# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2019

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

data_kasm-c3b
_database_code_depnum_ccdc_archive 'CCDC 1866430'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-08-01 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-07-13
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.25(C60 H88 O56 Tb8), 4(H2 O)'
_chemical_formula_sum            'C15 H30 O18 Tb2'
_chemical_formula_weight         816.23
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   7.9368(2)
_cell_length_b                   14.9436(3)
_cell_length_c                   19.6279(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.485(2)
_cell_angle_gamma                90
_cell_volume                     2320.83(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6843
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.3580
_cell_measurement_theta_min      3.2511
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.132
_exptl_absorpt_correction_T_max  0.399
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   multi-scan
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.336
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1576
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            8766
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.434
_diffrn_reflns_theta_min         3.431
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2336
_reflns_number_total             2453
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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         1.370
_refine_diff_density_min         -2.105
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2453
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0323
_refine_ls_restrained_S_all      1.077
_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)+(0.0533P)²+4.1990P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0873
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid body (RIGU) restrains
 O9, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: H8A(0.5) H8B(0.5)
4.a Riding coordinates:
 O9(H9A,H9B)
4.b Free rotating group:
 O8(H8C,H8D)
4.c Rotating group:
 O7(H7A,H7B)
4.d Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C8(H8A,H8B), C2(H2A,H2B), C7(H7C,H7D), C3(H3A,H3B)
;
_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 0.75642(2) 0.46278(2) 0.51225(2) 0.01394(11) Uani 1 1 d . . . . .
O3 O 0.8328(4) 0.3228(2) 0.57192(16) 0.0225(7) Uani 1 1 d . . . . .
O1 O 0.4949(4) 0.45518(18) 0.5612(2) 0.0230(8) Uani 1 1 d . . . . .
O4 O 0.8531(4) 0.44634(19) 0.63077(19) 0.0247(7) Uani 1 1 d . . . . .
O2 O 0.2362(4) 0.4533(2) 0.5915(2) 0.0270(8) Uani 1 1 d . . . . .
O5 O 0.4881(4) 0.07824(18) 0.53318(16) 0.0200(6) Uani 1 1 d . . . . .
O7 O 0.6159(4) 0.35489(19) 0.44009(18) 0.0259(7) Uani 1 1 d . . . . .
H7A H 0.668472 0.305062 0.443828 0.039 Uiso 1 1 d GR . . . .
H7B H 0.614735 0.373181 0.398844 0.039 Uiso 1 1 d GR . . . .
O6 O 0.2327(4) 0.11377(18) 0.55790(19) 0.0247(7) Uani 1 1 d . . . . .
C1 C 0.3858(5) 0.4269(2) 0.6006(2) 0.0141(8) Uani 1 1 d . . . . .
C5 C 0.3858(5) 0.1348(3) 0.5554(2) 0.0164(8) Uani 1 1 d . . . . .
C6 C 0.8711(5) 0.3628(3) 0.6278(2) 0.0164(8) Uani 1 1 d . . . . .
C4 C 0.4515(6) 0.2250(3) 0.5777(3) 0.0272(10) Uani 1 1 d . . . . .
H4A H 0.443022 0.264816 0.538612 0.033 Uiso 1 1 calc R . . . .
H4B H 0.570225 0.219360 0.592970 0.033 Uiso 1 1 calc R . . . .
C8 C 1.000000 0.3664(4) 0.750000 0.0244(13) Uani 1 2 d S T P . .
H8A H 0.911818 0.404603 0.765447 0.029 Uiso 0.5 1 calc R . . . .
C2 C 0.4312(5) 0.3598(3) 0.6557(2) 0.0193(8) Uani 1 1 d . . . . .
H2A H 0.385305 0.378569 0.697771 0.023 Uiso 1 1 calc R . . . .
H2B H 0.553168 0.356322 0.663836 0.023 Uiso 1 1 calc R . . . .
C7 C 0.9273(5) 0.3096(3) 0.6905(2) 0.0213(9) Uani 1 1 d . . . . .
H7C H 1.012037 0.266732 0.678822 0.026 Uiso 1 1 calc R . . . .
H7D H 0.831459 0.276260 0.704970 0.026 Uiso 1 1 calc R . . . .
C3 C 0.3601(7) 0.2671(3) 0.6344(3) 0.0263(10) Uani 1 1 d . . . . .
H3A H 0.368935 0.227812 0.673889 0.032 Uiso 1 1 calc R . . . .
H3B H 0.241227 0.273097 0.619460 0.032 Uiso 1 1 calc R . . . .
O8 O 0.610(2) 0.0925(4) 0.6998(4) 0.177(5) Uani 1 1 d . U . . .
H8C H 0.557629 0.045076 0.709785 0.265 Uiso 1 1 d G . . . .
H8D H 0.715019 0.082021 0.701077 0.265 Uiso 1 1 d G . . . .
O9 O 0.8810(15) 0.0708(7) 0.7853(7) 0.200(5) Uani 1 1 d . U . . .
H9A H 0.876319 0.083140 0.827370 0.299 Uiso 1 1 d R . . . .
H9B H 0.871919 0.014650 0.779490 0.299 Uiso 1 1 d 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 2.450(3) . ?
Tb1 O1 2.357(3) . ?
Tb1 O1 2.666(4) 5_666 ?
Tb1 O4 2.405(4) . ?
Tb1 O2 2.396(4) 5_666 ?
Tb1 O5 2.359(3) 7_656 ?
Tb1 O5 2.531(3) 3 ?
Tb1 O7 2.367(3) . ?
Tb1 O6 2.440(3) 3 ?
Tb1 C1 2.918(4) 5_666 ?
Tb1 C5 2.871(4) 3 ?
Tb1 C6 2.807(4) . ?
O3 C6 1.265(5) . ?
O1 C1 1.278(5) . ?
O4 C6 1.259(5) . ?
O2 C1 1.251(5) . ?
O5 C5 1.273(5) . ?
O7 H7A 0.8538 . ?
O7 H7B 0.8539 . ?
O6 C5 1.260(5) . ?
C1 C2 1.497(5) . ?
C5 C4 1.498(6) . ?
C6 C7 1.503(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.512(7) . ?
C8 H8A 0.9700 . ?
C8 C7 1.520(5) 2_756 ?
C8 C7 1.520(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.541(6) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O8 H8C 0.8498 . ?
O8 H8D 0.8501 . ?
O9 H9A 0.8504 . ?
O9 H9B 0.8496 . ?

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 O1 142.91(10) . 5_666 ?
O3 Tb1 O5 110.78(10) . 3 ?
O3 Tb1 C1 155.81(10) . 5_666 ?
O3 Tb1 C5 123.62(11) . 3 ?
O3 Tb1 C6 26.74(11) . . ?
O1 Tb1 O3 87.54(10) . . ?
O1 Tb1 O1 66.23(14) . 5_666 ?
O1 Tb1 O4 79.94(13) . . ?
O1 Tb1 O2 116.89(12) . 5_666 ?
O1 Tb1 O5 162.15(10) . 7_656 ?
O1 Tb1 O5 128.19(10) . 3 ?
O1 Tb1 O7 79.77(12) . . ?
O1 Tb1 O6 78.42(10) . 3 ?
O1 Tb1 C1 92.06(12) . 5_666 ?
O1 Tb1 C1 25.96(10) 5_666 5_666 ?
O1 Tb1 C5 103.23(11) . 3 ?
O1 Tb1 C5 89.03(10) 5_666 3 ?
O1 Tb1 C6 149.65(11) 5_666 . ?
O1 Tb1 C6 83.42(12) . . ?
O4 Tb1 O3 53.27(10) . . ?
O4 Tb1 O1 137.61(11) . 5_666 ?
O4 Tb1 O5 74.92(10) . 3 ?
O4 Tb1 O6 76.54(11) . 3 ?
O4 Tb1 C1 150.20(10) . 5_666 ?
O4 Tb1 C5 74.11(11) . 3 ?
O4 Tb1 C6 26.53(11) . . ?
O2 Tb1 O3 146.23(11) 5_666 . ?
O2 Tb1 O1 50.72(10) 5_666 5_666 ?
O2 Tb1 O4 148.07(11) 5_666 . ?
O2 Tb1 O5 73.49(11) 5_666 3 ?
O2 Tb1 O6 80.57(11) 5_666 3 ?
O2 Tb1 C1 24.83(11) 5_666 5_666 ?
O2 Tb1 C5 75.56(12) 5_666 3 ?
O2 Tb1 C6 159.58(11) 5_666 . ?
O5 Tb1 O3 76.76(10) 7_656 . ?
O5 Tb1 O1 122.95(11) 7_656 5_666 ?
O5 Tb1 O1 106.11(9) 3 5_666 ?
O5 Tb1 O4 96.92(11) 7_656 . ?
O5 Tb1 O2 74.68(10) 7_656 5_666 ?
O5 Tb1 O5 66.64(11) 7_656 3 ?
O5 Tb1 O7 88.60(11) 7_656 . ?
O5 Tb1 O6 118.18(10) 7_656 3 ?
O5 Tb1 C1 88.34(10) 3 5_666 ?
O5 Tb1 C1 98.79(11) 7_656 5_666 ?
O5 Tb1 C5 92.64(11) 7_656 3 ?
O5 Tb1 C5 26.29(10) 3 3 ?
O5 Tb1 C6 92.65(11) 3 . ?
O5 Tb1 C6 86.17(11) 7_656 . ?
O7 Tb1 O3 77.99(10) . . ?
O7 Tb1 O1 72.08(10) . 5_666 ?
O7 Tb1 O4 127.53(11) . . ?
O7 Tb1 O2 83.65(12) . 5_666 ?
O7 Tb1 O5 149.73(11) . 3 ?
O7 Tb1 O6 143.44(10) . 3 ?
O7 Tb1 C1 78.13(11) . 5_666 ?
O7 Tb1 C5 158.03(11) . 3 ?
O7 Tb1 C6 103.22(11) . . ?
O6 Tb1 O3 129.57(11) 3 . ?
O6 Tb1 O1 72.39(10) 3 5_666 ?
O6 Tb1 O5 52.13(9) 3 3 ?
O6 Tb1 C1 73.73(11) 3 5_666 ?
O6 Tb1 C5 25.84(10) 3 3 ?
O6 Tb1 C6 103.00(12) 3 . ?
C5 Tb1 C1 80.00(11) 3 5_666 ?
C6 Tb1 C1 174.93(11) . 5_666 ?
C6 Tb1 C5 98.75(12) . 3 ?
C6 O3 Tb1 92.6(2) . . ?
Tb1 O1 Tb1 113.77(14) . 5_666 ?
C1 O1 Tb1 88.1(2) . 5_666 ?
C1 O1 Tb1 157.3(3) . . ?
C6 O4 Tb1 94.9(3) . . ?
C1 O2 Tb1 101.6(3) . 5_666 ?
Tb1 O5 Tb1 113.36(11) 7_656 3_445 ?
C5 O5 Tb1 153.2(3) . 7_656 ?
C5 O5 Tb1 91.9(2) . 3_445 ?
Tb1 O7 H7A 109.8 . . ?
Tb1 O7 H7B 108.6 . . ?
H7A O7 H7B 109.2 . . ?
C5 O6 Tb1 96.6(2) . 3_445 ?
O1 C1 Tb1 66.0(2) . 5_666 ?
O1 C1 C2 121.5(4) . . ?
O2 C1 Tb1 53.6(2) . 5_666 ?
O2 C1 O1 119.3(4) . . ?
O2 C1 C2 119.2(4) . . ?
C2 C1 Tb1 169.6(3) . 5_666 ?
O5 C5 Tb1 61.8(2) . 3_445 ?
O5 C5 C4 118.8(4) . . ?
O6 C5 Tb1 57.6(2) . 3_445 ?
O6 C5 O5 119.4(4) . . ?
O6 C5 C4 121.9(4) . . ?
C4 C5 Tb1 179.4(3) . 3_445 ?
O3 C6 Tb1 60.7(2) . . ?
O3 C6 C7 119.8(4) . . ?
O4 C6 Tb1 58.6(2) . . ?
O4 C6 O3 119.2(4) . . ?
O4 C6 C7 120.9(4) . . ?
C7 C6 Tb1 178.2(3) . . ?
C5 C4 H4A 108.6 . . ?
C5 C4 H4B 108.6 . . ?
C5 C4 C3 114.4(4) . . ?
H4A C4 H4B 107.6 . . ?
C3 C4 H4A 108.6 . . ?
C3 C4 H4B 108.6 . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8A 109.2 2_756 . ?
C7 C8 C7 112.2(5) . 2_756 ?
C1 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C1 C2 C3 110.1(4) . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
C6 C7 C8 113.9(3) . . ?
C6 C7 H7C 108.8 . . ?
C6 C7 H7D 108.8 . . ?
C8 C7 H7C 108.8 . . ?
C8 C7 H7D 108.8 . . ?
H7C C7 H7D 107.7 . . ?
C4 C3 C2 112.8(4) . . ?
C4 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C2 C3 H3A 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
H8C O8 H8D 109.5 . . ?
H9A O9 H9B 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7A O3 0.85 1.94 2.700(4) 148.3 7_656 yes
O8 H8D O9 0.85 2.04 2.645(17) 127.7 . yes

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT417_kasm-c3b            
;
PROBLEM: Short Inter D-H..H-D       H8C      ..H8C      .       1.89 Ang.  
RESPONSE:X-ray data was not of sufficient quality to refine proton positions.The
geometrically estimated positions using the riding model. In a number of instanc to be correct,
in particular, for disordered solvent molecules
;
_vrf_PLAT420_kasm-c3b            
;
PROBLEM: D-H Without Acceptor       O7       --H7B      .     Please Check 
RESPONSE:X-ray data was not of sufficient quality to refine proton positions.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1866431'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-08-01 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H22 O14 Sm2, 4(H2 O)'
_chemical_formula_sum            'C15 H30 O18 Sm2'
_chemical_formula_weight         799.11

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   8.0028(5)
_cell_length_b                   15.0146(9)
_cell_length_c                   19.6729(12)
_cell_angle_alpha                90
_cell_angle_beta                 93.991(2)
_cell_angle_gamma                90
_cell_volume                     2358.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9163
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      28.35

_exptl_crystal_description       Needles
_exptl_crystal_colour            Colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.251
_exptl_crystal_F_000             1552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_exptl_absorpt_coefficient_mu    5.017
_shelx_estimated_absorpt_T_min   0.648
_shelx_estimated_absorpt_T_max   0.717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_T_max  0.434
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37693
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.1573
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.890
_diffrn_reflns_theta_max         28.368
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2958
_reflns_number_gt                2789
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0140P)²+8.4075P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2958
_refine_ls_number_parameters     177
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0694
_refine_ls_wR_factor_gt          0.0683
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_restrained_S_all      1.154
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3818(4) 0.42642(19) 0.60103(16) 0.0162(6) Uani 1 1 d . . . . .
C2 C 0.4295(5) 0.3596(2) 0.65602(17) 0.0200(6) Uani 1 1 d . . . . .
H2A H 0.385129 0.378159 0.698411 0.024 Uiso 1 1 calc R U . . .
H2B H 0.550552 0.356493 0.663134 0.024 Uiso 1 1 calc R U . . .
C3 C 0.3596(5) 0.2671(2) 0.6356(2) 0.0269(8) Uani 1 1 d . . . . .
H3A H 0.369892 0.228032 0.674929 0.032 Uiso 1 1 calc R U . . .
H3B H 0.241476 0.272561 0.621475 0.032 Uiso 1 1 calc R U . . .
C4 C 0.4500(5) 0.2255(2) 0.5781(2) 0.0284(8) Uani 1 1 d . . . . .
H4A H 0.440122 0.265087 0.539076 0.034 Uiso 1 1 calc R U . . .
H4B H 0.568053 0.220392 0.592463 0.034 Uiso 1 1 calc R U . . .
C5 C 0.3852(4) 0.13538(19) 0.55656(17) 0.0177(6) Uani 1 1 d . . . . .
C6 C 0.8676(4) 0.3627(2) 0.62906(17) 0.0185(6) Uani 1 1 d . . . . .
C7 C 0.9268(5) 0.3095(2) 0.69134(17) 0.0220(7) Uani 1 1 d . . . . .
H7A H 1.011026 0.267290 0.678749 0.026 Uiso 1 1 calc R U . . .
H7B H 0.833134 0.275755 0.706669 0.026 Uiso 1 1 calc R U . . .
C8 C 1.000000 0.3663(3) 0.750000 0.0277(11) Uani 1 2 d S T P . .
H8A H 1.086997 0.404279 0.733926 0.033 Uiso 0.5 1 calc R U P . .
H8B H 0.913003 0.404279 0.766074 0.033 Uiso 0.5 1 calc R U P . .
O1 O 0.4886(4) 0.45503(15) 0.56131(14) 0.0223(5) Uani 1 1 d . . . . .
O2 O 0.2330(4) 0.45125(18) 0.59325(16) 0.0300(6) Uani 1 1 d . . . . .
O1W O 0.6155(4) 0.35327(17) 0.43876(16) 0.0291(6) Uani 1 1 d D . . . .
H11W H 0.631(5) 0.3006(15) 0.432(2) 0.035 Uiso 1 1 d D U . . .
H12W H 0.516(3) 0.361(3) 0.428(3) 0.035 Uiso 1 1 d D U . . .
O3 O 0.4861(3) 0.07920(15) 0.53392(13) 0.0214(5) Uani 1 1 d . . . . .
O2W O 1.1032(18) 0.5918(4) 0.7009(4) 0.193(5) Uani 1 1 d D . . . .
H21W H 1.165(15) 0.632(6) 0.692(7) 0.232 Uiso 1 1 d D U . . .
H22W H 1.12(2) 0.554(7) 0.672(6) 0.232 Uiso 1 1 d D U . . .
O4 O 0.2323(3) 0.11519(16) 0.55924(15) 0.0256(5) Uani 1 1 d . . . . .
O3W O 1.3819(18) 0.5710(9) 0.7839(8) 0.225(6) Uani 1 1 d D . . . .
H31W H 1.36(2) 0.520(5) 0.794(10) 0.270 Uiso 1 1 d D U . . .
H32W H 1.306(18) 0.586(11) 0.757(10) 0.270 Uiso 1 1 d D U . . .
O5 O 0.8483(4) 0.44573(16) 0.63227(14) 0.0256(6) Uani 1 1 d . . . . .
O6 O 0.8325(3) 0.32242(16) 0.57289(13) 0.0234(5) Uani 1 1 d . . . . .
Sm1 Sm 0.75497(2) 0.46270(2) 0.51198(2) 0.01427(7) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O2 1.247(4) . ?
C1 O1 1.272(4) . ?
C1 C2 1.505(4) . ?
C1 Sm1 2.928(3) 5_666 ?
C2 C3 1.540(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.518(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.500(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 O4 1.266(4) . ?
C5 O3 1.269(4) . ?
C5 Sm1 2.907(3) 3_445 ?
C6 O5 1.259(4) . ?
C6 O6 1.274(4) . ?
C6 C7 1.511(4) . ?
C6 Sm1 2.843(3) . ?
C7 C8 1.519(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
O1 Sm1 2.406(3) . ?
O1 Sm1 2.648(3) 5_666 ?
O2 Sm1 2.448(3) 5_666 ?
O1W Sm1 2.408(2) . ?
O1W H11W 0.813(18) . ?
O1W H12W 0.816(18) . ?
O3 Sm1 2.401(2) 7_656 ?
O3 Sm1 2.560(2) 3_445 ?
O2W H21W 0.81(11) . ?
O2W H22W 0.82(11) . ?
O4 Sm1 2.483(2) 3_445 ?
O3W H31W 0.81(10) . ?
O3W H32W 0.81(16) . ?
O5 Sm1 2.445(3) . ?
O6 Sm1 2.481(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 C1 O1 120.0(3) . . ?
O2 C1 C2 118.7(3) . . ?
O1 C1 C2 121.3(3) . . ?
O2 C1 Sm1 55.49(18) . 5_666 ?
O1 C1 Sm1 64.73(18) . 5_666 ?
C2 C1 Sm1 170.9(2) . 5_666 ?
C1 C2 C3 110.1(3) . . ?
C1 C2 H2A 109.6 . . ?
C3 C2 H2A 109.6 . . ?
C1 C2 H2B 109.6 . . ?
C3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C4 C3 C2 112.4(3) . . ?
C4 C3 H3A 109.1 . . ?
C2 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
C2 C3 H3B 109.1 . . ?
H3A C3 H3B 107.8 . . ?
C5 C4 C3 114.1(3) . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
O4 C5 O3 119.7(3) . . ?
O4 C5 C4 121.4(3) . . ?
O3 C5 C4 118.9(3) . . ?
O4 C5 Sm1 58.09(16) . 3_445 ?
O3 C5 Sm1 61.63(16) . 3_445 ?
C4 C5 Sm1 178.6(3) . 3_445 ?
O5 C6 O6 119.6(3) . . ?
O5 C6 C7 121.0(3) . . ?
O6 C6 C7 119.4(3) . . ?
O5 C6 Sm1 58.95(18) . . ?
O6 C6 Sm1 60.63(17) . . ?
C7 C6 Sm1 179.8(3) . . ?
C6 C7 C8 113.7(3) . . ?
C6 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C7 C8 C7 111.7(4) 2_756 . ?
C7 C8 H8A 109.3 2_756 . ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 2_756 . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
C1 O1 Sm1 156.3(2) . . ?
C1 O1 Sm1 89.5(2) . 5_666 ?
Sm1 O1 Sm1 113.41(10) . 5_666 ?
C1 O2 Sm1 99.7(2) . 5_666 ?
Sm1 O1W H11W 134(3) . . ?
Sm1 O1W H12W 117(3) . . ?
H11W O1W H12W 105(3) . . ?
C5 O3 Sm1 153.2(2) . 7_656 ?
C5 O3 Sm1 92.51(19) . 3_445 ?
Sm1 O3 Sm1 112.94(9) 7_656 3_445 ?
H21W O2W H22W 104(13) . . ?
C5 O4 Sm1 96.27(19) . 3_445 ?
H31W O3W H32W 105(16) . . ?
C6 O5 Sm1 94.9(2) . . ?
C6 O6 Sm1 92.80(19) . . ?
O3 Sm1 O1 162.05(8) 7_656 . ?
O3 Sm1 O1W 88.43(9) 7_656 . ?
O1 Sm1 O1W 79.73(10) . . ?
O3 Sm1 O5 97.08(10) 7_656 . ?
O1 Sm1 O5 79.86(10) . . ?
O1W Sm1 O5 127.27(9) . . ?
O3 Sm1 O2 74.61(9) 7_656 5_666 ?
O1 Sm1 O2 117.03(9) . 5_666 ?
O1W Sm1 O2 84.15(11) . 5_666 ?
O5 Sm1 O2 147.82(10) . 5_666 ?
O3 Sm1 O6 76.46(9) 7_656 . ?
O1 Sm1 O6 87.89(9) . . ?
O1W Sm1 O6 78.43(9) . . ?
O5 Sm1 O6 52.74(8) . . ?
O2 Sm1 O6 146.46(9) 5_666 . ?
O3 Sm1 O4 118.03(8) 7_656 3 ?
O1 Sm1 O4 78.64(8) . 3 ?
O1W Sm1 O4 144.15(9) . 3 ?
O5 Sm1 O4 76.05(9) . 3 ?
O2 Sm1 O4 80.69(10) 5_666 3 ?
O6 Sm1 O4 128.64(9) . 3 ?
O3 Sm1 O3 67.06(9) 7_656 3 ?
O1 Sm1 O3 127.93(8) . 3 ?
O1W Sm1 O3 150.05(10) . 3 ?
O5 Sm1 O3 74.91(9) . 3 ?
O2 Sm1 O3 73.24(10) 5_666 3 ?
O6 Sm1 O3 110.20(8) . 3 ?
O4 Sm1 O3 51.51(8) 3 3 ?
O3 Sm1 O1 122.63(9) 7_656 5_666 ?
O1 Sm1 O1 66.59(10) . 5_666 ?
O1W Sm1 O1 72.51(8) . 5_666 ?
O5 Sm1 O1 137.67(9) . 5_666 ?
O2 Sm1 O1 50.51(9) 5_666 5_666 ?
O6 Sm1 O1 143.99(8) . 5_666 ?
O4 Sm1 O1 72.75(8) 3 5_666 ?
O3 Sm1 O1 105.59(8) 3 5_666 ?
O3 Sm1 C6 86.16(9) 7_656 . ?
O1 Sm1 C6 83.55(9) . . ?
O1W Sm1 C6 103.40(10) . . ?
O5 Sm1 C6 26.18(9) . . ?
O2 Sm1 C6 159.24(10) 5_666 . ?
O6 Sm1 C6 26.58(8) . . ?
O4 Sm1 C6 102.18(9) 3 . ?
O3 Sm1 C6 92.28(9) 3 . ?
O1 Sm1 C6 150.14(9) 5_666 . ?
O3 Sm1 C5 92.66(9) 7_656 3 ?
O1 Sm1 C5 103.31(9) . 3 ?
O1W Sm1 C5 158.55(9) . 3 ?
O5 Sm1 C5 73.86(9) . 3 ?
O2 Sm1 C5 75.53(10) 5_666 3 ?
O6 Sm1 C5 122.63(9) . 3 ?
O4 Sm1 C5 25.65(9) 3 3 ?
O3 Sm1 C5 25.86(8) 3 3 ?
O1 Sm1 C5 89.03(8) 5_666 3 ?
C6 Sm1 C5 98.05(9) . 3 ?
O3 Sm1 C1 98.64(9) 7_656 5_666 ?
O1 Sm1 C1 92.21(9) . 5_666 ?
O1W Sm1 C1 78.49(9) . 5_666 ?
O5 Sm1 C1 150.12(8) . 5_666 ?
O2 Sm1 C1 24.82(9) 5_666 5_666 ?
O6 Sm1 C1 156.53(8) . 5_666 ?
O4 Sm1 C1 74.14(9) 3 5_666 ?
O3 Sm1 C1 88.11(8) 3 5_666 ?
O1 Sm1 C1 25.75(9) 5_666 5_666 ?
C6 Sm1 C1 174.92(9) . 5_666 ?
C5 Sm1 C1 80.17(9) 3 5_666 ?

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
O2 C1 C2 C3 72.0(4) . . . . ?
O1 C1 C2 C3 -105.4(4) . . . . ?
C1 C2 C3 C4 71.0(4) . . . . ?
C2 C3 C4 C5 -179.8(3) . . . . ?
C3 C4 C5 O4 32.5(5) . . . . ?
C3 C4 C5 O3 -149.0(3) . . . . ?
O5 C6 C7 C8 -14.6(5) . . . . ?
O6 C6 C7 C8 167.3(3) . . . . ?
C6 C7 C8 C7 -174.4(4) . . . 2_756 ?
O2 C1 O1 Sm1 -171.2(4) . . . . ?
C2 C1 O1 Sm1 6.2(7) . . . . ?
Sm1 C1 O1 Sm1 -166.1(6) 5_666 . . . ?
O2 C1 O1 Sm1 -5.1(3) . . . 5_666 ?
C2 C1 O1 Sm1 172.3(3) . . . 5_666 ?
O1 C1 O2 Sm1 5.6(4) . . . 5_666 ?
C2 C1 O2 Sm1 -171.8(2) . . . 5_666 ?
O4 C5 O3 Sm1 162.1(4) . . . 7_656 ?
C4 C5 O3 Sm1 -16.5(7) . . . 7_656 ?
Sm1 C5 O3 Sm1 162.1(5) 3_445 . . 7_656 ?
O4 C5 O3 Sm1 0.1(3) . . . 3_445 ?
C4 C5 O3 Sm1 -178.5(3) . . . 3_445 ?
O3 C5 O4 Sm1 -0.1(3) . . . 3_445 ?
C4 C5 O4 Sm1 178.5(3) . . . 3_445 ?
O6 C6 O5 Sm1 -1.6(4) . . . . ?
C7 C6 O5 Sm1 -179.8(3) . . . . ?
O5 C6 O6 Sm1 1.6(4) . . . . ?
C7 C6 O6 Sm1 179.8(3) . . . . ?

_refine_diff_density_max         0.955
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.225

# start Validation Reply Form
_vrf_PLAT417_shelxl              
;
RESPONSE: This Alert is due to the presence of
disorder in the lattice water molecules.
;
_vrf_PLAT420_shelxl              
;
RESPONSE: This Alert is due to the presence of
disorder in the lattice water molecules.
;
# end Validation Reply Form




_vrf_PLAT417_shelx               
;
PROBLEM: Short Inter D-H..H-D       H21W     ..H32W     .       1.80 Ang.  
RESPONSE:X-ray data was not of sufficient quality to refine proton positions. Therefore proton atoms 
were placed in geometrically estimated positions using the riding model. In a number of instances the estimated positions 
are unlikely to be correct, in particular, for disordered solvent molecules.  
;
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor       O2W      --H21W     .     Please Check 
RESPONSE:X-ray data was not of sufficient quality to refine proton positions. H2O molecules were therefore refined without riding proton atoms. 
;
# end Validation Reply Form
####################################################################### 
# 
# 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_sub-kasm-C4
_database_code_depnum_ccdc_archive 'CCDC 1921926'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-01-22
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_chemical_formula_moiety         'C15 H22 Eu2 O14 [+ solvent]'
_chemical_formula_sum            'C15 H22 Eu2 O14'
_chemical_formula_weight         730.26
_chemical_absolute_configuration ?
_chemical_compound_source        synthesized
_chemical_oxdiff_formula         'Eu C H N O'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Eu -0.00847 3.77655 24.62740 19.08860 13.76030 2.92270 2.38790 0.19420 13.75460
123.17400 2.57450008392
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z+1/2
3 -x,-y,-z
4 x,-y,z-1/2
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z+1/2
7 -x+1/2,-y+1/2,-z
8 x+1/2,-y+1/2,z-1/2

_cell_length_a                   7.9832(1)
_cell_length_b                   15.0012(3)
_cell_length_c                   19.6694(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.119(2)
_cell_angle_gamma                90
_cell_volume                     2349.48(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13821
_cell_measurement_temperature    293
_cell_measurement_theta_max      27.3200
_cell_measurement_theta_min      3.4410
_exptl_absorpt_coefficient_mu    5.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48220
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.0643
_exptl_crystal_description       block
_exptl_crystal_F_000             1400.8264
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15063
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         3.14
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00 -16.00   0.50   12.00    --   -9.95 121.00  51.00   80
  2  ω    -47.00 -22.00   0.50   12.00    --   -9.95 153.00-149.00   50
  3  ω     23.00  48.00   0.50   12.00    --   10.22-153.00 169.00   50
  4  ω     20.00  47.00   0.50   12.00    --   10.22-121.00 -30.00   54
  5  ω    -22.00   4.00   0.50   12.00    --   -9.95  38.00  60.00   52
  6  ω    -58.00 -33.00   0.50   12.00    --   -9.95 125.00  90.00   50
  7  ω    -21.00  60.00   0.50   12.00    --   -9.95  19.00-150.00  162
  8  ω     18.00  43.00   0.50   12.00    --   -9.95  38.00  60.00   50
  9  ω    -14.00  54.00   0.50   12.00    --   -9.95  38.00 -60.00  136
 10  ω    -79.00 -46.00   0.50   12.00    --   -9.95 -19.00-150.00   66
 11  ω    -19.00  41.00   0.50   12.00    --   10.22 -99.00   0.00  120
 12  ω    -33.00   2.00   0.50   12.00    --   10.22 119.00  -1.06   70
 13  ω    -24.00   4.00   0.50   12.00    --   10.22 117.00-133.72   56
 14  ω    -52.00  23.00   0.50   12.00    --   10.22 -38.00  90.00  150
 15  ω     19.00  45.00   0.50   12.00    --   10.22-125.00-120.00   52
 16  ω     -8.00  43.00   0.50   12.00    --   10.22 -99.00-120.00  102
 17  ω    -31.00  -6.00   0.50   12.00    --   10.22 126.00  65.85   50
 18  ω     40.00  66.00   0.50   12.00    --   10.22  38.00-180.00   52
 19  ω     21.00  46.00   0.50   12.00    --   10.22  57.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0200027000
_diffrn_orient_matrix_UB_12      -0.0010015000
_diffrn_orient_matrix_UB_13      0.0357136000
_diffrn_orient_matrix_UB_21      -0.0752490000
_diffrn_orient_matrix_UB_22      -0.0237790000
_diffrn_orient_matrix_UB_23      0.0044244000
_diffrn_orient_matrix_UB_31      0.0432769000
_diffrn_orient_matrix_UB_32      -0.0408606000
_diffrn_orient_matrix_UB_33      -0.0034484000
_diffrn_oxdiff_ac3_digest_frames 
;
0161ad9c2442a51d4bef8614a8591745f90002536d3
;
_diffrn_oxdiff_ac3_digest_hkl    
;
012459c268292a67d7f8f49757fa3e60c95be9
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                2494
_reflns_number_total             2556
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.3711
_refine_diff_density_min         -2.2040
_refine_diff_density_rms         0.2580
_refine_ls_d_res_high            0.7723
_refine_ls_d_res_low             6.4911
_refine_ls_goodness_of_fit_ref   1.0090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2556
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.0090
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0271P)²+100.1241P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0955
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H8a(0.5) H8b(0.5)
3.a Rotating group:
 O7(H7a,H7b)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2a,H2b), C4(H4a,H4b), C7(H7c,H7d), C8(H8a,H8b), C3(H3a,H3b)
;
_atom_sites_solution_primary     dual
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_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Eu1 Eu 0.75528(4) 0.53722(2) 0.511975(16) 0.01241(11) Uani 1.000000 1 . . .
O1 O 0.4897(6) 0.5443(3) 0.5612(3) 0.0196(10) Uani 1.000000 1 . . .
O3 O 0.4866(6) 0.9204(3) 0.5333(3) 0.0190(10) Uani 1.000000 1 . . .
O6 O 0.8498(7) 0.5540(3) 0.6320(3) 0.0239(11) Uani 1.000000 1 . . .
O5 O 0.8333(6) 0.6775(3) 0.5726(2) 0.0200(10) Uani 1.000000 1 . . .
O2 O 0.2332(6) 0.5476(4) 0.5927(3) 0.0270(12) Uani 1.000000 1 . . .
O7 O 0.6139(7) 0.6463(3) 0.4393(3) 0.0261(11) Uani 1.000000 1 . . .
H7a H 0.572(8) 0.6214(9) 0.4024(16) 0.0391(17) Uiso 1.000000 1 GR . .
H7b H 0.684(2) 0.687(3) 0.429(3) 0.0391(17) Uiso 1.000000 1 GR . .
O4 O 0.2328(6) 0.8853(3) 0.5588(3) 0.0228(11) Uani 1.000000 1 . . .
C1 C 0.3828(8) 0.5733(4) 0.6015(3) 0.0145(12) Uani 1.000000 1 . . .
C5 C 0.3853(9) 0.8646(4) 0.5562(3) 0.0169(13) Uani 1.000000 1 . . .
C6 C 0.8690(8) 0.6373(4) 0.6290(3) 0.0156(12) Uani 1.000000 1 . . .
C2 C 0.4296(9) 0.6403(4) 0.6559(3) 0.0180(13) Uani 1.000000 1 . . .
H2a H 0.3845(9) 0.6221(4) 0.6982(3) 0.0216(16) Uiso 1.000000 1 R . .
H2b H 0.5509(9) 0.6433(4) 0.6634(3) 0.0216(16) Uiso 1.000000 1 R . .
C4 C 0.4493(10) 0.7746(5) 0.5775(4) 0.0256(16) Uani 1.000000 1 . . .
H4a H 0.4383(10) 0.7352(5) 0.5383(4) 0.0307(19) Uiso 1.000000 1 R . .
H4b H 0.5679(10) 0.7795(5) 0.5915(4) 0.0307(19) Uiso 1.000000 1 R . .
C7 C 0.9256(9) 0.6908(5) 0.6913(3) 0.0192(13) Uani 1.000000 1 . . .
H7c H 1.0093(9) 0.7337(5) 0.6791(3) 0.0230(16) Uiso 1.000000 1 R . .
H7d H 0.8306(9) 0.7237(5) 0.7064(3) 0.0230(16) Uiso 1.000000 1 R . .
C8 C 1.0 0.6330(7) 0.75 0.023(2) Uani 1.000000 2 S T P
H8a H 0.912976453499 0.5950(7) 0.766213111138 0.028(3) Uiso 0.500000 1 R . .
H8b H 1.0870235465 0.5950(7) 0.733786888862 0.028(3) Uiso 0.500000 1 R . .
C3 C 0.3602(10) 0.7327(5) 0.6351(4) 0.0257(16) Uani 1.000000 1 . . .
H3a H 0.2416(10) 0.7272(5) 0.6211(4) 0.0308(19) Uiso 1.000000 1 R . .
H3b H 0.3709(10) 0.7719(5) 0.6744(4) 0.0308(19) Uiso 1.000000 1 R . .


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 2.395(5) . ?
Eu1 O1 2.642(5) 3_666 ?
Eu1 O3 2.559(5) 5_545 ?
Eu1 O3 2.390(4) 7_666 ?
Eu1 O6 2.440(5) . ?
Eu1 O5 2.477(5) . ?
Eu1 O2 2.429(5) 3_666 ?
Eu1 O7 2.400(5) . ?
Eu1 O4 2.469(5) 5_545 ?
Eu1 C1 2.932(6) 3_666 ?
Eu1 C5 2.900(7) 5_545 ?
Eu1 C6 2.841(6) . ?
O1 C1 1.283(8) . ?
O3 C5 1.268(8) . ?
O6 C6 1.261(8) . ?
O5 C6 1.275(8) . ?
O2 C1 1.255(8) . ?
O7 H7a 0.8618 . ?
O7 H7b 0.8612 . ?
O4 C5 1.262(8) . ?
C1 C2 1.495(9) . ?
C5 C4 1.492(9) . ?
C6 C7 1.507(9) . ?
C2 H2a 0.9700 . ?
C2 H2b 0.9700 . ?
C2 C3 1.537(9) . ?
C4 H4a 0.9700 . ?
C4 H4b 0.9700 . ?
C4 C3 1.516(10) . ?
C7 H7c 0.9700 . ?
C7 H7d 0.9700 . ?
C7 C8 1.530(8) . ?
C8 H8a 0.9700 . ?
C8 H8a 0.9700 2_756 ?
C8 H8b 0.9700 2_756 ?
C8 H8b 0.9700 . ?
H8a H8b 0.0000 2_756 ?
C3 H3a 0.9700 . ?
C3 H3b 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
O3 Eu1 O1 162.00(16) 7_666 . ?
O3 Eu1 O1 122.99(16) 7_666 3_666 ?
O3 Eu1 O1 127.82(16) 5_545 . ?
O3 Eu1 O1 105.63(15) 5_545 3_666 ?
O6 Eu1 O1 79.98(18) . . ?
O6 Eu1 O1 137.73(16) . 3_666 ?
O6 Eu1 O3 96.79(18) . 7_666 ?
O6 Eu1 O3 75.07(17) . 5_545 ?
O5 Eu1 O1 88.13(17) . . ?
O5 Eu1 O1 143.71(15) . 3_666 ?
O5 Eu1 O3 76.08(16) . 7_666 ?
O5 Eu1 O3 110.46(16) . 5_545 ?
O5 Eu1 O6 52.88(16) . . ?
O2 Eu1 O1 117.01(17) 3_666 . ?
O2 Eu1 O1 50.78(15) 3_666 3_666 ?
O2 Eu1 O3 74.75(17) 3_666 7_666 ?
O2 Eu1 O3 73.10(18) 3_666 5_545 ?
O2 Eu1 O6 147.88(19) 3_666 . ?
O2 Eu1 O5 146.13(17) 3_666 . ?
O7 Eu1 O1 79.54(18) . . ?
O7 Eu1 O1 72.13(16) . 3_666 ?
O7 Eu1 O3 88.72(17) . 7_666 ?
O7 Eu1 O3 150.18(18) . 5_545 ?
O7 Eu1 O6 127.27(18) . . ?
O7 Eu1 O5 78.41(16) . . ?
O7 Eu1 O2 84.09(19) . 3_666 ?
O4 Eu1 O1 78.45(16) 5_545 . ?
O4 Eu1 O1 72.87(16) 5_545 3_666 ?
O4 Eu1 O3 118.20(15) 5_545 7_666 ?
O4 Eu1 O3 51.50(15) 5_545 5_545 ?
O4 Eu1 O6 76.10(17) 5_545 . ?
O4 Eu1 O5 128.82(17) 5_545 . ?
O4 Eu1 O2 80.85(19) 5_545 3_666 ?
O4 Eu1 O7 143.85(17) 5_545 . ?
C1 Eu1 O1 92.13(17) 3_666 . ?
C1 Eu1 O1 25.95(16) 3_666 3_666 ?
C1 Eu1 O3 98.84(17) 3_666 7_666 ?
C1 Eu1 O3 87.99(17) 3_666 5_545 ?
C1 Eu1 O6 150.30(17) 3_666 . ?
C1 Eu1 O5 156.24(16) 3_666 . ?
C1 Eu1 O2 24.88(17) 3_666 3_666 ?
C1 Eu1 O7 78.29(18) 3_666 . ?
C1 Eu1 O4 74.27(18) 3_666 5_545 ?
C5 Eu1 O1 103.09(17) 5_545 . ?
C5 Eu1 O1 89.14(17) 5_545 3_666 ?
C5 Eu1 O3 92.85(17) 5_545 7_666 ?
C5 Eu1 O3 25.90(17) 5_545 5_545 ?
C5 Eu1 O6 73.91(17) 5_545 . ?
C5 Eu1 O5 122.83(17) 5_545 . ?
C5 Eu1 O2 75.62(19) 5_545 3_666 ?
C5 Eu1 O7 158.43(19) 5_545 . ?
C5 Eu1 O4 25.60(17) 5_545 5_545 ?
C5 Eu1 C1 80.22(18) 5_545 3_666 ?
C6 Eu1 O1 83.70(17) . . ?
C6 Eu1 O1 150.02(16) . 3_666 ?
C6 Eu1 O3 85.83(18) . 7_666 ?
C6 Eu1 O3 92.54(17) . 5_545 ?
C6 Eu1 O6 26.24(18) . . ?
C6 Eu1 O5 26.64(17) . . ?
C6 Eu1 O2 159.13(17) . 3_666 ?
C6 Eu1 O7 103.38(18) . . ?
C6 Eu1 O4 102.30(19) . 5_545 ?
C6 Eu1 C1 175.11(18) . 3_666 ?
C6 Eu1 C5 98.19(19) . 5_545 ?
C1 O1 Eu1 155.8(4) . . ?
C1 O1 Eu1 89.7(4) . 3_666 ?
C5 O3 Eu1 153.7(4) . 7_666 ?
C5 O3 Eu1 92.3(4) . 5_455 ?
C6 O6 Eu1 94.9(4) . . ?
C6 O5 Eu1 92.8(4) . . ?
C1 O2 Eu1 100.6(4) . 3_666 ?
H7a O7 Eu1 110.1 . . ?
H7b O7 Eu1 109.7 . . ?
H7b O7 H7a 108.8 . . ?
C5 O4 Eu1 96.7(4) . 5_455 ?
O1 C1 Eu1 64.3(3) . 3_666 ?
O2 C1 Eu1 54.5(3) . 3_666 ?
O2 C1 O1 118.6(6) . . ?
C2 C1 Eu1 170.3(5) . 3_666 ?
C2 C1 O1 121.9(6) . . ?
C2 C1 O2 119.4(6) . . ?
O3 C5 Eu1 61.8(3) . 5_455 ?
O4 C5 Eu1 57.7(3) . 5_455 ?
O4 C5 O3 119.6(6) . . ?
C4 C5 Eu1 178.5(5) . 5_455 ?
C4 C5 O3 118.9(6) . . ?
C4 C5 O4 121.5(6) . . ?
O6 C6 Eu1 58.8(4) . . ?
O5 C6 Eu1 60.5(3) . . ?
O5 C6 O6 119.3(6) . . ?
C7 C6 Eu1 178.8(5) . . ?
C7 C6 O6 121.3(6) . . ?
C7 C6 O5 119.3(6) . . ?
H2a C2 C1 109.6(4) . . ?
H2b C2 C1 109.6(4) . . ?
H2b C2 H2a 108.1 . . ?
C3 C2 C1 110.4(6) . . ?
C3 C2 H2a 109.6(4) . . ?
C3 C2 H2b 109.6(4) . . ?
H4a C4 C5 108.6(4) . . ?
H4b C4 C5 108.6(4) . . ?
H4b C4 H4a 107.6 . . ?
C3 C4 C5 114.6(6) . . ?
C3 C4 H4a 108.6(4) . . ?
C3 C4 H4b 108.6(5) . . ?
H7c C7 C6 109.0(4) . . ?
H7d C7 C6 109.0(4) . . ?
H7d C7 H7c 107.8 . . ?
C8 C7 C6 112.9(6) . . ?
C8 C7 H7c 109.0(3) . . ?
C8 C7 H7d 109.0(3) . . ?
C7 C8 C7 110.9(8) 2_756 . ?
H8a C8 C7 109.5(3) 2_756 . ?
H8a C8 C7 109.5(3) . . ?
H8a C8 C7 109.5(3) . 2_756 ?
H8a C8 C7 109.5(3) 2_756 2_756 ?
H8a C8 H8a 108.0 2_756 . ?
H8b C8 C7 109.5(3) 2_756 2_756 ?
H8b C8 C7 109.5(3) 2_756 . ?
H8b C8 C7 109.5(3) . 2_756 ?
H8b C8 C7 109.5(3) . . ?
H8b C8 H8a 0.0 2_756 . ?
H8b C8 H8a 0.0 . 2_756 ?
H8b C8 H8a 108.0 2_756 2_756 ?
H8b C8 H8a 108.0 . . ?
H8b C8 H8b 108.0 . 2_756 ?
H8b H8a C8 0(50000) 2_756 . ?
H8a H8b C8 0(2100000) 2_756 2_756 ?
C4 C3 C2 113.2(6) . . ?
H3a C3 C2 108.9(4) . . ?
H3a C3 C4 108.9(5) . . ?
H3b C3 C2 108.9(4) . . ?
H3b C3 C4 108.9(4) . . ?
H3b C3 H3a 107.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O7 H7b O5 0.8612 2.04(4) 2.690(7) 131(4) 7_666

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.518 0.086 0.250 117.6 55.3 '1 water'
2 -0.320 -0.086 0.750 117.6 55.4 '1 water'
3 -0.521 0.414 0.750 117.6 55.4 '1 water'
4 -0.955 0.586 0.250 117.6 55.3 '1 water'


_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 1.651
_oxdiff_exptl_absorpt_empirical_full_min 0.655
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1866435'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-08-01 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-04-10
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H26 Gd2 O16'
_chemical_formula_sum            'C15 H26 Gd2 O16'
_chemical_formula_weight         776.86
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   8.7718(7)
_cell_length_b                   14.1478(11)
_cell_length_c                   23.0016(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2854.5(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9375
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      2.28
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.667
_exptl_absorpt_correction_T_max  0.476
_exptl_absorpt_correction_T_min  0.309
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.808
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Needles
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1163
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.97
_diffrn_reflns_Laue_measured_fraction_max 0.650
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            18614
_diffrn_reflns_point_group_measured_fraction_full 0.97
_diffrn_reflns_point_group_measured_fraction_max 0.573
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.504
_diffrn_reflns_theta_min         2.282
_diffrn_ambient_temperature      297.25
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.97
_diffrn_measured_fraction_theta_max 0.650
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.582
_reflns_Friedel_fraction_full    0.774
_reflns_Friedel_fraction_max     0.476
_reflns_number_gt                4309
_reflns_number_total             5172
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         3.953
_refine_diff_density_min         -1.778
_refine_diff_density_rms         0.225
_refine_ls_abs_structure_details 
;
 Flack x determined using 1320 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.54(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0545
_refine_ls_restrained_S_all      1.052
_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)+(0.0946P)²+1.5854P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1526
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O2W(H2WA,H2WB)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0411(17) 0.1636(13) 0.2977(6) 0.031(4) Uani 1 1 d . . . . .
C2 C 0.9379(17) 0.1613(12) 0.3500(6) 0.029(3) Uiso 1 1 d . . . . .
H2A H 0.909169 0.224908 0.361417 0.035 Uiso 1 1 calc R . . . .
H2B H 0.988191 0.130871 0.382550 0.035 Uiso 1 1 calc R . . . .
C3 C 0.7940(18) 0.1034(13) 0.3307(6) 0.035(4) Uani 1 1 d . . . . .
H3A H 0.738897 0.138346 0.301108 0.041 Uiso 1 1 calc R . . . .
H3B H 0.826211 0.043750 0.313894 0.041 Uiso 1 1 calc R . . . .
C4 C 0.6887(17) 0.0844(13) 0.3821(6) 0.034(4) Uani 1 1 d . . . . .
H4A H 0.739322 0.043376 0.409862 0.041 Uiso 1 1 calc R . . . .
H4B H 0.664458 0.143403 0.401538 0.041 Uiso 1 1 calc R . . . .
C5 C 0.5465(18) 0.0389(12) 0.3612(5) 0.028(4) Uani 1 1 d . . . . .
C6 C -0.0447(17) 0.0904(13) 0.1445(5) 0.035(4) Uani 1 1 d . . . . .
C7 C -0.196(2) 0.0432(16) 0.1221(7) 0.052(5) Uani 1 1 d . . . . .
H7A H -0.248409 0.086550 0.096179 0.062 Uiso 1 1 calc R . . . .
H7B H -0.171459 -0.013407 0.100221 0.062 Uiso 1 1 calc R . . . .
C8 C -0.2999(18) 0.0178(14) 0.1720(5) 0.041(5) Uani 1 1 d . . . . .
H8A H -0.245161 -0.023653 0.198341 0.049 Uiso 1 1 calc R . . . .
H8B H -0.324728 0.075058 0.193269 0.049 Uiso 1 1 calc R . . . .
C9 C -0.4405(18) -0.0281(13) 0.1548(6) 0.031(3) Uiso 1 1 d . . . . .
H9A H -0.417398 -0.090037 0.139110 0.038 Uiso 1 1 calc R . . . .
H9B H -0.488942 0.008745 0.124435 0.038 Uiso 1 1 calc R . . . .
C10 C 0.4520(17) -0.0384(13) 0.2047(6) 0.029(3) Uani 1 1 d . . . . .
C11 C 0.407(2) 0.1914(15) 0.0895(7) 0.044(5) Uani 1 1 d . . . . .
C12 C 0.490(2) 0.2296(15) 0.0400(6) 0.046(5) Uani 1 1 d . . . . .
H12A H 0.597297 0.215535 0.045149 0.056 Uiso 1 1 calc R . . . .
H12B H 0.478835 0.297786 0.040132 0.056 Uiso 1 1 calc R . . . .
C13 C 0.442(3) 0.1935(15) -0.0176(6) 0.059(6) Uani 1 1 d . . . . .
H13A H 0.488027 0.231451 -0.047887 0.071 Uiso 1 1 calc R . . . .
H13B H 0.331735 0.199373 -0.021186 0.071 Uiso 1 1 calc R . . . .
C14 C 0.013(2) -0.0895(16) 0.4742(8) 0.055(6) Uani 1 1 d . . . . .
H14A H 0.049681 -0.050653 0.505914 0.066 Uiso 1 1 calc R . . . .
H14B H -0.097120 -0.082786 0.471308 0.066 Uiso 1 1 calc R . . . .
C15 C 0.097(2) -0.0610(15) 0.4118(7) 0.045(5) Uani 1 1 d . . . . .
O1 O 0.1340(12) 0.0968(8) 0.2872(4) 0.027(2) Uiso 1 1 d . . . . .
O2 O 0.0391(14) 0.2348(10) 0.2631(4) 0.039(3) Uani 1 1 d . . . . .
O1W O 0.3864(14) 0.2311(9) 0.2664(5) 0.041(3) Uani 1 1 d . . . . .
H1WA H 0.432425 0.280773 0.254454 0.061 Uiso 1 1 d GR . . . .
H1WB H 0.452689 0.189356 0.275869 0.061 Uiso 1 1 d GR . . . .
O3 O 0.4402(15) 0.0893(9) 0.3415(5) 0.043(3) Uani 1 1 d . . . . .
O4 O 0.5307(14) -0.0509(11) 0.3606(6) 0.048(4) Uani 1 1 d . . . . .
O3W O 0.1122(15) -0.1023(10) 0.2389(5) 0.043(3) Uani 1 1 d . . . . .
H3WA H 0.145282 -0.086085 0.203657 0.065 Uiso 1 1 d GR . . . .
H3WB H 0.017028 -0.080527 0.242328 0.065 Uiso 1 1 d GR . . . .
O5 O 0.0666(14) 0.0377(10) 0.1623(5) 0.046(3) Uani 1 1 d . . . . .
O4W O 0.2794(14) -0.2063(8) 0.3383(5) 0.041(3) Uani 1 1 d . . . . .
H4WA H 0.291383 -0.241165 0.307541 0.062 Uiso 1 1 d GR . . . .
H4WB H 0.194558 -0.222208 0.354938 0.062 Uiso 1 1 d GR . . . .
O6 O -0.0303(10) 0.1778(7) 0.1441(3) 0.0167(17) Uiso 1 1 d . . . . .
O7 O 0.3656(12) 0.0317(8) 0.2173(4) 0.033(3) Uani 1 1 d . . . . .
O8 O 0.4581(15) -0.1069(11) 0.2414(5) 0.044(3) Uiso 1 1 d . . . . .
O9 O 0.4618(15) 0.2079(9) 0.1411(6) 0.044(3) Uani 1 1 d . . . . .
O10 O 0.2760(16) 0.1544(11) 0.0867(4) 0.059(4) Uani 1 1 d . . . . .
O11 O 0.2268(15) -0.0206(9) 0.4169(4) 0.046(3) Uani 1 1 d . . . . .
O12 O 0.0360(13) -0.0797(9) 0.3655(5) 0.035(3) Uani 1 1 d . . . . .
Gd1 Gd 0.22594(8) 0.17025(5) 0.19111(2) 0.0229(2) Uani 1 1 d . . . . .
Gd2 Gd 0.27323(8) -0.04244(5) 0.31275(2) 0.0234(2) Uani 1 1 d . . . . .
O2W O 0.2136(15) 0.3324(8) 0.1655(5) 0.045(3) Uiso 1 1 d . . . . .
H2WA H 0.280378 0.347112 0.136746 0.067 Uiso 1 1 d GR . . . .
H2WB H 0.236040 0.371339 0.195839 0.067 Uiso 1 1 d GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.506(18) 1_455 ?
C1 O1 1.272(19) . ?
C1 O2 1.28(2) . ?
C1 Gd1 2.941(14) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.57(2) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.525(19) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.48(2) . ?
C5 O3 1.259(19) . ?
C5 O4 1.28(2) . ?
C5 Gd2 2.884(16) . ?
C6 C7 1.57(2) . ?
C6 O5 1.29(2) . ?
C6 O6 1.24(2) . ?
C6 Gd1 2.838(13) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.510(18) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.45(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.492(19) 1_455 ?
C10 O7 1.282(19) . ?
C10 O8 1.29(2) . ?
C10 Gd2 2.940(14) . ?
C11 C12 1.455(19) . ?
C11 O9 1.30(2) . ?
C11 O10 1.26(2) . ?
C11 Gd1 2.841(16) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.48(2) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.54(3) 2_554 ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.66(2) . ?
C15 O11 1.28(2) . ?
C15 O12 1.22(2) . ?
C15 Gd2 2.764(16) . ?
O1 Gd1 2.573(9) . ?
O1 Gd2 2.390(11) . ?
O2 Gd1 2.502(10) . ?
O1W H1WA 0.8566 . ?
O1W H1WB 0.8564 . ?
O1W Gd1 2.392(11) . ?
O3 Gd2 2.460(13) . ?
O4 Gd2 2.516(11) . ?
O3W H3WA 0.8916 . ?
O3W H3WB 0.8932 . ?
O3W Gd2 2.366(11) . ?
O5 Gd1 2.430(13) . ?
O4W H4WA 0.8678 . ?
O4W H4WB 0.8671 . ?
O4W Gd2 2.393(12) . ?
O6 Gd1 2.496(9) . ?
O7 Gd1 2.389(11) . ?
O7 Gd2 2.564(10) . ?
O8 Gd2 2.481(13) . ?
O9 Gd1 2.426(14) . ?
O10 Gd1 2.453(10) . ?
O11 Gd2 2.450(10) . ?
O12 Gd2 2.465(11) . ?
Gd1 O2W 2.371(12) . ?
O2W H2WA 0.9080 . ?
O2W H2WB 0.9103 . ?

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
C2 C1 Gd1 176.5(11) 1_455 . ?
O1 C1 C2 121.4(15) . 1_455 ?
O1 C1 O2 118.3(12) . . ?
O1 C1 Gd1 60.8(7) . . ?
O2 C1 C2 120.3(15) . 1_455 ?
O2 C1 Gd1 57.7(7) . . ?
C1 C2 H2A 110.6 1_655 . ?
C1 C2 H2B 110.6 1_655 . ?
C1 C2 C3 105.6(11) 1_655 . ?
H2A C2 H2B 108.8 . . ?
C3 C2 H2A 110.6 . . ?
C3 C2 H2B 110.6 . . ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 C2 111.0(12) . . ?
C4 C3 H3A 109.4 . . ?
C4 C3 H3B 109.4 . . ?
C3 C4 H4A 109.8 . . ?
C3 C4 H4B 109.8 . . ?
H4A C4 H4B 108.2 . . ?
C5 C4 C3 109.5(11) . . ?
C5 C4 H4A 109.8 . . ?
C5 C4 H4B 109.8 . . ?
C4 C5 Gd2 175.9(10) . . ?
O3 C5 C4 119.6(16) . . ?
O3 C5 O4 118.6(16) . . ?
O3 C5 Gd2 58.0(9) . . ?
O4 C5 C4 121.7(15) . . ?
O4 C5 Gd2 60.6(9) . . ?
C7 C6 Gd1 176.8(10) . . ?
O5 C6 C7 119.7(16) . . ?
O5 C6 Gd1 58.6(8) . . ?
O6 C6 C7 120.3(16) . . ?
O6 C6 O5 119.9(13) . . ?
O6 C6 Gd1 61.5(7) . . ?
C6 C7 H7A 109.4 . . ?
C6 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C8 C7 C6 111.1(13) . . ?
C8 C7 H7A 109.4 . . ?
C8 C7 H7B 109.4 . . ?
C7 C8 H8A 108.7 . . ?
C7 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
C9 C8 C7 114.3(12) . . ?
C9 C8 H8A 108.7 . . ?
C9 C8 H8B 108.7 . . ?
C8 C9 H9A 109.2 . . ?
C8 C9 H9B 109.2 . . ?
C8 C9 C10 111.9(11) . 1_455 ?
H9A C9 H9B 107.9 . . ?
C10 C9 H9A 109.2 1_455 . ?
C10 C9 H9B 109.2 1_455 . ?
C9 C10 Gd2 171.5(11) 1_655 . ?
O7 C10 C9 118.2(15) . 1_655 ?
O7 C10 O8 117.3(13) . . ?
O7 C10 Gd2 60.5(7) . . ?
O8 C10 C9 123.5(15) . 1_655 ?
O8 C10 Gd2 56.8(8) . . ?
C12 C11 Gd1 164.2(15) . . ?
O9 C11 C12 117.3(17) . . ?
O9 C11 Gd1 58.4(9) . . ?
O10 C11 C12 124.8(17) . . ?
O10 C11 O9 117.3(15) . . ?
O10 C11 Gd1 59.4(8) . . ?
C11 C12 H12A 108.5 . . ?
C11 C12 H12B 108.5 . . ?
C11 C12 C13 115.3(17) . . ?
H12A C12 H12B 107.5 . . ?
C13 C12 H12A 108.5 . . ?
C13 C12 H12B 108.5 . . ?
C12 C13 H13A 109.3 . . ?
C12 C13 H13B 109.3 . . ?
C12 C13 C14 111.4(16) . 2_554 ?
H13A C13 H13B 108.0 . . ?
C14 C13 H13A 109.3 2_554 . ?
C14 C13 H13B 109.3 2_554 . ?
C13 C14 H14A 111.2 2 . ?
C13 C14 H14B 111.2 2 . ?
C13 C14 C15 102.8(15) 2 . ?
H14A C14 H14B 109.1 . . ?
C15 C14 H14A 111.2 . . ?
C15 C14 H14B 111.2 . . ?
C14 C15 Gd2 169.2(12) . . ?
O11 C15 C14 115.3(16) . . ?
O11 C15 Gd2 62.4(8) . . ?
O12 C15 C14 120.1(18) . . ?
O12 C15 O11 124.6(15) . . ?
O12 C15 Gd2 63.1(9) . . ?
C1 O1 Gd1 93.6(9) . . ?
C1 O1 Gd2 153.4(9) . . ?
Gd2 O1 Gd1 112.6(4) . . ?
C1 O2 Gd1 96.6(9) . . ?
H1WA O1W H1WB 109.1 . . ?
Gd1 O1W H1WA 109.9 . . ?
Gd1 O1W H1WB 109.6 . . ?
C5 O3 Gd2 96.3(10) . . ?
C5 O4 Gd2 93.1(10) . . ?
H3WA O3W H3WB 107.2 . . ?
Gd2 O3W H3WA 111.5 . . ?
Gd2 O3W H3WB 111.8 . . ?
C6 O5 Gd1 94.3(10) . . ?
H4WA O4W H4WB 108.5 . . ?
Gd2 O4W H4WA 110.7 . . ?
Gd2 O4W H4WB 109.9 . . ?
C6 O6 Gd1 92.6(8) . . ?
C10 O7 Gd1 151.7(9) . . ?
C10 O7 Gd2 93.7(9) . . ?
Gd1 O7 Gd2 113.0(4) . . ?
C10 O8 Gd2 97.5(10) . . ?
C11 O9 Gd1 94.4(11) . . ?
C11 O10 Gd1 94.3(10) . . ?
C15 O11 Gd2 90.1(9) . . ?
C15 O12 Gd2 90.6(11) . . ?
C6 Gd1 C1 80.8(4) . . ?
C6 Gd1 C11 101.4(5) . . ?
C11 Gd1 C1 175.7(6) . . ?
O1 Gd1 C1 25.6(4) . . ?
O1 Gd1 C6 84.3(3) . . ?
O1 Gd1 C11 157.7(5) . . ?
O2 Gd1 C1 25.7(4) . . ?
O2 Gd1 C6 81.2(4) . . ?
O2 Gd1 C11 150.6(5) . . ?
O2 Gd1 O1 51.2(3) . . ?
O1W Gd1 C1 74.5(4) . . ?
O1W Gd1 C6 155.3(4) . . ?
O1W Gd1 C11 103.3(5) . . ?
O1W Gd1 O1 73.0(4) . . ?
O1W Gd1 O2 77.0(4) . . ?
O1W Gd1 O5 144.4(4) . . ?
O1W Gd1 O6 145.9(4) . . ?
O1W Gd1 O9 76.3(5) . . ?
O1W Gd1 O10 129.6(4) . . ?
O5 Gd1 C1 83.4(5) . . ?
O5 Gd1 C6 27.1(5) . . ?
O5 Gd1 C11 100.2(5) . . ?
O5 Gd1 O1 75.1(4) . . ?
O5 Gd1 O2 94.9(5) . . ?
O5 Gd1 O6 52.9(4) . . ?
O5 Gd1 O10 76.4(4) . . ?
O6 Gd1 C1 82.3(4) . . ?
O6 Gd1 C6 25.9(4) . . ?
O6 Gd1 C11 98.1(4) . . ?
O6 Gd1 O1 96.2(3) . . ?
O6 Gd1 O2 71.4(3) . . ?
O7 Gd1 C1 92.6(4) . . ?
O7 Gd1 C6 101.4(5) . . ?
O7 Gd1 C11 90.5(5) . . ?
O7 Gd1 O1 67.2(3) . . ?
O7 Gd1 O2 117.9(3) . . ?
O7 Gd1 O1W 79.1(4) . . ?
O7 Gd1 O5 74.4(4) . . ?
O7 Gd1 O6 127.3(4) . . ?
O7 Gd1 O9 82.1(4) . . ?
O7 Gd1 O10 94.6(4) . . ?
O9 Gd1 C1 150.7(4) . . ?
O9 Gd1 C6 128.4(4) . . ?
O9 Gd1 C11 27.2(5) . . ?
O9 Gd1 O1 139.8(4) . . ?
O9 Gd1 O2 142.4(5) . . ?
O9 Gd1 O5 122.1(4) . . ?
O9 Gd1 O6 123.6(4) . . ?
O9 Gd1 O10 53.4(4) . . ?
O10 Gd1 C1 155.9(4) . . ?
O10 Gd1 C6 75.2(4) . . ?
O10 Gd1 C11 26.3(5) . . ?
O10 Gd1 O1 149.4(4) . . ?
O10 Gd1 O2 143.0(4) . . ?
O10 Gd1 O6 75.0(4) . . ?
O2W Gd1 C1 102.3(5) . . ?
O2W Gd1 C6 104.7(5) . . ?
O2W Gd1 C11 73.7(5) . . ?
O2W Gd1 O1 126.2(4) . . ?
O2W Gd1 O2 77.4(4) . . ?
O2W Gd1 O1W 81.9(4) . . ?
O2W Gd1 O5 130.7(4) . . ?
O2W Gd1 O6 79.0(4) . . ?
O2W Gd1 O7 151.7(4) . . ?
O2W Gd1 O9 73.1(4) . . ?
O2W Gd1 O10 81.6(5) . . ?
C5 Gd2 C10 82.9(4) . . ?
C15 Gd2 C5 100.5(5) . . ?
C15 Gd2 C10 175.3(6) . . ?
O1 Gd2 C5 101.0(4) . . ?
O1 Gd2 C10 92.8(4) . . ?
O1 Gd2 C15 89.7(4) . . ?
O1 Gd2 O3 75.3(4) . . ?
O1 Gd2 O4 127.3(4) . . ?
O1 Gd2 O4W 150.5(4) . . ?
O1 Gd2 O7 67.3(3) . . ?
O1 Gd2 O8 118.3(4) . . ?
O1 Gd2 O11 92.9(4) . . ?
O1 Gd2 O12 82.3(4) . . ?
O3 Gd2 C5 25.7(4) . . ?
O3 Gd2 C10 84.0(5) . . ?
O3 Gd2 C15 100.5(6) . . ?
O3 Gd2 O4 52.0(4) . . ?
O3 Gd2 O7 74.4(4) . . ?
O3 Gd2 O8 93.8(5) . . ?
O3 Gd2 O12 122.1(4) . . ?
O4 Gd2 C5 26.3(4) . . ?
O4 Gd2 C10 83.8(4) . . ?
O4 Gd2 C15 97.8(5) . . ?
O4 Gd2 O7 96.3(4) . . ?
O3W Gd2 C5 156.5(4) . . ?
O3W Gd2 C10 73.6(4) . . ?
O3W Gd2 C15 103.0(5) . . ?
O3W Gd2 O1 79.3(4) . . ?
O3W Gd2 O3 145.0(4) . . ?
O3W Gd2 O4 146.4(5) . . ?
O3W Gd2 O4W 80.9(4) . . ?
O3W Gd2 O7 73.8(4) . . ?
O3W Gd2 O8 77.5(4) . . ?
O3W Gd2 O11 130.4(4) . . ?
O3W Gd2 O12 76.9(4) . . ?
O4W Gd2 C5 105.8(4) . . ?
O4W Gd2 C10 102.4(5) . . ?
O4W Gd2 C15 73.6(5) . . ?
O4W Gd2 O3 130.9(4) . . ?
O4W Gd2 O4 80.0(5) . . ?
O4W Gd2 O7 126.8(4) . . ?
O4W Gd2 O8 77.9(5) . . ?
O4W Gd2 O11 83.5(4) . . ?
O4W Gd2 O12 72.0(4) . . ?
O7 Gd2 C5 84.6(4) . . ?
O7 Gd2 C10 25.8(4) . . ?
O7 Gd2 C15 157.1(4) . . ?
O8 Gd2 C5 81.9(4) . . ?
O8 Gd2 C10 25.7(4) . . ?
O8 Gd2 C15 151.0(5) . . ?
O8 Gd2 O4 71.6(4) . . ?
O8 Gd2 O7 51.5(4) . . ?
O11 Gd2 C5 73.1(4) . . ?
O11 Gd2 C10 156.0(4) . . ?
O11 Gd2 C15 27.5(5) . . ?
O11 Gd2 O3 75.0(4) . . ?
O11 Gd2 O4 74.2(4) . . ?
O11 Gd2 O7 146.9(4) . . ?
O11 Gd2 O8 143.3(4) . . ?
O11 Gd2 O12 53.5(4) . . ?
O12 Gd2 C5 126.6(4) . . ?
O12 Gd2 C10 150.5(4) . . ?
O12 Gd2 C15 26.3(5) . . ?
O12 Gd2 O4 122.2(4) . . ?
O12 Gd2 O7 140.8(4) . . ?
O12 Gd2 O8 143.0(5) . . ?
Gd1 O2W H2WA 111.9 . . ?
Gd1 O2W H2WB 112.7 . . ?
H2WA O2W H2WB 106.3 . . ?

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
C1 C2 C3 C4 172.5(14) 1_655 . . . ?
C2 C1 O1 Gd1 176.8(13) 1_455 . . . ?
C2 C1 O1 Gd2 -14(3) 1_455 . . . ?
C2 C1 O2 Gd1 -176.6(12) 1_455 . . . ?
C2 C3 C4 C5 173.9(14) . . . . ?
C3 C4 C5 O3 -83.3(17) . . . . ?
C3 C4 C5 O4 94.1(17) . . . . ?
C4 C5 O3 Gd2 176.1(10) . . . . ?
C4 C5 O4 Gd2 -176.0(10) . . . . ?
C6 C7 C8 C9 -178.6(17) . . . . ?
C7 C6 O5 Gd1 -176.8(10) . . . . ?
C7 C6 O6 Gd1 177.0(10) . . . . ?
C7 C8 C9 C10 -171.5(16) . . . 1_455 ?
C9 C10 O7 Gd1 29(3) 1_655 . . . ?
C9 C10 O7 Gd2 -170.4(11) 1_655 . . . ?
C9 C10 O8 Gd2 169.8(13) 1_655 . . . ?
C11 C12 C13 C14 -70(2) . . . 2_554 ?
C12 C11 O9 Gd1 162.5(17) . . . . ?
C12 C11 O10 Gd1 -161.9(19) . . . . ?
C13 C14 C15 O11 -96(2) 2 . . . ?
C13 C14 C15 O12 84(2) 2 . . . ?
C13 C14 C15 Gd2 -21(9) 2 . . . ?
C14 C15 O11 Gd2 168.2(14) . . . . ?
C14 C15 O12 Gd2 -168.3(16) . . . . ?
O1 C1 O2 Gd1 4.7(15) . . . . ?
O2 C1 O1 Gd1 -4.6(15) . . . . ?
O2 C1 O1 Gd2 164.9(15) . . . . ?
O3 C5 O4 Gd2 1.3(14) . . . . ?
O4 C5 O3 Gd2 -1.4(14) . . . . ?
O5 C6 C7 C8 82.8(19) . . . . ?
O5 C6 O6 Gd1 -4.6(13) . . . . ?
O6 C6 C7 C8 -98.7(18) . . . . ?
O6 C6 O5 Gd1 4.8(13) . . . . ?
O7 C10 O8 Gd2 1.6(15) . . . . ?
O8 C10 O7 Gd1 -162.6(16) . . . . ?
O8 C10 O7 Gd2 -1.5(14) . . . . ?
O9 C11 C12 C13 168.3(18) . . . . ?
O9 C11 O10 Gd1 9(2) . . . . ?
O10 C11 C12 C13 -21(3) . . . . ?
O10 C11 O9 Gd1 -9(2) . . . . ?
O11 C15 O12 Gd2 11(2) . . . . ?
O12 C15 O11 Gd2 -11(2) . . . . ?
Gd1 C1 O1 Gd2 169(2) . . . . ?
Gd1 C11 C12 C13 -122(5) . . . . ?
Gd2 C10 O7 Gd1 -161(2) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.767 -0.250 0.000 367.4 109.3 '1 DMF'
2 -0.572 0.250 0.500 367.4 108.3 '1 DMF'


_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT201_shelx               
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) .......          6 Report
RESPONSE: ...
;
_vrf_PLAT342_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.02083 Ang.  
RESPONSE: ...
;
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor       O3W      --H3WB     .     Please Check 
RESPONSE:The disordered water molecule occupies a cavity of the
structure with no suitable acceptor atoms in its surroundings.

;
_vrf_PLAT987_shelx               
;
PROBLEM: The Flack x is >> 0 -  Do a BASF/TWIN Refinement     Please Check 
RESPONSE: ...
;
# end Validation Reply Form
####################################################################### 
# 
# 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_sub-kasm-g1
_database_code_depnum_ccdc_archive 'CCDC 1921927'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-06-07 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-05-27
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.01.05 svn.r3372 for Rigaku Oxford Diffraction, GUI svn.r5289)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C7.5 H11 Gd O7, 2(H2 O)'
_chemical_formula_sum            'C7.50 H15 Gd O9'
_chemical_compound_source        synthesized
_chemical_formula_weight         406.44
_chemical_melting_point          ?
_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      293(2)
_chemical_oxdiff_formula         'Gd C H N O S'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'
_chemical_absolute_configuration ?
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   7.9593(2)
_cell_length_b                   14.9638(3)
_cell_length_c                   19.6391(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.266(2)
_cell_angle_gamma                90
_cell_volume                     2332.56(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    13669
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2790
_cell_measurement_theta_min      3.4510
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.724
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_density_diffrn    2.315
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15684
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.392
_diffrn_reflns_theta_min         3.427
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -56.00 -30.00   0.50   10.00    --   -9.95 126.00  84.00   52
  2  ω    -41.00 -13.00   0.50   10.00    --   -9.95 145.00-107.00   56
  3  ω     18.00  43.00   0.50   10.00    --   10.22-145.00-160.00   50
  4  ω     30.00  56.00   0.50   10.00    --   10.22-126.00   7.00   52
  5  ω    -19.00  54.00   0.50   10.00    --   -9.95  38.00 150.00  146
  6  ω    -74.00   4.00   0.50   10.00    --   -9.95 -38.00 -30.00  156
  7  ω    -51.00   2.00   0.50   10.00    --   -9.95 -57.00 -60.00  106
  8  ω    -29.00  37.00   0.50   10.00    --   -9.95  77.00 -90.00  132
  9  ω    -35.00   2.00   0.50   10.00    --   -9.95 -19.00  90.00   74
 10  ω    -58.00 -23.00   0.50   10.00    --   -9.95 125.00-180.00   70
 11  ω    -58.00 -31.00   0.50   10.00    --   -9.95 125.00  30.00   54
 12  ω    -26.00   1.00   0.50   10.00    --   10.22 120.00  27.24   54
 13  ω    -37.00  -6.00   0.50   10.00    --   10.22 132.00-125.00   62
 14  ω    -30.00  -5.00   0.50   10.00    --   10.22 120.00-174.75   50
 15  ω     17.00  71.00   0.50   10.00    --   10.22  57.00  90.00  108
 16  ω    -16.00  10.00   0.50   10.00    --   10.22 -99.00-150.00   52
 17  ω     -3.00  37.00   0.50   10.00    --   10.22 -99.00-180.00   80
 18  ω     -2.00  80.00   0.50   10.00    --   10.22  19.00 -60.00  164
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'SuperNova, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0592084000
_diffrn_orient_matrix_UB_12      0.0016734000
_diffrn_orient_matrix_UB_13      0.0252427000
_diffrn_orient_matrix_UB_21      0.0668979000
_diffrn_orient_matrix_UB_22      0.0028515000
_diffrn_orient_matrix_UB_23      0.0258651000
_diffrn_orient_matrix_UB_31      -0.0019522000
_diffrn_orient_matrix_UB_32      0.0472794000
_diffrn_orient_matrix_UB_33      -0.0024401000
_diffrn_oxdiff_ac3_digest_frames 
;
01c31b6b2bd7e45e8629cf35d29f62545e01518d9cb
;
_diffrn_oxdiff_ac3_digest_hkl    
;
012139b3ce7bc94677604cb4324fc01d804b10
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2446
_reflns_number_total             2541
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.136
_refine_diff_density_min         -2.633
_refine_diff_density_rms         0.241
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.295
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2541
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0447
_refine_ls_restrained_S_all      1.295
_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)+(0.0167P)²+97.6174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1162
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: H8A(0.5) H8B(0.5)
3.a Free rotating group:
 O8(H8C,H8D), O9(H9A,H9B)
3.b Rotating group:
 O7(H7A,H7B)
3.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C7(H7C,H7D), C8(H8A,H8B), C2(H2A,H2B), C3(H3A,H3B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.75555(5) 0.53712(3) 0.51201(2) 0.01401(14) Uani 1 1 d . . . . .
O1 O 0.5085(8) 0.4559(4) 0.4383(3) 0.0215(13) Uani 1 1 d . . . . .
O2 O 0.7660(8) 0.4525(5) 0.4071(4) 0.0286(15) Uani 1 1 d . . . . .
O5 O 0.8330(8) 0.6774(4) 0.5722(3) 0.0219(13) Uani 1 1 d . . . . .
O7 O 0.6153(8) 0.6455(4) 0.4396(4) 0.0267(15) Uani 1 1 d . . . . .
H7A H 0.598796 0.624775 0.398936 0.040 Uiso 1 1 d GR . . . .
H7B H 0.676041 0.692775 0.438645 0.040 Uiso 1 1 d GR . . . .
O3 O 0.5146(7) 0.0796(4) 0.4670(4) 0.0222(14) Uani 1 1 d . . . . .
O6 O 0.8516(9) 0.5535(4) 0.6315(4) 0.0258(14) Uani 1 1 d . . . . .
O4 O 0.7676(7) 0.1147(4) 0.4415(4) 0.0237(14) Uani 1 1 d . . . . .
C5 C 0.6147(11) 0.1353(5) 0.4446(4) 0.0175(17) Uani 1 1 d . . . . .
C1 C 0.6168(11) 0.4264(6) 0.3990(4) 0.0169(16) Uani 1 1 d . . . . .
C4 C 0.5506(13) 0.2254(6) 0.4226(6) 0.028(2) Uani 1 1 d . . . . .
H4A H 0.561109 0.265161 0.461768 0.034 Uiso 1 1 calc R . . . .
H4B H 0.431589 0.220365 0.408447 0.034 Uiso 1 1 calc R . . . .
C6 C 0.8686(10) 0.6369(6) 0.6285(5) 0.0178(17) Uani 1 1 d . . . . .
C7 C 0.9265(12) 0.6907(6) 0.6913(5) 0.0218(18) Uani 1 1 d . . . . .
H7C H 1.010617 0.733522 0.679167 0.026 Uiso 1 1 calc R . . . .
H7D H 0.831354 0.723954 0.706335 0.026 Uiso 1 1 calc R . . . .
C8 C 1.000000 0.6340(9) 0.750000 0.027(3) Uani 1 2 d S T P . .
H8A H 1.087445 0.595827 0.734025 0.032 Uiso 0.5 1 calc R . . . .
H8B H 0.912557 0.595826 0.765975 0.032 Uiso 0.5 1 calc R . . . .
C2 C 0.5690(12) 0.3602(6) 0.3442(5) 0.0214(18) Uani 1 1 d . . . . .
H2A H 0.614430 0.378582 0.301905 0.026 Uiso 1 1 calc R . . . .
H2B H 0.447253 0.357434 0.336613 0.026 Uiso 1 1 calc R . . . .
C3 C 0.6386(13) 0.2674(6) 0.3655(6) 0.029(2) Uani 1 1 d . . . . .
H3A H 0.628114 0.228077 0.326170 0.035 Uiso 1 1 calc R . . . .
H3B H 0.757582 0.273073 0.379559 0.035 Uiso 1 1 calc R . . . .
O8 O 0.892(4) 0.5922(10) 0.3000(8) 0.176(11) Uani 1 1 d . . . . .
H8C H 0.843903 0.615399 0.264342 0.264 Uiso 1 1 d G . . . .
H8D H 0.824972 0.556489 0.317792 0.264 Uiso 1 1 d G . . . .
O9 O 0.620(4) 0.570(2) 0.2142(16) 0.207(12) Uani 1 1 d . . . . .
H9A H 0.664376 0.532534 0.188663 0.311 Uiso 1 1 d G . . . .
H9B H 0.681076 0.575440 0.251474 0.311 Uiso 1 1 d G . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.385(6) 5_666 ?
Gd1 O1 2.649(6) . ?
Gd1 O2 2.426(7) . ?
Gd1 O5 2.465(6) . ?
Gd1 O7 2.381(6) . ?
Gd1 O3 2.541(6) 7_656 ?
Gd1 O3 2.390(6) 3 ?
Gd1 O6 2.426(7) . ?
Gd1 O4 2.460(6) 7_656 ?
Gd1 C5 2.884(8) 7_656 ?
Gd1 C1 2.920(9) . ?
Gd1 C6 2.822(9) . ?
O1 C1 1.278(10) . ?
O2 C1 1.249(11) . ?
O5 C6 1.273(11) . ?
O7 H7A 0.8572 . ?
O7 H7B 0.8574 . ?
O3 C5 1.255(10) . ?
O6 C6 1.257(11) . ?
O4 C5 1.261(10) . ?
C5 C4 1.495(12) . ?
C1 C2 1.491(12) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C3 1.504(14) . ?
C6 C7 1.516(12) . ?
C7 H7C 0.9700 . ?
C7 H7D 0.9700 . ?
C7 C8 1.513(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.541(13) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
O8 H8C 0.8489 . ?
O8 H8D 0.8503 . ?
O9 H9A 0.8496 . ?
O9 H9B 0.8512 . ?

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 Gd1 O1 66.6(2) 5_666 . ?
O1 Gd1 O2 117.3(2) 5_666 . ?
O1 Gd1 O5 87.9(2) 5_666 . ?
O1 Gd1 O3 127.5(2) 5_666 7_656 ?
O1 Gd1 O3 162.0(2) 5_666 3 ?
O1 Gd1 O6 79.8(2) 5_666 . ?
O1 Gd1 O4 78.2(2) 5_666 7_656 ?
O1 Gd1 C5 89.2(2) . 7_656 ?
O1 Gd1 C5 103.0(2) 5_666 7_656 ?
O1 Gd1 C1 92.4(2) 5_666 . ?
O1 Gd1 C1 25.9(2) . . ?
O1 Gd1 C6 149.9(2) . . ?
O1 Gd1 C6 83.3(2) 5_666 . ?
O2 Gd1 O1 50.7(2) . . ?
O2 Gd1 O5 146.0(2) . . ?
O2 Gd1 O3 73.1(2) . 7_656 ?
O2 Gd1 O6 147.9(2) . . ?
O2 Gd1 O4 80.9(2) . 7_656 ?
O2 Gd1 C5 75.5(2) . 7_656 ?
O2 Gd1 C1 24.9(2) . . ?
O2 Gd1 C6 159.4(2) . . ?
O5 Gd1 O1 143.3(2) . . ?
O5 Gd1 O3 110.9(2) . 7_656 ?
O5 Gd1 C5 123.3(2) . 7_656 ?
O5 Gd1 C1 156.2(2) . . ?
O5 Gd1 C6 26.8(2) . . ?
O7 Gd1 O1 71.9(2) . . ?
O7 Gd1 O1 80.0(2) . 5_666 ?
O7 Gd1 O2 83.8(2) . . ?
O7 Gd1 O5 78.2(2) . . ?
O7 Gd1 O3 88.7(2) . 3 ?
O7 Gd1 O3 150.0(2) . 7_656 ?
O7 Gd1 O6 127.5(2) . . ?
O7 Gd1 O4 143.7(2) . 7_656 ?
O7 Gd1 C5 158.1(2) . 7_656 ?
O7 Gd1 C1 78.4(2) . . ?
O7 Gd1 C6 103.4(2) . . ?
O3 Gd1 O1 105.6(2) 7_656 . ?
O3 Gd1 O1 123.1(2) 3 . ?
O3 Gd1 O2 74.9(2) 3 . ?
O3 Gd1 O5 76.1(2) 3 . ?
O3 Gd1 O3 67.2(2) 3 7_656 ?
O3 Gd1 O6 96.5(2) 3 . ?
O3 Gd1 O4 118.3(2) 3 7_656 ?
O3 Gd1 C5 92.7(2) 3 7_656 ?
O3 Gd1 C5 25.8(2) 7_656 7_656 ?
O3 Gd1 C1 87.7(2) 7_656 . ?
O3 Gd1 C1 99.1(2) 3 . ?
O3 Gd1 C6 92.9(2) 7_656 . ?
O3 Gd1 C6 85.8(2) 3 . ?
O6 Gd1 O1 138.0(2) . . ?
O6 Gd1 O5 53.1(2) . . ?
O6 Gd1 O3 75.0(2) . 7_656 ?
O6 Gd1 O4 76.2(2) . 7_656 ?
O6 Gd1 C5 74.0(2) . 7_656 ?
O6 Gd1 C1 150.1(2) . . ?
O6 Gd1 C6 26.3(2) . . ?
O4 Gd1 O1 72.9(2) 7_656 . ?
O4 Gd1 O5 129.1(2) 7_656 . ?
O4 Gd1 O3 51.53(19) 7_656 7_656 ?
O4 Gd1 C5 25.8(2) 7_656 7_656 ?
O4 Gd1 C1 74.0(2) 7_656 . ?
O4 Gd1 C6 102.5(2) 7_656 . ?
C5 Gd1 C1 79.9(2) 7_656 . ?
C6 Gd1 C5 98.5(2) . 7_656 ?
C6 Gd1 C1 174.9(2) . . ?
Gd1 O1 Gd1 113.4(2) 5_666 . ?
C1 O1 Gd1 88.9(5) . . ?
C1 O1 Gd1 156.6(6) . 5_666 ?
C1 O2 Gd1 100.3(5) . . ?
C6 O5 Gd1 92.4(5) . . ?
Gd1 O7 H7A 110.0 . . ?
Gd1 O7 H7B 109.5 . . ?
H7A O7 H7B 109.1 . . ?
Gd1 O3 Gd1 112.8(2) 3_445 7_656 ?
C5 O3 Gd1 153.4(6) . 3_445 ?
C5 O3 Gd1 92.6(5) . 7_656 ?
C6 O6 Gd1 94.7(6) . . ?
C5 O4 Gd1 96.2(5) . 7_656 ?
O3 C5 Gd1 61.7(4) . 7_656 ?
O3 C5 O4 119.7(8) . . ?
O3 C5 C4 119.2(8) . . ?
O4 C5 Gd1 58.0(4) . 7_656 ?
O4 C5 C4 121.1(8) . . ?
C4 C5 Gd1 178.9(7) . 7_656 ?
O1 C1 Gd1 65.1(5) . . ?
O1 C1 C2 121.2(8) . . ?
O2 C1 Gd1 54.8(5) . . ?
O2 C1 O1 119.5(8) . . ?
O2 C1 C2 119.3(8) . . ?
C2 C1 Gd1 170.9(6) . . ?
C5 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
C5 C4 C3 115.1(8) . . ?
H4A C4 H4B 107.5 . . ?
C3 C4 H4A 108.5 . . ?
C3 C4 H4B 108.5 . . ?
O5 C6 Gd1 60.8(5) . . ?
O5 C6 C7 119.2(8) . . ?
O6 C6 Gd1 58.9(5) . . ?
O6 C6 O5 119.7(8) . . ?
O6 C6 C7 121.0(8) . . ?
C7 C6 Gd1 179.1(6) . . ?
C6 C7 H7C 108.9 . . ?
C6 C7 H7D 108.9 . . ?
H7C C7 H7D 107.7 . . ?
C8 C7 C6 113.5(8) . . ?
C8 C7 H7C 108.9 . . ?
C8 C7 H7D 108.9 . . ?
C7 C8 C7 111.8(11) . 2_756 ?
C7 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 2_756 . ?
C7 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 2_756 . ?
H8A C8 H8B 107.9 . . ?
C1 C2 H2A 109.8 . . ?
C1 C2 H2B 109.8 . . ?
C1 C2 C3 109.6(8) . . ?
H2A C2 H2B 108.2 . . ?
C3 C2 H2A 109.8 . . ?
C3 C2 H2B 109.8 . . ?
C4 C3 C2 113.6(8) . . ?
C4 C3 H3A 108.8 . . ?
C4 C3 H3B 108.8 . . ?
C2 C3 H3A 108.8 . . ?
C2 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
H8C O8 H8D 109.5 . . ?
H9A O9 H9B 109.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O7 H7B O5 0.86 1.95 2.694(9) 143.6 7_666 yes
O8 H8C O9 0.85 2.08 2.67(4) 125.3 . yes
O9 H9B O8 0.85 1.89 2.67(4) 151.3 . yes

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.044
_oxdiff_exptl_absorpt_empirical_full_min 0.542
# start Validation Reply Form
_vrf_PLAT417_sub-kasm-g1         
;
PROBLEM: Short Inter D-H..H-D       H8C      ..H9B      .       1.43 Ang.  
RESPONSE:X-ray data was not of sufficient quality to refine proton positions and were placed in geometrically 
estimated positions using the riding model. The estimated positions are unlikely to be correct, 
due to disordered solvent molecules.  
;
_vrf_PLAT420_sub-kasm-g1         
;
PROBLEM: D-H Without Acceptor       O7       --H7A      .     Please Check 
RESPONSE:The disordered water molecule occupies a cavity of the
structure with no suitable acceptor atoms in its surroundings.

;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1866434'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-08-01 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-04-10
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H26 Eu2 O16'
_chemical_formula_sum            'C15 H26 Eu2 O16'
_chemical_formula_weight         766.28
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.768(3)
_cell_length_b                   14.156(4)
_cell_length_c                   22.898(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2842.1(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      30.97
_cell_measurement_theta_min      2.73
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.435
_exptl_absorpt_correction_T_max  0.456
_exptl_absorpt_correction_T_min  0.375
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0976
_diffrn_reflns_av_unetI/netI     0.0522
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.904
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            33729
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         31.394
_diffrn_reflns_theta_min         2.288
_diffrn_ambient_temperature      299.86
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.839
_reflns_number_gt                7220
_reflns_number_total             8211
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         1.966
_refine_diff_density_min         -2.086
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 
;
 Flack x determined using 2809 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         8211
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0480
_refine_ls_restrained_S_all      1.056
_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)+(0.0712P)²+11.2761P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1341
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5442(11) 0.6653(7) 0.7010(4) 0.0247(18) Uani 1 1 d . . . . .
C2 C 0.4394(12) 0.6618(9) 0.6500(5) 0.031(2) Uani 1 1 d . . . . .
H2A H 0.487712 0.629113 0.617675 0.037 Uiso 1 1 calc R . . . .
H2B H 0.413497 0.725222 0.637452 0.037 Uiso 1 1 calc R . . . .
C3 C 0.2941(13) 0.6082(8) 0.6695(5) 0.035(2) Uani 1 1 d . . . . .
H3A H 0.323420 0.550448 0.689370 0.042 Uiso 1 1 calc R . . . .
H3B H 0.237726 0.646935 0.697016 0.042 Uiso 1 1 calc R . . . .
C4 C 0.1904(13) 0.5837(9) 0.6175(5) 0.036(2) Uani 1 1 d . . . . .
H4A H 0.165461 0.640703 0.596033 0.043 Uiso 1 1 calc R . . . .
H4B H 0.243357 0.541032 0.591238 0.043 Uiso 1 1 calc R . . . .
C5 C 0.0486(13) 0.5385(8) 0.6387(5) 0.034(2) Uani 1 1 d . . . . .
C6 C 0.5941(14) 0.4428(10) 0.5841(6) 0.039(3) Uani 1 1 d . . . . .
C7 C 0.5185(18) 0.4091(13) 0.5278(6) 0.055(4) Uani 1 1 d . . . . .
H7A H 0.553036 0.447038 0.495118 0.066 Uiso 1 1 calc R . . . .
H7B H 0.408594 0.415289 0.530852 0.066 Uiso 1 1 calc R . . . .
C8 C 0.562(2) 0.3056(11) 0.5182(6) 0.055(4) Uani 1 1 d . . . . .
H8A H 0.671529 0.298788 0.520048 0.066 Uiso 1 1 calc R . . . .
H8B H 0.517277 0.267147 0.548894 0.066 Uiso 1 1 calc R . . . .
C9 C 0.506(2) 0.2725(13) 0.4609(6) 0.056(4) Uani 1 1 d . . . . .
H9A H 0.400310 0.291071 0.456901 0.068 Uiso 1 1 calc R . . . .
H9B H 0.509457 0.203958 0.460711 0.068 Uiso 1 1 calc R . . . .
C10 C 0.5913(13) 0.3074(8) 0.4091(5) 0.033(2) Uani 1 1 d . . . . .
C11 C 0.5454(11) 0.5372(7) 0.2945(5) 0.0242(18) Uani 1 1 d . . . . .
C12 C 0.4408(13) 0.5308(9) 0.3455(5) 0.034(2) Uani 1 1 d . . . . .
H12A H 0.417062 0.593496 0.359874 0.041 Uiso 1 1 calc R . . . .
H12B H 0.488912 0.495354 0.376721 0.041 Uiso 1 1 calc R . . . .
C13 C 0.2947(13) 0.4809(10) 0.3257(5) 0.043(3) Uani 1 1 d . . . . .
H13A H 0.241533 0.520304 0.297725 0.051 Uiso 1 1 calc R . . . .
H13B H 0.320933 0.421970 0.306555 0.051 Uiso 1 1 calc R . . . .
C14 C 0.1894(14) 0.4604(11) 0.3776(5) 0.046(3) Uani 1 1 d . . . . .
H14A H 0.163042 0.519004 0.397068 0.055 Uiso 1 1 calc R . . . .
H14B H 0.241205 0.419985 0.405426 0.055 Uiso 1 1 calc R . . . .
C15 C 0.0444(12) 0.4117(9) 0.3556(5) 0.032(2) Uani 1 1 d . . . . .
O1 O 0.6340(9) 0.5981(5) 0.7118(4) 0.0291(15) Uani 1 1 d . . . . .
O2 O 0.5402(11) 0.7338(6) 0.7369(4) 0.040(2) Uani 1 1 d . . . . .
O1W O 0.6082(11) 0.4004(6) 0.7605(4) 0.041(2) Uani 1 1 d . . . . .
H1WA H 0.630412 0.425730 0.793809 0.061 Uiso 1 1 d GR . . . .
H1WB H 0.617203 0.339742 0.763547 0.061 Uiso 1 1 d GR . . . .
O3 O 0.0353(10) 0.4521(7) 0.6400(5) 0.046(3) Uani 1 1 d . . . . .
O2W O 0.7795(10) 0.2952(5) 0.6624(4) 0.0397(18) Uani 1 1 d . . . . .
H2WA H 0.724893 0.261051 0.687366 0.060 Uiso 1 1 d GR . . . .
H2WB H 0.874167 0.272913 0.662981 0.060 Uiso 1 1 d GR . . . .
O4 O -0.0591(11) 0.5887(6) 0.6585(5) 0.045(2) Uani 1 1 d . . . . .
O3W O 0.6114(11) 0.2685(6) 0.2346(4) 0.042(2) Uani 1 1 d . . . . .
H3WA H 0.578899 0.213897 0.244365 0.063 Uiso 1 1 d GR . . . .
H3WB H 0.660806 0.264270 0.202605 0.063 Uiso 1 1 d GR . . . .
O5 O 0.5324(9) 0.4258(6) 0.6340(4) 0.0326(17) Uani 1 1 d . . . . .
O4W O 0.7823(10) 0.1648(5) 0.3339(4) 0.0390(18) Uani 1 1 d . . . . .
H4WA H 0.736223 0.153141 0.368039 0.058 Uiso 1 1 d GR . . . .
H4WB H 0.878439 0.144303 0.337073 0.058 Uiso 1 1 d GR . . . .
O6 O 0.7261(12) 0.4787(8) 0.5817(4) 0.055(3) Uani 1 1 d . . . . .
O7 O 0.7218(11) 0.3455(7) 0.4135(4) 0.047(2) Uani 1 1 d . . . . .
O8 O 0.5366(10) 0.2926(7) 0.3586(4) 0.0350(18) Uani 1 1 d . . . . .
O9 O 0.6351(9) 0.4674(5) 0.2837(4) 0.0290(16) Uani 1 1 d . . . . .
O10 O 0.5430(11) 0.6056(6) 0.2594(4) 0.040(2) Uani 1 1 d . . . . .
O11 O 0.0344(9) 0.3219(6) 0.3551(5) 0.0345(19) Uani 1 1 d . . . . .
O12 O -0.0654(11) 0.4628(6) 0.3396(4) 0.042(2) Uani 1 1 d . . . . .
Eu1 Eu 0.77318(6) 0.45855(3) 0.68678(2) 0.02301(11) Uani 1 1 d . . . . .
Eu2 Eu 0.77389(5) 0.32872(3) 0.30911(2) 0.02229(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.487(14) . ?
C1 O1 1.260(12) . ?
C1 O2 1.272(12) . ?
C1 Eu2 2.946(10) 2_665 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.549(15) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.539(16) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.480(15) . ?
C5 O3 1.229(15) . ?
C5 O4 1.266(14) . ?
C5 Eu1 2.885(11) 1_455 ?
C6 C7 1.525(17) . ?
C6 O5 1.288(15) . ?
C6 O6 1.266(15) . ?
C6 Eu1 2.837(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.53(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.47(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.487(16) . ?
C10 O7 1.269(14) . ?
C10 O8 1.268(16) . ?
C10 Eu2 2.809(10) . ?
C11 C12 1.487(14) . ?
C11 O9 1.287(11) . ?
C11 O10 1.258(13) . ?
C11 Eu1 2.935(10) 2_664 ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.531(15) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.531(15) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.531(16) . ?
C15 O11 1.274(14) . ?
C15 O12 1.259(15) . ?
C15 Eu2 2.853(11) 1_455 ?
O1 Eu1 2.392(7) . ?
O1 Eu2 2.586(8) 2_665 ?
O2 Eu2 2.485(9) 2_665 ?
O1W H1WA 0.8648 . ?
O1W H1WB 0.8648 . ?
O1W Eu1 2.371(9) . ?
O3 Eu1 2.538(9) 1_455 ?
O2W H2WA 0.8893 . ?
O2W H2WB 0.8884 . ?
O2W Eu1 2.379(7) . ?
O4 Eu1 2.444(8) 1_455 ?
O3W H3WA 0.8536 . ?
O3W H3WB 0.8538 . ?
O3W Eu2 2.380(9) . ?
O5 Eu1 2.477(8) . ?
O4W H4WA 0.8960 . ?
O4W H4WB 0.8949 . ?
O4W Eu2 2.389(7) . ?
O6 Eu1 2.457(9) . ?
O7 Eu2 2.446(8) . ?
O8 Eu2 2.424(8) . ?
O9 Eu1 2.583(8) 2_664 ?
O9 Eu2 2.382(7) . ?
O10 Eu1 2.487(9) 2_664 ?
O11 Eu2 2.517(8) 1_455 ?
O12 Eu2 2.464(8) 1_455 ?
Eu1 H1WA 2.7910 . ?
Eu1 H1WB 2.7909 . ?
Eu2 H3WA 2.7863 . ?
Eu2 H3WB 2.7863 . ?

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
C2 C1 Eu2 174.6(7) . 2_665 ?
O1 C1 C2 121.0(10) . . ?
O1 C1 O2 117.8(9) . . ?
O1 C1 Eu2 61.2(5) . 2_665 ?
O2 C1 C2 121.1(10) . . ?
O2 C1 Eu2 56.6(5) . 2_665 ?
C1 C2 H2A 110.2 . . ?
C1 C2 H2B 110.2 . . ?
C1 C2 C3 107.3(9) . . ?
H2A C2 H2B 108.5 . . ?
C3 C2 H2A 110.2 . . ?
C3 C2 H2B 110.2 . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 C2 111.9(9) . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C3 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C5 C4 C3 109.8(10) . . ?
C5 C4 H4A 109.7 . . ?
C5 C4 H4B 109.7 . . ?
C4 C5 Eu1 176.2(8) . 1_455 ?
O3 C5 C4 121.2(11) . . ?
O3 C5 O4 118.6(11) . . ?
O3 C5 Eu1 61.4(6) . 1_455 ?
O4 C5 C4 120.1(10) . . ?
O4 C5 Eu1 57.2(6) . 1_455 ?
C7 C6 Eu1 164.9(10) . . ?
O5 C6 C7 120.6(12) . . ?
O5 C6 Eu1 60.7(6) . . ?
O6 C6 C7 119.2(12) . . ?
O6 C6 O5 119.8(11) . . ?
O6 C6 Eu1 59.8(7) . . ?
C6 C7 H7A 110.0 . . ?
C6 C7 H7B 110.0 . . ?
C6 C7 C8 108.3(13) . . ?
H7A C7 H7B 108.4 . . ?
C8 C7 H7A 110.0 . . ?
C8 C7 H7B 110.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 C7 110.6(14) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C8 C9 H9A 108.3 . . ?
C8 C9 H9B 108.3 . . ?
C8 C9 C10 116.1(13) . . ?
H9A C9 H9B 107.4 . . ?
C10 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
C9 C10 Eu2 166.5(10) . . ?
O7 C10 C9 121.9(13) . . ?
O7 C10 Eu2 60.4(6) . . ?
O8 C10 C9 118.9(12) . . ?
O8 C10 O7 119.0(10) . . ?
O8 C10 Eu2 59.4(6) . . ?
C12 C11 Eu1 174.2(8) . 2_664 ?
O9 C11 C12 118.7(9) . . ?
O9 C11 Eu1 61.5(5) . 2_664 ?
O10 C11 C12 122.6(9) . . ?
O10 C11 O9 118.6(9) . . ?
O10 C11 Eu1 57.1(6) . 2_664 ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
C11 C12 C13 108.2(9) . . ?
H12A C12 H12B 108.4 . . ?
C13 C12 H12A 110.1 . . ?
C13 C12 H12B 110.1 . . ?
C12 C13 H13A 109.4 . . ?
C12 C13 H13B 109.4 . . ?
H13A C13 H13B 108.0 . . ?
C14 C13 C12 111.3(9) . . ?
C14 C13 H13A 109.4 . . ?
C14 C13 H13B 109.4 . . ?
C13 C14 H14A 109.8 . . ?
C13 C14 H14B 109.8 . . ?
C13 C14 C15 109.4(10) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
C14 C15 Eu2 176.6(9) . 1_455 ?
O11 C15 C14 120.7(12) . . ?
O11 C15 Eu2 61.9(6) . 1_455 ?
O12 C15 C14 118.1(11) . . ?
O12 C15 O11 121.2(10) . . ?
O12 C15 Eu2 59.5(6) . 1_455 ?
C1 O1 Eu1 153.6(7) . . ?
C1 O1 Eu2 93.5(6) . 2_665 ?
Eu1 O1 Eu2 112.2(3) . 2_665 ?
C1 O2 Eu2 98.1(6) . 2_665 ?
H1WA O1W H1WB 108.7 . . ?
Eu1 O1W H1WA 110.2 . . ?
Eu1 O1W H1WB 110.2 . . ?
C5 O3 Eu1 93.5(7) . 1_455 ?
H2WA O2W H2WB 107.4 . . ?
Eu1 O2W H2WA 111.4 . . ?
Eu1 O2W H2WB 111.3 . . ?
C5 O4 Eu1 96.9(7) . 1_455 ?
H3WA O3W H3WB 109.3 . . ?
Eu2 O3W H3WA 109.7 . . ?
Eu2 O3W H3WB 109.7 . . ?
C6 O5 Eu1 92.3(7) . . ?
H4WA O4W H4WB 107.0 . . ?
Eu2 O4W H4WA 111.9 . . ?
Eu2 O4W H4WB 111.3 . . ?
C6 O6 Eu1 93.8(8) . . ?
C10 O7 Eu2 92.8(7) . . ?
C10 O8 Eu2 93.8(6) . . ?
C11 O9 Eu1 92.5(6) . 2_664 ?
C11 O9 Eu2 153.9(7) . . ?
Eu2 O9 Eu1 112.7(3) . 2_664 ?
C11 O10 Eu1 97.8(6) . 2_664 ?
C15 O11 Eu2 91.6(7) . 1_455 ?
C15 O12 Eu2 94.4(7) . 1_455 ?
C5 Eu1 C11 81.9(3) 1_655 2_665 ?
C5 Eu1 H1WA 140.9 1_655 . ?
C5 Eu1 H1WB 152.5 1_655 . ?
C6 Eu1 C5 100.3(4) . 1_655 ?
C6 Eu1 C11 176.5(4) . 2_665 ?
C6 Eu1 H1WA 117.8 . . ?
C6 Eu1 H1WB 101.7 . . ?
C11 Eu1 H1WA 60.6 2_665 . ?
C11 Eu1 H1WB 75.4 2_665 . ?
O1 Eu1 C5 101.2(3) . 1_655 ?
O1 Eu1 C6 88.9(3) . . ?
O1 Eu1 C11 93.3(3) . 2_665 ?
O1 Eu1 H1WA 72.4 . . ?
O1 Eu1 H1WB 95.5 . . ?
O1 Eu1 O3 126.4(3) . 1_655 ?
O1 Eu1 O4 75.4(3) . 1_655 ?
O1 Eu1 O5 80.6(3) . . ?
O1 Eu1 O6 93.1(3) . . ?
O1 Eu1 O9 67.5(2) . 2_665 ?
O1 Eu1 O10 118.1(3) . 2_665 ?
O1W Eu1 C5 156.7(3) . 1_655 ?
O1W Eu1 C6 103.0(4) . . ?
O1W Eu1 C11 74.9(3) . 2_665 ?
O1W Eu1 O1 78.7(3) . . ?
O1W Eu1 H1WA 16.9 . . ?
O1W Eu1 H1WB 16.9 . . ?
O1W Eu1 O3 147.2(4) . 1_655 ?
O1W Eu1 O2W 81.0(3) . . ?
O1W Eu1 O4 144.8(3) . 1_655 ?
O1W Eu1 O5 76.2(3) . . ?
O1W Eu1 O6 129.4(3) . . ?
O1W Eu1 O9 73.7(3) . 2_665 ?
O1W Eu1 O10 78.0(3) . 2_665 ?
H1WA Eu1 H1WB 29.2 . . ?
O3 Eu1 C5 25.2(3) 1_655 1_655 ?
O3 Eu1 C6 98.5(4) 1_655 . ?
O3 Eu1 C11 82.2(3) 1_655 2_665 ?
O3 Eu1 H1WA 140.5 1_655 . ?
O3 Eu1 H1WB 133.5 1_655 . ?
O3 Eu1 O9 95.5(3) 1_655 2_665 ?
O2W Eu1 C5 105.8(3) . 1_655 ?
O2W Eu1 C6 75.0(4) . . ?
O2W Eu1 C11 101.8(3) . 2_665 ?
O2W Eu1 O1 150.6(3) . . ?
O2W Eu1 H1WA 93.2 . . ?
O2W Eu1 H1WB 64.8 . . ?
O2W Eu1 O3 81.1(3) . 1_655 ?
O2W Eu1 O4 131.0(3) . 1_655 ?
O2W Eu1 O5 73.9(3) . . ?
O2W Eu1 O6 83.5(4) . . ?
O2W Eu1 O9 126.1(3) . 2_665 ?
O2W Eu1 O10 77.7(3) . 2_665 ?
O4 Eu1 C5 25.8(3) 1_655 1_655 ?
O4 Eu1 C6 99.9(4) 1_655 . ?
O4 Eu1 C11 83.2(3) 1_655 2_665 ?
O4 Eu1 H1WA 128.9 1_655 . ?
O4 Eu1 H1WB 156.3 1_655 . ?
O4 Eu1 O3 51.0(3) 1_655 1_655 ?
O4 Eu1 O5 121.7(3) 1_655 . ?
O4 Eu1 O6 75.8(4) 1_655 . ?
O4 Eu1 O9 74.6(3) 1_655 2_665 ?
O4 Eu1 O10 93.6(4) 1_655 2_665 ?
O5 Eu1 C5 126.9(3) . 1_655 ?
O5 Eu1 C6 27.0(3) . . ?
O5 Eu1 C11 151.1(3) . 2_665 ?
O5 Eu1 H1WA 90.9 . . ?
O5 Eu1 H1WB 77.1 . . ?
O5 Eu1 O3 124.0(3) . 1_655 ?
O5 Eu1 O9 139.5(3) . 2_665 ?
O5 Eu1 O10 144.1(3) . 2_665 ?
O6 Eu1 C5 73.8(3) . 1_655 ?
O6 Eu1 C6 26.4(3) . . ?
O6 Eu1 C11 155.7(3) . 2_665 ?
O6 Eu1 H1WA 143.5 . . ?
O6 Eu1 H1WB 127.2 . . ?
O6 Eu1 O3 75.1(4) . 1_655 ?
O6 Eu1 O5 53.2(3) . . ?
O6 Eu1 O9 147.8(3) . 2_665 ?
O6 Eu1 O10 143.7(4) . 2_665 ?
O9 Eu1 C5 84.7(3) 2_665 1_655 ?
O9 Eu1 C6 156.5(3) 2_665 . ?
O9 Eu1 C11 26.0(2) 2_665 2_665 ?
O9 Eu1 H1WA 56.8 2_665 . ?
O9 Eu1 H1WB 81.7 2_665 . ?
O10 Eu1 C5 81.7(4) 2_665 1_655 ?
O10 Eu1 C6 152.2(3) 2_665 . ?
O10 Eu1 C11 25.1(3) 2_665 2_665 ?
O10 Eu1 H1WA 69.1 2_665 . ?
O10 Eu1 H1WB 71.1 2_665 . ?
O10 Eu1 O3 71.5(3) 2_665 1_655 ?
O10 Eu1 O9 51.1(2) 2_665 2_665 ?
C1 Eu2 H3WA 84.4 2_664 . ?
C1 Eu2 H3WB 57.8 2_664 . ?
C10 Eu2 C1 175.0(3) . 2_664 ?
C10 Eu2 C15 102.3(3) . 1_655 ?
C10 Eu2 H3WA 91.2 . . ?
C10 Eu2 H3WB 118.4 . . ?
C15 Eu2 C1 81.5(3) 1_655 2_664 ?
C15 Eu2 H3WA 161.6 1_655 . ?
C15 Eu2 H3WB 139.2 1_655 . ?
O1 Eu2 C1 25.3(2) 2_664 2_664 ?
O1 Eu2 C10 157.3(3) 2_664 . ?
O1 Eu2 C15 84.1(3) 2_664 1_655 ?
O1 Eu2 H3WA 88.1 2_664 . ?
O1 Eu2 H3WB 59.2 2_664 . ?
O2 Eu2 C1 25.3(3) 2_664 2_664 ?
O2 Eu2 C10 151.3(3) 2_664 . ?
O2 Eu2 C15 81.4(3) 2_664 1_655 ?
O2 Eu2 O1 50.6(2) 2_664 2_664 ?
O2 Eu2 H3WA 80.8 2_664 . ?
O2 Eu2 H3WB 62.3 2_664 . ?
O2 Eu2 O11 70.7(3) 2_664 1_655 ?
O3W Eu2 C1 74.5(3) . 2_664 ?
O3W Eu2 C10 101.8(4) . . ?
O3W Eu2 C15 155.9(3) . 1_655 ?
O3W Eu2 O1 73.3(3) . 2_664 ?
O3W Eu2 O2 77.8(3) . 2_664 ?
O3W Eu2 H3WA 16.8 . . ?
O3W Eu2 H3WB 16.8 . . ?
O3W Eu2 O4W 80.8(3) . . ?
O3W Eu2 O7 128.6(3) . . ?
O3W Eu2 O8 75.3(3) . . ?
O3W Eu2 O9 79.3(3) . . ?
O3W Eu2 O11 146.0(3) . 1_655 ?
O3W Eu2 O12 145.2(3) . 1_655 ?
H3WA Eu2 H3WB 28.9 . . ?
O4W Eu2 C1 102.1(3) . 2_664 ?
O4W Eu2 C10 73.7(3) . . ?
O4W Eu2 C15 106.6(3) . 1_655 ?
O4W Eu2 O1 125.7(3) . 2_664 ?
O4W Eu2 O2 78.0(3) . 2_664 ?
O4W Eu2 H3WA 65.1 . . ?
O4W Eu2 H3WB 84.3 . . ?
O4W Eu2 O7 82.4(3) . . ?
O4W Eu2 O8 73.2(3) . . ?
O4W Eu2 O11 80.5(3) . 1_655 ?
O4W Eu2 O12 131.5(3) . 1_655 ?
O7 Eu2 C1 156.9(3) . 2_664 ?
O7 Eu2 C10 26.8(3) . . ?
O7 Eu2 C15 75.6(3) . 1_655 ?
O7 Eu2 O1 149.5(3) . 2_664 ?
O7 Eu2 O2 143.9(3) . 2_664 ?
O7 Eu2 H3WA 117.5 . . ?
O7 Eu2 H3WB 145.2 . . ?
O7 Eu2 O11 76.4(3) . 1_655 ?
O7 Eu2 O12 75.9(3) . 1_655 ?
O8 Eu2 C1 149.7(3) . 2_664 ?
O8 Eu2 C10 26.8(3) . . ?
O8 Eu2 C15 128.7(3) . 1_655 ?
O8 Eu2 O1 139.1(3) . 2_664 ?
O8 Eu2 O2 143.0(3) . 2_664 ?
O8 Eu2 H3WA 66.4 . . ?
O8 Eu2 H3WB 92.0 . . ?
O8 Eu2 O7 53.3(3) . . ?
O8 Eu2 O11 125.1(3) . 1_655 ?
O8 Eu2 O12 121.4(3) . 1_655 ?
O9 Eu2 C1 92.7(3) . 2_664 ?
O9 Eu2 C10 89.8(3) . . ?
O9 Eu2 C15 100.2(3) . 1_655 ?
O9 Eu2 O1 67.6(2) . 2_664 ?
O9 Eu2 O2 117.8(3) . 2_664 ?
O9 Eu2 H3WA 92.1 . . ?
O9 Eu2 H3WB 82.8 . . ?
O9 Eu2 O4W 150.9(3) . . ?
O9 Eu2 O7 93.6(3) . . ?
O9 Eu2 O8 81.3(3) . . ?
O9 Eu2 O11 126.7(3) . 1_655 ?
O9 Eu2 O12 74.1(3) . 1_655 ?
O11 Eu2 C1 82.0(3) 1_655 2_664 ?
O11 Eu2 C10 99.9(4) 1_655 . ?
O11 Eu2 C15 26.5(3) 1_655 1_655 ?
O11 Eu2 O1 95.3(3) 1_655 2_664 ?
O11 Eu2 H3WA 139.2 1_655 . ?
O11 Eu2 H3WB 132.6 1_655 . ?
O12 Eu2 C1 84.6(3) 1_655 2_664 ?
O12 Eu2 C10 100.3(4) 1_655 . ?
O12 Eu2 C15 26.1(3) 1_655 1_655 ?
O12 Eu2 O1 75.9(3) 1_655 2_664 ?
O12 Eu2 O2 95.0(4) 1_655 2_664 ?
O12 Eu2 H3WA 161.9 1_655 . ?
O12 Eu2 H3WB 134.7 1_655 . ?
O12 Eu2 O11 52.6(3) 1_655 1_655 ?

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
C1 C2 C3 C4 -169.2(10) . . . . ?
C2 C1 O1 Eu1 18(2) . . . . ?
C2 C1 O1 Eu2 -174.3(8) . . . 2_665 ?
C2 C1 O2 Eu2 174.2(8) . . . 2_665 ?
C2 C3 C4 C5 -176.2(10) . . . . ?
C3 C4 C5 O3 -96.2(15) . . . . ?
C3 C4 C5 O4 80.6(15) . . . . ?
C4 C5 O3 Eu1 176.8(10) . . . 1_455 ?
C4 C5 O4 Eu1 -176.8(10) . . . 1_455 ?
C6 C7 C8 C9 -173.4(13) . . . . ?
C7 C6 O5 Eu1 162.6(12) . . . . ?
C7 C6 O6 Eu1 -162.6(12) . . . . ?
C7 C8 C9 C10 73.8(19) . . . . ?
C8 C9 C10 O7 15(2) . . . . ?
C8 C9 C10 O8 -170.0(14) . . . . ?
C8 C9 C10 Eu2 111(4) . . . . ?
C9 C10 O7 Eu2 164.5(12) . . . . ?
C9 C10 O8 Eu2 -164.5(11) . . . . ?
C11 C12 C13 C14 172.9(11) . . . . ?
C12 C11 O9 Eu1 173.4(9) . . . 2_664 ?
C12 C11 O9 Eu2 -22(2) . . . . ?
C12 C11 O10 Eu1 -173.1(9) . . . 2_664 ?
C12 C13 C14 C15 179.3(12) . . . . ?
C13 C14 C15 O11 93.8(15) . . . . ?
C13 C14 C15 O12 -87.9(15) . . . . ?
C14 C15 O11 Eu2 -177.3(9) . . . 1_455 ?
C14 C15 O12 Eu2 177.2(8) . . . 1_455 ?
O1 C1 C2 C3 85.4(12) . . . . ?
O1 C1 O2 Eu2 -2.0(11) . . . 2_665 ?
O2 C1 C2 C3 -90.7(13) . . . . ?
O2 C1 O1 Eu1 -165.8(11) . . . . ?
O2 C1 O1 Eu2 1.9(10) . . . 2_665 ?
O3 C5 O4 Eu1 0.1(14) . . . 1_455 ?
O4 C5 O3 Eu1 -0.1(14) . . . 1_455 ?
O5 C6 C7 C8 -82.4(16) . . . . ?
O5 C6 O6 Eu1 9.9(14) . . . . ?
O6 C6 C7 C8 90.0(18) . . . . ?
O6 C6 O5 Eu1 -9.8(13) . . . . ?
O7 C10 O8 Eu2 10.5(12) . . . . ?
O8 C10 O7 Eu2 -10.4(12) . . . . ?
O9 C11 C12 C13 -86.6(13) . . . . ?
O9 C11 O10 Eu1 2.3(11) . . . 2_664 ?
O10 C11 C12 C13 88.8(14) . . . . ?
O10 C11 O9 Eu1 -2.2(11) . . . 2_664 ?
O10 C11 O9 Eu2 162.9(11) . . . . ?
O11 C15 O12 Eu2 -4.5(12) . . . 1_455 ?
O12 C15 O11 Eu2 4.4(12) . . . 1_455 ?
Eu1 C6 C7 C8 8(5) . . . . ?
Eu1 C11 O9 Eu2 165.1(16) 2_664 . . . ?
Eu2 C1 O1 Eu1 -167.7(16) 2_665 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.412 0.250 0.000 363.2 360.6 '1 DMF'
2 -0.578 0.750 0.500 363.2 359.7 '1 DMF'


_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor       O3W      --H3WB     .     Please Check 
RESPONSE:The disordered water molecule occupies a cavity of the
structure with no suitable acceptor atoms in its surroundings.

;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1866432'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-08-01 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-04-10
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H27 Dy2 N O14, H2 O'
_chemical_formula_sum            'C18 H29 Dy2 N O15'
_chemical_formula_weight         824.42
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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                   13.7102(12)
_cell_length_b                   13.6658(12)
_cell_length_c                   15.8149(14)
_cell_angle_alpha                90
_cell_angle_beta                 114.841(2)
_cell_angle_gamma                90
_cell_volume                     2688.9(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.583
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.589
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            49408
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.390
_diffrn_reflns_theta_min         2.058
_diffrn_ambient_temperature      302.27
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5805
_reflns_number_total             6708
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.856
_refine_diff_density_min         -1.538
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6708
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0292
_refine_ls_restrained_S_all      1.077
_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)+(0.0506P)²+7.0496P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.0925
_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 C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O13-C18
 1.219 with sigma of 0.02
 O13-C18A
 1.219 with sigma of 0.02
 N1-C18
 1.342 with sigma of 0.02
 N1-C18A
 1.342 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C17) = Uanis(C17A)
Uanis(C18) = Uanis(C18A)
Uanis(C16) = Uanis(C16A)
4. Others
 Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(C18)=Sof(H18)=1-FVAR(3)
 Sof(C18A)=Sof(H18A)=FVAR(3)
5.a Free rotating group:
 O2W(H2WA,H2WB)
5.b Rotating group:
 O1W(H1WA,H1WB)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
5.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C18A(H18A)
5.e Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C17(H17A,H17B,H17C), C17A(H17D,
 H17E,H17F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3771(4) 0.4657(3) 0.6844(3) 0.0224(8) Uani 1 1 d . . . . .
C2 C 0.3845(4) 0.4421(3) 0.5949(3) 0.0261(9) Uani 1 1 d . . . . .
H2A H 0.430400 0.489619 0.583854 0.031 Uiso 1 1 calc R . . . .
H2B H 0.313621 0.446135 0.543833 0.031 Uiso 1 1 calc R . . . .
C3 C 0.4300(4) 0.3399(3) 0.5984(3) 0.0292(10) Uani 1 1 d . . . . .
H3A H 0.501410 0.337005 0.648845 0.035 Uiso 1 1 calc R . . . .
H3B H 0.385232 0.293227 0.612047 0.035 Uiso 1 1 calc R . . . .
C4 C 0.4364(4) 0.3102(3) 0.5084(3) 0.0266(9) Uani 1 1 d . . . . .
H4A H 0.367031 0.321497 0.456909 0.032 Uiso 1 1 calc R . . . .
H4B H 0.488400 0.351743 0.499076 0.032 Uiso 1 1 calc R . . . .
C5 C 0.4677(3) 0.2048(3) 0.5061(3) 0.0204(7) Uani 1 1 d . . . . .
C6 C 0.0636(3) 0.3701(3) 0.4248(3) 0.0205(7) Uani 1 1 d . . . . .
C7 C 0.1265(4) 0.2788(3) 0.4369(4) 0.0337(11) Uani 1 1 d . . . . .
H7A H 0.192499 0.283915 0.493322 0.040 Uiso 1 1 calc R . . . .
H7B H 0.145967 0.271848 0.384894 0.040 Uiso 1 1 calc R . . . .
C8 C 0.0661(4) 0.1878(3) 0.4429(3) 0.0284(9) Uani 1 1 d . . . . .
H8A H -0.004472 0.187315 0.391059 0.034 Uiso 1 1 calc R . . . .
H8B H 0.056112 0.189773 0.500075 0.034 Uiso 1 1 calc R . . . .
C9 C 0.1256(4) 0.0941(3) 0.4409(3) 0.0300(10) Uani 1 1 d . . . . .
H9A H 0.199264 0.098164 0.487393 0.036 Uiso 1 1 calc R . . . .
H9B H 0.091741 0.038807 0.456308 0.036 Uiso 1 1 calc R . . . .
C10 C 0.1247(4) 0.0783(3) 0.3468(3) 0.0225(8) Uani 1 1 d . . . . .
C11 C 0.6502(3) 0.0788(3) 0.4665(3) 0.0185(7) Uani 1 1 d . . . . .
C12 C 0.6531(5) 0.1267(4) 0.3824(3) 0.0370(13) Uani 1 1 d . . . . .
H12A H 0.682220 0.080204 0.352670 0.044 Uiso 1 1 calc R . . . .
H12B H 0.579886 0.140900 0.338705 0.044 Uiso 1 1 calc R . . . .
C13 C 0.7169(5) 0.2187(3) 0.3999(3) 0.0330(11) Uani 1 1 d . . . . .
H13A H 0.790575 0.205278 0.443118 0.040 Uiso 1 1 calc R . . . .
H13B H 0.687872 0.266170 0.428829 0.040 Uiso 1 1 calc R . . . .
C14 C 0.7158(4) 0.2617(3) 0.3119(3) 0.0303(10) Uani 1 1 d . . . . .
H14A H 0.750077 0.215686 0.286289 0.036 Uiso 1 1 calc R . . . .
H14B H 0.641615 0.268570 0.267011 0.036 Uiso 1 1 calc R . . . .
C15 C 0.7699(3) 0.3585(3) 0.3223(3) 0.0171(7) Uani 1 1 d . . . . .
C16 C 0.2133(18) 0.0359(11) 0.7756(17) 0.066(3) Uani 0.416(12) 1 d . . P A 1
H16A H 0.138153 0.024249 0.757687 0.099 Uiso 0.416(12) 1 calc GR . P A 1
H16B H 0.249834 0.039550 0.842314 0.099 Uiso 0.416(12) 1 calc GR . P A 1
H16C H 0.242869 -0.016765 0.753591 0.099 Uiso 0.416(12) 1 calc GR . P A 1
C16A C 0.1384(12) 0.0724(9) 0.6928(11) 0.066(3) Uani 0.584(12) 1 d . . P A 2
H16D H 0.134357 0.046641 0.634988 0.099 Uiso 0.584(12) 1 calc GR . P A 2
H16E H 0.074250 0.108735 0.681735 0.099 Uiso 0.584(12) 1 calc GR . P A 2
H16F H 0.145465 0.019521 0.734953 0.099 Uiso 0.584(12) 1 calc GR . P A 2
C17 C 0.3233(17) 0.1570(14) 0.7350(16) 0.073(3) Uani 0.441(14) 1 d . . P A 1
H17A H 0.375790 0.110846 0.773688 0.109 Uiso 0.441(14) 1 calc GR . P A 1
H17B H 0.343208 0.221644 0.760198 0.109 Uiso 0.441(14) 1 calc GR . P A 1
H17C H 0.319807 0.155013 0.673113 0.109 Uiso 0.441(14) 1 calc GR . P A 1
C17A C 0.3424(13) 0.0938(11) 0.7713(13) 0.073(3) Uani 0.559(14) 1 d . . P A 2
H17D H 0.348354 0.039954 0.812101 0.109 Uiso 0.559(14) 1 calc GR . P A 2
H17E H 0.392230 0.144230 0.805378 0.109 Uiso 0.559(14) 1 calc GR . P A 2
H17F H 0.358610 0.071809 0.720951 0.109 Uiso 0.559(14) 1 calc GR . P A 2
C18 C 0.1419(11) 0.1933(8) 0.7070(10) 0.0403(17) Uani 0.385(11) 1 d D . P A 1
H18 H 0.081218 0.168484 0.711686 0.048 Uiso 0.385(11) 1 calc R . P A 1
C18A C 0.2222(8) 0.2318(6) 0.7196(7) 0.0403(17) Uani 0.615(11) 1 d D . P A 2
H18A H 0.285799 0.267531 0.743354 0.048 Uiso 0.615(11) 1 calc R . P A 2
Dy1 Dy 0.10387(2) 0.45484(2) 0.65335(2) 0.02473(7) Uani 1 1 d . . . . .
Dy2 Dy 0.38253(2) -0.00626(2) 0.37249(2) 0.02064(7) Uani 1 1 d . . . . .
N1 N 0.2281(5) 0.1345(3) 0.7322(4) 0.0474(12) Uani 1 1 d D . . . .
O1 O 0.3047(3) 0.4235(2) 0.7022(2) 0.0260(6) Uani 1 1 d . . . . .
O2 O 0.4422(3) 0.5230(3) 0.7419(2) 0.0321(7) Uani 1 1 d . . . . .
O1W O -0.0758(3) 0.3784(3) 0.5882(3) 0.0451(11) Uani 1 1 d . . . . .
H1WA H -0.108068 0.392121 0.530309 0.068 Uiso 1 1 d GR . . . .
H1WB H -0.112323 0.400577 0.616455 0.068 Uiso 1 1 d GR . . . .
O3 O 0.4277(3) 0.1625(2) 0.4276(2) 0.0293(7) Uani 1 1 d . . . . .
O2W O 0.8918(5) 0.2121(5) 0.6634(4) 0.098(3) Uani 1 1 d . . . . .
H2WA H 0.929341 0.193836 0.719160 0.147 Uiso 1 1 d G . . . .
H2WB H 0.914980 0.184618 0.627247 0.147 Uiso 1 1 d G . . . .
O4 O 0.5321(3) 0.1665(2) 0.5807(2) 0.0269(7) Uani 1 1 d . . . . .
O5 O 0.0727(3) 0.4197(3) 0.4945(2) 0.0338(8) Uani 1 1 d . . . . .
O6 O 0.0000(3) 0.3952(3) 0.3440(2) 0.0325(7) Uani 1 1 d . . . . .
O7 O 0.0360(3) 0.0722(4) 0.2776(3) 0.0423(9) Uani 1 1 d . . . . .
O8 O 0.2106(3) 0.0735(2) 0.3356(2) 0.0262(6) Uani 1 1 d . . . . .
O9 O 0.5807(2) 0.0120(2) 0.4548(2) 0.0194(6) Uani 1 1 d . . . . .
O10 O 0.7146(3) 0.1019(2) 0.5459(2) 0.0285(7) Uani 1 1 d . . . . .
O11 O 0.8189(3) 0.3979(2) 0.4004(2) 0.0246(6) Uani 1 1 d . . . . .
O12 O 0.7648(2) 0.40105(19) 0.24911(18) 0.0174(5) Uani 1 1 d . . . . .
O13 O 0.1374(4) 0.2763(2) 0.6786(3) 0.0430(10) Uani 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.495(6) . ?
C1 Dy2 2.996(4) 4_566 ?
C1 O1 1.278(5) . ?
C1 O2 1.247(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.521(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.518(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.508(5) . ?
C5 O3 1.266(5) . ?
C5 O4 1.253(5) . ?
C6 C7 1.484(6) . ?
C6 O5 1.255(5) . ?
C6 O6 1.254(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.519(7) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.525(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.498(6) . ?
C10 Dy1 2.986(4) 4_565 ?
C10 O7 1.252(6) . ?
C10 O8 1.265(5) . ?
C11 C12 1.497(6) . ?
C11 Dy2 2.938(4) 3_656 ?
C11 O9 1.276(5) . ?
C11 O10 1.235(5) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.490(6) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.505(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.491(5) . ?
C15 Dy1 3.015(4) 3_666 ?
C15 O11 1.253(5) . ?
C15 O12 1.271(4) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16 N1 1.564(18) . ?
C16A H16D 0.9600 . ?
C16A H16E 0.9600 . ?
C16A H16F 0.9600 . ?
C16A N1 1.405(14) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N1 1.32(2) . ?
C17A H17D 0.9600 . ?
C17A H17E 0.9600 . ?
C17A H17F 0.9600 . ?
C17A N1 1.528(16) . ?
C18 H18 0.9300 . ?
C18 N1 1.344(12) . ?
C18 O13 1.212(12) . ?
C18A H18A 0.9300 . ?
C18A N1 1.343(9) . ?
C18A O13 1.228(9) . ?
Dy1 Dy2 3.9970(4) 4_566 ?
Dy1 O1 2.564(3) . ?
Dy1 O1W 2.468(3) . ?
Dy1 O5 2.413(3) . ?
Dy1 O6 2.506(4) 3_566 ?
Dy1 O7 2.530(4) 4_566 ?
Dy1 O8 2.657(3) 4_566 ?
Dy1 O11 2.579(3) 3_666 ?
Dy1 O12 2.677(3) 3_666 ?
Dy1 O13 2.484(3) . ?
Dy2 Dy2 3.9693(5) 3_656 ?
Dy2 O1 2.695(3) 4_565 ?
Dy2 O2 2.531(4) 4_565 ?
Dy2 O3 2.451(3) . ?
Dy2 O4 2.446(3) 3_656 ?
Dy2 O8 2.434(3) . ?
Dy2 O9 2.562(3) 3_656 ?
Dy2 O9 2.483(3) . ?
Dy2 O10 2.567(3) 3_656 ?
Dy2 O12 2.473(3) 2_645 ?
O1W H1WA 0.8539 . ?
O1W H1WB 0.8539 . ?
O2W H2WA 0.8503 . ?
O2W H2WB 0.8500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 Dy2 174.9(3) . 4_566 ?
O1 C1 C2 118.6(4) . . ?
O1 C1 Dy2 64.1(2) . 4_566 ?
O2 C1 C2 120.9(4) . . ?
O2 C1 Dy2 56.5(2) . 4_566 ?
O2 C1 O1 120.5(4) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 C3 110.7(4) . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C2 C3 H3A 108.9 . . ?
C2 C3 H3B 108.9 . . ?
H3A C3 H3B 107.7 . . ?
C4 C3 C2 113.4(4) . . ?
C4 C3 H3A 108.9 . . ?
C4 C3 H3B 108.9 . . ?
C3 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C5 C4 C3 114.1(4) . . ?
C5 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
O3 C5 C4 116.7(4) . . ?
O4 C5 C4 118.1(4) . . ?
O4 C5 O3 125.2(4) . . ?
O5 C6 C7 120.2(4) . . ?
O6 C6 C7 118.6(4) . . ?
O6 C6 O5 121.1(4) . . ?
C6 C7 H7A 108.9 . . ?
C6 C7 H7B 108.9 . . ?
C6 C7 C8 113.2(4) . . ?
H7A C7 H7B 107.8 . . ?
C8 C7 H7A 108.9 . . ?
C8 C7 H7B 108.9 . . ?
C7 C8 H8A 109.2 . . ?
C7 C8 H8B 109.2 . . ?
C7 C8 C9 112.0(4) . . ?
H8A C8 H8B 107.9 . . ?
C9 C8 H8A 109.2 . . ?
C9 C8 H8B 109.2 . . ?
C8 C9 H9A 109.4 . . ?
C8 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
C10 C9 C8 111.1(4) . . ?
C10 C9 H9A 109.4 . . ?
C10 C9 H9B 109.4 . . ?
C9 C10 Dy1 175.4(3) . 4_565 ?
O7 C10 C9 118.5(4) . . ?
O7 C10 Dy1 56.9(2) . 4_565 ?
O7 C10 O8 119.6(4) . . ?
O8 C10 C9 121.8(4) . . ?
O8 C10 Dy1 62.7(2) . 4_565 ?
C12 C11 Dy2 171.1(4) . 3_656 ?
O9 C11 C12 118.7(4) . . ?
O9 C11 Dy2 60.5(2) . 3_656 ?
O10 C11 C12 121.2(4) . . ?
O10 C11 Dy2 60.6(2) . 3_656 ?
O10 C11 O9 120.1(4) . . ?
C11 C12 H12A 108.3 . . ?
C11 C12 H12B 108.3 . . ?
H12A C12 H12B 107.4 . . ?
C13 C12 C11 115.9(4) . . ?
C13 C12 H12A 108.3 . . ?
C13 C12 H12B 108.3 . . ?
C12 C13 H13A 109.1 . . ?
C12 C13 H13B 109.1 . . ?
C12 C13 C14 112.4(4) . . ?
H13A C13 H13B 107.9 . . ?
C14 C13 H13A 109.1 . . ?
C14 C13 H13B 109.1 . . ?
C13 C14 H14A 108.4 . . ?
C13 C14 H14B 108.4 . . ?
H14A C14 H14B 107.4 . . ?
C15 C14 C13 115.7(4) . . ?
C15 C14 H14A 108.4 . . ?
C15 C14 H14B 108.4 . . ?
C14 C15 Dy1 175.3(3) . 3_666 ?
O11 C15 C14 121.7(4) . . ?
O11 C15 Dy1 57.95(19) . 3_666 ?
O11 C15 O12 120.2(3) . . ?
O12 C15 C14 118.1(3) . . ?
O12 C15 Dy1 62.51(19) . 3_666 ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
N1 C16A H16D 109.5 . . ?
N1 C16A H16E 109.5 . . ?
N1 C16A H16F 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
N1 C17A H17D 109.5 . . ?
N1 C17A H17E 109.5 . . ?
N1 C17A H17F 109.5 . . ?
N1 C18 H18 117.6 . . ?
O13 C18 H18 117.6 . . ?
O13 C18 N1 124.9(12) . . ?
N1 C18A H18A 118.2 . . ?
O13 C18A H18A 118.2 . . ?
O13 C18A N1 123.6(8) . . ?
C10 Dy1 C15 101.24(11) 4_566 3_666 ?
C10 Dy1 Dy2 59.54(9) 4_566 4_566 ?
C15 Dy1 Dy2 56.79(7) 3_666 4_566 ?
O1 Dy1 C10 92.16(12) . 4_566 ?
O1 Dy1 C15 67.48(10) . 3_666 ?
O1 Dy1 Dy2 41.76(7) . 4_566 ?
O1 Dy1 O8 67.45(10) . 4_566 ?
O1 Dy1 O11 72.08(10) . 3_666 ?
O1 Dy1 O12 64.67(9) . 3_666 ?
O1W Dy1 C10 90.71(12) . 4_566 ?
O1W Dy1 C15 146.12(13) . 3_666 ?
O1W Dy1 Dy2 149.24(8) . 4_566 ?
O1W Dy1 O1 144.33(14) . . ?
O1W Dy1 O6 83.02(15) . 3_566 ?
O1W Dy1 O7 68.51(13) . 4_566 ?
O1W Dy1 O8 112.93(11) . 4_566 ?
O1W Dy1 O11 131.97(11) . 3_666 ?
O1W Dy1 O12 149.75(13) . 3_666 ?
O1W Dy1 O13 74.71(15) . . ?
O5 Dy1 C10 159.32(11) . 4_566 ?
O5 Dy1 C15 98.19(11) . 3_666 ?
O5 Dy1 Dy2 128.65(10) . 4_566 ?
O5 Dy1 O1 88.76(12) . . ?
O5 Dy1 O1W 76.83(13) . . ?
O5 Dy1 O6 109.06(12) . 3_566 ?
O5 Dy1 O7 144.82(13) . 4_566 ?
O5 Dy1 O8 151.25(12) . 4_566 ?
O5 Dy1 O11 74.32(11) . 3_666 ?
O5 Dy1 O12 121.89(11) . 3_666 ?
O5 Dy1 O13 84.95(13) . . ?
O6 Dy1 C10 85.27(11) 3_566 4_566 ?
O6 Dy1 C15 66.76(12) 3_566 3_666 ?
O6 Dy1 Dy2 100.64(8) 3_566 4_566 ?
O6 Dy1 O1 132.66(11) 3_566 . ?
O6 Dy1 O7 73.12(14) 3_566 4_566 ?
O6 Dy1 O8 99.15(11) 3_566 4_566 ?
O6 Dy1 O11 71.45(12) 3_566 3_666 ?
O6 Dy1 O12 68.79(10) 3_566 3_666 ?
O7 Dy1 C10 24.49(12) 4_566 4_566 ?
O7 Dy1 C15 113.78(13) 4_566 3_666 ?
O7 Dy1 Dy2 83.22(9) 4_566 4_566 ?
O7 Dy1 O1 116.15(11) 4_566 . ?
O7 Dy1 O8 49.52(11) 4_566 4_566 ?
O7 Dy1 O11 134.91(13) 4_566 3_666 ?
O7 Dy1 O12 92.18(12) 4_566 3_666 ?
O8 Dy1 C10 25.04(11) 4_566 4_566 ?
O8 Dy1 C15 87.68(10) 4_566 3_666 ?
O8 Dy1 Dy2 36.34(7) 4_566 4_566 ?
O8 Dy1 O12 63.34(9) 4_566 3_666 ?
O11 Dy1 C10 125.49(10) 3_666 4_566 ?
O11 Dy1 C15 24.32(9) 3_666 3_666 ?
O11 Dy1 Dy2 76.91(7) 3_666 4_566 ?
O11 Dy1 O8 110.86(9) 3_666 4_566 ?
O11 Dy1 O12 49.15(9) 3_666 3_666 ?
O12 Dy1 C10 76.68(10) 3_666 4_566 ?
O12 Dy1 C15 24.90(9) 3_666 3_666 ?
O12 Dy1 Dy2 37.30(5) 3_666 4_566 ?
O13 Dy1 C10 75.78(13) . 4_566 ?
O13 Dy1 C15 138.85(13) . 3_666 ?
O13 Dy1 Dy2 89.32(10) . 4_566 ?
O13 Dy1 O1 71.60(12) . . ?
O13 Dy1 O6 150.32(14) . 3_566 ?
O13 Dy1 O7 80.51(15) . 4_566 ?
O13 Dy1 O8 72.66(12) . 4_566 ?
O13 Dy1 O11 138.23(13) . 3_666 ?
O13 Dy1 O12 126.55(11) . 3_666 ?
C1 Dy2 Dy2 132.21(8) 4_565 3_656 ?
C11 Dy2 C1 166.94(11) 3_656 4_565 ?
C11 Dy2 Dy2 59.20(8) 3_656 3_656 ?
O1 Dy2 C1 25.24(11) 4_565 4_565 ?
O1 Dy2 C11 150.20(11) 4_565 3_656 ?
O1 Dy2 Dy2 144.02(7) 4_565 3_656 ?
O2 Dy2 C1 24.27(12) 4_565 4_565 ?
O2 Dy2 C11 153.67(12) 4_565 3_656 ?
O2 Dy2 Dy2 115.49(8) 4_565 3_656 ?
O2 Dy2 O1 49.49(10) 4_565 4_565 ?
O2 Dy2 O9 151.73(11) 4_565 3_656 ?
O2 Dy2 O10 141.05(12) 4_565 3_656 ?
O3 Dy2 C1 94.37(11) . 4_565 ?
O3 Dy2 C11 96.71(11) . 3_656 ?
O3 Dy2 Dy2 67.79(8) . 3_656 ?
O3 Dy2 O1 84.00(10) . 4_565 ?
O3 Dy2 O2 104.80(13) . 4_565 ?
O3 Dy2 O9 70.21(11) . . ?
O3 Dy2 O9 75.08(10) . 3_656 ?
O3 Dy2 O10 114.02(12) . 3_656 ?
O3 Dy2 O12 139.48(10) . 2_645 ?
O4 Dy2 C1 105.97(12) 3_656 4_565 ?
O4 Dy2 C11 70.36(12) 3_656 3_656 ?
O4 Dy2 Dy2 69.53(7) 3_656 3_656 ?
O4 Dy2 O1 128.06(10) 3_656 4_565 ?
O4 Dy2 O2 83.57(12) 3_656 4_565 ?
O4 Dy2 O3 135.82(11) 3_656 . ?
O4 Dy2 O9 78.18(10) 3_656 3_656 ?
O4 Dy2 O9 69.66(10) 3_656 . ?
O4 Dy2 O10 71.08(12) 3_656 3_656 ?
O4 Dy2 O12 84.69(10) 3_656 2_645 ?
O8 Dy2 C1 93.54(12) . 4_565 ?
O8 Dy2 C11 82.73(11) . 3_656 ?
O8 Dy2 Dy2 120.98(8) . 3_656 ?
O8 Dy2 O1 68.63(10) . 4_565 ?
O8 Dy2 O2 117.22(11) . 4_565 ?
O8 Dy2 O3 74.86(12) . . ?
O8 Dy2 O4 139.92(12) . 3_656 ?
O8 Dy2 O9 90.36(10) . 3_656 ?
O8 Dy2 O9 144.72(10) . . ?
O8 Dy2 O10 72.17(11) . 3_656 ?
O8 Dy2 O12 69.57(10) . 2_645 ?
O9 Dy2 C1 93.84(11) . 4_565 ?
O9 Dy2 C1 167.39(10) 3_656 4_565 ?
O9 Dy2 C11 25.67(10) 3_656 3_656 ?
O9 Dy2 C11 96.41(10) . 3_656 ?
O9 Dy2 Dy2 37.42(7) 3_656 3_656 ?
O9 Dy2 Dy2 38.83(7) . 3_656 ?
O9 Dy2 O1 153.73(9) 3_656 4_565 ?
O9 Dy2 O1 111.61(10) . 4_565 ?
O9 Dy2 O2 77.24(11) . 4_565 ?
O9 Dy2 O9 76.25(11) . 3_656 ?
O9 Dy2 O10 118.17(10) . 3_656 ?
O9 Dy2 O10 50.19(9) 3_656 3_656 ?
O10 Dy2 C1 142.34(10) 3_656 4_565 ?
O10 Dy2 C11 24.78(10) 3_656 3_656 ?
O10 Dy2 Dy2 83.23(7) 3_656 3_656 ?
O10 Dy2 O1 130.17(10) 3_656 4_565 ?
O12 Dy2 C1 69.59(10) 2_645 4_565 ?
O12 Dy2 C11 97.42(10) 2_645 3_656 ?
O12 Dy2 Dy2 149.43(6) 2_645 3_656 ?
O12 Dy2 O1 65.58(9) 2_645 4_565 ?
O12 Dy2 O2 75.96(11) 2_645 4_565 ?
O12 Dy2 O9 144.60(9) 2_645 . ?
O12 Dy2 O9 122.95(9) 2_645 3_656 ?
O12 Dy2 O10 72.76(9) 2_645 3_656 ?
C16A N1 C17A 121.2(9) . . ?
C17 N1 C16 119.6(13) . . ?
C17 N1 C18 127.0(11) . . ?
C18 N1 C16 112.7(11) . . ?
C18A N1 C16A 123.1(8) . . ?
C18A N1 C17A 114.1(8) . . ?
C1 O1 Dy1 133.9(3) . . ?
C1 O1 Dy2 90.7(3) . 4_566 ?
Dy1 O1 Dy2 98.92(11) . 4_566 ?
C1 O2 Dy2 99.2(3) . 4_566 ?
Dy1 O1W H1WA 109.3 . . ?
Dy1 O1W H1WB 109.5 . . ?
H1WA O1W H1WB 109.3 . . ?
C5 O3 Dy2 136.0(3) . . ?
H2WA O2W H2WB 109.5 . . ?
C5 O4 Dy2 135.8(3) . 3_656 ?
C6 O5 Dy1 158.6(3) . . ?
C6 O6 Dy1 111.3(3) . 3_566 ?
C10 O7 Dy1 98.6(3) . 4_565 ?
C10 O8 Dy1 92.2(3) . 4_565 ?
C10 O8 Dy2 148.8(3) . . ?
Dy2 O8 Dy1 103.38(11) . 4_565 ?
C11 O9 Dy2 137.3(3) . . ?
C11 O9 Dy2 93.8(2) . 3_656 ?
Dy2 O9 Dy2 103.75(11) . 3_656 ?
C11 O10 Dy2 94.7(2) . 3_656 ?
C15 O11 Dy1 97.7(2) . 3_666 ?
C15 O12 Dy1 92.6(2) . 3_666 ?
C15 O12 Dy2 131.1(3) . 2_655 ?
Dy2 O12 Dy1 101.72(9) 2_655 3_666 ?
C18 O13 Dy1 163.0(8) . . ?
C18A O13 Dy1 129.9(5) . . ?

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
C1 C2 C3 C4 178.2(4) . . . . ?
C2 C1 O1 Dy1 -81.8(5) . . . . ?
C2 C1 O1 Dy2 175.1(3) . . . 4_566 ?
C2 C1 O2 Dy2 -174.8(3) . . . 4_566 ?
C2 C3 C4 C5 -172.6(4) . . . . ?
C3 C4 C5 O3 147.3(4) . . . . ?
C3 C4 C5 O4 -33.9(6) . . . . ?
C4 C5 O3 Dy2 -152.8(3) . . . . ?
C4 C5 O4 Dy2 -178.9(3) . . . 3_656 ?
C6 C7 C8 C9 171.6(4) . . . . ?
C7 C6 O5 Dy1 -29.5(12) . . . . ?
C7 C6 O6 Dy1 176.0(3) . . . 3_566 ?
C7 C8 C9 C10 -69.6(6) . . . . ?
C8 C9 C10 O7 -58.4(6) . . . . ?
C8 C9 C10 O8 119.9(5) . . . . ?
C9 C10 O7 Dy1 -179.4(3) . . . 4_565 ?
C9 C10 O8 Dy1 179.6(4) . . . 4_565 ?
C9 C10 O8 Dy2 58.9(7) . . . . ?
C11 C12 C13 C14 179.8(5) . . . . ?
C12 C11 O9 Dy2 -169.9(4) . . . 3_656 ?
C12 C11 O9 Dy2 -54.8(6) . . . . ?
C12 C11 O10 Dy2 169.9(4) . . . 3_656 ?
C12 C13 C14 C15 174.9(5) . . . . ?
C13 C14 C15 O11 4.4(7) . . . . ?
C13 C14 C15 O12 -175.2(4) . . . . ?
C14 C15 O11 Dy1 174.5(4) . . . 3_666 ?
C14 C15 O12 Dy1 -174.8(4) . . . 3_666 ?
C14 C15 O12 Dy2 77.2(5) . . . 2_655 ?
Dy1 C10 O8 Dy2 -120.7(5) 4_565 . . . ?
Dy1 C15 O12 Dy2 -108.0(3) 3_666 . . 2_655 ?
Dy2 C1 O1 Dy1 103.1(3) 4_566 . . . ?
Dy2 C11 O9 Dy2 115.1(4) 3_656 . . . ?
N1 C18 O13 Dy1 -134.8(19) . . . . ?
N1 C18A O13 Dy1 176.5(6) . . . . ?
O1 C1 C2 C3 -72.5(5) . . . . ?
O1 C1 O2 Dy2 3.0(5) . . . 4_566 ?
O2 C1 C2 C3 105.4(5) . . . . ?
O2 C1 O1 Dy1 100.3(5) . . . . ?
O2 C1 O1 Dy2 -2.8(4) . . . 4_566 ?
O3 C5 O4 Dy2 -0.2(7) . . . 3_656 ?
O4 C5 O3 Dy2 28.5(7) . . . . ?
O5 C6 C7 C8 93.2(5) . . . . ?
O5 C6 O6 Dy1 -2.5(5) . . . 3_566 ?
O6 C6 C7 C8 -85.3(6) . . . . ?
O6 C6 O5 Dy1 149.0(7) . . . . ?
O7 C10 O8 Dy1 -2.1(5) . . . 4_565 ?
O7 C10 O8 Dy2 -122.8(5) . . . . ?
O8 C10 O7 Dy1 2.3(5) . . . 4_565 ?
O9 C11 C12 C13 166.0(5) . . . . ?
O9 C11 O10 Dy2 -11.2(4) . . . 3_656 ?
O10 C11 C12 C13 -15.1(8) . . . . ?
O10 C11 O9 Dy2 126.3(4) . . . . ?
O10 C11 O9 Dy2 11.2(4) . . . 3_656 ?
O11 C15 O12 Dy1 5.6(4) . . . 3_666 ?
O11 C15 O12 Dy2 -102.4(4) . . . 2_655 ?
O12 C15 O11 Dy1 -5.9(4) . . . 3_666 ?
O13 C18 N1 C16 173.9(14) . . . . ?
O13 C18 N1 C17 3(2) . . . . ?
O13 C18A N1 C16A 5.4(15) . . . . ?
O13 C18A N1 C17A 170.8(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.310 0.644 0.414 26.6 4.4 '1 water'
2 0.310 0.856 0.914 26.6 3.4 '1 water'
3 0.690 0.144 0.086 26.6 5.0 '1 water'
4 0.690 0.356 0.586 26.6 4.0 '1 water'


_olex2_submission_special_instructions 'No special instructions were received'
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Without Acceptor       O2W      --H2WB     .     Please Check 
RESPONSE:The disordered water molecule occupies a cavity of the
structure with no suitable acceptor atoms in its surroundings
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx_CCDC4
_database_code_depnum_ccdc_archive 'CCDC 1866433'
loop_
_audit_author_name
_audit_author_address
'subash Chandra Sahoo'
;Panjab University chandigarh
India
;
_audit_update_record             
;
2019-08-01 deposited with the CCDC.	2019-08-13 downloaded from the CCDC.
;
_audit_creation_date             2019-04-10
_audit_creation_method           
;
Olex2 1.2-ac3
(compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H27 N O14 Pr2, H2 O'
_chemical_formula_sum            'C18 H29 N O15 Pr2'
_chemical_formula_weight         781.24
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 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                   13.700(6)
_cell_length_b                   13.662(6)
_cell_length_c                   15.835(7)
_cell_angle_alpha                90
_cell_angle_beta                 114.812(10)
_cell_angle_gamma                90
_cell_volume                     2690.2(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8088
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.21
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.648
_exptl_absorpt_correction_T_max  0.725
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_process_details   
'SADABS-2008/1 - Bruker AXS area detector scaling and absorption correction'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.929
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       bLOCK
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48527
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.383
_diffrn_reflns_theta_min         2.057
_diffrn_ambient_temperature      302.27
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-III CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6107
_reflns_number_total             6724
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.563
_refine_diff_density_min         -1.266
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         6724
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0207
_refine_ls_restrained_S_all      1.133
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0223P)²+2.5799P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0514
_refine_ls_wR_factor_ref         0.0532
_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 C(H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C18A) = Uanis(C18)
Uanis(C16A) = Uanis(C16)
Uanis(C17) = Uanis(C17A)
3. Others
 Sof(C18)=Sof(H18)=1-FVAR(1)
 Sof(C18A)=Sof(H18A)=FVAR(1)
 Sof(C16)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(2)
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(2)
 Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(3)
 Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(3)
4.a Free rotating group:
 O2W(H2WA,H2WB)
4.b Rotating group:
 O1W(H1WA,H1WB)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B)
4.d Aromatic/amide H refined with riding coordinates:
 C18A(H18A), C18(H18)
4.e Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C16(H16D,H16E,H16F), C17(H17A,H17B,H17C), C17A(H17D,
 H17E,H17F)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.26964(18) 0.35845(17) 0.82220(16) 0.0237(4) Uani 1 1 d . . . . .
C2 C 0.2155(3) 0.2616(2) 0.81144(19) 0.0382(7) Uani 1 1 d . . . . .
H2A H 0.249950 0.215612 0.785873 0.046 Uiso 1 1 calc R . . . .
H2B H 0.141301 0.268385 0.766647 0.046 Uiso 1 1 calc R . . . .
C3 C 0.2170(3) 0.2188(2) 0.9001(2) 0.0405(7) Uani 1 1 d . . . . .
H3A H 0.290749 0.205037 0.943004 0.049 Uiso 1 1 calc R . . . .
H3B H 0.188352 0.266437 0.929103 0.049 Uiso 1 1 calc R . . . .
C4 C 0.1524(3) 0.1266(2) 0.88208(19) 0.0452(8) Uani 1 1 d . . . . .
H4A H 0.079027 0.141293 0.838868 0.054 Uiso 1 1 calc R . . . .
H4B H 0.180899 0.080146 0.851919 0.054 Uiso 1 1 calc R . . . .
C5 C 0.15005(19) 0.07874(18) 0.96622(16) 0.0247(5) Uani 1 1 d . . . . .
C6 C 0.3756(2) 0.57847(19) 0.65355(17) 0.0286(5) Uani 1 1 d . . . . .
C7 C 0.3738(3) 0.5941(2) 0.55875(19) 0.0378(6) Uani 1 1 d . . . . .
H7A H 0.299911 0.598905 0.512723 0.045 Uiso 1 1 calc R . . . .
H7B H 0.406706 0.538430 0.542795 0.045 Uiso 1 1 calc R . . . .
C8 C 0.4346(3) 0.6877(2) 0.5570(2) 0.0360(6) Uani 1 1 d . . . . .
H8A H 0.505010 0.687241 0.608975 0.043 Uiso 1 1 calc R . . . .
H8B H 0.444832 0.689843 0.499997 0.043 Uiso 1 1 calc R . . . .
C9 C 0.3731(2) 0.7780(2) 0.5629(2) 0.0410(7) Uani 1 1 d . . . . .
H9A H 0.307281 0.783064 0.506426 0.049 Uiso 1 1 calc R . . . .
H9B H 0.353505 0.770751 0.614705 0.049 Uiso 1 1 calc R . . . .
C10 C 0.4368(2) 0.87033(19) 0.57540(17) 0.0276(5) Uani 1 1 d . . . . .
C11 C 0.0323(2) 0.70440(18) 0.49415(17) 0.0269(5) Uani 1 1 d . . . . .
C12 C 0.0644(2) 0.8100(2) 0.49158(18) 0.0336(6) Uani 1 1 d . . . . .
H12A H 0.134264 0.820879 0.542525 0.040 Uiso 1 1 calc R . . . .
H12B H 0.013160 0.851986 0.501628 0.040 Uiso 1 1 calc R . . . .
C13 C 0.0699(3) 0.8399(2) 0.40135(19) 0.0358(6) Uani 1 1 d . . . . .
H13A H -0.001801 0.837152 0.351297 0.043 Uiso 1 1 calc R . . . .
H13B H 0.114456 0.793442 0.387214 0.043 Uiso 1 1 calc R . . . .
C14 C 0.1152(2) 0.9421(2) 0.40533(19) 0.0327(6) Uani 1 1 d . . . . .
H14A H 0.068846 0.989514 0.416047 0.039 Uiso 1 1 calc R . . . .
H14B H 0.185836 0.946264 0.456685 0.039 Uiso 1 1 calc R . . . .
C15 C 0.1234(2) 0.96590(19) 0.31555(17) 0.0282(5) Uani 1 1 d . . . . .
C18A C 0.3601(7) 0.6934(6) 0.2931(6) 0.0470(10) Uani 0.415(6) 1 d . . P A 1
H18A H 0.420985 0.669010 0.288337 0.056 Uiso 0.415(6) 1 calc R . P A 1
C18 C 0.2765(5) 0.7321(4) 0.2790(4) 0.0470(10) Uani 0.585(6) 1 d . . P A 2
H18 H 0.212757 0.767707 0.254067 0.056 Uiso 0.585(6) 1 calc R . P A 2
C16A C 0.1768(9) 0.6597(9) 0.2656(9) 0.082(2) Uani 0.444(8) 1 d . . P A 1
H16A H 0.173021 0.639203 0.322097 0.122 Uiso 0.444(8) 1 calc GR . P A 1
H16B H 0.120477 0.628727 0.213484 0.122 Uiso 0.444(8) 1 calc GR . P A 1
H16C H 0.168562 0.729507 0.259495 0.122 Uiso 0.444(8) 1 calc GR . P A 1
C16 C 0.1595(7) 0.5925(7) 0.2308(7) 0.082(2) Uani 0.556(8) 1 d . . P A 2
H16D H 0.147236 0.564571 0.281090 0.122 Uiso 0.556(8) 1 calc GR . P A 2
H16E H 0.151549 0.542819 0.185509 0.122 Uiso 0.556(8) 1 calc GR . P A 2
H16F H 0.108294 0.643839 0.202229 0.122 Uiso 0.556(8) 1 calc GR . P A 2
C17 C 0.3618(7) 0.5726(6) 0.3076(7) 0.0757(19) Uani 0.577(7) 1 d . . P A 2
H17A H 0.364146 0.529024 0.260888 0.114 Uiso 0.577(7) 1 calc GR . P A 2
H17B H 0.356389 0.535192 0.356741 0.114 Uiso 0.577(7) 1 calc GR . P A 2
H17C H 0.426246 0.611281 0.332285 0.114 Uiso 0.577(7) 1 calc GR . P A 2
C17A C 0.2865(10) 0.5349(7) 0.2237(10) 0.0757(19) Uani 0.423(7) 1 d . . P A 1
H17D H 0.327601 0.546091 0.188233 0.114 Uiso 0.423(7) 1 calc GR . P A 1
H17E H 0.217077 0.509406 0.183679 0.114 Uiso 0.423(7) 1 calc GR . P A 1
H17F H 0.323426 0.488558 0.272313 0.114 Uiso 0.423(7) 1 calc GR . P A 1
N1 N 0.2724(3) 0.6343(2) 0.2679(2) 0.0568(8) Uani 1 1 d . . . . .
O1 O 0.26474(13) 0.40107(12) 0.74887(11) 0.0245(3) Uani 1 1 d . . . . .
O2 O 0.31884(16) 0.39801(14) 0.90033(12) 0.0318(4) Uani 1 1 d . . . . .
O1W O 0.57659(18) 0.8799(2) 0.41166(15) 0.0549(7) Uani 1 1 d . . . . .
H1WA H 0.575135 0.821416 0.387711 0.082 Uiso 1 1 d GR . . . .
H1WB H 0.601114 0.873344 0.472422 0.082 Uiso 1 1 d GR . . . .
O3 O 0.08043(14) 0.01181(13) 0.95468(12) 0.0266(4) Uani 1 1 d . . . . .
O2W O 0.6068(3) 0.7115(3) 0.3372(2) 0.1144(18) Uani 1 1 d . . . . .
H2WA H 0.654670 0.673941 0.375021 0.172 Uiso 1 1 d G . . . .
H2WB H 0.590842 0.692870 0.281812 0.172 Uiso 1 1 d G . . . .
O4 O 0.21447(16) 0.10269(15) 1.04615(13) 0.0363(4) Uani 1 1 d . . . . .
O5 O 0.28967(15) 0.57370(15) 0.66432(13) 0.0335(4) Uani 1 1 d . . . . .
O6 O 0.46355(18) 0.5719(2) 0.72227(15) 0.0524(6) Uani 1 1 d . . . . .
O7 O 0.42741(19) 0.91994(16) 0.50545(15) 0.0429(5) Uani 1 1 d . . . . .
O8 O 0.50064(17) 0.89526(17) 0.65611(14) 0.0418(5) Uani 1 1 d . . . . .
O9 O 0.07239(17) 0.66201(14) 0.57224(14) 0.0375(4) Uani 1 1 d . . . . .
O10 O -0.03184(16) 0.66605(14) 0.41920(13) 0.0342(4) Uani 1 1 d . . . . .
O11 O 0.19577(16) 0.92347(14) 0.29786(14) 0.0337(4) Uani 1 1 d . . . . .
O12 O 0.05783(16) 1.02317(18) 0.25773(14) 0.0399(5) Uani 1 1 d . . . . .
O13 O 0.3630(2) 0.77652(16) 0.32168(18) 0.0524(6) Uani 1 1 d . . . . .
Pr1 Pr 0.11746(2) 0.49374(2) 0.62747(2) 0.01928(4) Uani 1 1 d . . . . .
Pr2 Pr 0.39610(2) 0.95488(2) 0.34657(2) 0.02331(4) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.491(3) . ?
C1 O1 1.275(3) . ?
C1 O2 1.256(3) . ?
C1 Pr2 3.015(2) 4_576 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.513(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.497(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.496(3) . ?
C5 O3 1.278(3) . ?
C5 O4 1.245(3) . ?
C5 Pr1 2.942(3) 4_566 ?
C6 C7 1.506(3) . ?
C6 O5 1.260(3) . ?
C6 O6 1.243(3) . ?
C6 Pr2 2.984(3) 4_576 ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.534(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.519(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C9 C10 1.499(4) . ?
C10 O7 1.258(3) . ?
C10 O8 1.255(3) . ?
C11 C12 1.514(3) . ?
C11 O9 1.263(3) . ?
C11 O10 1.257(3) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C12 C13 1.518(4) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C13 C14 1.519(4) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C14 C15 1.508(4) . ?
C15 O11 1.277(3) . ?
C15 O12 1.252(3) . ?
C15 Pr1 2.996(3) 4_575 ?
C18A H18A 0.9300 . ?
C18A N1 1.361(9) . ?
C18A O13 1.217(8) . ?
C18 H18 0.9300 . ?
C18 N1 1.346(6) . ?
C18 O13 1.248(6) . ?
C16A H16A 0.9600 . ?
C16A H16B 0.9600 . ?
C16A H16C 0.9600 . ?
C16A N1 1.340(12) . ?
C16 H16D 0.9600 . ?
C16 H16E 0.9600 . ?
C16 H16F 0.9600 . ?
C16 N1 1.517(9) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17 N1 1.400(8) . ?
C17A H17D 0.9600 . ?
C17A H17E 0.9600 . ?
C17A H17F 0.9600 . ?
C17A N1 1.576(11) . ?
O1 Pr1 2.4727(17) . ?
O1 Pr2 2.6775(18) 4_576 ?
O2 Pr2 2.5768(19) 4_576 ?
O1W H1WA 0.8810 . ?
O1W H1WB 0.8805 . ?
O1W Pr2 2.467(2) . ?
O3 Pr1 2.479(2) 2_546 ?
O3 Pr1 2.566(2) 4_566 ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8499 . ?
O4 Pr1 2.568(2) 4_566 ?
O5 Pr1 2.438(2) . ?
O5 Pr2 2.660(2) 4_576 ?
O6 Pr2 2.528(2) 4_576 ?
O7 Pr2 2.416(2) . ?
O8 Pr2 2.499(2) 3_676 ?
O9 Pr1 2.445(2) . ?
O10 Pr1 2.441(2) 3_566 ?
O11 Pr1 2.698(2) 4_575 ?
O11 Pr2 2.556(2) . ?
O12 Pr1 2.528(2) 4_575 ?
O13 Pr2 2.480(2) . ?
Pr1 Pr1 3.9725(13) 3_566 ?

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
C2 C1 Pr2 175.19(19) . 4_576 ?
O1 C1 C2 117.9(2) . . ?
O1 C1 Pr2 62.51(12) . 4_576 ?
O2 C1 C2 122.0(2) . . ?
O2 C1 O1 120.1(2) . . ?
O2 C1 Pr2 57.85(12) . 4_576 ?
C1 C2 H2A 108.5 . . ?
C1 C2 H2B 108.5 . . ?
C1 C2 C3 115.1(2) . . ?
H2A C2 H2B 107.5 . . ?
C3 C2 H2A 108.5 . . ?
C3 C2 H2B 108.5 . . ?
C2 C3 H3A 109.2 . . ?
C2 C3 H3B 109.2 . . ?
H3A C3 H3B 107.9 . . ?
C4 C3 C2 111.8(2) . . ?
C4 C3 H3A 109.2 . . ?
C4 C3 H3B 109.2 . . ?
C3 C4 H4A 108.4 . . ?
C3 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
C5 C4 C3 115.5(2) . . ?
C5 C4 H4A 108.4 . . ?
C5 C4 H4B 108.4 . . ?
C4 C5 Pr1 170.9(2) . 4_566 ?
O3 C5 C4 118.6(2) . . ?
O3 C5 Pr1 60.48(12) . 4_566 ?
O4 C5 C4 121.3(2) . . ?
O4 C5 O3 120.1(2) . . ?
O4 C5 Pr1 60.48(13) . 4_566 ?
C7 C6 Pr2 175.9(2) . 4_576 ?
O5 C6 C7 121.1(2) . . ?
O5 C6 Pr2 62.96(13) . 4_576 ?
O6 C6 C7 119.1(3) . . ?
O6 C6 O5 119.7(2) . . ?
O6 C6 Pr2 56.79(15) . 4_576 ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 C8 110.8(2) . . ?
H7A C7 H7B 108.1 . . ?
C8 C7 H7A 109.5 . . ?
C8 C7 H7B 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 108.0 . . ?
C9 C8 C7 110.9(2) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
C8 C9 H9A 109.1 . . ?
C8 C9 H9B 109.1 . . ?
H9A C9 H9B 107.8 . . ?
C10 C9 C8 112.6(2) . . ?
C10 C9 H9A 109.1 . . ?
C10 C9 H9B 109.1 . . ?
O7 C10 C9 119.9(3) . . ?
O8 C10 C9 118.8(2) . . ?
O8 C10 O7 121.4(3) . . ?
O9 C11 C12 116.8(2) . . ?
O10 C11 C12 117.9(2) . . ?
O10 C11 O9 125.3(2) . . ?
C11 C12 H12A 108.7 . . ?
C11 C12 H12B 108.7 . . ?
C11 C12 C13 114.3(2) . . ?
H12A C12 H12B 107.6 . . ?
C13 C12 H12A 108.7 . . ?
C13 C12 H12B 108.7 . . ?
C12 C13 H13A 109.0 . . ?
C12 C13 H13B 109.0 . . ?
C12 C13 C14 112.9(2) . . ?
H13A C13 H13B 107.8 . . ?
C14 C13 H13A 109.0 . . ?
C14 C13 H13B 109.0 . . ?
C13 C14 H14A 109.6 . . ?
C13 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
C15 C14 C13 110.5(2) . . ?
C15 C14 H14A 109.6 . . ?
C15 C14 H14B 109.6 . . ?
C14 C15 Pr1 174.37(18) . 4_575 ?
O11 C15 C14 118.8(2) . . ?
O11 C15 Pr1 64.23(13) . 4_575 ?
O12 C15 C14 120.6(3) . . ?
O12 C15 O11 120.6(2) . . ?
O12 C15 Pr1 56.37(14) . 4_575 ?
N1 C18A H18A 118.3 . . ?
O13 C18A H18A 118.3 . . ?
O13 C18A N1 123.3(7) . . ?
N1 C18 H18 119.0 . . ?
O13 C18 H18 119.0 . . ?
O13 C18 N1 122.1(5) . . ?
H16A C16A H16B 109.5 . . ?
H16A C16A H16C 109.5 . . ?
H16B C16A H16C 109.5 . . ?
N1 C16A H16A 109.5 . . ?
N1 C16A H16B 109.5 . . ?
N1 C16A H16C 109.5 . . ?
H16D C16 H16E 109.5 . . ?
H16D C16 H16F 109.5 . . ?
H16E C16 H16F 109.5 . . ?
N1 C16 H16D 109.5 . . ?
N1 C16 H16E 109.5 . . ?
N1 C16 H16F 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
N1 C17A H17D 109.5 . . ?
N1 C17A H17E 109.5 . . ?
N1 C17A H17F 109.5 . . ?
C18A N1 C17A 112.6(6) . . ?
C18 N1 C16 113.8(5) . . ?
C18 N1 C17 124.0(5) . . ?
C16A N1 C18A 125.9(7) . . ?
C16A N1 C17A 120.8(7) . . ?
C17 N1 C16 120.4(5) . . ?
C1 O1 Pr1 130.97(16) . . ?
C1 O1 Pr2 92.50(14) . 4_576 ?
Pr1 O1 Pr2 101.78(6) . 4_576 ?
C1 O2 Pr2 97.78(15) . 4_576 ?
H1WA O1W H1WB 107.9 . . ?
Pr2 O1W H1WA 111.0 . . ?
Pr2 O1W H1WB 110.8 . . ?
C5 O3 Pr1 93.84(14) . 4_566 ?
C5 O3 Pr1 137.11(16) . 2_546 ?
Pr1 O3 Pr1 103.88(7) 2_546 4_566 ?
H2WA O2W H2WB 109.5 . . ?
C5 O4 Pr1 94.57(15) . 4_566 ?
C6 O5 Pr1 148.87(18) . . ?
C6 O5 Pr2 92.09(15) . 4_576 ?
Pr1 O5 Pr2 103.22(7) . 4_576 ?
C6 O6 Pr2 98.92(17) . 4_576 ?
C10 O7 Pr2 158.6(2) . . ?
C10 O8 Pr2 111.24(18) . 3_676 ?
C11 O9 Pr1 136.21(18) . . ?
C11 O10 Pr1 135.66(17) . 3_566 ?
C15 O11 Pr1 90.55(15) . 4_575 ?
C15 O11 Pr2 133.76(17) . . ?
Pr2 O11 Pr1 99.05(6) . 4_575 ?
C15 O12 Pr1 99.27(17) . 4_575 ?
C18A O13 Pr2 162.1(5) . . ?
C18 O13 Pr2 129.3(3) . . ?
C5 Pr1 C15 166.87(7) 4_565 4_576 ?
C5 Pr1 Pr1 59.06(5) 4_565 3_566 ?
C15 Pr1 Pr1 132.44(5) 4_576 3_566 ?
O1 Pr1 C5 97.52(7) . 4_565 ?
O1 Pr1 C15 69.42(7) . 4_576 ?
O1 Pr1 O3 123.06(6) . 4_565 ?
O1 Pr1 O3 144.59(6) . 2_556 ?
O1 Pr1 O4 72.66(6) . 4_565 ?
O1 Pr1 O11 65.47(6) . 4_576 ?
O1 Pr1 O12 75.91(7) . 4_576 ?
O1 Pr1 Pr1 149.42(4) . 3_566 ?
O3 Pr1 C5 96.25(7) 2_556 4_565 ?
O3 Pr1 C5 25.68(6) 4_565 4_565 ?
O3 Pr1 C15 167.45(6) 4_565 4_576 ?
O3 Pr1 C15 94.06(7) 2_556 4_576 ?
O3 Pr1 O3 76.12(7) 2_556 4_565 ?
O3 Pr1 O4 50.40(6) 4_565 4_565 ?
O3 Pr1 O4 118.04(6) 2_556 4_565 ?
O3 Pr1 O11 153.68(6) 4_565 4_576 ?
O3 Pr1 O11 111.80(6) 2_556 4_576 ?
O3 Pr1 O12 77.32(7) 2_556 4_576 ?
O3 Pr1 Pr1 37.28(4) 4_565 3_566 ?
O3 Pr1 Pr1 38.84(4) 2_556 3_566 ?
O4 Pr1 C5 24.95(6) 4_565 4_565 ?
O4 Pr1 C15 142.07(6) 4_565 4_576 ?
O4 Pr1 O11 130.09(6) 4_565 4_576 ?
O4 Pr1 Pr1 83.20(5) 4_565 3_566 ?
O5 Pr1 C5 82.79(7) . 4_565 ?
O5 Pr1 C15 93.42(7) . 4_576 ?
O5 Pr1 O1 69.60(7) . . ?
O5 Pr1 O3 144.73(7) . 2_556 ?
O5 Pr1 O3 90.39(6) . 4_565 ?
O5 Pr1 O4 72.39(7) . 4_565 ?
O5 Pr1 O9 74.82(7) . . ?
O5 Pr1 O10 140.07(7) . 3_566 ?
O5 Pr1 O11 68.54(6) . 4_576 ?
O5 Pr1 O12 117.21(7) . 4_576 ?
O5 Pr1 Pr1 120.92(5) . 3_566 ?
O9 Pr1 C5 96.52(7) . 4_565 ?
O9 Pr1 C15 94.59(7) . 4_576 ?
O9 Pr1 O1 139.53(6) . . ?
O9 Pr1 O3 70.26(7) . 2_556 ?
O9 Pr1 O3 74.88(6) . 4_565 ?
O9 Pr1 O4 114.15(7) . 4_565 ?
O9 Pr1 O11 84.16(7) . 4_576 ?
O9 Pr1 O12 104.97(8) . 4_576 ?
O9 Pr1 Pr1 67.71(5) . 3_566 ?
O10 Pr1 C5 70.42(7) 3_566 4_565 ?
O10 Pr1 C15 105.94(7) 3_566 4_576 ?
O10 Pr1 O1 84.79(6) 3_566 . ?
O10 Pr1 O3 78.22(6) 3_566 4_565 ?
O10 Pr1 O3 69.47(6) 3_566 2_556 ?
O10 Pr1 O4 70.95(8) 3_566 4_565 ?
O10 Pr1 O9 135.67(7) 3_566 . ?
O10 Pr1 O11 128.06(6) 3_566 4_576 ?
O10 Pr1 O12 83.48(7) 3_566 4_576 ?
O10 Pr1 Pr1 69.47(5) 3_566 3_566 ?
O11 Pr1 C5 150.16(7) 4_576 4_565 ?
O11 Pr1 C15 25.22(7) 4_576 4_576 ?
O11 Pr1 Pr1 144.17(4) 4_576 3_566 ?
O12 Pr1 C5 153.65(7) 4_576 4_565 ?
O12 Pr1 C15 24.36(7) 4_576 4_576 ?
O12 Pr1 O3 151.69(6) 4_576 4_565 ?
O12 Pr1 O4 140.77(7) 4_576 4_565 ?
O12 Pr1 O11 49.57(7) 4_576 4_576 ?
O12 Pr1 Pr1 115.58(6) 4_576 3_566 ?
C1 Pr2 Pr1 56.80(4) 4_575 4_575 ?
C6 Pr2 C1 101.29(7) 4_575 4_575 ?
C6 Pr2 Pr1 59.52(6) 4_575 4_575 ?
O1 Pr2 C1 24.99(5) 4_575 4_575 ?
O1 Pr2 C6 76.63(6) 4_575 4_575 ?
O1 Pr2 Pr1 37.26(4) 4_575 4_575 ?
O2 Pr2 C1 24.37(6) 4_575 4_575 ?
O2 Pr2 C6 125.60(6) 4_575 4_575 ?
O2 Pr2 O1 49.30(6) 4_575 4_575 ?
O2 Pr2 O5 111.02(6) 4_575 4_575 ?
O2 Pr2 Pr1 76.98(4) 4_575 4_575 ?
O1W Pr2 C1 145.68(8) . 4_575 ?
O1W Pr2 C6 90.67(7) . 4_575 ?
O1W Pr2 O1 149.25(8) . 4_575 ?
O1W Pr2 O2 131.64(7) . 4_575 ?
O1W Pr2 O5 112.91(7) . 4_575 ?
O1W Pr2 O6 68.62(8) . 4_575 ?
O1W Pr2 O8 82.65(9) . 3_676 ?
O1W Pr2 O11 144.81(8) . . ?
O1W Pr2 O13 75.10(9) . . ?
O1W Pr2 Pr1 149.31(5) . 4_575 ?
O5 Pr2 C1 87.78(6) 4_575 4_575 ?
O5 Pr2 C6 24.94(7) 4_575 4_575 ?
O5 Pr2 O1 63.35(6) 4_575 4_575 ?
O5 Pr2 Pr1 36.41(4) 4_575 4_575 ?
O6 Pr2 C1 113.63(8) 4_575 4_575 ?
O6 Pr2 C6 24.29(7) 4_575 4_575 ?
O6 Pr2 O1 91.90(8) 4_575 4_575 ?
O6 Pr2 O2 134.85(8) 4_575 4_575 ?
O6 Pr2 O5 49.23(7) 4_575 4_575 ?
O6 Pr2 O11 115.96(7) 4_575 . ?
O6 Pr2 Pr1 82.97(6) 4_575 4_575 ?
O7 Pr2 C1 98.15(7) . 4_575 ?
O7 Pr2 C6 159.34(7) . 4_575 ?
O7 Pr2 O1 121.97(7) . 4_575 ?
O7 Pr2 O2 74.22(7) . 4_575 ?
O7 Pr2 O1W 76.94(8) . . ?
O7 Pr2 O5 151.38(8) . 4_575 ?
O7 Pr2 O6 145.01(8) . 4_575 ?
O7 Pr2 O8 108.98(7) . 3_676 ?
O7 Pr2 O11 88.85(7) . . ?
O7 Pr2 O13 84.95(8) . . ?
O7 Pr2 Pr1 128.75(6) . 4_575 ?
O8 Pr2 C1 66.67(8) 3_676 4_575 ?
O8 Pr2 C6 85.32(7) 3_676 4_575 ?
O8 Pr2 O1 68.66(7) 3_676 4_575 ?
O8 Pr2 O2 71.38(8) 3_676 4_575 ?
O8 Pr2 O5 99.11(7) 3_676 4_575 ?
O8 Pr2 O6 73.19(8) 3_676 4_575 ?
O8 Pr2 O11 132.54(7) 3_676 . ?
O8 Pr2 Pr1 100.52(5) 3_676 4_575 ?
O11 Pr2 C1 67.48(7) . 4_575 ?
O11 Pr2 C6 92.15(7) . 4_575 ?
O11 Pr2 O1 64.71(6) . 4_575 ?
O11 Pr2 O2 72.11(7) . 4_575 ?
O11 Pr2 O5 67.52(6) . 4_575 ?
O11 Pr2 Pr1 41.79(5) . 4_575 ?
O13 Pr2 C1 138.91(8) . 4_575 ?
O13 Pr2 C6 75.81(8) . 4_575 ?
O13 Pr2 O1 126.63(7) . 4_575 ?
O13 Pr2 O2 138.22(8) . 4_575 ?
O13 Pr2 O5 72.71(7) . 4_575 ?
O13 Pr2 O6 80.58(9) . 4_575 ?
O13 Pr2 O8 150.40(9) . 3_676 ?
O13 Pr2 O11 71.66(8) . . ?
O13 Pr2 Pr1 89.43(6) . 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
C1 C2 C3 C4 174.5(3) . . . . ?
C2 C1 O1 Pr1 77.4(3) . . . . ?
C2 C1 O1 Pr2 -174.6(2) . . . 4_576 ?
C2 C1 O2 Pr2 174.3(2) . . . 4_576 ?
C2 C3 C4 C5 179.6(3) . . . . ?
C3 C4 C5 O3 166.3(3) . . . . ?
C3 C4 C5 O4 -14.0(5) . . . . ?
C4 C5 O3 Pr1 -54.4(4) . . . 2_546 ?
C4 C5 O3 Pr1 -169.6(2) . . . 4_566 ?
C4 C5 O4 Pr1 169.6(3) . . . 4_566 ?
C6 C7 C8 C9 -70.2(3) . . . . ?
C7 C6 O5 Pr1 59.2(5) . . . . ?
C7 C6 O5 Pr2 179.4(2) . . . 4_576 ?
C7 C6 O6 Pr2 -179.2(2) . . . 4_576 ?
C7 C8 C9 C10 171.6(2) . . . . ?
C8 C9 C10 O7 93.3(3) . . . . ?
C8 C9 C10 O8 -85.1(3) . . . . ?
C9 C10 O7 Pr2 -29.8(7) . . . . ?
C9 C10 O8 Pr2 176.05(19) . . . 3_676 ?
C11 C12 C13 C14 -173.1(2) . . . . ?
C12 C11 O9 Pr1 -152.4(2) . . . . ?
C12 C11 O10 Pr1 -179.12(18) . . . 3_566 ?
C12 C13 C14 C15 177.4(3) . . . . ?
C13 C14 C15 O11 -72.0(3) . . . . ?
C13 C14 C15 O12 105.2(3) . . . . ?
C14 C15 O11 Pr1 174.6(2) . . . 4_575 ?
C14 C15 O11 Pr2 -82.2(3) . . . . ?
C14 C15 O12 Pr1 -174.4(2) . . . 4_575 ?
N1 C18A O13 Pr2 -136.6(11) . . . . ?
N1 C18 O13 Pr2 176.8(3) . . . . ?
O1 C1 C2 C3 -175.5(3) . . . . ?
O1 C1 O2 Pr2 -5.7(3) . . . 4_576 ?
O2 C1 C2 C3 4.5(4) . . . . ?
O2 C1 O1 Pr1 -102.6(3) . . . . ?
O2 C1 O1 Pr2 5.4(2) . . . 4_576 ?
O3 C5 O4 Pr1 -10.7(3) . . . 4_566 ?
O4 C5 O3 Pr1 10.7(3) . . . 4_566 ?
O4 C5 O3 Pr1 125.8(2) . . . 2_546 ?
O5 C6 C7 C8 120.7(3) . . . . ?
O5 C6 O6 Pr2 2.0(3) . . . 4_576 ?
O6 C6 C7 C8 -58.1(4) . . . . ?
O6 C6 O5 Pr1 -122.1(3) . . . . ?
O6 C6 O5 Pr2 -1.9(3) . . . 4_576 ?
O7 C10 O8 Pr2 -2.3(3) . . . 3_676 ?
O8 C10 O7 Pr2 148.5(4) . . . . ?
O9 C11 C12 C13 147.5(3) . . . . ?
O9 C11 O10 Pr1 0.7(4) . . . 3_566 ?
O10 C11 C12 C13 -32.6(4) . . . . ?
O10 C11 O9 Pr1 27.7(4) . . . . ?
O11 C15 O12 Pr1 2.7(3) . . . 4_575 ?
O12 C15 O11 Pr1 -2.5(3) . . . 4_575 ?
O12 C15 O11 Pr2 100.6(3) . . . . ?
O13 C18A N1 C16A 4.0(13) . . . . ?
O13 C18A N1 C17A 173.9(8) . . . . ?
O13 C18 N1 C16 168.9(6) . . . . ?
O13 C18 N1 C17 4.5(9) . . . . ?
Pr1 C5 O3 Pr1 115.2(2) 4_566 . . 2_546 ?
Pr1 C15 O11 Pr2 103.12(19) 4_575 . . . ?
Pr2 C1 O1 Pr1 -107.98(17) 4_576 . . . ?
Pr2 C6 O5 Pr1 -120.2(3) 4_576 . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.183 0.134 0.582 24.6 5.2 '1 water'
2 0.183 0.366 0.082 24.6 4.5 '1 water'
3 0.817 0.634 0.918 24.6 4.8 '1 water'
4 0.817 0.866 0.418 24.6 4.2 '1 water'


_olex2_submission_special_instructions 'No special instructions were received'
