# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

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

data_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1882984'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV/EHU)
Spain
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6


_chemical_name_systematic        
;
[tetraaqua(5-bromonicotinato-k2O,O')bis(5-bromonicotinato-kO)dysprosium(III)] 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17 Br3 Dy N3 O10'
_chemical_formula_weight         837.57

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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.4580(4)
_cell_length_b                   10.6630(6)
_cell_length_c                   15.6770(7)
_cell_angle_alpha                82.162(2)
_cell_angle_beta                 87.933(2)
_cell_angle_gamma                72.310(2)
_cell_volume                     1176.64(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    31777
_cell_measurement_theta_min      2.487
_cell_measurement_theta_max      28.784

_exptl_crystal_description       'rectangular plate'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_F_000             794
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    8.329
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6211
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

_exptl_special_details           
;
 The following wavelength and cell were deduced by SADABS from the
 direction cosines etc. They are given here for emergency use only:
 CELL 0.71082    7.465   10.675   15.689   82.112   87.873   72.231
;
_diffrn_ambient_temperature      100(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  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            37807
_diffrn_reflns_av_unetI/netI     0.0479
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.551
_diffrn_reflns_theta_max         28.759
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6083
_reflns_number_gt                4961
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_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)+(0.0131P)²+0.4076P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6083
_refine_ls_number_parameters     316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0275
_refine_ls_wR_factor_ref         0.0448
_refine_ls_wR_factor_gt          0.0418
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_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
Dy1 Dy 0.15871(2) 0.57579(2) 0.14838(2) 0.00732(4) Uani 1 1 d . . . . .
Br1A Br 0.32575(5) 0.20460(4) 0.56334(2) 0.01908(8) Uani 1 1 d . . . . .
Br1B Br 0.18149(5) 0.00515(4) 0.40465(2) 0.02012(8) Uani 1 1 d . . . . .
Br1C Br -0.38772(5) 1.19053(3) 0.36998(2) 0.01824(8) Uani 1 1 d . . . . .
C2A C -0.2603(4) 0.4479(3) 0.45512(19) 0.0130(7) Uani 1 1 d . . . . .
H2A H -0.3788 0.4977 0.4336 0.016 Uiso 1 1 calc R U . . .
C2B C 0.3915(4) 0.0013(3) 0.12574(19) 0.0146(7) Uani 1 1 d . . . . .
H2B H 0.4314 -0.0014 0.0689 0.018 Uiso 1 1 calc R U . . .
C2C C -0.1229(4) 1.0896(3) 0.1089(2) 0.0145(7) Uani 1 1 d . . . . .
H2C H -0.0723 1.0698 0.0554 0.017 Uiso 1 1 calc R U . . .
C3A C -0.1086(4) 0.4271(3) 0.39870(18) 0.0104(6) Uani 1 1 d . . . . .
C3B C 0.3261(4) 0.1246(3) 0.15569(19) 0.0101(6) Uani 1 1 d . . . . .
C3C C -0.1171(4) 0.9855(3) 0.17343(19) 0.0107(6) Uani 1 1 d . . . . .
C31A C -0.1247(4) 0.4869(3) 0.30501(19) 0.0108(6) Uani 1 1 d . . . . .
C31B C 0.3259(4) 0.2502(3) 0.0975(2) 0.0118(7) Uani 1 1 d . . . . .
C31C C -0.0237(4) 0.8440(3) 0.15943(19) 0.0103(6) Uani 1 1 d . . . . .
C4A C 0.0687(4) 0.3532(3) 0.43066(18) 0.0098(6) Uani 1 1 d . . . . .
H4A H 0.1734 0.3384 0.3950 0.012 Uiso 1 1 calc R U . . .
C4B C 0.2610(4) 0.1290(3) 0.23959(18) 0.0109(6) Uani 1 1 d . . . . .
H4B H 0.2141 0.2094 0.2616 0.013 Uiso 1 1 calc R U . . .
C4C C -0.1949(4) 1.0149(3) 0.25258(19) 0.0121(7) Uani 1 1 d . . . . .
H4C H -0.1929 0.9475 0.2973 0.015 Uiso 1 1 calc R U . . .
C5A C 0.0850(4) 0.3022(3) 0.51676(18) 0.0108(6) Uani 1 1 d . . . . .
C5B C 0.2683(4) 0.0098(3) 0.28971(18) 0.0123(7) Uani 1 1 d . . . . .
C5C C -0.2756(4) 1.1465(3) 0.26353(19) 0.0119(7) Uani 1 1 d . . . . .
C6A C -0.0725(5) 0.3259(3) 0.5691(2) 0.0151(7) Uani 1 1 d . . . . .
H6A H -0.0589 0.2897 0.6268 0.018 Uiso 1 1 calc R U . . .
C6B C 0.3401(4) -0.1080(3) 0.25612(19) 0.0126(7) Uani 1 1 d . . . . .
H6B H 0.3473 -0.1871 0.2912 0.015 Uiso 1 1 calc R U . . .
C6C C -0.2738(4) 1.2450(3) 0.1969(2) 0.0147(7) Uani 1 1 d . . . . .
H6C H -0.3263 1.3334 0.2054 0.018 Uiso 1 1 calc R U . . .
N1A N -0.2437(4) 0.3994(3) 0.53928(16) 0.0155(6) Uani 1 1 d . . . . .
N1B N 0.3997(4) -0.1130(3) 0.17497(17) 0.0156(6) Uani 1 1 d . . . . .
N1C N -0.1983(4) 1.2169(3) 0.12014(17) 0.0158(6) Uani 1 1 d . . . . .
O1A O 0.0299(3) 0.4753(2) 0.26633(13) 0.0124(5) Uani 1 1 d . . . . .
O1B O 0.2764(3) 0.3568(2) 0.13160(14) 0.0167(5) Uani 1 1 d . . . . .
O1C O 0.0105(3) 0.7564(2) 0.22539(13) 0.0158(5) Uani 1 1 d . . . . .
O2A O -0.2833(3) 0.5421(2) 0.27082(13) 0.0162(5) Uani 1 1 d . . . . .
O2B O 0.3769(3) 0.2410(2) 0.02161(13) 0.0170(5) Uani 1 1 d . . . . .
O2C O 0.0202(3) 0.8147(2) 0.08526(13) 0.0151(5) Uani 1 1 d . . . . .
O1W O -0.1556(3) 0.5997(2) 0.11114(12) 0.0121(5) Uani 1 1 d . . . . .
O2W O 0.3635(3) 0.5376(2) 0.27035(13) 0.0174(5) Uani 1 1 d . . . . .
O3W O 0.4209(3) 0.6543(2) 0.10958(13) 0.0127(5) Uani 1 1 d . . . . .
O4W O 0.1757(3) 0.5828(2) -0.00058(13) 0.0190(5) Uani 1 1 d . . . . .
H11W H -0.2298 0.6586 0.0763 0.029 Uiso 1 1 d . U . . .
H12W H -0.2200 0.5939 0.1568 0.029 Uiso 1 1 d . U . . .
H21W H 0.4749 0.5421 0.2698 0.029 Uiso 1 1 d . U . . .
H22W H 0.3315 0.5361 0.3231 0.029 Uiso 1 1 d . U . . .
H31W H 0.4672 0.6737 0.0612 0.029 Uiso 1 1 d . U . . .
H32W H 0.4153 0.7189 0.1371 0.029 Uiso 1 1 d . U . . .
H41W H 0.1655 0.6477 -0.0397 0.029 Uiso 1 1 d . U . . .
H42W H 0.1632 0.5285 -0.0326 0.029 Uiso 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 O1B 2.280(2) . ?
Dy1 O4W 2.326(2) . ?
Dy1 O1A 2.3342(19) . ?
Dy1 O1W 2.366(2) . ?
Dy1 O1C 2.373(2) . ?
Dy1 O3W 2.380(2) . ?
Dy1 O2W 2.403(2) . ?
Dy1 O2C 2.514(2) . ?
Dy1 C31C 2.795(3) . ?
Br1A C5A 1.895(3) . ?
Br1B C5B 1.892(3) . ?
Br1C C5C 1.892(3) . ?
C2A N1A 1.345(4) . ?
C2A C3A 1.393(4) . ?
C2A H2A 0.9300 . ?
C2B N1B 1.337(4) . ?
C2B C3B 1.396(4) . ?
C2B H2B 0.9300 . ?
C2C N1C 1.336(4) . ?
C2C C3C 1.388(4) . ?
C2C H2C 0.9300 . ?
C3A C4A 1.388(4) . ?
C3A C31A 1.513(4) . ?
C3B C4B 1.387(4) . ?
C3B C31B 1.514(4) . ?
C3C C4C 1.385(4) . ?
C3C C31C 1.500(4) . ?
C31A O2A 1.253(4) . ?
C31A O1A 1.263(3) . ?
C31B O2B 1.244(3) . ?
C31B O1B 1.269(4) . ?
C31C O2C 1.252(3) . ?
C31C O1C 1.272(3) . ?
C4A C5A 1.380(4) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.387(4) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.380(4) . ?
C4C H4C 0.9300 . ?
C5A C6A 1.387(4) . ?
C5B C6B 1.376(4) . ?
C5C C6C 1.380(4) . ?
C6A N1A 1.341(4) . ?
C6A H6A 0.9300 . ?
C6B N1B 1.335(4) . ?
C6B H6B 0.9300 . ?
C6C N1C 1.342(4) . ?
C6C H6C 0.9300 . ?
O1W H11W 0.8456 . ?
O1W H12W 0.8527 . ?
O2W H21W 0.8464 . ?
O2W H22W 0.8519 . ?
O3W H31W 0.8478 . ?
O3W H32W 0.8521 . ?
O4W H41W 0.8460 . ?
O4W H42W 0.8432 . ?

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
O1B Dy1 O4W 77.51(8) . . ?
O1B Dy1 O1A 78.22(8) . . ?
O4W Dy1 O1A 139.58(8) . . ?
O1B Dy1 O1W 96.25(8) . . ?
O4W Dy1 O1W 77.95(8) . . ?
O1A Dy1 O1W 73.13(7) . . ?
O1B Dy1 O1C 154.70(7) . . ?
O4W Dy1 O1C 126.31(8) . . ?
O1A Dy1 O1C 77.26(8) . . ?
O1W Dy1 O1C 82.54(8) . . ?
O1B Dy1 O3W 101.87(8) . . ?
O4W Dy1 O3W 75.70(8) . . ?
O1A Dy1 O3W 141.21(7) . . ?
O1W Dy1 O3W 143.71(7) . . ?
O1C Dy1 O3W 93.38(8) . . ?
O1B Dy1 O2W 89.51(8) . . ?
O4W Dy1 O2W 139.54(8) . . ?
O1A Dy1 O2W 71.51(7) . . ?
O1W Dy1 O2W 142.12(7) . . ?
O1C Dy1 O2W 76.90(8) . . ?
O3W Dy1 O2W 69.71(7) . . ?
O1B Dy1 O2C 150.32(7) . . ?
O4W Dy1 O2C 73.04(7) . . ?
O1A Dy1 O2C 123.30(7) . . ?
O1W Dy1 O2C 74.17(7) . . ?
O1C Dy1 O2C 53.53(7) . . ?
O3W Dy1 O2C 74.56(7) . . ?
O2W Dy1 O2C 115.52(8) . . ?
O1B Dy1 C31C 173.29(8) . . ?
O4W Dy1 C31C 99.54(8) . . ?
O1A Dy1 C31C 100.86(8) . . ?
O1W Dy1 C31C 77.18(8) . . ?
O1C Dy1 C31C 26.94(8) . . ?
O3W Dy1 C31C 83.05(8) . . ?
O2W Dy1 C31C 96.52(9) . . ?
O2C Dy1 C31C 26.60(7) . . ?
N1A C2A C3A 123.2(3) . . ?
N1A C2A H2A 118.4 . . ?
C3A C2A H2A 118.4 . . ?
N1B C2B C3B 123.0(3) . . ?
N1B C2B H2B 118.5 . . ?
C3B C2B H2B 118.5 . . ?
N1C C2C C3C 122.8(3) . . ?
N1C C2C H2C 118.6 . . ?
C3C C2C H2C 118.6 . . ?
C4A C3A C2A 118.6(3) . . ?
C4A C3A C31A 117.9(3) . . ?
C2A C3A C31A 123.4(3) . . ?
C4B C3B C2B 118.4(3) . . ?
C4B C3B C31B 121.0(3) . . ?
C2B C3B C31B 120.5(3) . . ?
C4C C3C C2C 118.6(3) . . ?
C4C C3C C31C 120.2(3) . . ?
C2C C3C C31C 121.2(3) . . ?
O2A C31A O1A 124.5(3) . . ?
O2A C31A C3A 120.2(3) . . ?
O1A C31A C3A 115.2(3) . . ?
O2B C31B O1B 125.4(3) . . ?
O2B C31B C3B 118.2(3) . . ?
O1B C31B C3B 116.4(3) . . ?
O2C C31C O1C 121.8(3) . . ?
O2C C31C C3C 120.6(3) . . ?
O1C C31C C3C 117.6(3) . . ?
O2C C31C Dy1 64.07(16) . . ?
O1C C31C Dy1 57.71(16) . . ?
C3C C31C Dy1 175.1(2) . . ?
C5A C4A C3A 118.1(3) . . ?
C5A C4A H4A 120.9 . . ?
C3A C4A H4A 120.9 . . ?
C3B C4B C5B 117.9(3) . . ?
C3B C4B H4B 121.0 . . ?
C5B C4B H4B 121.0 . . ?
C5C C4C C3C 118.5(3) . . ?
C5C C4C H4C 120.8 . . ?
C3C C4C H4C 120.8 . . ?
C4A C5A C6A 120.2(3) . . ?
C4A C5A Br1A 119.3(2) . . ?
C6A C5A Br1A 120.5(2) . . ?
C6B C5B C4B 120.0(3) . . ?
C6B C5B Br1B 118.7(2) . . ?
C4B C5B Br1B 121.2(2) . . ?
C4C C5C C6C 119.8(3) . . ?
C4C C5C Br1C 119.7(2) . . ?
C6C C5C Br1C 120.4(2) . . ?
N1A C6A C5A 122.2(3) . . ?
N1A C6A H6A 118.9 . . ?
C5A C6A H6A 118.9 . . ?
N1B C6B C5B 122.4(3) . . ?
N1B C6B H6B 118.8 . . ?
C5B C6B H6B 118.8 . . ?
N1C C6C C5C 121.8(3) . . ?
N1C C6C H6C 119.1 . . ?
C5C C6C H6C 119.1 . . ?
C6A N1A C2A 117.7(3) . . ?
C6B N1B C2B 118.1(3) . . ?
C2C N1C C6C 118.5(3) . . ?
C31A O1A Dy1 140.7(2) . . ?
C31B O1B Dy1 161.6(2) . . ?
C31C O1C Dy1 95.36(18) . . ?
C31C O2C Dy1 89.33(18) . . ?
Dy1 O1W H11W 129.6 . . ?
Dy1 O1W H12W 109.7 . . ?
H11W O1W H12W 104.8 . . ?
Dy1 O2W H21W 126.9 . . ?
Dy1 O2W H22W 126.7 . . ?
H21W O2W H22W 104.7 . . ?
Dy1 O3W H31W 132.2 . . ?
Dy1 O3W H32W 108.8 . . ?
H31W O3W H32W 104.6 . . ?
Dy1 O4W H41W 130.4 . . ?
Dy1 O4W H42W 130.7 . . ?
H41W O4W H42W 97.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O2B 0.85 1.91 2.742(3) 165.6 2_565
O1W H12W O2A 0.85 1.88 2.704(3) 160.7 .
O2W H21W O2A 0.85 1.80 2.649(3) 176.8 1_655
O2W H22W N1A 0.85 2.36 3.185(3) 162.3 2_566
O3W H31W O2B 0.85 2.02 2.815(3) 156.0 2_665
O3W H32W N1B 0.85 1.93 2.771(4) 167.6 1_565
O4W H41W N1C 0.85 1.85 2.685(3) 167.5 2_575

_refine_diff_density_max         0.662
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.159

_shelxl_version_number           2014-3


_exptl_crystal_preparation       'Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1882986'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV/EHU)
Spain
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6

_chemical_name_systematic        
;
[tetraaquabis(5-bromonicotinato-kO)ytterbium(III)] 
[diaquabis(5-bromonicotinato-k2O,O')bis(5-bromonicotinato-kO)dysprosium(III)]
bis(5-bromonicotinic acid)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H19 Br4 N4 O11 Yb'
_chemical_formula_weight         1032.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.6100(5)
_cell_length_b                   15.8524(8)
_cell_length_c                   16.6978(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.443(3)
_cell_angle_gamma                90
_cell_volume                     3073.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    31777
_cell_measurement_theta_min      2.487
_cell_measurement_theta_max      28.784

_exptl_crystal_description       'rectangular plate'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_F_000             1956
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    8.307
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0683
_exptl_absorpt_correction_T_max  0.4765
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      100(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  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            31777
_diffrn_reflns_av_unetI/netI     0.1247
_diffrn_reflns_av_R_equivalents  0.1487
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.487
_diffrn_reflns_theta_max         28.784
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7958
_reflns_number_gt                5138
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
One of the carboxylate carbon atoms (C31B) as well as an carboxylate oxygen atoms
(O1A) present quite prolate anisotropic ellipsoids probably influenced by 
the large electron density of the ytterbium ions in the vicinity. 
Therefore, its thermal anisotropic displacement parameters
have been refined with an ISOR restraint. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0172P)²+4.9210P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7958
_refine_ls_number_parameters     398
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0558
_refine_ls_wR_factor_ref         0.0847
_refine_ls_wR_factor_gt          0.0721
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.022
_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
Yb1 Yb 0.0000 0.35374(3) 0.2500 0.00647(10) Uani 1 2 d S T P . .
Yb2 Yb 0.5000 0.38697(3) 0.2500 0.00574(10) Uani 1 2 d S T P . .
Br1A Br -0.15922(7) -0.14933(5) 0.18792(6) 0.0309(2) Uani 1 1 d . . . . .
Br1B Br -0.43049(6) 0.25808(5) 0.60856(5) 0.01793(19) Uani 1 1 d . . . . .
Br1C Br 0.03758(6) 0.71312(5) 0.11902(4) 0.01673(18) Uani 1 1 d . . . . .
Br1D Br 0.38178(7) -0.08307(5) 0.17662(5) 0.02017(19) Uani 1 1 d . . . . .
C2A C 0.0116(6) 0.1033(5) 0.1259(4) 0.0139(16) Uani 1 1 d . . . . .
H2A H 0.0466 0.1543 0.1133 0.017 Uiso 1 1 calc R U . . .
C2B C -0.1493(6) 0.4403(4) 0.5254(4) 0.0110(16) Uani 1 1 d . . . . .
H2B H -0.0933 0.4783 0.5089 0.013 Uiso 1 1 calc R U . . .
C2C C 0.3642(6) 0.5844(4) 0.0253(4) 0.0094(15) Uani 1 1 d . . . . .
H2C H 0.4319 0.5607 0.0061 0.011 Uiso 1 1 calc R U . . .
C2D C 0.5797(6) 0.1413(5) 0.0741(4) 0.0122(15) Uani 1 1 d . . . . .
H2D H 0.6177 0.1876 0.0526 0.015 Uiso 1 1 calc R U . . .
C3A C -0.0889(6) 0.1047(4) 0.1687(4) 0.0087(15) Uani 1 1 d . . . . .
C3B C -0.1756(5) 0.3728(4) 0.4750(4) 0.0065(15) Uani 1 1 d . . . . .
C3C C 0.3296(6) 0.5645(4) 0.1024(4) 0.0083(15) Uani 1 1 d . . . . .
C3D C 0.6261(6) 0.0621(5) 0.0605(4) 0.0124(16) Uani 1 1 d . . . . .
C4A C -0.1423(6) 0.0288(4) 0.1886(4) 0.0137(17) Uani 1 1 d . . . . .
H4A H -0.2111 0.0276 0.2168 0.016 Uiso 1 1 calc R U . . .
C4B C -0.2602(6) 0.3159(5) 0.4989(4) 0.0111(16) Uani 1 1 d . . . . .
H4B H -0.2805 0.2700 0.4672 0.013 Uiso 1 1 calc R U . . .
C4C C 0.2284(6) 0.6013(4) 0.1310(4) 0.0088(15) Uani 1 1 d . . . . .
H4C H 0.2013 0.5886 0.1819 0.011 Uiso 1 1 calc R U . . .
C4D C 0.5687(6) -0.0083(5) 0.0914(4) 0.0163(17) Uani 1 1 d . . . . .
H4D H 0.5961 -0.0627 0.0831 0.020 Uiso 1 1 calc R U . . .
C5A C -0.0885(6) -0.0444(4) 0.1647(4) 0.0142(17) Uani 1 1 d . . . . .
C5B C -0.3131(6) 0.3306(4) 0.5720(4) 0.0111(16) Uani 1 1 d . . . . .
C5C C 0.1699(6) 0.6567(4) 0.0820(4) 0.0121(16) Uani 1 1 d . . . . .
C5D C 0.4692(6) 0.0064(5) 0.1350(4) 0.0137(16) Uani 1 1 d . . . . .
C6A C 0.0110(6) -0.0416(5) 0.1205(4) 0.0166(18) Uani 1 1 d . . . . .
H6A H 0.0439 -0.0919 0.1035 0.020 Uiso 1 1 calc R U . . .
C6B C -0.2819(6) 0.4002(4) 0.6179(4) 0.0112(16) Uani 1 1 d . . . . .
H6B H -0.3199 0.4099 0.6659 0.013 Uiso 1 1 calc R U . . .
C6C C 0.2079(6) 0.6715(4) 0.0055(4) 0.0139(17) Uani 1 1 d . . . . .
H6C H 0.1650 0.7071 -0.0275 0.017 Uiso 1 1 calc R U . . .
C6D C 0.4311(6) 0.0881(5) 0.1469(4) 0.0159(17) Uani 1 1 d . . . . .
H6D H 0.3657 0.0966 0.1777 0.019 Uiso 1 1 calc R U . . .
C31A C -0.1456(6) 0.1871(4) 0.1908(4) 0.0120(16) Uani 1 1 d . . . . .
C31B C -0.1163(6) 0.3649(4) 0.3953(4) 0.0087(14) Uani 1 1 d . U . . .
C31C C 0.3965(6) 0.5049(4) 0.1531(4) 0.0121(16) Uani 1 1 d . . . . .
C31D C 0.7334(6) 0.0548(5) 0.0122(4) 0.0110(16) Uani 1 1 d . . . . .
N1A N 0.0617(5) 0.0315(4) 0.1013(4) 0.0175(15) Uani 1 1 d . . . . .
N1B N -0.1989(5) 0.4536(4) 0.5955(3) 0.0128(14) Uani 1 1 d . . . . .
N1C N 0.3036(5) 0.6369(4) -0.0231(4) 0.0131(14) Uani 1 1 d . . . . .
N1D N 0.4842(5) 0.1555(4) 0.1158(4) 0.0174(15) Uani 1 1 d . . . . .
O1W O 0.1383(4) 0.4500(3) 0.2752(3) 0.0116(11) Uani 1 1 d . . . . .
H11W H 0.2053 0.4528 0.2554 0.017 Uiso 1 1 d . U . . .
H12W H 0.1452 0.4760 0.3201 0.017 Uiso 1 1 d . U . . .
O2W O 0.3627(4) 0.3291(3) 0.3254(3) 0.0127(11) Uani 1 1 d . . . . .
H21W H 0.3152 0.2909 0.3115 0.019 Uiso 1 1 d . U . . .
H22W H 0.3505 0.3367 0.3751 0.019 Uiso 1 1 d . U . . .
O3W O 0.3951(4) 0.3037(3) 0.1657(3) 0.0146(12) Uani 1 1 d . . . . .
H31W H 0.3222 0.3004 0.1685 0.018 Uiso 1 1 d . U . . .
H32W H 0.4170 0.2542 0.1541 0.018 Uiso 1 1 d . U . . .
O1A O -0.0870(4) 0.2539(3) 0.1800(3) 0.0096(10) Uani 1 1 d . U . . .
O1B O -0.0279(4) 0.4088(3) 0.3826(3) 0.0123(11) Uani 1 1 d . . . . .
O1C O 0.4918(4) 0.4770(3) 0.1307(3) 0.0118(11) Uani 1 1 d . . . . .
O2D O 0.7920(4) 0.1151(3) -0.0040(3) 0.0184(12) Uani 1 1 d . . . . .
O2A O -0.2472(4) 0.1850(3) 0.2149(3) 0.0127(11) Uani 1 1 d . . . . .
O2B O -0.1572(4) 0.3147(3) 0.3431(3) 0.0095(11) Uani 1 1 d . . . . .
O2C O 0.3547(4) 0.4831(3) 0.2204(3) 0.0122(11) Uani 1 1 d . . . . .
O1D O 0.7550(4) -0.0241(3) -0.0088(3) 0.0157(12) Uani 1 1 d . . . . .
H1D H 0.8123 -0.0267 -0.0319 0.019 Uiso 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
Yb1 O1A 2.207(5) . ?
Yb1 O1A 2.207(5) 2 ?
Yb1 O1W 2.253(5) . ?
Yb1 O1W 2.253(5) 2 ?
Yb1 O1B 2.404(4) 2 ?
Yb1 O1B 2.404(4) . ?
Yb1 O2B 2.485(4) . ?
Yb1 O2B 2.485(4) 2 ?
Yb1 C31B 2.791(6) . ?
Yb1 C31B 2.791(6) 2 ?
Yb2 O2W 2.236(4) 2_655 ?
Yb2 O2W 2.236(4) . ?
Yb2 O3W 2.276(5) . ?
Yb2 O3W 2.276(5) 2_655 ?
Yb2 O2C 2.324(5) . ?
Yb2 O2C 2.324(5) 2_655 ?
Yb2 O1C 2.452(5) . ?
Yb2 O1C 2.452(5) 2_655 ?
Yb2 C31C 2.743(7) . ?
Yb2 C31C 2.743(7) 2_655 ?
Br1A C5A 1.896(7) . ?
Br1B C5B 1.888(7) . ?
Br1C C5C 1.886(7) . ?
Br1D C5D 1.880(7) . ?
C2A N1A 1.343(9) . ?
C2A C3A 1.374(9) . ?
C2A H2A 0.9300 . ?
C2B N1B 1.325(8) . ?
C2B C3B 1.394(9) . ?
C2B H2B 0.9300 . ?
C2C N1C 1.354(9) . ?
C2C C3C 1.387(9) . ?
C2C H2C 0.9300 . ?
C2D N1D 1.333(8) . ?
C2D C3D 1.385(10) . ?
C2D H2D 0.9300 . ?
C3A C4A 1.395(9) . ?
C3A C31A 1.510(9) . ?
C3B C4B 1.394(9) . ?
C3B C31B 1.508(8) . ?
C3C C4C 1.400(8) . ?
C3C C31C 1.485(10) . ?
C3D C4D 1.400(10) . ?
C3D C31D 1.494(9) . ?
C4A C5A 1.378(9) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.391(9) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.377(9) . ?
C4C H4C 0.9300 . ?
C4D C5D 1.390(9) . ?
C4D H4D 0.9300 . ?
C5A C6A 1.376(9) . ?
C5B C6B 1.389(10) . ?
C5C C6C 1.374(9) . ?
C5D C6D 1.383(10) . ?
C6A N1A 1.341(9) . ?
C6A H6A 0.9300 . ?
C6B N1B 1.339(8) . ?
C6B H6B 0.9300 . ?
C6C N1C 1.332(8) . ?
C6C H6C 0.9300 . ?
C6D N1D 1.341(9) . ?
C6D H6D 0.9300 . ?
C31A O2A 1.250(8) . ?
C31A O1A 1.273(8) . ?
C31B O1B 1.259(8) . ?
C31B O2B 1.270(8) . ?
C31C O1C 1.252(8) . ?
C31C O2C 1.274(8) . ?
C31D O2D 1.204(8) . ?
C31D O1D 1.325(8) . ?
O1W H11W 0.8479 . ?
O1W H12W 0.8584 . ?
O2W H21W 0.8494 . ?
O2W H22W 0.8529 . ?
O3W H31W 0.8497 . ?
O3W H32W 0.8484 . ?
O1D H1D 0.7731 . ?

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
O1A Yb1 O1A 88.4(2) . 2 ?
O1A Yb1 O1W 155.11(15) . . ?
O1A Yb1 O1W 93.68(17) 2 . ?
O1A Yb1 O1W 93.68(17) . 2 ?
O1A Yb1 O1W 155.12(15) 2 2 ?
O1W Yb1 O1W 94.7(2) . 2 ?
O1A Yb1 O1B 80.63(16) . 2 ?
O1A Yb1 O1B 133.13(15) 2 2 ?
O1W Yb1 O1B 79.91(16) . 2 ?
O1W Yb1 O1B 71.51(15) 2 2 ?
O1A Yb1 O1B 133.14(15) . . ?
O1A Yb1 O1B 80.63(16) 2 . ?
O1W Yb1 O1B 71.52(15) . . ?
O1W Yb1 O1B 79.91(16) 2 . ?
O1B Yb1 O1B 137.4(2) 2 . ?
O1A Yb1 O2B 79.48(15) . . ?
O1A Yb1 O2B 79.96(16) 2 . ?
O1W Yb1 O2B 125.31(15) . . ?
O1W Yb1 O2B 76.07(15) 2 . ?
O1B Yb1 O2B 140.47(15) 2 . ?
O1B Yb1 O2B 53.81(15) . . ?
O1A Yb1 O2B 79.96(15) . 2 ?
O1A Yb1 O2B 79.48(15) 2 2 ?
O1W Yb1 O2B 76.07(15) . 2 ?
O1W Yb1 O2B 125.31(15) 2 2 ?
O1B Yb1 O2B 53.81(15) 2 2 ?
O1B Yb1 O2B 140.47(15) . 2 ?
O2B Yb1 O2B 151.2(2) . 2 ?
O1A Yb1 C31B 106.46(18) . . ?
O1A Yb1 C31B 78.90(18) 2 . ?
O1W Yb1 C31B 98.26(18) . . ?
O1W Yb1 C31B 76.73(18) 2 . ?
O1B Yb1 C31B 147.88(17) 2 . ?
O1B Yb1 C31B 26.75(17) . . ?
O2B Yb1 C31B 27.06(17) . . ?
O2B Yb1 C31B 157.23(17) 2 . ?
O1A Yb1 C31B 78.90(18) . 2 ?
O1A Yb1 C31B 106.46(18) 2 2 ?
O1W Yb1 C31B 76.73(18) . 2 ?
O1W Yb1 C31B 98.26(18) 2 2 ?
O1B Yb1 C31B 26.75(17) 2 2 ?
O1B Yb1 C31B 147.88(18) . 2 ?
O2B Yb1 C31B 157.23(17) . 2 ?
O2B Yb1 C31B 27.06(17) 2 2 ?
C31B Yb1 C31B 172.7(3) . 2 ?
O2W Yb2 O2W 131.5(2) 2_655 . ?
O2W Yb2 O3W 78.11(17) 2_655 . ?
O2W Yb2 O3W 74.32(17) . . ?
O2W Yb2 O3W 74.32(17) 2_655 2_655 ?
O2W Yb2 O3W 78.11(17) . 2_655 ?
O3W Yb2 O3W 109.1(2) . 2_655 ?
O2W Yb2 O2C 131.99(16) 2_655 . ?
O2W Yb2 O2C 82.50(16) . . ?
O3W Yb2 O2C 82.20(17) . . ?
O3W Yb2 O2C 153.63(16) 2_655 . ?
O2W Yb2 O2C 82.50(16) 2_655 2_655 ?
O2W Yb2 O2C 131.99(16) . 2_655 ?
O3W Yb2 O2C 153.63(16) . 2_655 ?
O3W Yb2 O2C 82.20(17) 2_655 2_655 ?
O2C Yb2 O2C 98.1(2) . 2_655 ?
O2W Yb2 O1C 78.76(15) 2_655 . ?
O2W Yb2 O1C 132.31(16) . . ?
O3W Yb2 O1C 79.51(17) . . ?
O3W Yb2 O1C 149.02(15) 2_655 . ?
O2C Yb2 O1C 54.68(15) . . ?
O2C Yb2 O1C 79.32(16) 2_655 . ?
O2W Yb2 O1C 132.31(16) 2_655 2_655 ?
O2W Yb2 O1C 78.76(15) . 2_655 ?
O3W Yb2 O1C 149.02(15) . 2_655 ?
O3W Yb2 O1C 79.51(17) 2_655 2_655 ?
O2C Yb2 O1C 79.32(16) . 2_655 ?
O2C Yb2 O1C 54.68(15) 2_655 2_655 ?
O1C Yb2 O1C 108.8(2) . 2_655 ?
O2W Yb2 C31C 105.01(18) 2_655 . ?
O2W Yb2 C31C 107.50(19) . . ?
O3W Yb2 C31C 78.49(19) . . ?
O3W Yb2 C31C 171.79(19) 2_655 . ?
O2C Yb2 C31C 27.57(17) . . ?
O2C Yb2 C31C 89.59(19) 2_655 . ?
O1C Yb2 C31C 27.16(16) . . ?
O1C Yb2 C31C 95.52(18) 2_655 . ?
O2W Yb2 C31C 107.50(19) 2_655 2_655 ?
O2W Yb2 C31C 105.01(18) . 2_655 ?
O3W Yb2 C31C 171.79(19) . 2_655 ?
O3W Yb2 C31C 78.49(19) 2_655 2_655 ?
O2C Yb2 C31C 89.59(19) . 2_655 ?
O2C Yb2 C31C 27.57(17) 2_655 2_655 ?
O1C Yb2 C31C 95.52(18) . 2_655 ?
O1C Yb2 C31C 27.15(16) 2_655 2_655 ?
C31C Yb2 C31C 94.1(3) . 2_655 ?
N1A C2A C3A 123.0(7) . . ?
N1A C2A H2A 118.5 . . ?
C3A C2A H2A 118.5 . . ?
N1B C2B C3B 124.2(6) . . ?
N1B C2B H2B 117.9 . . ?
C3B C2B H2B 117.9 . . ?
N1C C2C C3C 122.7(6) . . ?
N1C C2C H2C 118.6 . . ?
C3C C2C H2C 118.6 . . ?
N1D C2D C3D 124.4(7) . . ?
N1D C2D H2D 117.8 . . ?
C3D C2D H2D 117.8 . . ?
C2A C3A C4A 119.4(6) . . ?
C2A C3A C31A 121.0(6) . . ?
C4A C3A C31A 119.5(6) . . ?
C2B C3B C4B 118.3(6) . . ?
C2B C3B C31B 119.8(6) . . ?
C4B C3B C31B 121.8(6) . . ?
C2C C3C C4C 118.2(6) . . ?
C2C C3C C31C 121.4(6) . . ?
C4C C3C C31C 120.4(6) . . ?
C2D C3D C4D 118.3(6) . . ?
C2D C3D C31D 119.0(6) . . ?
C4D C3D C31D 122.6(7) . . ?
C5A C4A C3A 117.0(6) . . ?
C5A C4A H4A 121.5 . . ?
C3A C4A H4A 121.5 . . ?
C5B C4B C3B 117.4(7) . . ?
C5B C4B H4B 121.3 . . ?
C3B C4B H4B 121.3 . . ?
C5C C4C C3C 118.3(6) . . ?
C5C C4C H4C 120.9 . . ?
C3C C4C H4C 120.9 . . ?
C5D C4D C3D 117.4(7) . . ?
C5D C4D H4D 121.3 . . ?
C3D C4D H4D 121.3 . . ?
C6A C5A C4A 120.8(7) . . ?
C6A C5A Br1A 120.3(6) . . ?
C4A C5A Br1A 118.8(5) . . ?
C6B C5B C4B 120.1(6) . . ?
C6B C5B Br1B 119.4(5) . . ?
C4B C5B Br1B 120.4(6) . . ?
C6C C5C C4C 120.1(6) . . ?
C6C C5C Br1C 119.5(6) . . ?
C4C C5C Br1C 120.4(5) . . ?
C6D C5D C4D 120.0(7) . . ?
C6D C5D Br1D 118.6(5) . . ?
C4D C5D Br1D 121.4(6) . . ?
N1A C6A C5A 121.9(7) . . ?
N1A C6A H6A 119.1 . . ?
C5A C6A H6A 119.1 . . ?
N1B C6B C5B 122.2(6) . . ?
N1B C6B H6B 118.9 . . ?
C5B C6B H6B 118.9 . . ?
N1C C6C C5C 122.5(7) . . ?
N1C C6C H6C 118.7 . . ?
C5C C6C H6C 118.7 . . ?
N1D C6D C5D 122.9(6) . . ?
N1D C6D H6D 118.6 . . ?
C5D C6D H6D 118.6 . . ?
O2A C31A O1A 125.1(6) . . ?
O2A C31A C3A 118.1(6) . . ?
O1A C31A C3A 116.8(6) . . ?
O1B C31B O2B 122.1(6) . . ?
O1B C31B C3B 118.7(6) . . ?
O2B C31B C3B 119.1(6) . . ?
O1B C31B Yb1 59.2(3) . . ?
O2B C31B Yb1 62.9(3) . . ?
C3B C31B Yb1 177.9(5) . . ?
O1C C31C O2C 120.8(7) . . ?
O1C C31C C3C 120.9(6) . . ?
O2C C31C C3C 118.4(6) . . ?
O1C C31C Yb2 63.4(4) . . ?
O2C C31C Yb2 57.6(3) . . ?
C3C C31C Yb2 174.4(5) . . ?
O2D C31D O1D 125.6(6) . . ?
O2D C31D C3D 122.3(7) . . ?
O1D C31D C3D 112.1(6) . . ?
C6A N1A C2A 117.8(6) . . ?
C2B N1B C6B 117.7(6) . . ?
C6C N1C C2C 118.1(6) . . ?
C2D N1D C6D 117.0(6) . . ?
Yb1 O1W H11W 128.1 . . ?
Yb1 O1W H12W 123.3 . . ?
H11W O1W H12W 103.7 . . ?
Yb2 O2W H21W 127.1 . . ?
Yb2 O2W H22W 127.9 . . ?
H21W O2W H22W 104.8 . . ?
Yb2 O3W H31W 122.0 . . ?
Yb2 O3W H32W 121.2 . . ?
H31W O3W H32W 104.8 . . ?
C31A O1A Yb1 139.9(4) . . ?
C31B O1B Yb1 94.0(4) . . ?
C31C O1C Yb2 89.5(4) . . ?
C31B O2B Yb1 90.0(4) . . ?
C31C O2C Yb2 94.9(4) . . ?
C31D O1D H1D 110.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O2C 0.85 1.90 2.731(6) 167.6 .
O1W H12W N1B 0.86 1.90 2.733(7) 163.2 3_566
O2W H22W N1C 0.85 1.84 2.681(7) 170.6 4_566
O2W H21W O2A 0.85 1.91 2.729(6) 163.2 2
O3W H31W O2B 0.85 1.94 2.770(6) 166.4 2
O3W H32W N1D 0.85 1.86 2.701(7) 169.2 .

_refine_diff_density_max         1.678
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.286

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Compound4
_database_code_depnum_ccdc_archive 'CCDC 1882987'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV/EHU)
Spain
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6

_chemical_name_systematic        
;
poly-{[triaquabis(mu-5-bromonicotinato-kO:kO')(5-bromonicotinato-kO)neodymium(III)] 
hydrate}
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H17 Br3 N3 Nd O10'
_chemical_formula_weight         819.31

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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1630(5)
_cell_length_b                   11.5260(6)
_cell_length_c                   11.6110(6)
_cell_angle_alpha                88.319(2)
_cell_angle_beta                 85.525(2)
_cell_angle_gamma                69.254(2)
_cell_volume                     1268.03(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30674
_cell_measurement_theta_min      2.306
_cell_measurement_theta_max      26.411

_exptl_crystal_description       'rectangular plate'
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_F_000             782
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    6.830
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1297
_exptl_absorpt_correction_T_max  0.5664
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(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  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            30674
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.306
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5222
_reflns_number_gt                4343
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
O4w crystallization water molecule presents a significant large and prolate 
ellipsoid that suggests it could be involved in a disorder. Indeed, taking
into account that it shows two quite large residual density peaks in its surroundig
it has been disordered into two equivalent dispositions (with 50% occupancy according
to a previous simulation with SUMP order), both of which satisfy well the 
accurate hydrogen bonding scheme. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0158P)²+0.8166P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5222
_refine_ls_number_parameters     325
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0500
_refine_ls_wR_factor_gt          0.0465
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.002
_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
Nd1 Nd 0.72538(2) 0.02851(2) 0.47476(2) 0.00540(5) Uani 1 1 d . . . . .
Br1A Br 1.10517(4) -0.50958(4) 0.28722(4) 0.02283(10) Uani 1 1 d . . . . .
Br1B Br 0.18225(4) 0.36186(4) 0.94187(4) 0.03505(13) Uani 1 1 d . . . . .
Br1C Br 0.48587(4) 0.51886(4) 0.78908(4) 0.02820(11) Uani 1 1 d . . . . .
C2A C 0.6658(4) -0.4571(3) 0.4556(3) 0.0146(8) Uani 1 1 d . . . . .
H2A H 0.5770 -0.4484 0.4898 0.017 Uiso 1 1 calc R U . . .
C2B C 0.6259(4) 0.0828(3) 0.9925(3) 0.0121(8) Uani 1 1 d . . . . .
H2B H 0.7153 0.0260 1.0041 0.014 Uiso 1 1 calc R U . . .
C2C C 0.9026(4) 0.2050(3) 0.8492(3) 0.0124(8) Uani 1 1 d . . . . .
H2C H 0.9897 0.1445 0.8610 0.015 Uiso 1 1 calc R U . . .
C3A C 0.7021(3) -0.3515(3) 0.4428(3) 0.0080(7) Uani 1 1 d . . . . .
C3B C 0.5830(4) 0.1003(3) 0.8801(3) 0.0108(8) Uani 1 1 d . . . . .
C3C C 0.8519(3) 0.2138(3) 0.7405(3) 0.0098(7) Uani 1 1 d . . . . .
C31A C 0.5944(3) -0.2277(3) 0.4778(3) 0.0078(7) Uani 1 1 d . . . . .
C31B C 0.6780(3) 0.0270(3) 0.7808(3) 0.0096(7) Uani 1 1 d . . . . .
C31C C 0.9373(3) 0.1320(3) 0.6440(3) 0.0093(7) Uani 1 1 d . . . . .
C4A C 0.8358(3) -0.3639(3) 0.3939(3) 0.0109(8) Uani 1 1 d . . . . .
H4A H 0.8651 -0.2961 0.3851 0.013 Uiso 1 1 calc R U . . .
C4B C 0.4503(4) 0.1859(3) 0.8631(3) 0.0132(8) Uani 1 1 d . . . . .
H4B H 0.4179 0.2018 0.7895 0.016 Uiso 1 1 calc R U . . .
C4C C 0.7230(3) 0.3045(3) 0.7219(3) 0.0102(7) Uani 1 1 d . . . . .
H4C H 0.6839 0.3117 0.6511 0.012 Uiso 1 1 calc R U . . .
C5A C 0.9231(3) -0.4812(3) 0.3591(3) 0.0121(8) Uani 1 1 d . . . . .
C5B C 0.3667(4) 0.2473(3) 0.9586(3) 0.0164(8) Uani 1 1 d . . . . .
C5C C 0.6540(4) 0.3840(3) 0.8123(3) 0.0139(8) Uani 1 1 d . . . . .
C6A C 0.8792(4) -0.5806(3) 0.3731(3) 0.0164(8) Uani 1 1 d . . . . .
H6A H 0.9404 -0.6582 0.3480 0.020 Uiso 1 1 calc R U . . .
C6B C 0.4173(4) 0.2240(3) 1.0672(3) 0.0159(8) Uani 1 1 d . . . . .
H6B H 0.3601 0.2659 1.1305 0.019 Uiso 1 1 calc R U . . .
C6C C 0.7113(4) 0.3686(3) 0.9184(3) 0.0155(8) Uani 1 1 d . . . . .
H6C H 0.6634 0.4229 0.9781 0.019 Uiso 1 1 calc R U . . .
N1A N 0.7516(3) -0.5704(3) 0.4215(3) 0.0191(7) Uani 1 1 d . . . . .
N1B N 0.5467(3) 0.1425(3) 1.0839(3) 0.0153(7) Uani 1 1 d . . . . .
N1C N 0.8334(3) 0.2783(3) 0.9380(3) 0.0170(7) Uani 1 1 d . . . . .
O1A O 0.4699(2) -0.2239(2) 0.5003(2) 0.0113(5) Uani 1 1 d . . . . .
O1C O 1.0676(2) 0.0801(2) 0.6529(2) 0.0121(5) Uani 1 1 d . . . . .
O2A O 0.6327(2) -0.1352(2) 0.4815(2) 0.0115(5) Uani 1 1 d . . . . .
O1B O 0.7969(2) -0.0471(2) 0.8016(2) 0.0173(6) Uani 1 1 d . . . . .
O2B O 0.6286(2) 0.0455(2) 0.6814(2) 0.0101(5) Uani 1 1 d . . . . .
O2C O 0.8724(2) 0.1233(2) 0.5577(2) 0.0107(5) Uani 1 1 d . . . . .
O1W O 0.8996(2) -0.1370(2) 0.5879(2) 0.0121(5) Uani 1 1 d . . . . .
O2W O 0.6106(2) 0.0251(2) 0.2985(2) 0.0126(5) Uani 1 1 d . . . . .
O3W O 0.7612(3) 0.1883(2) 0.3416(2) 0.0155(6) Uani 1 1 d . . . . .
O4W1 O 0.9283(10) 0.1959(8) 0.1569(9) 0.029(2) Uani 0.5 1 d . . P A 1
O4W2 O 0.9190(11) 0.1408(7) 0.1434(9) 0.023(2) Uani 0.5 1 d . . P B 2
H11W H 0.8794 -0.1192 0.6590 0.035 Uiso 1 1 d . U . . .
H12W H 0.9811 -0.1324 0.5734 0.035 Uiso 1 1 d . U . . .
H21W H 0.5437 -0.0025 0.3098 0.035 Uiso 1 1 d . U . . .
H22W H 0.5864 0.0743 0.2415 0.035 Uiso 1 1 d . U . . .
H31W H 0.8040 0.1838 0.2761 0.035 Uiso 1 1 d . U . . .
H32W H 0.7370 0.2619 0.3639 0.035 Uiso 1 1 d . U . . .
H41W H 1.0113 0.1427 0.1497 0.035 Uiso 1 1 d . U . . .
H42W H 0.9005 0.2058 0.0885 0.035 Uiso 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
Nd1 O2A 2.386(2) . ?
Nd1 O2C 2.407(2) . ?
Nd1 O1A 2.424(2) 2_656 ?
Nd1 O1C 2.439(2) 2_756 ?
Nd1 O2W 2.442(2) . ?
Nd1 O3W 2.477(2) . ?
Nd1 O2B 2.507(2) . ?
Nd1 O1W 2.515(2) . ?
Br1A C5A 1.890(3) . ?
Br1B C5B 1.893(4) . ?
Br1C C5C 1.891(3) . ?
C2A N1A 1.339(4) . ?
C2A C3A 1.392(5) . ?
C2A H2A 0.9300 . ?
C2B N1B 1.329(4) . ?
C2B C3B 1.394(5) . ?
C2B H2B 0.9300 . ?
C2C N1C 1.337(4) . ?
C2C C3C 1.388(5) . ?
C2C H2C 0.9300 . ?
C3A C4A 1.392(5) . ?
C3A C31A 1.502(4) . ?
C3B C4B 1.386(5) . ?
C3B C31B 1.510(5) . ?
C3C C4C 1.384(5) . ?
C3C C31C 1.492(5) . ?
C31A O1A 1.257(4) . ?
C31A O2A 1.261(4) . ?
C31B O1B 1.245(4) . ?
C31B O2B 1.276(4) . ?
C31C O1C 1.256(4) . ?
C31C O2C 1.267(4) . ?
C4A C5A 1.381(5) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.387(5) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.385(5) . ?
C4C H4C 0.9300 . ?
C5A C6A 1.371(5) . ?
C5B C6B 1.382(5) . ?
C5C C6C 1.384(5) . ?
C6A N1A 1.339(5) . ?
C6A H6A 0.9300 . ?
C6B N1B 1.343(4) . ?
C6B H6B 0.9300 . ?
C6C N1C 1.338(4) . ?
C6C H6C 0.9300 . ?
O1A Nd1 2.424(2) 2_656 ?
O1C Nd1 2.439(2) 2_756 ?
O1W H11W 0.8479 . ?
O1W H12W 0.8522 . ?
O2W H21W 0.8470 . ?
O2W H22W 0.8504 . ?
O3W H31W 0.8400 . ?
O3W H32W 0.8375 . ?
O4W1 H41W 0.8480 . ?
O4W1 H42W 0.8541 . ?
O4W2 H41W 0.9544 . ?
O4W2 H42W 0.9443 . ?

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
O2A Nd1 O2C 147.95(8) . . ?
O2A Nd1 O1A 108.40(8) . 2_656 ?
O2C Nd1 O1A 88.49(8) . 2_656 ?
O2A Nd1 O1C 95.18(8) . 2_756 ?
O2C Nd1 O1C 86.04(8) . 2_756 ?
O1A Nd1 O1C 142.63(8) 2_656 2_756 ?
O2A Nd1 O2W 69.28(8) . . ?
O2C Nd1 O2W 141.83(8) . . ?
O1A Nd1 O2W 81.39(8) 2_656 . ?
O1C Nd1 O2W 80.42(8) 2_756 . ?
O2A Nd1 O3W 141.01(8) . . ?
O2C Nd1 O3W 70.05(8) . . ?
O1A Nd1 O3W 69.19(8) 2_656 . ?
O1C Nd1 O3W 74.21(8) 2_756 . ?
O2W Nd1 O3W 71.95(8) . . ?
O2A Nd1 O2B 80.16(8) . . ?
O2C Nd1 O2B 79.83(8) . . ?
O1A Nd1 O2B 71.45(8) 2_656 . ?
O1C Nd1 O2B 142.91(7) 2_756 . ?
O2W Nd1 O2B 129.76(7) . . ?
O3W Nd1 O2B 130.27(7) . . ?
O2A Nd1 O1W 77.24(8) . . ?
O2C Nd1 O1W 72.93(8) . . ?
O1A Nd1 O1W 141.47(8) 2_656 . ?
O1C Nd1 O1W 70.90(8) 2_756 . ?
O2W Nd1 O1W 133.23(8) . . ?
O3W Nd1 O1W 130.06(8) . . ?
O2B Nd1 O1W 72.19(7) . . ?
N1A C2A C3A 123.7(3) . . ?
N1A C2A H2A 118.1 . . ?
C3A C2A H2A 118.1 . . ?
N1B C2B C3B 123.9(3) . . ?
N1B C2B H2B 118.1 . . ?
C3B C2B H2B 118.1 . . ?
N1C C2C C3C 123.8(3) . . ?
N1C C2C H2C 118.1 . . ?
C3C C2C H2C 118.1 . . ?
C4A C3A C2A 118.6(3) . . ?
C4A C3A C31A 122.2(3) . . ?
C2A C3A C31A 119.2(3) . . ?
C4B C3B C2B 117.8(3) . . ?
C4B C3B C31B 121.4(3) . . ?
C2B C3B C31B 120.8(3) . . ?
C4C C3C C2C 118.4(3) . . ?
C4C C3C C31C 120.6(3) . . ?
C2C C3C C31C 121.0(3) . . ?
O1A C31A O2A 124.4(3) . . ?
O1A C31A C3A 116.6(3) . . ?
O2A C31A C3A 119.0(3) . . ?
O1B C31B O2B 125.1(3) . . ?
O1B C31B C3B 118.2(3) . . ?
O2B C31B C3B 116.8(3) . . ?
O1C C31C O2C 125.0(3) . . ?
O1C C31C C3C 118.0(3) . . ?
O2C C31C C3C 116.9(3) . . ?
C5A C4A C3A 117.1(3) . . ?
C5A C4A H4A 121.5 . . ?
C3A C4A H4A 121.5 . . ?
C3B C4B C5B 118.4(3) . . ?
C3B C4B H4B 120.8 . . ?
C5B C4B H4B 120.8 . . ?
C3C C4C C5C 117.9(3) . . ?
C3C C4C H4C 121.1 . . ?
C5C C4C H4C 121.1 . . ?
C6A C5A C4A 121.0(3) . . ?
C6A C5A Br1A 117.8(3) . . ?
C4A C5A Br1A 121.2(3) . . ?
C6B C5B C4B 120.0(3) . . ?
C6B C5B Br1B 119.5(3) . . ?
C4B C5B Br1B 120.5(3) . . ?
C6C C5C C4C 120.2(3) . . ?
C6C C5C Br1C 119.6(3) . . ?
C4C C5C Br1C 120.2(3) . . ?
N1A C6A C5A 122.6(3) . . ?
N1A C6A H6A 118.7 . . ?
C5A C6A H6A 118.7 . . ?
N1B C6B C5B 121.8(3) . . ?
N1B C6B H6B 119.1 . . ?
C5B C6B H6B 119.1 . . ?
N1C C6C C5C 122.1(3) . . ?
N1C C6C H6C 119.0 . . ?
C5C C6C H6C 119.0 . . ?
C2A N1A C6A 117.1(3) . . ?
C2B N1B C6B 118.1(3) . . ?
C2C N1C C6C 117.5(3) . . ?
C31A O1A Nd1 121.5(2) . 2_656 ?
C31C O1C Nd1 136.9(2) . 2_756 ?
C31A O2A Nd1 174.0(2) . . ?
C31B O2B Nd1 137.0(2) . . ?
C31C O2C Nd1 147.4(2) . . ?
Nd1 O1W H11W 107.8 . . ?
Nd1 O1W H12W 108.8 . . ?
H11W O1W H12W 104.9 . . ?
Nd1 O2W H21W 112.5 . . ?
Nd1 O2W H22W 134.4 . . ?
H21W O2W H22W 103.5 . . ?
Nd1 O3W H31W 132.4 . . ?
Nd1 O3W H32W 119.9 . . ?
H31W O3W H32W 107.2 . . ?
H41W O4W1 H42W 104.7 . . ?
H41W O4W2 H42W 90.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O1B 0.85 1.87 2.702(3) 165.6 .
O1W H12W O2C 0.85 2.07 2.808(3) 144.3 2_756
O2W H22W N1B 0.85 1.98 2.809(4) 163.3 1_554
O2W H21W O2B 0.85 1.98 2.816(3) 170.7 2_656
O3W H32W N1A 0.84 2.12 2.923(4) 160.3 1_565

_refine_diff_density_max         0.549
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.137

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_Compound2
_database_code_depnum_ccdc_archive 'CCDC 1882985'
loop_
_audit_author_name
_audit_author_address
'Javier Cepeda'
;University of the Basque Country (UPV/EHU)
Spain
;
_audit_update_record             
;
2018-12-26 deposited with the CCDC.	2019-05-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6

_chemical_name_systematic        
"[tetraaquabis(5-bromonicotinato-kO)terbium(III)][diaquabis(5-bromonicotinato-k2O,O')bis(5-bromonicotinato-kO)terbium(III)] bis(5-bromonicotinic acid)"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H19 Br4 N4 O11 Tb'
_chemical_formula_weight         1017.99

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'
Br Br -0.2901 2.4595 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   11.6860(6)
_cell_length_b                   15.9703(9)
_cell_length_c                   16.7415(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.246(2)
_cell_angle_gamma                90
_cell_volume                     3124.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    82273
_cell_measurement_theta_min      2.433
_cell_measurement_theta_max      28.775

_exptl_crystal_description       'rectangular plate'
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_F_000             1936
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    7.441
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1325
_exptl_absorpt_correction_T_max  0.6100
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_absorpt_special_details   ?

_exptl_special_details           
;
 ?
;
_diffrn_ambient_temperature      100(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  'Bruker Venture'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            82273
_diffrn_reflns_av_unetI/netI     0.0511
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.433
_diffrn_reflns_theta_max         28.775
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8124
_reflns_number_gt                6299
_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 APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_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)+(0.0181P)²+10.5823P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8124
_refine_ls_number_parameters     398
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0597
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_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
Tb1 Tb 0.0000 0.35128(2) 0.2500 0.00649(6) Uani 1 2 d S T P . .
Tb2 Tb 0.5000 0.38576(2) 0.2500 0.00634(6) Uani 1 2 d S T P . .
Br1A Br -0.15964(4) -0.15145(3) 0.18910(4) 0.03360(14) Uani 1 1 d . . . . .
Br1B Br -0.43104(4) 0.25872(3) 0.61025(3) 0.01900(10) Uani 1 1 d . . . . .
Br1C Br 0.03692(3) 0.71187(3) 0.12004(3) 0.01779(10) Uani 1 1 d . . . . .
Br1D Br 0.38412(4) -0.08368(3) 0.17562(3) 0.02114(10) Uani 1 1 d . . . . .
C2A C 0.0102(3) 0.0993(3) 0.1257(2) 0.0122(8) Uani 1 1 d . . . . .
H2A H 0.0455 0.1498 0.1133 0.015 Uiso 1 1 calc R U . . .
C2B C -0.1501(3) 0.4399(3) 0.5267(2) 0.0120(8) Uani 1 1 d . . . . .
H2B H -0.0937 0.4773 0.5106 0.014 Uiso 1 1 calc R U . . .
C2C C 0.3615(3) 0.5852(3) 0.0240(2) 0.0127(8) Uani 1 1 d . . . . .
H2C H 0.4282 0.5612 0.0042 0.015 Uiso 1 1 calc R U . . .
C2D C 0.5791(3) 0.1411(3) 0.0730(3) 0.0171(9) Uani 1 1 d . . . . .
H2D H 0.6164 0.1873 0.0516 0.021 Uiso 1 1 calc R U . . .
C3A C -0.0915(3) 0.1010(3) 0.1688(2) 0.0088(8) Uani 1 1 d . . . . .
C3B C -0.1768(3) 0.3732(3) 0.4764(2) 0.0107(8) Uani 1 1 d . . . . .
C3C C 0.3273(3) 0.5653(3) 0.1010(2) 0.0095(8) Uani 1 1 d . . . . .
C3D C 0.6253(3) 0.0624(3) 0.0602(2) 0.0134(8) Uani 1 1 d . . . . .
C4A C -0.1425(3) 0.0256(3) 0.1886(2) 0.0116(8) Uani 1 1 d . . . . .
H4A H -0.2103 0.0243 0.2174 0.014 Uiso 1 1 calc R U . . .
C4B C -0.2602(3) 0.3160(3) 0.5011(2) 0.0112(8) Uani 1 1 d . . . . .
H4B H -0.2789 0.2695 0.4703 0.013 Uiso 1 1 calc R U . . .
C4C C 0.2273(3) 0.6013(3) 0.1306(2) 0.0110(8) Uani 1 1 d . . . . .
H4C H 0.2012 0.5886 0.1816 0.013 Uiso 1 1 calc R U . . .
C4D C 0.5696(3) -0.0079(3) 0.0907(2) 0.0142(9) Uani 1 1 d . . . . .
H4D H 0.5975 -0.0617 0.0821 0.017 Uiso 1 1 calc R U . . .
C5A C -0.0906(4) -0.0474(3) 0.1645(3) 0.0158(9) Uani 1 1 d . . . . .
C5B C -0.3141(3) 0.3313(3) 0.5735(2) 0.0118(8) Uani 1 1 d . . . . .
C5C C 0.1684(3) 0.6563(3) 0.0822(2) 0.0116(8) Uani 1 1 d . . . . .
C5D C 0.4710(3) 0.0061(3) 0.1343(2) 0.0147(9) Uani 1 1 d . . . . .
C6A C 0.0092(3) -0.0452(3) 0.1205(3) 0.0152(9) Uani 1 1 d . . . . .
H6A H 0.0424 -0.0951 0.1039 0.018 Uiso 1 1 calc R U . . .
C6B C -0.2834(3) 0.3995(3) 0.6192(2) 0.0134(9) Uani 1 1 d . . . . .
H6B H -0.3211 0.4086 0.6673 0.016 Uiso 1 1 calc R U . . .
C6C C 0.2062(4) 0.6723(3) 0.0053(3) 0.0158(9) Uani 1 1 d . . . . .
H6C H 0.1638 0.7079 -0.0274 0.019 Uiso 1 1 calc R U . . .
C6D C 0.4310(4) 0.0873(3) 0.1453(3) 0.0180(9) Uani 1 1 d . . . . .
H6D H 0.3651 0.0956 0.1753 0.022 Uiso 1 1 calc R U . . .
C31A C -0.1481(3) 0.1833(3) 0.1899(2) 0.0099(8) Uani 1 1 d . . . . .
C31B C -0.1164(3) 0.3634(3) 0.3982(2) 0.0105(8) Uani 1 1 d . . . . .
C31C C 0.3951(3) 0.5061(2) 0.1512(2) 0.0091(8) Uani 1 1 d . . . . .
C31D C 0.7338(3) 0.0554(3) 0.0125(2) 0.0128(8) Uani 1 1 d . . . . .
N1A N 0.0591(3) 0.0280(2) 0.1014(2) 0.0154(8) Uani 1 1 d . . . . .
N1B N -0.2012(3) 0.4530(2) 0.5970(2) 0.0145(7) Uani 1 1 d . . . . .
N1C N 0.3019(3) 0.6377(2) -0.0232(2) 0.0146(8) Uani 1 1 d . . . . .
N1D N 0.4836(3) 0.1534(2) 0.1146(2) 0.0191(8) Uani 1 1 d . . . . .
O1W O 0.1401(2) 0.45078(19) 0.27575(16) 0.0128(6) Uani 1 1 d . . . . .
H11W H 0.2044 0.4525 0.2528 0.019 Uiso 1 1 d . U . . .
H12W H 0.1497 0.4769 0.3193 0.019 Uiso 1 1 d . U . . .
O2W O 0.3594(2) 0.32595(18) 0.32580(16) 0.0120(6) Uani 1 1 d . . . . .
H21W H 0.3551 0.3295 0.3764 0.018 Uiso 1 1 d . U . . .
H22W H 0.3236 0.2813 0.3142 0.018 Uiso 1 1 d . U . . .
O3W O 0.3932(2) 0.30153(18) 0.16339(17) 0.0129(6) Uani 1 1 d . . . . .
H31W H 0.3208 0.2974 0.1644 0.019 Uiso 1 1 d . U . . .
H32W H 0.4164 0.2538 0.1482 0.019 Uiso 1 1 d . U . . .
O1A O -0.0893(2) 0.24935(18) 0.17825(16) 0.0130(6) Uani 1 1 d . . . . .
O1B O -0.0284(2) 0.40655(19) 0.38534(16) 0.0137(6) Uani 1 1 d . . . . .
O1C O 0.4896(2) 0.47887(18) 0.12880(16) 0.0120(6) Uani 1 1 d . . . . .
O1D O 0.7568(2) -0.0227(2) -0.00903(18) 0.0181(7) Uani 1 1 d . . . . .
H1D H 0.8141 -0.0253 -0.0321 0.022 Uiso 1 1 d . U . . .
O2A O -0.2480(2) 0.18127(18) 0.21440(18) 0.0149(6) Uani 1 1 d . . . . .
O2B O -0.1570(2) 0.31354(18) 0.34589(15) 0.0102(6) Uani 1 1 d . . . . .
O2C O 0.3527(2) 0.48360(18) 0.21860(16) 0.0116(6) Uani 1 1 d . . . . .
O2D O 0.7910(2) 0.1164(2) -0.00426(18) 0.0192(7) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1A 2.274(3) . ?
Tb1 O1A 2.274(3) 2 ?
Tb1 O1W 2.320(3) 2 ?
Tb1 O1W 2.320(3) . ?
Tb1 O1B 2.455(3) 2 ?
Tb1 O1B 2.456(3) . ?
Tb1 O2B 2.517(3) . ?
Tb1 O2B 2.517(3) 2 ?
Tb1 C31B 2.841(4) . ?
Tb1 C31B 2.841(4) 2 ?
Tb2 O2W 2.290(3) 2_655 ?
Tb2 O2W 2.290(3) . ?
Tb2 O3W 2.335(3) . ?
Tb2 O3W 2.335(3) 2_655 ?
Tb2 O2C 2.382(3) . ?
Tb2 O2C 2.382(3) 2_655 ?
Tb2 O1C 2.518(3) 2_655 ?
Tb2 O1C 2.518(3) . ?
Tb2 C31C 2.813(4) . ?
Tb2 C31C 2.813(4) 2_655 ?
Br1A C5A 1.894(4) . ?
Br1B C5B 1.897(4) . ?
Br1C C5C 1.886(4) . ?
Br1D C5D 1.890(4) . ?
C2A N1A 1.338(5) . ?
C2A C3A 1.393(5) . ?
C2A H2A 0.9300 . ?
C2B N1B 1.338(5) . ?
C2B C3B 1.392(6) . ?
C2B H2B 0.9300 . ?
C2C N1C 1.345(5) . ?
C2C C3C 1.389(5) . ?
C2C H2C 0.9300 . ?
C2D N1D 1.333(5) . ?
C2D C3D 1.384(6) . ?
C2D H2D 0.9300 . ?
C3A C4A 1.386(6) . ?
C3A C31A 1.514(5) . ?
C3B C4B 1.399(5) . ?
C3B C31B 1.499(5) . ?
C3C C4C 1.396(5) . ?
C3C C31C 1.491(5) . ?
C3D C4D 1.396(6) . ?
C3D C31D 1.506(5) . ?
C4A C5A 1.374(6) . ?
C4A H4A 0.9300 . ?
C4B C5B 1.389(5) . ?
C4B H4B 0.9300 . ?
C4C C5C 1.378(6) . ?
C4C H4C 0.9300 . ?
C4D C5D 1.385(5) . ?
C4D H4D 0.9300 . ?
C5A C6A 1.383(5) . ?
C5B C6B 1.378(6) . ?
C5C C6C 1.387(6) . ?
C5D C6D 1.392(6) . ?
C6A N1A 1.345(5) . ?
C6A H6A 0.9300 . ?
C6B N1B 1.341(5) . ?
C6B H6B 0.9300 . ?
C6C N1C 1.338(5) . ?
C6C H6C 0.9300 . ?
C6D N1D 1.326(6) . ?
C6D H6D 0.9300 . ?
C31A O2A 1.239(5) . ?
C31A O1A 1.275(5) . ?
C31B O1B 1.257(5) . ?
C31B O2B 1.274(5) . ?
C31C O1C 1.245(4) . ?
C31C O2C 1.285(5) . ?
C31D O2D 1.214(5) . ?
C31D O1D 1.327(5) . ?
O1W H11W 0.8468 . ?
O1W H12W 0.8482 . ?
O2W H21W 0.8514 . ?
O2W H22W 0.8486 . ?
O3W H31W 0.8489 . ?
O3W H32W 0.8487 . ?
O1D H1D 0.7760 . ?

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
O1A Tb1 O1A 88.56(15) . 2 ?
O1A Tb1 O1W 94.04(10) . 2 ?
O1A Tb1 O1W 155.51(9) 2 2 ?
O1A Tb1 O1W 155.51(9) . . ?
O1A Tb1 O1W 94.04(10) 2 . ?
O1W Tb1 O1W 93.56(14) 2 . ?
O1A Tb1 O1B 80.41(10) . 2 ?
O1A Tb1 O1B 132.95(9) 2 2 ?
O1W Tb1 O1B 71.37(9) 2 2 ?
O1W Tb1 O1B 80.05(10) . 2 ?
O1A Tb1 O1B 132.95(9) . . ?
O1A Tb1 O1B 80.41(10) 2 . ?
O1W Tb1 O1B 80.05(10) 2 . ?
O1W Tb1 O1B 71.37(9) . . ?
O1B Tb1 O1B 137.87(14) 2 . ?
O1A Tb1 O2B 80.30(9) . . ?
O1A Tb1 O2B 79.96(9) 2 . ?
O1W Tb1 O2B 76.51(9) 2 . ?
O1W Tb1 O2B 124.14(9) . . ?
O1B Tb1 O2B 140.95(9) 2 . ?
O1B Tb1 O2B 52.81(9) . . ?
O1A Tb1 O2B 79.96(9) . 2 ?
O1A Tb1 O2B 80.30(9) 2 2 ?
O1W Tb1 O2B 124.14(9) 2 2 ?
O1W Tb1 O2B 76.51(9) . 2 ?
O1B Tb1 O2B 52.81(9) 2 2 ?
O1B Tb1 O2B 140.95(9) . 2 ?
O2B Tb1 O2B 152.29(13) . 2 ?
O1A Tb1 C31B 106.85(11) . . ?
O1A Tb1 C31B 78.92(10) 2 . ?
O1W Tb1 C31B 77.03(10) 2 . ?
O1W Tb1 C31B 97.54(11) . . ?
O1B Tb1 C31B 148.03(10) 2 . ?
O1B Tb1 C31B 26.18(10) . . ?
O2B Tb1 C31B 26.63(10) . . ?
O2B Tb1 C31B 157.91(10) 2 . ?
O1A Tb1 C31B 78.92(10) . 2 ?
O1A Tb1 C31B 106.85(11) 2 2 ?
O1W Tb1 C31B 97.53(11) 2 2 ?
O1W Tb1 C31B 77.02(10) . 2 ?
O1B Tb1 C31B 26.18(10) 2 2 ?
O1B Tb1 C31B 148.04(10) . 2 ?
O2B Tb1 C31B 157.91(10) . 2 ?
O2B Tb1 C31B 26.63(10) 2 2 ?
C31B Tb1 C31B 172.18(16) . 2 ?
O2W Tb2 O2W 130.69(15) 2_655 . ?
O2W Tb2 O3W 78.37(10) 2_655 . ?
O2W Tb2 O3W 73.80(10) . . ?
O2W Tb2 O3W 73.80(10) 2_655 2_655 ?
O2W Tb2 O3W 78.37(10) . 2_655 ?
O3W Tb2 O3W 109.65(15) . 2_655 ?
O2W Tb2 O2C 132.16(9) 2_655 . ?
O2W Tb2 O2C 82.88(10) . . ?
O3W Tb2 O2C 81.79(10) . . ?
O3W Tb2 O2C 153.98(9) 2_655 . ?
O2W Tb2 O2C 82.89(10) 2_655 2_655 ?
O2W Tb2 O2C 132.16(9) . 2_655 ?
O3W Tb2 O2C 153.98(9) . 2_655 ?
O3W Tb2 O2C 81.79(10) 2_655 2_655 ?
O2C Tb2 O2C 98.01(14) . 2_655 ?
O2W Tb2 O1C 131.34(9) 2_655 2_655 ?
O2W Tb2 O1C 80.34(9) . 2_655 ?
O3W Tb2 O1C 149.82(9) . 2_655 ?
O3W Tb2 O1C 79.39(10) 2_655 2_655 ?
O2C Tb2 O1C 79.80(9) . 2_655 ?
O2C Tb2 O1C 53.30(8) 2_655 2_655 ?
O2W Tb2 O1C 80.34(9) 2_655 . ?
O2W Tb2 O1C 131.34(9) . . ?
O3W Tb2 O1C 79.39(10) . . ?
O3W Tb2 O1C 149.82(9) 2_655 . ?
O2C Tb2 O1C 53.30(8) . . ?
O2C Tb2 O1C 79.80(9) 2_655 . ?
O1C Tb2 O1C 107.62(13) 2_655 . ?
O2W Tb2 C31C 105.73(10) 2_655 . ?
O2W Tb2 C31C 107.39(10) . . ?
O3W Tb2 C31C 78.37(11) . . ?
O3W Tb2 C31C 171.44(11) 2_655 . ?
O2C Tb2 C31C 27.06(10) . . ?
O2C Tb2 C31C 89.67(10) 2_655 . ?
O1C Tb2 C31C 95.15(10) 2_655 . ?
O1C Tb2 C31C 26.28(9) . . ?
O2W Tb2 C31C 107.39(10) 2_655 2_655 ?
O2W Tb2 C31C 105.73(10) . 2_655 ?
O3W Tb2 C31C 171.44(11) . 2_655 ?
O3W Tb2 C31C 78.37(11) 2_655 2_655 ?
O2C Tb2 C31C 89.67(10) . 2_655 ?
O2C Tb2 C31C 27.05(10) 2_655 2_655 ?
O1C Tb2 C31C 26.28(9) 2_655 2_655 ?
O1C Tb2 C31C 95.15(10) . 2_655 ?
C31C Tb2 C31C 93.80(16) . 2_655 ?
N1A C2A C3A 122.8(4) . . ?
N1A C2A H2A 118.6 . . ?
C3A C2A H2A 118.6 . . ?
N1B C2B C3B 123.5(4) . . ?
N1B C2B H2B 118.2 . . ?
C3B C2B H2B 118.2 . . ?
N1C C2C C3C 122.5(4) . . ?
N1C C2C H2C 118.7 . . ?
C3C C2C H2C 118.7 . . ?
N1D C2D C3D 122.9(4) . . ?
N1D C2D H2D 118.5 . . ?
C3D C2D H2D 118.5 . . ?
C4A C3A C2A 118.4(4) . . ?
C4A C3A C31A 120.7(3) . . ?
C2A C3A C31A 120.9(4) . . ?
C2B C3B C4B 118.4(4) . . ?
C2B C3B C31B 120.2(4) . . ?
C4B C3B C31B 121.5(4) . . ?
C2C C3C C4C 118.7(4) . . ?
C2C C3C C31C 121.0(3) . . ?
C4C C3C C31C 120.4(3) . . ?
C2D C3D C4D 119.4(4) . . ?
C2D C3D C31D 118.6(4) . . ?
C4D C3D C31D 121.9(4) . . ?
C5A C4A C3A 118.4(4) . . ?
C5A C4A H4A 120.8 . . ?
C3A C4A H4A 120.8 . . ?
C5B C4B C3B 117.5(4) . . ?
C5B C4B H4B 121.2 . . ?
C3B C4B H4B 121.2 . . ?
C5C C4C C3C 118.1(4) . . ?
C5C C4C H4C 120.9 . . ?
C3C C4C H4C 120.9 . . ?
C5D C4D C3D 117.0(4) . . ?
C5D C4D H4D 121.5 . . ?
C3D C4D H4D 121.5 . . ?
C4A C5A C6A 120.6(4) . . ?
C4A C5A Br1A 119.4(3) . . ?
C6A C5A Br1A 119.9(3) . . ?
C6B C5B C4B 120.4(4) . . ?
C6B C5B Br1B 119.3(3) . . ?
C4B C5B Br1B 120.4(3) . . ?
C4C C5C C6C 120.2(4) . . ?
C4C C5C Br1C 120.6(3) . . ?
C6C C5C Br1C 119.2(3) . . ?
C4D C5D C6D 120.0(4) . . ?
C4D C5D Br1D 121.4(3) . . ?
C6D C5D Br1D 118.5(3) . . ?
N1A C6A C5A 121.1(4) . . ?
N1A C6A H6A 119.5 . . ?
C5A C6A H6A 119.5 . . ?
N1B C6B C5B 122.3(4) . . ?
N1B C6B H6B 118.8 . . ?
C5B C6B H6B 118.8 . . ?
N1C C6C C5C 121.7(4) . . ?
N1C C6C H6C 119.2 . . ?
C5C C6C H6C 119.2 . . ?
N1D C6D C5D 122.3(4) . . ?
N1D C6D H6D 118.9 . . ?
C5D C6D H6D 118.9 . . ?
O2A C31A O1A 125.6(4) . . ?
O2A C31A C3A 117.9(4) . . ?
O1A C31A C3A 116.4(3) . . ?
O1B C31B O2B 121.8(3) . . ?
O1B C31B C3B 118.8(4) . . ?
O2B C31B C3B 119.4(3) . . ?
O1B C31B Tb1 59.5(2) . . ?
O2B C31B Tb1 62.33(19) . . ?
C3B C31B Tb1 177.9(3) . . ?
O1C C31C O2C 120.8(4) . . ?
O1C C31C C3C 121.4(3) . . ?
O2C C31C C3C 117.8(3) . . ?
O1C C31C Tb2 63.5(2) . . ?
O2C C31C Tb2 57.45(19) . . ?
C3C C31C Tb2 173.6(3) . . ?
O2D C31D O1D 125.4(4) . . ?
O2D C31D C3D 121.9(4) . . ?
O1D C31D C3D 112.7(3) . . ?
C2A N1A C6A 118.7(3) . . ?
C2B N1B C6B 117.9(4) . . ?
C6C N1C C2C 118.7(4) . . ?
C6D N1D C2D 118.4(4) . . ?
Tb1 O1W H11W 124.4 . . ?
Tb1 O1W H12W 126.1 . . ?
H11W O1W H12W 105.0 . . ?
Tb2 O2W H21W 124.7 . . ?
Tb2 O2W H22W 125.3 . . ?
H21W O2W H22W 104.6 . . ?
Tb2 O3W H31W 124.2 . . ?
Tb2 O3W H32W 122.2 . . ?
H31W O3W H32W 104.8 . . ?
C31A O1A Tb1 139.3(2) . . ?
C31B O1B Tb1 94.3(2) . . ?
C31C O1C Tb2 90.2(2) . . ?
C31D O1D H1D 111.2 . . ?
C31B O2B Tb1 91.0(2) . . ?
C31C O2C Tb2 95.5(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H11W O2C 0.85 1.89 2.717(4) 164.1 .
O1W H12W N1B 0.85 1.89 2.720(4) 166.1 3_566
O2W H21W N1C 0.85 1.87 2.682(4) 159.3 4_566
O2W H22W O2A 0.85 1.89 2.735(4) 178.0 2
O3W H31W O2B 0.85 1.94 2.771(4) 166.4 2
O3W H32W N1D 0.85 1.87 2.717(5) 173.7 .

_refine_diff_density_max         1.342
_refine_diff_density_min         -1.216
_refine_diff_density_rms         0.182

_shelxl_version_number           2014-3


_exptl_crystal_preparation       Luminescent
