# 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 2024

####################################################################### 
# 
# 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 2201687'
loop_
_audit_author_name
_audit_author_address
'H. N. Sheikh'
;University of Jammu
India
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2024-01-12 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         'C9 H10 Dy N2 O9'
_chemical_formula_sum            'C9 H10 Dy N2 O9'
_chemical_formula_weight         452.69

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.980(3)
_cell_length_b                   10.190(2)
_cell_length_c                   10.555(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.591(6)
_cell_angle_gamma                90
_cell_volume                     1160.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4425
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      26.38

_exptl_crystal_description       Block
_exptl_crystal_colour            White
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.590
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    6.493
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_process_details   
'SADABS-2016/2 - 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-III CCD'
_diffrn_measurement_method       'φ and ω scans'

_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5413
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.0789
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.749
_diffrn_reflns_theta_max         26.379
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measured_fraction_theta_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.944
_reflns_number_total             2240
_reflns_number_gt                2068
_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)+(0.0384P)²+26.2292P] 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         2240
_refine_ls_number_parameters     211
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1278
_refine_ls_wR_factor_gt          0.1225
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.001

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 0.4157(11) 0.2099(12) 0.3793(11) 0.037(3) Uani 1 1 d . . . . .
C2 C 0.4681(10) 0.0898(11) 0.4471(12) 0.038(3) Uani 1 1 d D . . . .
C3 C 0.4621(14) 0.084(2) 0.5761(14) 0.134(13) Uani 1 1 d D . . . .
H3 H 0.432869 0.158377 0.612051 0.160 Uiso 1 1 calc R U . . .
C4 C 0.5061(16) 0.0175(16) 0.3458(16) 0.074(5) Uani 1 1 d D . . . .
H4 H 0.507886 0.034494 0.259561 0.089 Uiso 1 1 calc R U . . .
C5 C 0.1841(9) 0.7884(10) 0.3817(9) 0.0225(19) Uani 1 1 d . . . . .
C6 C 0.1754(8) 0.8988(9) 0.4727(9) 0.0190(18) Uani 1 1 d . . . . .
C7 C 0.1595(9) 1.0334(9) 0.4539(9) 0.0201(19) Uani 1 1 d . . . . .
H7 H 0.149754 1.079053 0.376452 0.024 Uiso 1 1 calc R U . . .
C8 C 0.1613(8) 1.0848(9) 0.5770(9) 0.0191(18) Uani 1 1 d . . . . .
C9 C 0.1420(8) 1.2174(9) 0.6252(9) 0.0195(18) Uani 1 1 d . . . . .
Dy1 Dy 0.21231(4) 0.44686(4) 0.39791(4) 0.01883(17) Uani 1 1 d . . . . .
N1 N 0.1899(8) 0.8780(8) 0.6019(8) 0.0236(17) Uani 1 1 d D . . . .
H1A H 0.195(11) 0.810(7) 0.647(9) 0.028 Uiso 1 1 d D U . . .
N2 N 0.1809(8) 0.9893(8) 0.6669(8) 0.0216(17) Uani 1 1 d . . . . .
O1 O 0.3676(8) 0.2909(8) 0.4428(10) 0.047(2) Uani 1 1 d . . . . .
O2 O 0.4179(14) 0.2121(13) 0.2605(11) 0.086(4) Uani 1 1 d . . . . .
O1W O 0.4029(7) 0.5536(9) 0.3716(10) 0.042(2) Uani 1 1 d D . . . .
H11W H 0.461(9) 0.543(11) 0.432(10) 0.050 Uiso 1 1 d D U . . .
H12W H 0.406(12) 0.633(4) 0.358(12) 0.050 Uiso 1 1 d D U . . .
O3 O 0.1809(7) 0.6731(7) 0.4236(7) 0.0281(16) Uani 1 1 d . . . . .
O2W O 0.3134(8) 0.5035(9) 0.6128(7) 0.0351(18) Uani 1 1 d D . . . .
H21W H 0.334(13) 0.442(8) 0.662(9) 0.042 Uiso 1 1 d D U . . .
H22W H 0.296(13) 0.560(8) 0.661(9) 0.042 Uiso 1 1 d D U . . .
O4 O 0.1915(7) 0.8215(7) 0.2680(7) 0.0310(17) Uani 1 1 d . . . . .
O3W O 0.0001(6) 0.4840(7) 0.3541(7) 0.0245(15) Uani 1 1 d D . . . .
H31W H -0.038(8) 0.547(7) 0.375(10) 0.029 Uiso 1 1 d D U . . .
H32W H -0.050(7) 0.447(9) 0.299(8) 0.029 Uiso 1 1 d D U . . .
O5 O 0.1248(7) 1.3119(6) 0.5469(7) 0.0261(15) Uani 1 1 d . . . . .
O6 O 0.1395(7) 1.2269(7) 0.7443(7) 0.0287(16) 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 O1 1.241(14) . ?
C1 O2 1.258(15) . ?
C1 C2 1.480(15) . ?
C2 C3 1.377(15) . ?
C2 C4 1.422(15) . ?
C2 C3 1.96(3) 3_656 ?
C3 C4 1.330(13) 3_656 ?
C3 H3 0.9300 . ?
C4 H4 0.9300 . ?
C5 O3 1.258(12) . ?
C5 O4 1.263(12) . ?
C5 C6 1.494(13) . ?
C6 N1 1.360(12) . ?
C6 C7 1.392(12) . ?
C7 C8 1.398(13) . ?
C7 H7 0.9300 . ?
C8 N2 1.349(12) . ?
C8 C9 1.472(12) . ?
C9 O5 1.260(11) . ?
C9 O6 1.266(12) . ?
Dy1 O1 2.315(7) . ?
Dy1 O3W 2.322(6) . ?
Dy1 O3 2.354(7) . ?
Dy1 O2W 2.405(8) . ?
Dy1 O5 2.417(7) 1_545 ?
Dy1 O1W 2.419(8) . ?
Dy1 O6 2.434(7) 4_575 ?
Dy1 N2 2.486(8) 4_575 ?
N1 N2 1.338(11) . ?
N1 H1A 0.84(8) . ?
O1W H11W 0.82(11) . ?
O1W H12W 0.82(5) . ?
O2W H21W 0.82(9) . ?
O2W H22W 0.81(9) . ?
O3W H31W 0.82(8) . ?
O3W H32W 0.81(8) . ?

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 C1 O2 127.9(13) . . ?
O1 C1 C2 117.0(11) . . ?
O2 C1 C2 114.8(12) . . ?
C3 C2 C4 142.7(13) . . ?
C3 C2 C1 115.4(13) . . ?
C4 C2 C1 101.9(11) . . ?
C3 C2 C3 100.1(15) . 3_656 ?
C1 C2 C3 144.3(11) . 3_656 ?
C4 C3 C2 126(2) 3_656 . ?
C4 C3 C2 46.4(10) 3_656 3_656 ?
C2 C3 C2 79.9(15) . 3_656 ?
C4 C3 H3 116.9 3_656 . ?
C2 C3 H3 116.9 . . ?
C2 C3 H3 163.2 3_656 . ?
C3 C4 C2 91.0(16) 3_656 . ?
C3 C4 H4 134.5 3_656 . ?
C2 C4 H4 134.5 . . ?
O3 C5 O4 126.5(9) . . ?
O3 C5 C6 117.9(9) . . ?
O4 C5 C6 115.6(9) . . ?
N1 C6 C7 106.5(8) . . ?
N1 C6 C5 121.2(8) . . ?
C7 C6 C5 132.2(9) . . ?
C6 C7 C8 104.9(8) . . ?
C6 C7 H7 127.5 . . ?
C8 C7 H7 127.5 . . ?
N2 C8 C7 110.8(8) . . ?
N2 C8 C9 115.7(8) . . ?
C7 C8 C9 133.4(9) . . ?
O5 C9 O6 124.4(9) . . ?
O5 C9 C8 119.2(8) . . ?
O6 C9 C8 116.3(8) . . ?
O1 Dy1 O3W 145.8(3) . . ?
O1 Dy1 O3 140.1(3) . . ?
O3W Dy1 O3 72.6(3) . . ?
O1 Dy1 O2W 77.1(3) . . ?
O3W Dy1 O2W 114.9(3) . . ?
O3 Dy1 O2W 73.0(3) . . ?
O1 Dy1 O5 80.9(3) . 1_545 ?
O3W Dy1 O5 73.6(3) . 1_545 ?
O3 Dy1 O5 113.5(2) . 1_545 ?
O2W Dy1 O5 72.1(3) . 1_545 ?
O1 Dy1 O1W 73.3(3) . . ?
O3W Dy1 O1W 139.6(3) . . ?
O3 Dy1 O1W 73.8(3) . . ?
O2W Dy1 O1W 75.0(3) . . ?
O5 Dy1 O1W 141.8(3) 1_545 . ?
O1 Dy1 O6 77.1(3) . 4_575 ?
O3W Dy1 O6 78.0(3) . 4_575 ?
O3 Dy1 O6 138.8(2) . 4_575 ?
O2W Dy1 O6 147.2(3) . 4_575 ?
O5 Dy1 O6 84.2(2) 1_545 4_575 ?
O1W Dy1 O6 115.8(3) . 4_575 ?
O1 Dy1 N2 110.1(3) . 4_575 ?
O3W Dy1 N2 79.0(3) . 4_575 ?
O3 Dy1 N2 81.9(3) . 4_575 ?
O2W Dy1 N2 145.0(3) . 4_575 ?
O5 Dy1 N2 141.9(3) 1_545 4_575 ?
O1W Dy1 N2 74.7(3) . 4_575 ?
O6 Dy1 N2 64.4(2) 4_575 4_575 ?
N2 N1 C6 112.1(8) . . ?
N2 N1 H1A 114(8) . . ?
C6 N1 H1A 133(8) . . ?
N1 N2 C8 105.6(8) . . ?
N1 N2 Dy1 135.6(6) . 4_576 ?
C8 N2 Dy1 118.4(6) . 4_576 ?
C1 O1 Dy1 135.8(8) . . ?
Dy1 O1W H11W 115(10) . . ?
Dy1 O1W H12W 122(10) . . ?
H11W O1W H12W 102(12) . . ?
C5 O3 Dy1 149.3(7) . . ?
Dy1 O2W H21W 116(9) . . ?
Dy1 O2W H22W 130(9) . . ?
H21W O2W H22W 102(9) . . ?
Dy1 O3W H31W 128(7) . . ?
Dy1 O3W H32W 126(7) . . ?
H31W O3W H32W 104(9) . . ?
C9 O5 Dy1 146.3(6) . 1_565 ?
C9 O6 Dy1 122.8(6) . 4_576 ?

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
O1 C1 C2 C3 -2.6(17) . . . . ?
O2 C1 C2 C3 -177.7(13) . . . . ?
O1 C1 C2 C4 176.1(13) . . . . ?
O2 C1 C2 C4 1.0(16) . . . . ?
O1 C1 C2 C3 170.5(12) . . . 3_656 ?
O2 C1 C2 C3 -5(2) . . . 3_656 ?
C4 C2 C3 C4 -4(3) . . . 3_656 ?
C1 C2 C3 C4 174.4(15) . . . 3_656 ?
C3 C2 C3 C4 -1.6(16) 3_656 . . 3_656 ?
C4 C2 C3 C2 -2.0(19) . . . 3_656 ?
C1 C2 C3 C2 175.9(12) . . . 3_656 ?
C3 C2 C3 C2 0.000(1) 3_656 . . 3_656 ?
C3 C2 C4 C3 3(3) . . . 3_656 ?
C1 C2 C4 C3 -175.2(12) . . . 3_656 ?
O3 C5 C6 N1 13.7(14) . . . . ?
O4 C5 C6 N1 -167.8(9) . . . . ?
O3 C5 C6 C7 -170.0(10) . . . . ?
O4 C5 C6 C7 8.5(16) . . . . ?
N1 C6 C7 C8 -2.1(10) . . . . ?
C5 C6 C7 C8 -178.8(10) . . . . ?
C6 C7 C8 N2 1.8(11) . . . . ?
C6 C7 C8 C9 -175.6(10) . . . . ?
N2 C8 C9 O5 179.0(9) . . . . ?
C7 C8 C9 O5 -3.7(16) . . . . ?
N2 C8 C9 O6 -3.4(12) . . . . ?
C7 C8 C9 O6 173.8(10) . . . . ?
C7 C6 N1 N2 1.8(11) . . . . ?
C5 C6 N1 N2 178.9(8) . . . . ?
C6 N1 N2 C8 -0.6(11) . . . . ?
C6 N1 N2 Dy1 -173.2(7) . . . 4_576 ?
C7 C8 N2 N1 -0.8(11) . . . . ?
C9 C8 N2 N1 177.1(8) . . . . ?
C7 C8 N2 Dy1 173.3(6) . . . 4_576 ?
C9 C8 N2 Dy1 -8.8(11) . . . 4_576 ?
O2 C1 O1 Dy1 23(2) . . . . ?
C2 C1 O1 Dy1 -151.7(9) . . . . ?
O4 C5 O3 Dy1 16(2) . . . . ?
C6 C5 O3 Dy1 -165.7(9) . . . . ?
O6 C9 O5 Dy1 118.2(11) . . . 1_565 ?
C8 C9 O5 Dy1 -64.5(15) . . . 1_565 ?
O5 C9 O6 Dy1 -167.7(7) . . . 4_576 ?
C8 C9 O6 Dy1 14.9(11) . . . 4_576 ?

_refine_diff_density_max         1.879
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.236

####################################################################### 
# 
# 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 2201688'
loop_
_audit_author_name
_audit_author_address
'H. N. Sheikh'
;University of Jammu
India
;
_audit_update_record             
;
2022-08-16 deposited with the CCDC.	2024-01-12 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         ?
_chemical_formula_sum            'C8 H9 Gd N2 O9'
_chemical_formula_weight         434.42

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'
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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.911(3)
_cell_length_b                   10.217(3)
_cell_length_c                   10.524(3)
_cell_angle_alpha                90
_cell_angle_beta                 100.378(6)
_cell_angle_gamma                90
_cell_volume                     1154.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1298
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      23.01

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.500
_exptl_crystal_F_000             828
_exptl_transmission_factor_min   0.167
_exptl_transmission_factor_max   0.444
_exptl_crystal_size_max          0.470
_exptl_crystal_size_mid          0.270
_exptl_crystal_size_min          0.140
_exptl_absorpt_coefficient_mu    5.799
_shelx_estimated_absorpt_T_min   0.171
_shelx_estimated_absorpt_T_max   0.497
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   Sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_number            10118
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.179
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_full        24.998
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             2010
_reflns_number_gt                1768
_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_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_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)+(0.0282P)²+21.8611P] 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         2010
_refine_ls_number_parameters     186
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_restrained_S_all      1.106
_refine_ls_shift/su_max          0.000
_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 0.6832(8) 0.7902(8) 0.3813(7) 0.0116(17) Uani 1 1 d . . . . .
C2 C 0.6770(8) 0.9006(8) 0.4711(7) 0.0106(16) Uani 1 1 d . . . . .
C3 C 0.6585(8) 1.0336(8) 0.4525(8) 0.0126(17) Uani 1 1 d . . . . .
H3 H 0.647102 1.079787 0.375184 0.015 Uiso 1 1 calc R U . . .
C4 C 0.6609(8) 1.0825(8) 0.5772(8) 0.0130(17) Uani 1 1 d . . . . .
C5 C 0.6423(7) 1.2175(8) 0.6242(8) 0.0112(17) Uani 1 1 d . . . . .
C6 C 0.9159(9) 0.2078(9) 0.3773(9) 0.020(2) Uani 1 1 d . . . . .
C7 C 0.9697(8) 0.0886(9) 0.4489(10) 0.022(2) Uani 1 1 d . . . . .
C8 C 0.9565(15) 0.0969(16) 0.5869(15) 0.010(2) Uiso 0.5 1 d . U P . .
H8 H 0.926462 0.170982 0.622510 0.012 Uiso 0.5 1 calc R U P . .
C9 C 0.9898(15) -0.0058(15) 0.6517(15) 0.010(2) Uiso 0.5 1 d . U P . .
H9 H 0.988959 -0.024145 0.738147 0.012 Uiso 0.5 1 calc R U P . .
Gd1 Gd 0.71279(4) 0.44846(4) 0.39951(4) 0.01002(15) Uani 1 1 d . . . . .
N1 N 0.6909(6) 0.8779(6) 0.6003(7) 0.0114(14) Uani 1 1 d . . . . .
N2 N 0.6815(7) 0.9880(7) 0.6657(7) 0.0131(15) Uani 1 1 d . . . . .
O1 O 0.6816(5) 0.6754(5) 0.4230(5) 0.0136(12) Uani 1 1 d . . . . .
O2 O 0.6917(5) 0.8225(5) 0.2662(5) 0.0141(12) Uani 1 1 d . . . . .
O3 O 0.6398(6) 1.2259(5) 0.7452(5) 0.0178(13) Uani 1 1 d . . . . .
O4 O 0.6253(6) 1.3110(5) 0.5464(5) 0.0151(13) Uani 1 1 d . . . . .
O5 O 0.8738(6) 0.2938(6) 0.4420(7) 0.0315(17) Uani 1 1 d . . . . .
O6 O 0.9161(10) 0.2116(9) 0.2578(8) 0.062(3) Uani 1 1 d . . . . .
O7 O 0.9051(6) 0.5598(7) 0.3773(6) 0.0295(16) Uani 1 1 d . . . . .
H7A H 0.897557 0.641081 0.391123 0.044 Uiso 1 1 d R U . . .
H7B H 0.915392 0.555472 0.299177 0.044 Uiso 1 1 d R U . . .
O8 O 0.4956(5) 0.4859(6) 0.3531(5) 0.0138(12) Uani 1 1 d . . . . .
H8A H 0.466722 0.486477 0.422945 0.021 Uiso 1 1 d R U . . .
H8B H 0.460095 0.421037 0.311109 0.021 Uiso 1 1 d R U . . .
O9 O 0.8142(5) 0.5054(6) 0.6165(6) 0.0191(14) Uani 1 1 d . . . . .
H9A H 0.820075 0.437838 0.664344 0.029 Uiso 1 1 d R U . . .
H9B H 0.767446 0.557099 0.649359 0.029 Uiso 1 1 d R U . . .
H1 H 0.700(10) 0.793(11) 0.654(10) 0.03(3) Uiso 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 O1 1.254(10) . ?
C1 O2 1.275(10) . ?
C1 C2 1.481(11) . ?
C2 N1 1.360(10) . ?
C2 C3 1.382(11) . ?
C3 C4 1.400(12) . ?
C3 H3 0.9300 . ?
C4 N2 1.333(11) . ?
C4 C5 1.492(11) . ?
C5 O4 1.250(10) . ?
C5 O3 1.281(10) . ?
C6 O5 1.249(11) . ?
C6 O6 1.258(12) . ?
C6 C7 1.496(12) . ?
C7 C9 1.484(18) 3_756 ?
C7 C8 1.487(18) . ?
C8 C9 1.27(2) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
Gd1 O5 2.345(6) . ?
Gd1 O1 2.363(5) . ?
Gd1 O8 2.363(6) . ?
Gd1 O4 2.410(6) 1_545 ?
Gd1 O9 2.423(6) . ?
Gd1 O7 2.435(7) . ?
Gd1 O3 2.445(6) 4_575 ?
Gd1 N2 2.508(7) 4_575 ?
N1 N2 1.332(9) . ?
N1 H1 1.03(11) . ?
O7 H7A 0.8501 . ?
O7 H7B 0.8501 . ?
O8 H8A 0.8500 . ?
O8 H8B 0.8501 . ?
O9 H9A 0.8501 . ?
O9 H9B 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
O1 C1 O2 125.7(7) . . ?
O1 C1 C2 118.9(7) . . ?
O2 C1 C2 115.4(7) . . ?
N1 C2 C3 107.2(7) . . ?
N1 C2 C1 119.9(7) . . ?
C3 C2 C1 132.9(7) . . ?
C2 C3 C4 103.9(7) . . ?
C2 C3 H3 128.0 . . ?
C4 C3 H3 128.0 . . ?
N2 C4 C3 111.6(7) . . ?
N2 C4 C5 117.0(7) . . ?
C3 C4 C5 131.3(7) . . ?
O4 C5 O3 125.0(7) . . ?
O4 C5 C4 120.1(7) . . ?
O3 C5 C4 114.8(7) . . ?
O5 C6 O6 126.2(10) . . ?
O5 C6 C7 116.5(8) . . ?
O6 C6 C7 117.2(9) . . ?
C9 C7 C8 145.4(11) 3_756 . ?
C9 C7 C6 104.1(9) 3_756 . ?
C8 C7 C6 110.3(9) . . ?
C9 C8 C7 114.2(14) . . ?
C9 C8 H8 122.9 . . ?
C7 C8 H8 122.9 . . ?
C8 C9 C7 100.4(13) . 3_756 ?
C8 C9 H9 129.8 . . ?
C7 C9 H9 129.8 3_756 . ?
O5 Gd1 O1 139.3(2) . . ?
O5 Gd1 O8 146.9(2) . . ?
O1 Gd1 O8 72.8(2) . . ?
O5 Gd1 O4 81.6(2) . 1_545 ?
O1 Gd1 O4 115.1(2) . 1_545 ?
O8 Gd1 O4 74.2(2) . 1_545 ?
O5 Gd1 O9 77.4(2) . . ?
O1 Gd1 O9 73.5(2) . . ?
O8 Gd1 O9 115.3(2) . . ?
O4 Gd1 O9 72.7(2) 1_545 . ?
O5 Gd1 O7 72.8(3) . . ?
O1 Gd1 O7 72.2(2) . . ?
O8 Gd1 O7 139.0(2) . . ?
O4 Gd1 O7 141.4(2) 1_545 . ?
O9 Gd1 O7 73.9(2) . . ?
O5 Gd1 O3 77.2(2) . 4_575 ?
O1 Gd1 O3 138.47(19) . 4_575 ?
O8 Gd1 O3 77.7(2) . 4_575 ?
O4 Gd1 O3 83.22(19) 1_545 4_575 ?
O9 Gd1 O3 147.1(2) . 4_575 ?
O7 Gd1 O3 117.4(2) . 4_575 ?
O5 Gd1 N2 109.1(2) . 4_575 ?
O1 Gd1 N2 81.5(2) . 4_575 ?
O8 Gd1 N2 78.5(2) . 4_575 ?
O4 Gd1 N2 141.3(2) 1_545 4_575 ?
O9 Gd1 N2 145.2(2) . 4_575 ?
O7 Gd1 N2 75.6(2) . 4_575 ?
O3 Gd1 N2 64.3(2) 4_575 4_575 ?
N2 N1 C2 111.6(7) . . ?
N2 N1 H1 116(6) . . ?
C2 N1 H1 133(6) . . ?
N1 N2 C4 105.6(7) . . ?
N1 N2 Gd1 135.8(5) . 4_576 ?
C4 N2 Gd1 118.3(5) . 4_576 ?
C1 O1 Gd1 150.5(5) . . ?
C5 O3 Gd1 123.3(5) . 4_576 ?
C5 O4 Gd1 146.8(5) . 1_565 ?
C6 O5 Gd1 134.9(6) . . ?
Gd1 O7 H7A 109.1 . . ?
Gd1 O7 H7B 109.5 . . ?
H7A O7 H7B 104.5 . . ?
Gd1 O8 H8A 109.7 . . ?
Gd1 O8 H8B 109.1 . . ?
H8A O8 H8B 104.5 . . ?
Gd1 O9 H9A 109.6 . . ?
Gd1 O9 H9B 109.1 . . ?
H9A O9 H9B 104.5 . . ?

_refine_diff_density_max         4.498
_refine_diff_density_min         -0.972
_refine_diff_density_rms         0.233

