 C7 C8 171(2) . . . . ?
Dy2 O5 C7 C8 -40(5) 3_766 . . . ?
Dy2 O6 C7 O5 7(3) . . . . ?
Dy2 O6 C7 C8 -170.2(17) . . . . ?
O1 C1 C2 C2 132(2) . . . 4_565 ?
O1 C1 C2 C3 -156(3) . . . . ?
O2 C1 C2 C2 -54(3) . . . 4_565 ?
O2 C1 C2 C3 19(4) . . . . ?
O3 C4 C5 C5 62(2) . . . 4_575 ?
O3 C4 C5 C6 -9(3) . . . . ?
O4 C4 C5 C5 -120.1(15) . . . 4_575 ?
O4 C4 C5 C6 168.5(17) . . . . ?
O5 C7 C8 C8 44(3) . . . 4_575 ?
O5 C7 C8 C9 -28(3) . . . . ?
O6 C7 C8 C8 -138.9(16) . . . 4_575 ?
O6 C7 C8 C9 149(2) . . . . ?
C1 C2 C3 C2 -113(2) . . . 4_565 ?
C4 C5 C6 C5 110.6(16) . . . 4_575 ?
C7 C8 C9 C8 116.0(18) . . . 4_575 ?

_olex2_submission_special_instructions 'No special instructions were received'
