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

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

data_14
_database_code_depnum_ccdc_archive 'CCDC 2035253'
loop_
_audit_author_name
_audit_author_address
'Ying-Bing Lu'
;College of Chemistry and Chemical Engineering, Gannan Normal University
China
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 '[Eu(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2' 
;
_chemical_name_common            '[Eu(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[Eu(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_formula_sum            'C54 H38 Cl4 Eu2 N16 O12'
_chemical_formula_weight         1548.72

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.0689(3)
_cell_length_b                   11.6727(3)
_cell_length_c                   21.7296(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5420(10)
_cell_angle_gamma                90.00
_cell_volume                     3051.58(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blcok
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1528
_exptl_absorpt_coefficient_mu    2.285
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6328
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44951
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0192
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.40
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6951
_reflns_number_gt                5897
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0349P)²+13.2785P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6951
_refine_ls_number_parameters     397
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0346
_refine_ls_wR_factor_ref         0.0922
_refine_ls_wR_factor_gt          0.0829
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.008
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.605572(16) 0.872744(17) 0.492215(9) 0.02692(7) Uani 1 1 d . . .
Cl2 Cl 0.72227(11) 0.70591(13) 0.76878(6) 0.0498(3) Uani 1 1 d . . .
Cl1 Cl 0.37640(8) 0.89609(9) 0.47918(5) 0.0340(2) Uani 1 1 d . . .
C17 C 0.6714(5) 0.3841(4) 0.4622(3) 0.0572(15) Uani 1 1 d . . .
H17 H 0.6982 0.3112 0.4723 0.069 Uiso 1 1 calc R . .
C12 C 0.8904(4) 0.8671(4) 0.5274(2) 0.0359(9) Uani 1 1 d . . .
C25 C 0.4895(4) 0.9459(4) 0.6232(2) 0.0356(9) Uani 1 1 d . . .
C7 C 0.9769(4) 0.8087(5) 0.4336(3) 0.0479(12) Uani 1 1 d . . .
C1 C 0.8054(4) 0.9300(5) 0.6123(2) 0.0430(11) Uani 1 1 d . . .
H1 H 0.7414 0.9503 0.6308 0.052 Uiso 1 1 calc R . .
C11 C 0.8804(4) 0.8337(4) 0.4639(2) 0.0365(10) Uani 1 1 d . . .
C22 C 0.4925(4) 0.7251(5) 0.3638(2) 0.0443(11) Uani 1 1 d . . .
H22 H 0.4580 0.7953 0.3558 0.053 Uiso 1 1 calc R . .
C24 C 0.6394(4) 0.5828(4) 0.4926(2) 0.0322(9) Uani 1 1 d . . .
C23 C 0.5899(4) 0.6033(4) 0.4314(2) 0.0329(9) Uani 1 1 d . . .
C20 C 0.5337(5) 0.5390(5) 0.3286(3) 0.0539(14) Uani 1 1 d . . .
H20 H 0.5325 0.4841 0.2976 0.065 Uiso 1 1 calc R . .
C21 C 0.4857(5) 0.6432(5) 0.3173(3) 0.0531(14) Uani 1 1 d . . .
H21 H 0.4488 0.6593 0.2790 0.064 Uiso 1 1 calc R . .
C19 C 0.5853(4) 0.5150(4) 0.3876(2) 0.0429(11) Uani 1 1 d . . .
C10 C 0.7704(5) 0.8054(5) 0.3736(2) 0.0514(13) Uani 1 1 d . . .
H10 H 0.7006 0.8054 0.3522 0.062 Uiso 1 1 calc R . .
C4 C 0.9958(4) 0.8752(4) 0.5589(3) 0.0458(12) Uani 1 1 d . . .
C2 C 0.9083(5) 0.9403(5) 0.6468(3) 0.0508(13) Uani 1 1 d . . .
H2 H 0.9116 0.9666 0.6873 0.061 Uiso 1 1 calc R . .
C13 C 0.6840(5) 0.6491(5) 0.5910(2) 0.0455(12) Uani 1 1 d . . .
H13 H 0.6888 0.7093 0.6191 0.055 Uiso 1 1 calc R . .
C15 C 0.7161(5) 0.4524(5) 0.5698(3) 0.0550(14) Uani 1 1 d . . .
H15 H 0.7410 0.3800 0.5823 0.066 Uiso 1 1 calc R . .
C14 C 0.7186(5) 0.5407(5) 0.6115(3) 0.0555(14) Uani 1 1 d . . .
H14 H 0.7430 0.5286 0.6527 0.067 Uiso 1 1 calc R . .
C26 C 0.4924(6) 0.9158(6) 0.6913(2) 0.0598(16) Uani 1 1 d . . .
H26A H 0.4776 0.8345 0.6951 0.072 Uiso 1 1 calc R . .
H26B H 0.5667 0.9301 0.7101 0.072 Uiso 1 1 calc R . .
C16 C 0.6761(4) 0.4715(4) 0.5088(2) 0.0431(11) Uani 1 1 d . . .
N5 N 0.4147(5) 0.9778(6) 0.7250(2) 0.0759(18) Uani 1 1 d . . .
C3 C 1.0018(5) 0.9119(5) 0.6208(3) 0.0560(14) Uani 1 1 d . . .
H3 H 1.0703 0.9165 0.6435 0.067 Uiso 1 1 calc R . .
C18 C 0.6292(5) 0.4051(5) 0.4045(3) 0.0581(15) Uani 1 1 d . . .
H18 H 0.6286 0.3473 0.3751 0.070 Uiso 1 1 calc R . .
C8 C 0.9641(5) 0.7789(6) 0.3714(3) 0.0602(16) Uani 1 1 d . . .
H8 H 1.0260 0.7599 0.3505 0.072 Uiso 1 1 calc R . .
C9 C 0.8621(5) 0.7779(6) 0.3415(3) 0.0617(16) Uani 1 1 d . . .
H9 H 0.8530 0.7589 0.2998 0.074 Uiso 1 1 calc R . .
C5 C 1.0923(4) 0.8508(5) 0.5266(3) 0.0600(16) Uani 1 1 d . . .
H5 H 1.1626 0.8576 0.5471 0.072 Uiso 1 1 calc R . .
C6 C 1.0829(4) 0.8186(6) 0.4674(3) 0.0602(16) Uani 1 1 d . . .
H6 H 1.1468 0.8022 0.4478 0.072 Uiso 1 1 calc R . .
N3 N 0.6447(3) 0.6709(3) 0.53350(17) 0.0355(8) Uani 1 1 d . . .
N1 N 0.7951(3) 0.8926(3) 0.55428(17) 0.0340(8) Uani 1 1 d . . .
N4 N 0.5457(3) 0.7089(3) 0.41914(17) 0.0352(8) Uani 1 1 d . . .
N2 N 0.7772(3) 0.8316(4) 0.43340(18) 0.0385(9) Uani 1 1 d . . .
N6 N 0.3059(8) 0.9530(9) 0.7229(4) 0.120(3) Uani 1 1 d U . .
N8 N 0.3460(12) 1.1077(11) 0.7812(5) 0.153(4) Uani 1 1 d U . .
N7 N 0.2707(8) 1.0361(9) 0.7618(4) 0.116(3) Uani 1 1 d U . .
C27 C 0.4324(13) 1.0677(11) 0.7603(4) 0.140(5) Uani 1 1 d . . .
H27A H 0.5026 1.0994 0.7691 0.168 Uiso 1 1 calc R . .
O1 O 0.5503(3) 0.8844(3) 0.59318(14) 0.0369(7) Uani 1 1 d . . .
O2 O 0.4311(3) 1.0291(3) 0.60393(14) 0.0368(7) Uani 1 1 d . . .
O4 O 0.7213(6) 0.7461(8) 0.8264(3) 0.144(3) Uani 1 1 d U . .
O6 O 0.7688(7) 0.7715(8) 0.7263(3) 0.155(3) Uani 1 1 d U . .
O5 O 0.7971(8) 0.6158(9) 0.7767(6) 0.185(4) Uani 1 1 d U . .
O3 O 0.6175(4) 0.6635(5) 0.7451(2) 0.0731(13) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Eu1 O1 2.347(3) . ?
Eu1 O2 2.393(3) 3_676 ?
Eu1 N3 2.552(4) . ?
Eu1 N4 2.553(4) . ?
Eu1 N2 2.564(4) . ?
Eu1 N1 2.572(4) . ?
Eu1 Cl1 2.7713(10) . ?
Eu1 Cl1 2.7736(11) 3_676 ?
Eu1 Eu1 3.9460(4) 3_676 ?
Cl2 O4 1.338(6) . ?
Cl2 O6 1.355(6) . ?
Cl2 O5 1.388(9) . ?
Cl2 O3 1.417(4) . ?
Cl1 Eu1 2.7736(11) 3_676 ?
C17 C18 1.337(9) . ?
C17 C16 1.435(8) . ?
C17 H17 0.9300 . ?
C12 N1 1.364(6) . ?
C12 C4 1.400(6) . ?
C12 C11 1.430(7) . ?
C25 O1 1.247(5) . ?
C25 O2 1.254(5) . ?
C25 C26 1.518(7) . ?
C7 C8 1.392(8) . ?
C7 C11 1.413(6) . ?
C7 C6 1.429(8) . ?
C1 N1 1.330(6) . ?
C1 C2 1.405(7) . ?
C1 H1 0.9300 . ?
C11 N2 1.364(6) . ?
C22 N4 1.331(6) . ?
C22 C21 1.388(7) . ?
C22 H22 0.9300 . ?
C24 N3 1.357(6) . ?
C24 C16 1.409(6) . ?
C24 C23 1.434(6) . ?
C23 N4 1.361(6) . ?
C23 C19 1.401(6) . ?
C20 C21 1.361(8) . ?
C20 C19 1.407(8) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C19 C18 1.425(7) . ?
C10 N2 1.331(6) . ?
C10 C9 1.393(7) . ?
C10 H10 0.9300 . ?
C4 C3 1.407(8) . ?
C4 C5 1.435(8) . ?
C2 C3 1.344(8) . ?
C2 H2 0.9300 . ?
C13 N3 1.326(6) . ?
C13 C14 1.394(7) . ?
C13 H13 0.9300 . ?
C15 C14 1.371(8) . ?
C15 C16 1.393(8) . ?
C15 H15 0.9300 . ?
C14 H14 0.9300 . ?
C26 N5 1.431(8) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
N5 N6 1.343(11) . ?
N5 C27 1.307(14) . ?
C3 H3 0.9300 . ?
C18 H18 0.9300 . ?
C8 C9 1.346(9) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C5 C6 1.336(9) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
N6 N7 1.376(12) . ?
N8 N7 1.281(14) . ?
N8 C27 1.260(14) . ?
C27 H27A 0.9300 . ?
O2 Eu1 2.393(3) 3_676 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Eu1 O2 137.88(10) . 3_676 ?
O1 Eu1 N3 77.49(11) . . ?
O2 Eu1 N3 139.91(12) 3_676 . ?
O1 Eu1 N4 122.52(12) . . ?
O2 Eu1 N4 77.98(12) 3_676 . ?
N3 Eu1 N4 64.05(12) . . ?
O1 Eu1 N2 141.02(12) . . ?
O2 Eu1 N2 75.83(12) 3_676 . ?
N3 Eu1 N2 82.43(13) . . ?
N4 Eu1 N2 75.51(13) . . ?
O1 Eu1 N1 79.12(12) . . ?
O2 Eu1 N1 120.66(12) 3_676 . ?
N3 Eu1 N1 76.53(12) . . ?
N4 Eu1 N1 126.15(12) . . ?
N2 Eu1 N1 63.79(12) . . ?
O1 Eu1 Cl1 74.62(8) . . ?
O2 Eu1 Cl1 75.50(8) 3_676 . ?
N3 Eu1 Cl1 106.38(9) . . ?
N4 Eu1 Cl1 77.24(9) . . ?
N2 Eu1 Cl1 143.77(9) . . ?
N1 Eu1 Cl1 152.07(9) . . ?
O1 Eu1 Cl1 75.94(8) . 3_676 ?
O2 Eu1 Cl1 74.68(8) 3_676 3_676 ?
N3 Eu1 Cl1 144.14(9) . 3_676 ?
N4 Eu1 Cl1 151.80(9) . 3_676 ?
N2 Eu1 Cl1 103.98(10) . 3_676 ?
N1 Eu1 Cl1 75.16(9) . 3_676 ?
Cl1 Eu1 Cl1 89.26(3) . 3_676 ?
O1 Eu1 Eu1 69.08(7) . 3_676 ?
O2 Eu1 Eu1 68.80(7) 3_676 3_676 ?
N3 Eu1 Eu1 140.15(9) . 3_676 ?
N4 Eu1 Eu1 117.67(8) . 3_676 ?
N2 Eu1 Eu1 137.42(10) . 3_676 ?
N1 Eu1 Eu1 116.14(8) . 3_676 ?
Cl1 Eu1 Eu1 44.66(2) . 3_676 ?
Cl1 Eu1 Eu1 44.61(2) 3_676 3_676 ?
O4 Cl2 O6 118.3(5) . . ?
O4 Cl2 O5 101.8(6) . . ?
O6 Cl2 O5 102.3(7) . . ?
O4 Cl2 O3 112.9(4) . . ?
O6 Cl2 O3 110.8(4) . . ?
O5 Cl2 O3 109.5(5) . . ?
Eu1 Cl1 Eu1 90.74(3) . 3_676 ?
C18 C17 C16 121.4(5) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
N1 C12 C4 122.7(5) . . ?
N1 C12 C11 117.6(4) . . ?
C4 C12 C11 119.7(4) . . ?
O1 C25 O2 127.6(4) . . ?
O1 C25 C26 114.1(4) . . ?
O2 C25 C26 118.3(4) . . ?
C8 C7 C11 118.1(5) . . ?
C8 C7 C6 123.1(5) . . ?
C11 C7 C6 118.7(5) . . ?
N1 C1 C2 123.2(5) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
N2 C11 C7 121.7(5) . . ?
N2 C11 C12 118.5(4) . . ?
C7 C11 C12 119.8(4) . . ?
N4 C22 C21 123.8(5) . . ?
N4 C22 H22 118.1 . . ?
C21 C22 H22 118.1 . . ?
N3 C24 C16 122.5(4) . . ?
N3 C24 C23 118.4(4) . . ?
C16 C24 C23 119.0(4) . . ?
N4 C23 C19 122.6(4) . . ?
N4 C23 C24 117.4(4) . . ?
C19 C23 C24 120.0(4) . . ?
C21 C20 C19 119.6(5) . . ?
C21 C20 H20 120.2 . . ?
C19 C20 H20 120.2 . . ?
C20 C21 C22 118.9(5) . . ?
C20 C21 H21 120.6 . . ?
C22 C21 H21 120.6 . . ?
C23 C19 C20 117.6(5) . . ?
C23 C19 C18 119.5(5) . . ?
C20 C19 C18 122.9(5) . . ?
N2 C10 C9 123.5(5) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
C12 C4 C3 117.6(5) . . ?
C12 C4 C5 119.2(5) . . ?
C3 C4 C5 123.1(5) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
N3 C13 C14 123.4(5) . . ?
N3 C13 H13 118.3 . . ?
C14 C13 H13 118.3 . . ?
C14 C15 C16 119.8(5) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C14 C13 118.7(5) . . ?
C15 C14 H14 120.6 . . ?
C13 C14 H14 120.6 . . ?
N5 C26 C25 114.7(4) . . ?
N5 C26 H26A 108.6 . . ?
C25 C26 H26A 108.6 . . ?
N5 C26 H26B 108.6 . . ?
C25 C26 H26B 108.6 . . ?
H26A C26 H26B 107.6 . . ?
C15 C16 C24 117.6(5) . . ?
C15 C16 C17 123.3(5) . . ?
C24 C16 C17 119.0(5) . . ?
N6 N5 C27 107.9(8) . . ?
N6 N5 C26 123.5(8) . . ?
C27 N5 C26 128.5(9) . . ?
C2 C3 C4 119.8(5) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C17 C18 C19 120.9(5) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C9 C8 C7 119.8(5) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.3(6) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C6 C5 C4 121.1(5) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 121.5(5) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C13 N3 C24 117.9(4) . . ?
C13 N3 Eu1 123.4(3) . . ?
C24 N3 Eu1 118.1(3) . . ?
C1 N1 C12 117.3(4) . . ?
C1 N1 Eu1 122.6(3) . . ?
C12 N1 Eu1 120.0(3) . . ?
C22 N4 C23 117.3(4) . . ?
C22 N4 Eu1 123.2(3) . . ?
C23 N4 Eu1 118.0(3) . . ?
C10 N2 C11 117.5(4) . . ?
C10 N2 Eu1 122.7(3) . . ?
C11 N2 Eu1 119.8(3) . . ?
N7 N6 N5 100.1(9) . . ?
N7 N8 C27 103.0(13) . . ?
N6 N7 N8 114.6(10) . . ?
N5 C27 N8 114.1(15) . . ?
N5 C27 H27A 123.0 . . ?
N8 C27 H27A 123.0 . . ?
C25 O1 Eu1 138.2(3) . . ?
C25 O2 Eu1 136.3(3) . 3_676 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.281
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.110

####################################################################### 
# 
# 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_14_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2035255'
loop_
_audit_author_name
_audit_author_address
'Ying-Bing Lu'
;College of Chemistry and Chemical Engineering, Gannan Normal University
China
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 '[Gd(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2' 
;
_chemical_name_common            '[Gd(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[Gd(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_formula_sum            'C54 H38 Cl4 Gd2 N16 O12'
_chemical_formula_weight         1559.30

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.0381(4)
_cell_length_b                   11.6511(3)
_cell_length_c                   21.7206(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.5441(10)
_cell_angle_gamma                90.00
_cell_volume                     3036.89(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9907
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.47

_exptl_crystal_description       blcok
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1532
_exptl_absorpt_coefficient_mu    2.414
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.5708
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            45382
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0162
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6923
_reflns_number_gt                6031
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0394P)²+8.3951P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6923
_refine_ls_number_parameters     397
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0992
_refine_ls_wR_factor_gt          0.0915
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_restrained_S_all      1.245
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.394509(15) 0.872946(16) 0.007533(9) 0.02618(8) Uani 1 1 d . . .
Cl2 Cl -0.22158(11) 0.79289(13) 0.23116(6) 0.0477(3) Uani 1 1 d . . .
N5 N 0.3546(3) 0.6720(3) -0.03381(17) 0.0349(8) Uani 1 1 d . . .
O1 O 0.4496(3) 0.8847(3) -0.09322(14) 0.0362(7) Uani 1 1 d . . .
N8 N 0.2056(3) 0.8936(3) -0.05460(17) 0.0331(8) Uani 1 1 d . . .
N6 N 0.4549(3) 0.7091(3) 0.08039(17) 0.0339(8) Uani 1 1 d . . .
C26 C 0.1098(4) 0.8671(4) -0.0281(2) 0.0351(9) Uani 1 1 d . . .
C19 C 0.0231(4) 0.8078(5) 0.0656(3) 0.0474(12) Uani 1 1 d . . .
C1 C 0.5110(4) 0.9469(4) -0.1230(2) 0.0351(9) Uani 1 1 d . . .
C25 C 0.1949(4) 0.9315(5) -0.1125(2) 0.0421(11) Uani 1 1 d . . .
H25 H 0.2591 0.9522 -0.1309 0.051 Uiso 1 1 calc R . .
N7 N 0.2234(3) 0.8316(4) 0.06615(18) 0.0379(8) Uani 1 1 d . . .
C21 C -0.0929(4) 0.8506(5) -0.0271(3) 0.0592(16) Uani 1 1 d . . .
H21 H -0.1634 0.8578 -0.0475 0.071 Uiso 1 1 calc R . .
C13 C 0.5088(4) 0.7253(4) 0.1357(2) 0.0434(11) Uani 1 1 d . . .
H13 H 0.5444 0.7952 0.1435 0.052 Uiso 1 1 calc R . .
C27 C 0.1199(4) 0.8330(4) 0.0356(2) 0.0357(9) Uani 1 1 d . . .
C14 C 0.4102(3) 0.6044(4) 0.0681(2) 0.0319(9) Uani 1 1 d . . .
C22 C 0.0042(4) 0.8754(4) -0.0598(3) 0.0447(12) Uani 1 1 d . . .
C20 C -0.0833(4) 0.8175(6) 0.0319(3) 0.0593(15) Uani 1 1 d . . .
H20 H -0.1472 0.8004 0.0515 0.071 Uiso 1 1 calc R . .
C12 C 0.5145(5) 0.6434(5) 0.1822(3) 0.0510(13) Uani 1 1 d . . .
H12 H 0.5503 0.6598 0.2207 0.061 Uiso 1 1 calc R . .
C16 C 0.2306(5) 0.8045(5) 0.1257(2) 0.0505(13) Uani 1 1 d . . .
H16 H 0.3006 0.8042 0.1471 0.061 Uiso 1 1 calc R . .
C10 C 0.4143(4) 0.5152(4) 0.1121(2) 0.0416(11) Uani 1 1 d . . .
C15 C 0.3601(4) 0.5835(4) 0.0070(2) 0.0316(9) Uani 1 1 d . . .
O6 O -0.1172(4) 0.8357(4) 0.2548(2) 0.0705(12) Uani 1 1 d . . .
C5 C 0.2794(5) 0.5423(5) -0.1116(3) 0.0550(14) Uani 1 1 d . . .
H5 H 0.2538 0.5305 -0.1527 0.066 Uiso 1 1 calc R . .
C4 C 0.3155(5) 0.6503(5) -0.0914(2) 0.0451(11) Uani 1 1 d . . .
H4 H 0.3120 0.7102 -0.1198 0.054 Uiso 1 1 calc R . .
C23 C -0.0020(5) 0.9122(5) -0.1212(3) 0.0536(14) Uani 1 1 d . . .
H23 H -0.0706 0.9164 -0.1440 0.064 Uiso 1 1 calc R . .
C11 C 0.4672(5) 0.5388(5) 0.1709(3) 0.0537(14) Uani 1 1 d . . .
H11 H 0.4697 0.4832 0.2017 0.064 Uiso 1 1 calc R . .
C2 C 0.5088(6) 0.9163(6) -0.1910(2) 0.0602(16) Uani 1 1 d . . .
H2A H 0.5242 0.8350 -0.1946 0.072 Uiso 1 1 calc R . .
H2B H 0.4343 0.9300 -0.2099 0.072 Uiso 1 1 calc R . .
C18 C 0.0355(5) 0.7777(6) 0.1280(3) 0.0586(15) Uani 1 1 d . . .
H18 H -0.0265 0.7588 0.1489 0.070 Uiso 1 1 calc R . .
O5 O -0.2224(6) 0.7581(7) 0.1717(3) 0.120(2) Uani 1 1 d U . .
C17 C 0.1386(5) 0.7763(6) 0.1579(3) 0.0601(15) Uani 1 1 d . . .
H17 H 0.1480 0.7568 0.1995 0.072 Uiso 1 1 calc R . .
Cl1 Cl 0.37669(8) 1.10394(9) -0.02052(5) 0.0335(2) Uani 1 1 d . . .
N1 N 0.5865(5) 0.9788(6) -0.2246(2) 0.0681(16) Uani 1 1 d . . .
C7 C 0.3223(4) 0.4727(4) -0.0091(2) 0.0423(11) Uani 1 1 d . . .
C24 C 0.0925(5) 0.9419(5) -0.1474(3) 0.0501(13) Uani 1 1 d . . .
H24 H 0.0894 0.9687 -0.1878 0.060 Uiso 1 1 calc R . .
C6 C 0.2821(5) 0.4536(5) -0.0704(3) 0.0545(14) Uani 1 1 d . . .
H6 H 0.2573 0.3810 -0.0829 0.065 Uiso 1 1 calc R . .
O3 O -0.2673(7) 0.7237(8) 0.2740(4) 0.136(3) Uani 1 1 d U . .
N2 N 0.6974(8) 0.9530(8) -0.2223(4) 0.112(3) Uani 1 1 d U . .
O4 O -0.3004(8) 0.8827(9) 0.2265(5) 0.174(4) Uani 1 1 d U . .
C3 C 0.5690(11) 1.0704(10) -0.2600(4) 0.116(4) Uani 1 1 d . . .
H3 H 0.4997 1.1041 -0.2693 0.140 Uiso 1 1 calc R . .
O2 O 0.5697(3) 1.0291(3) -0.10341(14) 0.0360(7) Uani 1 1 d . . .
N4 N 0.6604(11) 1.1070(10) -0.2800(5) 0.133(3) Uani 1 1 d U . .
N3 N 0.7327(8) 1.0363(9) -0.2609(4) 0.109(3) Uani 1 1 d U . .
C8 C 0.3268(6) 0.3850(4) 0.0371(3) 0.0569(15) Uani 1 1 d . . .
H8 H 0.2998 0.3121 0.0269 0.068 Uiso 1 1 calc R . .
C9 C 0.3694(5) 0.4061(5) 0.0949(3) 0.0575(15) Uani 1 1 d . . .
H9 H 0.3695 0.3481 0.1243 0.069 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.341(3) . ?
Gd1 O2 2.384(3) 3_675 ?
Gd1 N5 2.540(4) . ?
Gd1 N6 2.549(4) . ?
Gd1 N7 2.551(4) . ?
Gd1 N8 2.562(4) . ?
Gd1 Cl1 2.7595(10) 3_675 ?
Gd1 Cl1 2.7640(11) . ?
Gd1 Gd1 3.9313(4) 3_675 ?
Cl2 O5 1.352(7) . ?
Cl2 O3 1.379(8) . ?
Cl2 O4 1.410(9) . ?
Cl2 O6 1.410(4) . ?
N5 C4 1.327(6) . ?
N5 C15 1.358(6) . ?
O1 C1 1.251(5) . ?
N8 C25 1.329(6) . ?
N8 C26 1.365(6) . ?
N6 C13 1.332(6) . ?
N6 C14 1.351(6) . ?
C26 C22 1.402(6) . ?
C26 C27 1.434(7) . ?
C19 C18 1.397(8) . ?
C19 C27 1.410(6) . ?
C19 C20 1.428(8) . ?
C1 O2 1.246(5) . ?
C1 C2 1.517(7) . ?
C25 C24 1.400(7) . ?
C25 H25 0.9300 . ?
N7 C16 1.328(6) . ?
N7 C27 1.365(6) . ?
C21 C20 1.335(10) . ?
C21 C22 1.444(8) . ?
C21 H21 0.9300 . ?
C13 C12 1.388(7) . ?
C13 H13 0.9300 . ?
C14 C10 1.410(6) . ?
C14 C15 1.436(6) . ?
C22 C23 1.396(8) . ?
C20 H20 0.9300 . ?
C12 C11 1.360(8) . ?
C12 H12 0.9300 . ?
C16 C17 1.395(7) . ?
C16 H16 0.9300 . ?
C10 C11 1.408(8) . ?
C10 C9 1.420(8) . ?
C15 C7 1.403(6) . ?
C5 C6 1.367(8) . ?
C5 C4 1.391(7) . ?
C5 H5 0.9300 . ?
C4 H4 0.9300 . ?
C23 C24 1.356(8) . ?
C23 H23 0.9300 . ?
C11 H11 0.9300 . ?
C2 N1 1.431(7) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C18 C17 1.354(9) . ?
C18 H18 0.9300 . ?
C17 H17 0.9300 . ?
Cl1 Gd1 2.7595(10) 3_675 ?
N1 C3 1.323(12) . ?
N1 N2 1.365(10) . ?
C7 C6 1.398(8) . ?
C7 C8 1.430(8) . ?
C24 H24 0.9300 . ?
C6 H6 0.9300 . ?
N2 N3 1.371(12) . ?
C3 N4 1.286(13) . ?
C3 H3 0.9300 . ?
O2 Gd1 2.384(3) 3_675 ?
N4 N3 1.246(13) . ?
C8 C9 1.339(9) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O2 138.07(10) . 3_675 ?
O1 Gd1 N5 77.46(11) . . ?
O2 Gd1 N5 140.00(12) 3_675 . ?
O1 Gd1 N6 122.42(12) . . ?
O2 Gd1 N6 78.06(11) 3_675 . ?
N5 Gd1 N6 64.25(12) . . ?
O1 Gd1 N7 141.03(12) . . ?
O2 Gd1 N7 75.60(12) 3_675 . ?
N5 Gd1 N7 82.23(13) . . ?
N6 Gd1 N7 75.56(13) . . ?
O1 Gd1 N8 78.91(12) . . ?
O2 Gd1 N8 120.43(12) 3_675 . ?
N5 Gd1 N8 76.42(12) . . ?
N6 Gd1 N8 126.52(11) . . ?
N7 Gd1 N8 64.07(12) . . ?
O1 Gd1 Cl1 74.65(8) . 3_675 ?
O2 Gd1 Cl1 75.78(8) 3_675 3_675 ?
N5 Gd1 Cl1 106.58(9) . 3_675 ?
N6 Gd1 Cl1 77.07(9) . 3_675 ?
N7 Gd1 Cl1 143.70(9) . 3_675 ?
N8 Gd1 Cl1 151.86(9) . 3_675 ?
O1 Gd1 Cl1 76.10(8) . . ?
O2 Gd1 Cl1 74.46(8) 3_675 . ?
N5 Gd1 Cl1 144.14(9) . . ?
N6 Gd1 Cl1 151.60(9) . . ?
N7 Gd1 Cl1 104.02(10) . . ?
N8 Gd1 Cl1 75.07(8) . . ?
Cl1 Gd1 Cl1 89.25(3) 3_675 . ?
O1 Gd1 Gd1 69.22(7) . 3_675 ?
O2 Gd1 Gd1 68.85(7) 3_675 3_675 ?
N5 Gd1 Gd1 140.37(9) . 3_675 ?
N6 Gd1 Gd1 117.47(8) . 3_675 ?
N7 Gd1 Gd1 137.40(10) . 3_675 ?
N8 Gd1 Gd1 115.96(8) . 3_675 ?
Cl1 Gd1 Gd1 44.67(2) 3_675 3_675 ?
Cl1 Gd1 Gd1 44.58(2) . 3_675 ?
O5 Cl2 O3 119.7(5) . . ?
O5 Cl2 O4 101.5(6) . . ?
O3 Cl2 O4 100.4(6) . . ?
O5 Cl2 O6 113.1(4) . . ?
O3 Cl2 O6 110.7(4) . . ?
O4 Cl2 O6 109.8(5) . . ?
C4 N5 C15 117.7(4) . . ?
C4 N5 Gd1 123.6(3) . . ?
C15 N5 Gd1 118.2(3) . . ?
C1 O1 Gd1 137.8(3) . . ?
C25 N8 C26 116.9(4) . . ?
C25 N8 Gd1 123.0(3) . . ?
C26 N8 Gd1 120.0(3) . . ?
C13 N6 C14 117.7(4) . . ?
C13 N6 Gd1 123.2(3) . . ?
C14 N6 Gd1 117.6(3) . . ?
N8 C26 C22 122.7(5) . . ?
N8 C26 C27 117.4(4) . . ?
C22 C26 C27 119.9(5) . . ?
C18 C19 C27 118.2(5) . . ?
C18 C19 C20 122.6(5) . . ?
C27 C19 C20 119.2(5) . . ?
O2 C1 O1 127.7(4) . . ?
O2 C1 C2 118.6(4) . . ?
O1 C1 C2 113.7(4) . . ?
N8 C25 C24 123.8(5) . . ?
N8 C25 H25 118.1 . . ?
C24 C25 H25 118.1 . . ?
C16 N7 C27 117.6(4) . . ?
C16 N7 Gd1 122.6(3) . . ?
C27 N7 Gd1 119.8(3) . . ?
C20 C21 C22 121.3(5) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 H21 119.4 . . ?
N6 C13 C12 123.4(5) . . ?
N6 C13 H13 118.3 . . ?
C12 C13 H13 118.3 . . ?
N7 C27 C19 121.9(5) . . ?
N7 C27 C26 118.4(4) . . ?
C19 C27 C26 119.5(4) . . ?
N6 C14 C10 122.6(4) . . ?
N6 C14 C15 117.9(4) . . ?
C10 C14 C15 119.4(4) . . ?
C26 C22 C23 117.9(5) . . ?
C26 C22 C21 118.8(5) . . ?
C23 C22 C21 123.2(5) . . ?
C21 C20 C19 121.3(5) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C11 C12 C13 119.3(5) . . ?
C11 C12 H12 120.4 . . ?
C13 C12 H12 120.4 . . ?
N7 C16 C17 123.5(5) . . ?
N7 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C11 C10 C14 117.4(5) . . ?
C11 C10 C9 123.3(5) . . ?
C14 C10 C9 119.3(5) . . ?
N5 C15 C7 122.6(4) . . ?
N5 C15 C14 118.0(4) . . ?
C7 C15 C14 119.3(4) . . ?
C6 C5 C4 119.1(5) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
N5 C4 C5 123.3(5) . . ?
N5 C4 H4 118.4 . . ?
C5 C4 H4 118.4 . . ?
C24 C23 C22 119.8(5) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C12 C11 C10 119.4(5) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N1 C2 C1 114.6(4) . . ?
N1 C2 H2A 108.6 . . ?
C1 C2 H2A 108.6 . . ?
N1 C2 H2B 108.6 . . ?
C1 C2 H2B 108.6 . . ?
H2A C2 H2B 107.6 . . ?
C17 C18 C19 119.5(5) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C18 C17 C16 119.3(5) . . ?
C18 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
Gd1 Cl1 Gd1 90.75(3) 3_675 . ?
C3 N1 N2 108.0(8) . . ?
C3 N1 C2 128.9(8) . . ?
N2 N1 C2 123.1(7) . . ?
C6 C7 C15 117.6(5) . . ?
C6 C7 C8 123.0(5) . . ?
C15 C7 C8 119.3(5) . . ?
C23 C24 C25 118.8(5) . . ?
C23 C24 H24 120.6 . . ?
C25 C24 H24 120.6 . . ?
C5 C6 C7 119.5(5) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
N3 N2 N1 99.9(8) . . ?
N4 C3 N1 111.3(12) . . ?
N4 C3 H3 124.4 . . ?
N1 C3 H3 124.4 . . ?
C1 O2 Gd1 136.5(3) . 3_675 ?
C3 N4 N3 105.2(11) . . ?
N2 N3 N4 115.4(9) . . ?
C9 C8 C7 121.1(5) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 121.3(5) . . ?
C8 C9 H9 119.3 . . ?
C10 C9 H9 119.3 . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         1.741
_refine_diff_density_min         -0.936
_refine_diff_density_rms         0.119

####################################################################### 
# 
# 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_14_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2035256'
loop_
_audit_author_name
_audit_author_address
'Ying-Bing Lu'
;College of Chemistry and Chemical Engineering, Gannan Normal University
China
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 '[Dy(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2' 
;
_chemical_name_common            '[Dy(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[Dy(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_formula_sum            'C54 H38 Cl4 Dy2 N16 O12'
_chemical_formula_weight         1569.80

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Dy Dy -0.1890 4.4100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.0165(11)
_cell_length_b                   11.6234(11)
_cell_length_c                   24.035(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.388(5)
_cell_angle_gamma                90.00
_cell_volume                     3032.8(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blcok
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1540
_exptl_absorpt_coefficient_mu    2.695
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.4464
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            96523
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0144
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.88
_diffrn_reflns_theta_max         27.50
_reflns_number_total             6884
_reflns_number_gt                5973
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+5.7942P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6884
_refine_ls_number_parameters     416
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0365
_refine_ls_wR_factor_ref         0.1150
_refine_ls_wR_factor_gt          0.1069
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      1.018
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.886905(13) -0.625669(13) -0.007779(6) 0.02831(5) Uani 1 1 d . . .
Cl1 Cl 1.10141(8) -0.60376(8) -0.02065(4) 0.03672(18) Uani 1 1 d . . .
O1 O 0.8272(2) -0.5285(2) -0.10236(11) 0.0383(6) Uani 1 1 d . . .
O2 O 0.9587(3) -0.3832(2) -0.09154(12) 0.0384(6) Uani 1 1 d . . .
N1 N 0.6892(4) -0.4709(5) -0.22264(19) 0.0757(14) Uani 1 1 d . . .
N2 N 0.5830(7) -0.4500(7) -0.2199(4) 0.121(2) Uani 1 1 d U . .
N3 N 0.5058(7) -0.5273(7) -0.2604(4) 0.117(2) Uani 1 1 d U . .
N4 N 0.5521(11) -0.5972(10) -0.2778(5) 0.150(3) Uani 1 1 d U . .
N11 N 0.7623(3) -0.6050(3) 0.05450(15) 0.0362(7) Uani 1 1 d . . .
N12 N 0.6591(3) -0.6668(3) -0.06612(15) 0.0401(7) Uani 1 1 d . . .
N13 N 0.8889(3) -0.8258(3) 0.03347(13) 0.0361(7) Uani 1 1 d . . .
N14 N 0.8738(3) -0.7877(3) -0.08066(14) 0.0360(6) Uani 1 1 d . . .
C1 C 0.6689(9) -0.5647(9) -0.2600(4) 0.112(2) Uani 1 1 d U . .
H1 H 0.7252 -0.6004 -0.2714 0.055(15) Uiso 1 1 d R . .
C2 C 0.8015(5) -0.4127(5) -0.1892(2) 0.0613(13) Uani 1 1 d . . .
H2A H 0.7845 -0.3308 -0.1921 0.15(4) Uiso 1 1 d R . .
H2B H 0.8573 -0.4270 -0.2080 0.070(16) Uiso 1 1 d R . .
C3 C 0.8670(3) -0.4449(3) -0.12141(16) 0.0364(8) Uani 1 1 d . . .
C11 C 0.8094(4) -0.5685(4) 0.11214(18) 0.0444(9) Uani 1 1 d . . .
H11 H 0.8919 -0.5470 0.1304 0.047(12) Uiso 1 1 d R . .
C12 C 0.7419(4) -0.5584(4) 0.1472(2) 0.0521(10) Uani 1 1 d . . .
H12 H 0.7791 -0.5300 0.1872 0.053(13) Uiso 1 1 d R . .
C13 C 0.6222(4) -0.5889(5) 0.1217(2) 0.0572(11) Uani 1 1 d . . .
H13 H 0.5784 -0.5877 0.1456 0.09(2) Uiso 1 1 d R . .
C14 C 0.5661(4) -0.6253(3) 0.0599(2) 0.0474(10) Uani 1 1 d . . .
C15 C 0.4364(4) -0.6514(5) 0.0275(3) 0.0628(12) Uani 1 1 d . . .
H15 H 0.3875 -0.6445 0.0486 0.076(18) Uiso 1 1 d R . .
C16 C 0.3870(4) -0.6828(5) -0.0315(3) 0.0631(13) Uani 1 1 d . . .
H16 H 0.3033 -0.6997 -0.0508 0.10(2) Uiso 1 1 d R . .
C17 C 0.4600(4) -0.6912(4) -0.0649(2) 0.0493(10) Uani 1 1 d . . .
C18 C 0.4095(4) -0.7225(5) -0.1274(2) 0.0619(13) Uani 1 1 d . . .
H18 H 0.3274 -0.7440 -0.1478 0.047(12) Uiso 1 1 d R . .
C19 C 0.4820(4) -0.7214(5) -0.1577(2) 0.0630(13) Uani 1 1 d . . .
H19 H 0.4494 -0.7384 -0.1995 0.084(19) Uiso 1 1 d R . .
C20 C 0.6059(4) -0.6922(4) -0.1259(2) 0.0530(11) Uani 1 1 d . . .
H20 H 0.6542 -0.6908 -0.1475 0.061(15) Uiso 1 1 d R . .
C21 C 0.5866(3) -0.6658(3) -0.03529(18) 0.0388(8) Uani 1 1 d . . .
C22 C 0.6404(4) -0.6319(3) 0.0279(2) 0.0375(8) Uani 1 1 d . . .
C23 C 0.9071(4) -0.8475(4) 0.0913(2) 0.0477(10) Uani 1 1 d . . .
H23 H 0.9290 -0.7865 0.1190 0.056(14) Uiso 1 1 d R . .
C24 C 0.8945(5) -0.9560(4) 0.1119(2) 0.0561(11) Uani 1 1 d . . .
H24 H 0.9128 -0.9686 0.1531 0.10(2) Uiso 1 1 d R . .
C25 C 0.8547(4) -1.0453(4) 0.0701(2) 0.0546(11) Uani 1 1 d . . .
H25 H 0.8414 -1.1179 0.0823 0.068(18) Uiso 1 1 d R . .
C26 C 0.8325(4) -1.0262(3) 0.0092(2) 0.0446(9) Uani 1 1 d . . .
C27 C 0.7913(5) -1.1137(4) -0.0372(3) 0.0595(13) Uani 1 1 d . . .
H27 H 0.7732 -1.1866 -0.0275 0.09(2) Uiso 1 1 d R . .
C28 C 0.7759(5) -1.0922(4) -0.0953(2) 0.0608(12) Uani 1 1 d . . .
H28 H 0.7484 -1.1503 -0.1247 0.063(15) Uiso 1 1 d R . .
C29 C 0.8025(4) -0.9828(4) -0.11202(19) 0.0450(9) Uani 1 1 d . . .
C30 C 0.7958(4) -0.9586(4) -0.1711(2) 0.0560(11) Uani 1 1 d . . .
H30 H 0.7658 -1.0137 -0.2020 0.046(12) Uiso 1 1 d R . .
C31 C 0.8329(5) -0.8532(4) -0.1822(2) 0.0543(11) Uani 1 1 d . . .
H31 H 0.8299 -0.8361 -0.2206 0.036(10) Uiso 1 1 d R . .
C32 C 0.8728(4) -0.7713(4) -0.13555(18) 0.0461(9) Uani 1 1 d . . .
H32 H 0.9009 -0.7011 -0.1431 0.030(9) Uiso 1 1 d R . .
C33 C 0.8423(3) -0.8932(3) -0.06838(18) 0.0348(7) Uani 1 1 d . . .
C34 C 0.8532(3) -0.9144(3) -0.00734(17) 0.0348(7) Uani 1 1 d . . .
Cl2 Cl 1.04889(9) -0.70766(10) -0.23097(4) 0.0497(2) Uani 1 1 d . . .
O3 O 1.1083(6) -0.7426(6) -0.1712(3) 0.1169(11) Uani 1 1 d U . .
O4 O 1.1302(4) -0.6642(4) -0.25406(17) 0.0731(10) Uani 1 1 d . . .
O5 O 0.9619(6) -0.7822(6) -0.2737(3) 0.1339(12) Uani 1 1 d U . .
O6 O 0.9794(9) -0.6118(7) -0.2236(5) 0.1611(13) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2 2.314(3) 3_745 ?
Dy1 O1 2.358(2) . ?
Dy1 N13 2.525(3) . ?
Dy1 N14 2.530(3) . ?
Dy1 N12 2.530(3) . ?
Dy1 N11 2.542(3) . ?
Dy1 Cl1 2.7364(9) . ?
Dy1 Cl1 2.7415(9) 3_745 ?
Dy1 Dy1 3.8975(4) 3_745 ?
Cl1 Dy1 2.7415(9) 3_745 ?
O1 C3 1.253(5) . ?
O2 C3 1.252(4) . ?
O2 Dy1 2.314(3) 3_745 ?
N1 N2 1.329(10) . ?
N1 C1 1.366(11) . ?
N1 C2 1.412(7) . ?
N2 N3 1.357(11) . ?
N3 N4 1.159(13) . ?
N4 C1 1.335(14) . ?
N11 C11 1.322(5) . ?
N11 C22 1.360(5) . ?
N12 C20 1.331(5) . ?
N12 C21 1.364(5) . ?
N13 C23 1.336(5) . ?
N13 C34 1.359(5) . ?
N14 C32 1.328(5) . ?
N14 C33 1.353(5) . ?
C1 H1 0.9294 . ?
C2 C3 1.522(6) . ?
C2 H2A 0.9697 . ?
C2 H2B 0.9702 . ?
C11 C12 1.402(6) . ?
C11 H11 0.9299 . ?
C12 C13 1.347(7) . ?
C12 H12 0.9298 . ?
C13 C14 1.407(7) . ?
C13 H13 0.9310 . ?
C14 C22 1.408(6) . ?
C14 C15 1.444(7) . ?
C15 C16 1.332(8) . ?
C15 H15 0.9297 . ?
C16 C17 1.425(7) . ?
C16 H16 0.9302 . ?
C17 C21 1.407(5) . ?
C17 C18 1.405(7) . ?
C18 C19 1.353(8) . ?
C18 H18 0.9281 . ?
C19 C20 1.393(6) . ?
C19 H19 0.9297 . ?
C20 H20 0.9301 . ?
C21 C22 1.427(6) . ?
C23 C24 1.387(6) . ?
C23 H23 0.9301 . ?
C24 C25 1.378(7) . ?
C24 H24 0.9293 . ?
C25 C26 1.390(7) . ?
C25 H25 0.9294 . ?
C26 C34 1.411(5) . ?
C26 C27 1.432(7) . ?
C27 C28 1.349(8) . ?
C27 H27 0.9291 . ?
C28 C29 1.412(7) . ?
C28 H28 0.9296 . ?
C29 C33 1.408(5) . ?
C29 C30 1.416(7) . ?
C30 C31 1.369(7) . ?
C30 H30 0.9285 . ?
C31 C32 1.390(6) . ?
C31 H31 0.9293 . ?
C32 H32 0.9299 . ?
C33 C34 1.437(5) . ?
Cl2 O3 1.363(6) . ?
Cl2 O5 1.406(7) . ?
Cl2 O4 1.409(4) . ?
Cl2 O6 1.448(9) . ?

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 Dy1 O1 138.70(9) 3_745 . ?
O2 Dy1 N13 76.57(9) 3_745 . ?
O1 Dy1 N13 140.13(9) . . ?
O2 Dy1 N14 122.15(10) 3_745 . ?
O1 Dy1 N14 77.64(9) . . ?
N13 Dy1 N14 64.75(10) . . ?
O2 Dy1 N12 141.15(11) 3_745 . ?
O1 Dy1 N12 75.32(10) . . ?
N13 Dy1 N12 82.48(11) . . ?
N14 Dy1 N12 75.17(10) . . ?
O2 Dy1 N11 78.59(10) 3_745 . ?
O1 Dy1 N11 120.67(10) . . ?
N13 Dy1 N11 76.37(10) . . ?
N14 Dy1 N11 126.88(10) . . ?
N12 Dy1 N11 64.76(10) . . ?
O2 Dy1 Cl1 74.64(8) 3_745 . ?
O1 Dy1 Cl1 76.02(7) . . ?
N13 Dy1 Cl1 106.22(7) . . ?
N14 Dy1 Cl1 76.90(7) . . ?
N12 Dy1 Cl1 143.42(8) . . ?
N11 Dy1 Cl1 151.51(7) . . ?
O2 Dy1 Cl1 76.51(6) 3_745 3_745 ?
O1 Dy1 Cl1 74.71(7) . 3_745 ?
N13 Dy1 Cl1 143.86(7) . 3_745 ?
N14 Dy1 Cl1 151.38(7) . 3_745 ?
N12 Dy1 Cl1 104.45(8) . 3_745 ?
N11 Dy1 Cl1 75.03(7) . 3_745 ?
Cl1 Dy1 Cl1 89.29(3) . 3_745 ?
O2 Dy1 Dy1 69.50(6) 3_745 3_745 ?
O1 Dy1 Dy1 69.20(6) . 3_745 ?
N13 Dy1 Dy1 139.84(7) . 3_745 ?
N14 Dy1 Dy1 117.27(7) . 3_745 ?
N12 Dy1 Dy1 137.68(8) . 3_745 ?
N11 Dy1 Dy1 115.81(7) . 3_745 ?
Cl1 Dy1 Dy1 44.696(19) . 3_745 ?
Cl1 Dy1 Dy1 44.591(19) 3_745 3_745 ?
Dy1 Cl1 Dy1 90.71(3) . 3_745 ?
C3 O1 Dy1 135.9(2) . . ?
C3 O2 Dy1 137.5(2) . 3_745 ?
N2 N1 C1 105.9(7) . . ?
N2 N1 C2 126.0(6) . . ?
C1 N1 C2 127.9(7) . . ?
N1 N2 N3 102.7(8) . . ?
N4 N3 N2 115.9(9) . . ?
N3 N4 C1 106.7(10) . . ?
C11 N11 C22 117.2(4) . . ?
C11 N11 Dy1 123.5(3) . . ?
C22 N11 Dy1 119.3(3) . . ?
C20 N12 C21 117.7(3) . . ?
C20 N12 Dy1 123.0(3) . . ?
C21 N12 Dy1 119.3(2) . . ?
C23 N13 C34 117.9(3) . . ?
C23 N13 Dy1 123.5(3) . . ?
C34 N13 Dy1 117.9(2) . . ?
C32 N14 C33 117.5(3) . . ?
C32 N14 Dy1 123.6(3) . . ?
C33 N14 Dy1 117.7(2) . . ?
N4 C1 N1 107.7(10) . . ?
N4 C1 H1 125.3 . . ?
N1 C1 H1 127.0 . . ?
N1 C2 C3 114.8(4) . . ?
N1 C2 H2A 108.0 . . ?
C3 C2 H2A 108.3 . . ?
N1 C2 H2B 109.6 . . ?
C3 C2 H2B 108.3 . . ?
H2A C2 H2B 107.5 . . ?
O1 C3 O2 128.0(3) . . ?
O1 C3 C2 118.6(3) . . ?
O2 C3 C2 113.4(3) . . ?
N11 C11 C12 123.9(4) . . ?
N11 C11 H11 118.2 . . ?
C12 C11 H11 117.9 . . ?
C13 C12 C11 119.0(4) . . ?
C13 C12 H12 120.7 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 H13 119.4 . . ?
C14 C13 H13 120.9 . . ?
C13 C14 C22 117.6(4) . . ?
C13 C14 C15 123.3(4) . . ?
C22 C14 C15 119.0(5) . . ?
C16 C15 C14 121.1(5) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 H15 118.5 . . ?
C15 C16 C17 121.2(4) . . ?
C15 C16 H16 118.8 . . ?
C17 C16 H16 120.0 . . ?
C21 C17 C18 118.3(4) . . ?
C21 C17 C16 119.6(4) . . ?
C18 C17 C16 122.2(4) . . ?
C19 C18 C17 119.3(4) . . ?
C19 C18 H18 120.1 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 119.3(5) . . ?
C18 C19 H19 120.6 . . ?
C20 C19 H19 120.1 . . ?
N12 C20 C19 123.5(4) . . ?
N12 C20 H20 118.2 . . ?
C19 C20 H20 118.3 . . ?
N12 C21 C17 121.8(4) . . ?
N12 C21 C22 118.5(3) . . ?
C17 C21 C22 119.7(4) . . ?
N11 C22 C14 122.6(4) . . ?
N11 C22 C21 118.0(4) . . ?
C14 C22 C21 119.4(4) . . ?
N13 C23 C24 123.3(4) . . ?
N13 C23 H23 118.1 . . ?
C24 C23 H23 118.6 . . ?
C25 C24 C23 118.8(4) . . ?
C25 C24 H24 120.5 . . ?
C23 C24 H24 120.7 . . ?
C24 C25 C26 119.8(4) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C34 117.8(4) . . ?
C25 C26 C27 123.6(4) . . ?
C34 C26 C27 118.6(4) . . ?
C28 C27 C26 121.4(4) . . ?
C28 C27 H27 119.0 . . ?
C26 C27 H27 119.5 . . ?
C27 C28 C29 121.0(4) . . ?
C27 C28 H28 119.8 . . ?
C29 C28 H28 119.2 . . ?
C33 C29 C30 117.1(4) . . ?
C33 C29 C28 120.0(4) . . ?
C30 C29 C28 122.9(4) . . ?
C31 C30 C29 119.3(4) . . ?
C31 C30 H30 120.6 . . ?
C29 C30 H30 120.1 . . ?
C30 C31 C32 119.0(4) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.6 . . ?
N14 C32 C31 123.9(4) . . ?
N14 C32 H32 118.0 . . ?
C31 C32 H32 118.2 . . ?
N14 C33 C29 123.0(4) . . ?
N14 C33 C34 117.8(3) . . ?
C29 C33 C34 119.1(3) . . ?
N13 C34 C26 122.3(4) . . ?
N13 C34 C33 118.0(3) . . ?
C26 C34 C33 119.7(4) . . ?
O3 Cl2 O5 118.4(4) . . ?
O3 Cl2 O4 112.6(3) . . ?
O5 Cl2 O4 110.9(3) . . ?
O3 Cl2 O6 99.7(5) . . ?
O5 Cl2 O6 106.1(5) . . ?
O4 Cl2 O6 107.8(4) . . ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.708
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.150


####################################################################### 
# 
# 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_14_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2035254'
loop_
_audit_author_name
_audit_author_address
'Ying-Bing Lu'
;College of Chemistry and Chemical Engineering, Gannan Normal University
China
;
_audit_update_record             
;
2020-10-03 deposited with the CCDC.	2020-11-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 '[Tb(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2' 
;
_chemical_name_common            '[Tb(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[Tb(C12N2H8)4(C3N4H3O2)2(Cl)2](ClO4)2'
_chemical_formula_sum            'C54 H38 Cl4 N16 O12 Tb2'
_chemical_formula_weight         1562.64

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   12.0288(4)
_cell_length_b                   11.6329(3)
_cell_length_c                   21.7452(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4880(10)
_cell_angle_gamma                90.00
_cell_volume                     3033.47(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       blcok
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.711
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6801
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44124
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.32
_diffrn_reflns_theta_max         27.49
_reflns_number_total             6898
_reflns_number_gt                5932
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0376P)²+9.7771P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6898
_refine_ls_number_parameters     397
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0849
_refine_ls_wR_factor_gt          0.0789
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.028
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Tb1 Tb 0.605422(13) 0.626313(14) 0.492331(7) 0.02583(4) Uani 1 1 d . . .
Cl1 Cl 0.62272(7) 0.39620(7) 0.52051(4) 0.03276(18) Uani 1 1 d . . .
Cl2 Cl 0.77912(9) 0.29249(11) 0.73113(5) 0.0483(3) Uani 1 1 d . . .
C24 C 0.8885(3) 0.6324(3) 0.52795(19) 0.0345(8) Uani 1 1 d . . .
C13 C 0.8030(4) 0.5679(4) 0.61243(18) 0.0412(9) Uani 1 1 d . . .
H13 H 0.7388 0.5468 0.6308 0.049 Uiso 1 1 calc R . .
C19 C 0.9761(3) 0.6914(4) 0.4343(2) 0.0465(10) Uani 1 1 d . . .
C25 C 0.4882(3) 0.5545(3) 0.62201(16) 0.0341(8) Uani 1 1 d . . .
C16 C 0.9948(3) 0.6247(4) 0.5598(2) 0.0453(10) Uani 1 1 d . . .
C17 C 1.0906(4) 0.6504(4) 0.5278(3) 0.0593(14) Uani 1 1 d . . .
H17 H 1.1609 0.6443 0.5486 0.071 Uiso 1 1 calc R . .
C10 C 0.4915(3) 0.7728(4) 0.36439(19) 0.0428(10) Uani 1 1 d . . .
H10 H 0.4565 0.7025 0.3564 0.051 Uiso 1 1 calc R . .
C11 C 0.5896(3) 0.8943(3) 0.43192(17) 0.0309(8) Uani 1 1 d . . .
C7 C 0.5851(3) 0.9834(3) 0.3882(2) 0.0418(9) Uani 1 1 d . . .
C23 C 0.8791(3) 0.6663(3) 0.46450(19) 0.0348(8) Uani 1 1 d . . .
C12 C 0.6398(3) 0.9148(3) 0.49289(17) 0.0321(8) Uani 1 1 d . . .
C15 C 1.0005(4) 0.5879(4) 0.6212(2) 0.0535(12) Uani 1 1 d . . .
H15 H 1.0691 0.5837 0.6441 0.064 Uiso 1 1 calc R . .
C18 C 1.0825(4) 0.6831(5) 0.4687(3) 0.0601(14) Uani 1 1 d . . .
H18 H 1.1469 0.7007 0.4496 0.072 Uiso 1 1 calc R . .
C9 C 0.4849(4) 0.8554(4) 0.3181(2) 0.0518(12) Uani 1 1 d . . .
H9 H 0.4479 0.8395 0.2799 0.062 Uiso 1 1 calc R . .
C2 C 0.7201(4) 0.9567(4) 0.6116(2) 0.0516(11) Uani 1 1 d . . .
H2 H 0.7453 0.9688 0.6526 0.062 Uiso 1 1 calc R . .
C22 C 0.7689(4) 0.6937(4) 0.3740(2) 0.0502(11) Uani 1 1 d . . .
H22 H 0.6991 0.6928 0.3525 0.060 Uiso 1 1 calc R . .
C1 C 0.6850(4) 0.8480(4) 0.59140(19) 0.0426(10) Uani 1 1 d . . .
H1 H 0.6894 0.7878 0.6196 0.051 Uiso 1 1 calc R . .
C8 C 0.5329(4) 0.9596(4) 0.3294(2) 0.0530(12) Uani 1 1 d . . .
H8 H 0.5314 1.0149 0.2984 0.064 Uiso 1 1 calc R . .
C26 C 0.4907(5) 0.5861(5) 0.6898(2) 0.0603(13) Uani 1 1 d . . .
H26A H 0.5652 0.5723 0.7088 0.072 Uiso 1 1 calc R . .
H26B H 0.4755 0.6677 0.6931 0.072 Uiso 1 1 calc R . .
C20 C 0.9631(4) 0.7219(5) 0.3722(2) 0.0587(13) Uani 1 1 d . . .
H20 H 1.0250 0.7419 0.3515 0.070 Uiso 1 1 calc R . .
C21 C 0.8613(4) 0.7224(5) 0.3422(2) 0.0594(13) Uani 1 1 d . . .
H21 H 0.8524 0.7418 0.3006 0.071 Uiso 1 1 calc R . .
N5 N 0.4123(4) 0.5237(5) 0.72383(18) 0.0698(13) Uani 1 1 d . . .
C5 C 0.6721(5) 1.1145(4) 0.4630(3) 0.0575(13) Uani 1 1 d . . .
H5 H 0.6985 1.1877 0.4734 0.069 Uiso 1 1 calc R . .
C4 C 0.6773(4) 1.0261(3) 0.5094(2) 0.0419(9) Uani 1 1 d . . .
C14 C 0.9068(4) 0.5588(4) 0.6472(2) 0.0505(11) Uani 1 1 d . . .
H14 H 0.9102 0.5327 0.6877 0.061 Uiso 1 1 calc R . .
C6 C 0.6298(5) 1.0936(4) 0.4052(3) 0.0582(13) Uani 1 1 d . . .
H6 H 0.6297 1.1516 0.3758 0.070 Uiso 1 1 calc R . .
C3 C 0.7170(4) 1.0455(4) 0.5702(2) 0.0531(12) Uani 1 1 d . . .
H3 H 0.7414 1.1183 0.5827 0.064 Uiso 1 1 calc R . .
N1 N 0.6456(3) 0.8262(3) 0.53369(14) 0.0343(7) Uani 1 1 d . . .
N3 N 0.7933(3) 0.6054(3) 0.55457(14) 0.0332(7) Uani 1 1 d . . .
N2 N 0.5452(2) 0.7888(3) 0.41947(14) 0.0332(7) Uani 1 1 d . . .
N4 N 0.7760(3) 0.6675(3) 0.43390(15) 0.0359(7) Uani 1 1 d . . .
N6 N 0.3034(6) 0.5479(7) 0.7212(3) 0.117(2) Uani 1 1 d U . .
C27 C 0.4303(9) 0.4336(9) 0.7598(3) 0.134(4) Uani 1 1 d . . .
H27A H 0.5007 0.4024 0.7695 0.161 Uiso 1 1 calc R . .
N8 N 0.3413(9) 0.3932(8) 0.7801(4) 0.146(3) Uani 1 1 d U . .
N7 N 0.2666(6) 0.4671(7) 0.7604(3) 0.115(2) Uani 1 1 d U . .
O1 O 0.5504(2) 0.6158(2) 0.59216(12) 0.0353(6) Uani 1 1 d . . .
O2 O 0.4300(2) 0.4710(2) 0.60294(11) 0.0350(6) Uani 1 1 d . . .
O5 O 0.8840(3) 0.3357(4) 0.75456(17) 0.0701(11) Uani 1 1 d . . .
O4 O 0.7785(4) 0.2577(7) 0.6724(2) 0.136(2) Uani 1 1 d U . .
O6 O 0.7349(5) 0.2239(6) 0.7730(3) 0.153(2) Uani 1 1 d U . .
O3 O 0.7016(7) 0.3828(7) 0.7265(4) 0.177(3) Uani 1 1 d U . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.322(3) . ?
Tb1 O2 2.370(2) 3_666 ?
Tb1 N1 2.526(3) . ?
Tb1 N2 2.535(3) . ?
Tb1 N4 2.542(3) . ?
Tb1 N3 2.553(3) . ?
Tb1 Cl1 2.7491(8) 3_666 ?
Tb1 Cl1 2.7504(9) . ?
Tb1 Tb1 3.9131(3) 3_666 ?
Cl1 Tb1 2.7491(8) 3_666 ?
Cl2 O4 1.340(5) . ?
Cl2 O6 1.350(5) . ?
Cl2 O3 1.403(7) . ?
Cl2 O5 1.416(4) . ?
C24 N3 1.359(5) . ?
C24 C16 1.410(5) . ?
C24 C23 1.431(6) . ?
C13 N3 1.328(5) . ?
C13 C14 1.412(6) . ?
C13 H13 0.9300 . ?
C19 C20 1.393(7) . ?
C19 C23 1.414(5) . ?
C19 C18 1.435(6) . ?
C25 O2 1.250(4) . ?
C25 O1 1.251(4) . ?
C25 C26 1.517(5) . ?
C16 C15 1.399(7) . ?
C16 C17 1.424(7) . ?
C17 C18 1.335(8) . ?
C17 H17 0.9300 . ?
C10 N2 1.329(5) . ?
C10 C9 1.389(6) . ?
C10 H10 0.9300 . ?
C11 N2 1.357(4) . ?
C11 C7 1.405(5) . ?
C11 C12 1.433(5) . ?
C7 C8 1.408(6) . ?
C7 C6 1.428(6) . ?
C23 N4 1.361(5) . ?
C12 N1 1.358(5) . ?
C12 C4 1.408(5) . ?
C15 C14 1.344(7) . ?
C15 H15 0.9300 . ?
C18 H18 0.9300 . ?
C9 C8 1.356(7) . ?
C9 H9 0.9300 . ?
C2 C3 1.368(7) . ?
C2 C1 1.393(6) . ?
C2 H2 0.9300 . ?
C22 N4 1.333(5) . ?
C22 C21 1.395(6) . ?
C22 H22 0.9300 . ?
C1 N1 1.331(5) . ?
C1 H1 0.9300 . ?
C8 H8 0.9300 . ?
C26 N5 1.440(6) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C20 C21 1.341(7) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
N5 N6 1.336(9) . ?
N5 C27 1.316(11) . ?
C5 C6 1.341(7) . ?
C5 C4 1.438(6) . ?
C5 H5 0.9300 . ?
C4 C3 1.390(6) . ?
C14 H14 0.9300 . ?
C6 H6 0.9300 . ?
C3 H3 0.9300 . ?
N6 N7 1.365(10) . ?
C27 N8 1.279(12) . ?
C27 H27A 0.9300 . ?
N8 N7 1.292(12) . ?
O2 Tb1 2.370(2) 3_666 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tb1 O2 138.35(9) . 3_666 ?
O1 Tb1 N1 77.09(9) . . ?
O2 Tb1 N1 140.09(10) 3_666 . ?
O1 Tb1 N2 122.36(10) . . ?
O2 Tb1 N2 77.69(9) 3_666 . ?
N1 Tb1 N2 64.75(10) . . ?
O1 Tb1 N4 141.06(10) . . ?
O2 Tb1 N4 75.51(10) 3_666 . ?
N1 Tb1 N4 82.25(11) . . ?
N2 Tb1 N4 75.49(10) . . ?
O1 Tb1 N3 78.74(10) . . ?
O2 Tb1 N3 120.58(10) 3_666 . ?
N1 Tb1 N3 76.26(10) . . ?
N2 Tb1 N3 126.87(10) . . ?
N4 Tb1 N3 64.37(10) . . ?
O1 Tb1 Cl1 74.60(7) . 3_666 ?
O2 Tb1 Cl1 75.89(7) 3_666 3_666 ?
N1 Tb1 Cl1 106.59(7) . 3_666 ?
N2 Tb1 Cl1 76.91(7) . 3_666 ?
N4 Tb1 Cl1 143.66(8) . 3_666 ?
N3 Tb1 Cl1 151.62(7) . 3_666 ?
O1 Tb1 Cl1 76.25(7) . . ?
O2 Tb1 Cl1 74.65(7) 3_666 . ?
N1 Tb1 Cl1 143.86(7) . . ?
N2 Tb1 Cl1 151.38(7) . . ?
N4 Tb1 Cl1 104.16(8) . . ?
N3 Tb1 Cl1 74.96(7) . . ?
Cl1 Tb1 Cl1 89.28(3) 3_666 . ?
O1 Tb1 Tb1 69.29(6) . 3_666 ?
O2 Tb1 Tb1 69.06(6) 3_666 3_666 ?
N1 Tb1 Tb1 140.19(7) . 3_666 ?
N2 Tb1 Tb1 117.25(7) . 3_666 ?
N4 Tb1 Tb1 137.56(8) . 3_666 ?
N3 Tb1 Tb1 115.84(7) . 3_666 ?
Cl1 Tb1 Tb1 44.653(18) 3_666 3_666 ?
Cl1 Tb1 Tb1 44.627(18) . 3_666 ?
Tb1 Cl1 Tb1 90.72(3) 3_666 . ?
O4 Cl2 O6 119.5(4) . . ?
O4 Cl2 O3 101.8(5) . . ?
O6 Cl2 O3 101.3(5) . . ?
O4 Cl2 O5 112.9(3) . . ?
O6 Cl2 O5 110.7(3) . . ?
O3 Cl2 O5 109.1(4) . . ?
N3 C24 C16 122.6(4) . . ?
N3 C24 C23 118.0(3) . . ?
C16 C24 C23 119.4(4) . . ?
N3 C13 C14 122.7(4) . . ?
N3 C13 H13 118.6 . . ?
C14 C13 H13 118.6 . . ?
C20 C19 C23 118.0(4) . . ?
C20 C19 C18 123.4(4) . . ?
C23 C19 C18 118.6(4) . . ?
O2 C25 O1 127.8(3) . . ?
O2 C25 C26 118.6(3) . . ?
O1 C25 C26 113.5(3) . . ?
C15 C16 C24 117.6(4) . . ?
C15 C16 C17 123.4(4) . . ?
C24 C16 C17 119.0(4) . . ?
C18 C17 C16 122.0(4) . . ?
C18 C17 H17 119.0 . . ?
C16 C17 H17 119.0 . . ?
N2 C10 C9 123.5(4) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N2 C11 C7 122.6(3) . . ?
N2 C11 C12 117.8(3) . . ?
C7 C11 C12 119.6(3) . . ?
C8 C7 C11 117.4(4) . . ?
C8 C7 C6 123.0(4) . . ?
C11 C7 C6 119.6(4) . . ?
N4 C23 C19 121.6(4) . . ?
N4 C23 C24 118.3(3) . . ?
C19 C23 C24 119.9(4) . . ?
N1 C12 C4 122.2(3) . . ?
N1 C12 C11 118.3(3) . . ?
C4 C12 C11 119.5(3) . . ?
C14 C15 C16 119.9(4) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C17 C18 C19 121.1(4) . . ?
C17 C18 H18 119.5 . . ?
C19 C18 H18 119.5 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2 120.5 . . ?
C1 C2 H2 120.5 . . ?
N4 C22 C21 123.2(4) . . ?
N4 C22 H22 118.4 . . ?
C21 C22 H22 118.4 . . ?
N1 C1 C2 123.1(4) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C9 C8 C7 119.5(4) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
N5 C26 C25 114.4(4) . . ?
N5 C26 H26A 108.7 . . ?
C25 C26 H26A 108.7 . . ?
N5 C26 H26B 108.7 . . ?
C25 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
C21 C20 C19 120.1(4) . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C20 C21 C22 119.3(5) . . ?
C20 C21 H21 120.3 . . ?
C22 C21 H21 120.3 . . ?
N6 N5 C27 108.0(6) . . ?
N6 N5 C26 123.5(6) . . ?
C27 N5 C26 128.5(6) . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C3 C4 C12 118.1(4) . . ?
C3 C4 C5 123.0(4) . . ?
C12 C4 C5 119.0(4) . . ?
C15 C14 C13 119.5(4) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C5 C6 C7 120.9(4) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C1 N1 C12 117.9(3) . . ?
C1 N1 Tb1 123.7(3) . . ?
C12 N1 Tb1 117.9(2) . . ?
C13 N3 C24 117.7(3) . . ?
C13 N3 Tb1 122.8(3) . . ?
C24 N3 Tb1 119.5(2) . . ?
C10 N2 C11 117.5(3) . . ?
C10 N2 Tb1 123.6(3) . . ?
C11 N2 Tb1 117.5(2) . . ?
C22 N4 C23 117.8(3) . . ?
C22 N4 Tb1 122.6(3) . . ?
C23 N4 Tb1 119.6(2) . . ?
N7 N6 N5 101.1(7) . . ?
N5 C27 N8 113.2(10) . . ?
N5 C27 H27A 123.4 . . ?
N8 C27 H27A 123.4 . . ?
N7 N8 C27 102.8(9) . . ?
N6 N7 N8 114.5(7) . . ?
C25 O1 Tb1 137.8(2) . . ?
C25 O2 Tb1 136.0(2) . 3_666 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.840
_refine_diff_density_rms         0.102

