# Electronic Supplementary Material (ESI) for Dalton Transactions.
# 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_mo_i06ub99_0m_ba_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1555187'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C96 H90 Cl6 Dy Mn6 N6 Na2 O20, 3(C H4 O), 4.75(H2 O)'
_chemical_formula_sum            'C96 H103 Cl6 Gd Mn6 N6 Na2 O25'
_chemical_formula_weight         2486.41

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'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   19.6406(6)
_cell_length_b                   19.6406(6)
_cell_length_c                   28.4472(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9503.4(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5334
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      26.08

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_F_000             3777
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.046
_exptl_absorpt_coefficient_mu    1.289
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6905
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 The value of sine(theta_max)/wavelength is 0.5621, because
crystals were poorly diffracting at high angles. This poor 
diffraction is likely related to the crystal size. Other attempts of 
crystallization were done, but no single crystals of better quality were obtained.

;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30639
_diffrn_reflns_av_R_equivalents  0.0923
_diffrn_reflns_av_sigmaI/netI    0.0915
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.148
_diffrn_reflns_theta_max         23.548
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.817
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.817
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_point_group_measured_fraction_full 0.764
_reflns_number_total             5874
_reflns_number_gt                5342
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.871
_reflns_Friedel_fraction_max     0.868
_reflns_Friedel_fraction_full    0.711

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0486P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
  At the end of refinement, large voids remained in 
 the structure containing only diffuse electron 
 density that could not be modelled satisfactorily. 
 These voids were thus analyzed and taken into account 
 by PLATON/SQUEEZE, occupying a total of 772 Å3 (main voids 
 volumes are 257 Å3 ), resulting in a significant improvement 
 both in R1 and wR2 factors. 
 The derived figures (electro/volumes) would reasonably 
 account for a number of diffuse small solvent molecules, 
 e.g water or methanol
;
_refine_ls_abs_structure_Flack   0.024(18)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         5874
_refine_ls_number_parameters     399
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0924
_refine_ls_wR_factor_gt          0.0904
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.300 249 18 ' '
2 0.333 0.667 0.967 247 18 ' '
3 0.667 0.333 0.633 250 18 ' '
_platon_squeeze_details          ?

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.3333 0.6667 0.49408(3) 0.01602(19) Uani 1 3 d S T P . .
Mn1 Mn 0.24558(8) 0.56402(7) 0.60742(4) 0.0129(3) Uani 1 1 d . . . . .
Mn2 Mn 0.33299(8) 0.56837(7) 0.39287(4) 0.0129(3) Uani 1 1 d . . . . .
Na1 Na 0.3333 0.6667 0.2901(2) 0.0169(13) Uani 1 3 d S T P . .
Na2 Na 0.3333 0.6667 0.7089(2) 0.0208(14) Uani 1 3 d S T P . .
O1 O 0.2408(3) 0.5657(3) 0.54075(19) 0.0135(13) Uani 1 1 d . . . . .
O2 O 0.2411(3) 0.5499(4) 0.6737(2) 0.0159(14) Uani 1 1 d . . . . .
O3 O 0.2951(4) 0.5559(4) 0.7576(2) 0.0243(16) Uani 1 1 d . . . . .
O4 O 0.3324(3) 0.5615(3) 0.4597(2) 0.0142(13) Uani 1 1 d . . . . .
O5 O 0.3399(3) 0.5644(3) 0.3262(2) 0.0171(15) Uani 1 1 d . . . . .
O6 O 0.4031(4) 0.6217(4) 0.2437(2) 0.0287(17) Uani 1 1 d . . . . .
O7 O 0.3333 0.6667 0.6101(3) 0.015(2) Uani 1 3 d S T P . .
O8 O 0.3333 0.6667 0.3994(4) 0.022(3) Uani 1 3 d S T P . .
N1 N 0.1549(4) 0.4553(4) 0.5989(2) 0.0153(16) Uani 1 1 d . . . . .
N2 N 0.3196(4) 0.4610(4) 0.3966(2) 0.0129(15) Uani 1 1 d . . . . .
C1 C 0.1635(5) 0.5145(5) 0.5241(3) 0.016(2) Uani 1 1 d . . . . .
H1A H 0.1647 0.5065 0.4898 0.019 Uiso 1 1 calc R U . . .
H1B H 0.1299 0.5379 0.5300 0.019 Uiso 1 1 calc R U . . .
C2 C 0.1298(5) 0.4353(5) 0.5498(3) 0.0230(19) Uani 1 1 d . U . . .
H2 H 0.1569 0.4078 0.5368 0.028 Uiso 1 1 calc R U . . .
C3 C 0.0434(7) 0.3836(7) 0.5404(4) 0.0535(14) Uani 1 1 d . U . . .
C4 C 0.0140(7) 0.3257(7) 0.5084(5) 0.0535(14) Uani 1 1 d . . . . .
H4 H 0.0511 0.3159 0.4928 0.064 Uiso 1 1 calc R U . . .
C5 C -0.0605(8) 0.2804(8) 0.4960(5) 0.0535(14) Uani 1 1 d . . . . .
H5 H -0.0752 0.2425 0.4716 0.064 Uiso 1 1 calc R U . . .
C6 C -0.1108(8) 0.2895(8) 0.5179(5) 0.0535(14) Uani 1 1 d . U . . .
H6 H -0.1648 0.2544 0.5115 0.064 Uiso 1 1 calc R U . . .
C7 C -0.0930(7) 0.3437(7) 0.5482(4) 0.0535(14) Uani 1 1 d . U . . .
H7 H -0.1338 0.3502 0.5613 0.064 Uiso 1 1 calc R U . . .
C8 C -0.0090(7) 0.3980(7) 0.5641(4) 0.0535(14) Uani 1 1 d . U . . .
H8A H 0.0047 0.4533 0.5589 0.064 Uiso 1 1 calc R U . . .
H8B H -0.0049 0.3908 0.5983 0.064 Uiso 1 1 calc R U . . .
C9 C 0.1271(5) 0.4036(5) 0.6315(3) 0.0175(19) Uani 1 1 d . . . . .
H9 H 0.0854 0.3532 0.6227 0.021 Uiso 1 1 calc R U . . .
C10 C 0.1511(5) 0.4125(5) 0.6793(3) 0.017(2) Uani 1 1 d . . . . .
C11 C 0.1163(6) 0.3445(5) 0.7083(3) 0.028(2) Uani 1 1 d . . . . .
H11 H 0.0758 0.2958 0.6963 0.033 Uiso 1 1 calc R U . . .
C12 C 0.1422(6) 0.3498(6) 0.7550(4) 0.032(3) Uani 1 1 d . . . . .
H12 H 0.1191 0.3046 0.7747 0.039 Uiso 1 1 calc R U . . .
C13 C 0.1976(6) 0.4164(5) 0.7712(3) 0.023(2) Uani 1 1 d . . . . .
H13 H 0.2150 0.4192 0.8027 0.028 Uiso 1 1 calc R U . . .
C14 C 0.2316(6) 0.4829(6) 0.7440(3) 0.020(2) Uani 1 1 d . . . . .
C15 C 0.2085(5) 0.4833(5) 0.6978(3) 0.016(2) Uani 1 1 d . . . . .
C16 C 0.3308(7) 0.5547(7) 0.8028(4) 0.046(3) Uani 1 1 d . . . . .
H16A H 0.3304 0.5049 0.8060 0.069 Uiso 1 1 calc R U . . .
H16B H 0.3007 0.5601 0.8285 0.069 Uiso 1 1 calc R U . . .
H16C H 0.3852 0.5984 0.8039 0.069 Uiso 1 1 calc R U . . .
C17 C 0.3293(6) 0.4917(5) 0.4781(3) 0.020(2) Uani 1 1 d . . . . .
H17A H 0.3034 0.4783 0.5092 0.023 Uiso 1 1 calc R U . . .
H17B H 0.3831 0.4999 0.4816 0.023 Uiso 1 1 calc R U . . .
C18 C 0.2825(5) 0.4261(5) 0.4431(3) 0.020(2) Uani 1 1 d . . . . .
H18 H 0.2280 0.4178 0.4425 0.024 Uiso 1 1 calc R U . . .
C19 C 0.2751(6) 0.3450(6) 0.4536(3) 0.029(2) Uani 1 1 d . . . . .
C20 C 0.3292(6) 0.3368(6) 0.4807(4) 0.035(3) Uani 1 1 d . . . . .
H20 H 0.3746 0.3812 0.4931 0.042 Uiso 1 1 calc R U . . .
C21 C 0.3144(7) 0.2620(7) 0.4890(4) 0.047(3) Uani 1 1 d . U . . .
H21 H 0.3507 0.2543 0.5071 0.057 Uiso 1 1 calc R U . . .
C22 C 0.2529(9) 0.2023(8) 0.4730(5) 0.061(4) Uani 1 1 d . U . . .
H22 H 0.2466 0.1521 0.4796 0.073 Uiso 1 1 calc R U . . .
C23 C 0.1975(8) 0.2040(7) 0.4481(5) 0.058(4) Uani 1 1 d . . . . .
H23 H 0.1522 0.1570 0.4381 0.069 Uiso 1 1 calc R U . . .
C24 C 0.2080(7) 0.2766(6) 0.4371(4) 0.042(3) Uani 1 1 d . . . . .
H24 H 0.1701 0.2809 0.4185 0.051 Uiso 1 1 calc R U . . .
C25 C 0.3405(5) 0.4290(5) 0.3665(3) 0.019(2) Uani 1 1 d . . . . .
H25 H 0.3346 0.3792 0.3742 0.023 Uiso 1 1 calc R U . . .
C26 C 0.3727(5) 0.4610(5) 0.3213(3) 0.019(2) Uani 1 1 d . . . . .
C27 C 0.4025(5) 0.4227(5) 0.2932(3) 0.023(2) Uani 1 1 d . . . . .
H27 H 0.4021 0.3772 0.3050 0.027 Uiso 1 1 calc R U . . .
C28 C 0.4323(5) 0.4501(5) 0.2489(3) 0.017(2) Uani 1 1 d . . . . .
H28 H 0.4533 0.4243 0.2308 0.021 Uiso 1 1 calc R U . . .
C29 C 0.4316(6) 0.5146(6) 0.2312(3) 0.025(2) Uani 1 1 d . . . . .
H29 H 0.4502 0.5323 0.2003 0.031 Uiso 1 1 calc R U . . .
C30 C 0.4037(5) 0.5542(6) 0.2585(3) 0.020(2) Uani 1 1 d . . . . .
C31 C 0.3712(5) 0.5276(5) 0.3034(3) 0.0111(18) Uani 1 1 d . . . . .
C32 C 0.4407(8) 0.6563(8) 0.1987(4) 0.050(3) Uani 1 1 d . . . . .
H32A H 0.4149 0.6176 0.1735 0.075 Uiso 1 1 calc R U . . .
H32B H 0.4964 0.6716 0.2000 0.075 Uiso 1 1 calc R U . . .
H32C H 0.4359 0.7028 0.1923 0.075 Uiso 1 1 calc R U . . .
Cl1 Cl 0.35851(13) 0.52587(13) 0.60726(7) 0.0180(5) Uani 1 1 d . . . . .
Cl2 Cl 0.48594(13) 0.66793(12) 0.39190(7) 0.0176(5) Uani 1 1 d . . . . .
O1W O 0.0049(14) 0.1846(14) 0.4124(8) 0.111(8) Uiso 0.5 1 d . . P . .
O2W O 0.1574(11) 0.3990(11) 0.2844(7) 0.077(6) Uiso 0.5 1 d . . P . .
O3W O 0.0000 0.0000 0.4159(9) 0.043(6) Uiso 0.5 3 d S . P . .
O4W O 0.4525(8) 0.5142(8) 0.7133(5) 0.038(4) Uiso 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O4 2.277(6) 3_565 ?
Gd1 O4 2.277(6) 2_665 ?
Gd1 O4 2.277(6) . ?
Gd1 O1 2.322(6) . ?
Gd1 O1 2.322(6) 3_565 ?
Gd1 O1 2.322(6) 2_665 ?
Gd1 O8 2.694(11) . ?
Gd1 Mn2 3.4646(14) 3_565 ?
Gd1 Mn2 3.4645(14) . ?
Gd1 Mn2 3.4646(14) 2_665 ?
Mn1 O7 1.8884(14) . ?
Mn1 O1 1.900(6) . ?
Mn1 O2 1.902(6) . ?
Mn1 N1 1.997(7) . ?
Mn1 Cl1 2.648(3) 3_565 ?
Mn1 Cl1 2.673(3) . ?
Mn1 Na2 3.449(5) . ?
Mn2 O4 1.906(6) . ?
Mn2 O5 1.907(6) . ?
Mn2 O8 1.9360(16) . ?
Mn2 N2 1.994(6) . ?
Mn2 Cl2 2.602(3) 3_565 ?
Mn2 Cl2 2.641(3) . ?
Mn2 Na1 3.502(5) . ?
Na1 O5 2.317(6) 3_565 ?
Na1 O5 2.317(6) 2_665 ?
Na1 O5 2.317(6) . ?
Na1 O6 2.369(7) . ?
Na1 O6 2.369(7) 3_565 ?
Na1 O6 2.369(7) 2_665 ?
Na1 Mn2 3.501(5) 3_565 ?
Na1 Mn2 3.502(5) 2_665 ?
Na2 O2 2.322(7) . ?
Na2 O2 2.322(7) 3_565 ?
Na2 O2 2.322(7) 2_665 ?
Na2 O3 2.363(7) 3_565 ?
Na2 O3 2.363(7) 2_665 ?
Na2 O3 2.363(7) . ?
Na2 O7 2.810(12) . ?
Na2 Mn1 3.449(5) 3_565 ?
Na2 Mn1 3.449(5) 2_665 ?
O1 C1 1.418(10) . ?
O2 C15 1.323(10) . ?
O3 C14 1.406(12) . ?
O3 C16 1.469(13) . ?
O4 C17 1.440(10) . ?
O5 C31 1.328(10) . ?
O6 C30 1.395(11) . ?
O6 C32 1.466(13) . ?
O7 Mn1 1.8883(13) 3_565 ?
O7 Mn1 1.8885(13) 2_665 ?
O8 Mn2 1.9360(16) 3_565 ?
O8 Mn2 1.9360(16) 2_665 ?
N1 C9 1.278(10) . ?
N1 C2 1.469(10) . ?
N2 C25 1.246(10) . ?
N2 C18 1.501(10) . ?
C1 C2 1.536(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.503(15) . ?
C2 H2 1.0000 . ?
C3 C4 1.341(17) . ?
C3 C8 1.375(17) . ?
C4 C5 1.325(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.253(18) . ?
C5 H5 0.9500 . ?
C6 C7 1.276(17) . ?
C6 H6 0.9500 . ?
C7 C8 1.518(16) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.421(12) . ?
C9 H9 0.9500 . ?
C10 C15 1.384(13) . ?
C10 C11 1.422(12) . ?
C11 C12 1.408(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.299(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.370(13) . ?
C13 H13 0.9500 . ?
C14 C15 1.391(12) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.520(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.554(12) . ?
C18 H18 1.0000 . ?
C19 C20 1.386(14) . ?
C19 C24 1.411(14) . ?
C20 C21 1.368(15) . ?
C20 H20 0.9500 . ?
C21 C22 1.276(18) . ?
C21 H21 0.9500 . ?
C22 C23 1.312(18) . ?
C22 H22 0.9500 . ?
C23 C24 1.372(16) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.433(12) . ?
C25 H25 0.9500 . ?
C26 C27 1.410(12) . ?
C26 C31 1.417(12) . ?
C27 C28 1.380(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.370(13) . ?
C28 H28 0.9500 . ?
C29 C30 1.392(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.406(12) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Cl1 Mn1 2.648(3) 2_665 ?
Cl2 Mn2 2.602(3) 2_665 ?

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
O4 Gd1 O4 102.93(18) 3_565 2_665 ?
O4 Gd1 O4 102.93(18) 3_565 . ?
O4 Gd1 O4 102.93(18) 2_665 . ?
O4 Gd1 O1 85.9(2) 3_565 . ?
O4 Gd1 O1 169.7(2) 2_665 . ?
O4 Gd1 O1 79.8(2) . . ?
O4 Gd1 O1 79.8(2) 3_565 3_565 ?
O4 Gd1 O1 85.9(2) 2_665 3_565 ?
O4 Gd1 O1 169.7(2) . 3_565 ?
O1 Gd1 O1 90.6(2) . 3_565 ?
O4 Gd1 O1 169.7(2) 3_565 2_665 ?
O4 Gd1 O1 79.8(2) 2_665 2_665 ?
O4 Gd1 O1 85.9(2) . 2_665 ?
O1 Gd1 O1 90.6(2) . 2_665 ?
O1 Gd1 O1 90.6(2) 3_565 2_665 ?
O4 Gd1 O8 64.59(15) 3_565 . ?
O4 Gd1 O8 64.59(15) 2_665 . ?
O4 Gd1 O8 64.59(15) . . ?
O1 Gd1 O8 124.87(14) . . ?
O1 Gd1 O8 124.87(14) 3_565 . ?
O1 Gd1 O8 124.87(14) 2_665 . ?
O4 Gd1 Mn2 30.79(15) 3_565 3_565 ?
O4 Gd1 Mn2 84.07(15) 2_665 3_565 ?
O4 Gd1 Mn2 83.83(15) . 3_565 ?
O1 Gd1 Mn2 106.17(14) . 3_565 ?
O1 Gd1 Mn2 102.52(14) 3_565 3_565 ?
O1 Gd1 Mn2 158.45(15) 2_665 3_565 ?
O8 Gd1 Mn2 33.80(2) . 3_565 ?
O4 Gd1 Mn2 84.07(15) 3_565 . ?
O4 Gd1 Mn2 83.83(15) 2_665 . ?
O4 Gd1 Mn2 30.79(15) . . ?
O1 Gd1 Mn2 102.52(14) . . ?
O1 Gd1 Mn2 158.45(15) 3_565 . ?
O1 Gd1 Mn2 106.17(14) 2_665 . ?
O8 Gd1 Mn2 33.80(2) . . ?
Mn2 Gd1 Mn2 57.60(4) 3_565 . ?
O4 Gd1 Mn2 83.83(15) 3_565 2_665 ?
O4 Gd1 Mn2 30.79(15) 2_665 2_665 ?
O4 Gd1 Mn2 84.07(15) . 2_665 ?
O1 Gd1 Mn2 158.45(15) . 2_665 ?
O1 Gd1 Mn2 106.17(14) 3_565 2_665 ?
O1 Gd1 Mn2 102.52(14) 2_665 2_665 ?
O8 Gd1 Mn2 33.80(2) . 2_665 ?
Mn2 Gd1 Mn2 57.60(4) 3_565 2_665 ?
Mn2 Gd1 Mn2 57.60(4) . 2_665 ?
O7 Mn1 O1 92.8(4) . . ?
O7 Mn1 O2 93.8(4) . . ?
O1 Mn1 O2 173.3(3) . . ?
O7 Mn1 N1 175.2(4) . . ?
O1 Mn1 N1 82.7(3) . . ?
O2 Mn1 N1 90.7(3) . . ?
O7 Mn1 Cl1 82.46(6) . 3_565 ?
O1 Mn1 Cl1 86.57(19) . 3_565 ?
O2 Mn1 Cl1 95.03(19) . 3_565 ?
N1 Mn1 Cl1 98.7(2) . 3_565 ?
O7 Mn1 Cl1 81.78(6) . . ?
O1 Mn1 Cl1 93.36(19) . . ?
O2 Mn1 Cl1 86.86(19) . . ?
N1 Mn1 Cl1 97.0(2) . . ?
Cl1 Mn1 Cl1 164.21(8) 3_565 . ?
O7 Mn1 Na2 54.5(3) . . ?
O1 Mn1 Na2 147.13(19) . . ?
O2 Mn1 Na2 39.52(19) . . ?
N1 Mn1 Na2 130.1(2) . . ?
Cl1 Mn1 Na2 85.96(6) 3_565 . ?
Cl1 Mn1 Na2 85.59(6) . . ?
O4 Mn2 O5 171.1(3) . . ?
O4 Mn2 O8 88.4(4) . . ?
O5 Mn2 O8 99.9(4) . . ?
O4 Mn2 N2 83.0(3) . . ?
O5 Mn2 N2 89.0(3) . . ?
O8 Mn2 N2 169.4(3) . . ?
O4 Mn2 Cl2 90.92(18) . 3_565 ?
O5 Mn2 Cl2 93.62(19) . 3_565 ?
O8 Mn2 Cl2 81.07(7) . 3_565 ?
N2 Mn2 Cl2 92.7(2) . 3_565 ?
O4 Mn2 Cl2 91.57(18) . . ?
O5 Mn2 Cl2 86.66(19) . . ?
O8 Mn2 Cl2 80.05(6) . . ?
N2 Mn2 Cl2 106.4(2) . . ?
Cl2 Mn2 Cl2 160.88(8) 3_565 . ?
O4 Mn2 Gd1 37.71(17) . . ?
O5 Mn2 Gd1 150.42(18) . . ?
O8 Mn2 Gd1 50.7(3) . . ?
N2 Mn2 Gd1 120.53(19) . . ?
Cl2 Mn2 Gd1 85.50(6) 3_565 . ?
Cl2 Mn2 Gd1 84.92(6) . . ?
O4 Mn2 Na1 150.51(19) . . ?
O5 Mn2 Na1 37.95(18) . . ?
O8 Mn2 Na1 62.1(3) . . ?
N2 Mn2 Na1 126.2(2) . . ?
Cl2 Mn2 Na1 84.54(6) 3_565 . ?
Cl2 Mn2 Na1 83.98(6) . . ?
Gd1 Mn2 Na1 112.81(6) . . ?
O5 Na1 O5 101.9(2) 3_565 2_665 ?
O5 Na1 O5 101.9(2) 3_565 . ?
O5 Na1 O5 101.9(2) 2_665 . ?
O5 Na1 O6 156.4(2) 3_565 . ?
O5 Na1 O6 101.2(2) 2_665 . ?
O5 Na1 O6 68.2(2) . . ?
O5 Na1 O6 68.2(2) 3_565 3_565 ?
O5 Na1 O6 156.4(2) 2_665 3_565 ?
O5 Na1 O6 101.2(2) . 3_565 ?
O6 Na1 O6 92.0(3) . 3_565 ?
O5 Na1 O6 101.2(2) 3_565 2_665 ?
O5 Na1 O6 68.2(2) 2_665 2_665 ?
O5 Na1 O6 156.4(2) . 2_665 ?
O6 Na1 O6 92.0(3) . 2_665 ?
O6 Na1 O6 92.0(3) 3_565 2_665 ?
O5 Na1 Mn2 30.40(16) 3_565 3_565 ?
O5 Na1 Mn2 81.5(2) 2_665 3_565 ?
O5 Na1 Mn2 84.3(2) . 3_565 ?
O6 Na1 Mn2 152.4(2) . 3_565 ?
O6 Na1 Mn2 95.81(17) 3_565 3_565 ?
O6 Na1 Mn2 114.01(19) 2_665 3_565 ?
O5 Na1 Mn2 84.3(2) 3_565 2_665 ?
O5 Na1 Mn2 30.40(16) 2_665 2_665 ?
O5 Na1 Mn2 81.5(2) . 2_665 ?
O6 Na1 Mn2 114.00(19) . 2_665 ?
O6 Na1 Mn2 152.5(2) 3_565 2_665 ?
O6 Na1 Mn2 95.81(17) 2_665 2_665 ?
Mn2 Na1 Mn2 56.93(9) 3_565 2_665 ?
O5 Na1 Mn2 81.5(2) 3_565 . ?
O5 Na1 Mn2 84.3(2) 2_665 . ?
O5 Na1 Mn2 30.40(16) . . ?
O6 Na1 Mn2 95.81(17) . . ?
O6 Na1 Mn2 114.01(19) 3_565 . ?
O6 Na1 Mn2 152.5(2) 2_665 . ?
Mn2 Na1 Mn2 56.93(9) 3_565 . ?
Mn2 Na1 Mn2 56.93(9) 2_665 . ?
O2 Na2 O2 102.8(2) . 3_565 ?
O2 Na2 O2 102.8(2) . 2_665 ?
O2 Na2 O2 102.8(2) 3_565 2_665 ?
O2 Na2 O3 105.7(2) . 3_565 ?
O2 Na2 O3 67.1(2) 3_565 3_565 ?
O2 Na2 O3 151.3(2) 2_665 3_565 ?
O2 Na2 O3 151.3(2) . 2_665 ?
O2 Na2 O3 105.7(2) 3_565 2_665 ?
O2 Na2 O3 67.1(2) 2_665 2_665 ?
O3 Na2 O3 89.1(3) 3_565 2_665 ?
O2 Na2 O3 67.1(2) . . ?
O2 Na2 O3 151.3(2) 3_565 . ?
O2 Na2 O3 105.7(2) 2_665 . ?
O3 Na2 O3 89.1(3) 3_565 . ?
O3 Na2 O3 89.1(3) 2_665 . ?
O2 Na2 O7 64.5(2) . . ?
O2 Na2 O7 64.5(2) 3_565 . ?
O2 Na2 O7 64.5(2) 2_665 . ?
O3 Na2 O7 125.9(2) 3_565 . ?
O3 Na2 O7 125.9(2) 2_665 . ?
O3 Na2 O7 125.9(2) . . ?
O2 Na2 Mn1 85.0(2) . 3_565 ?
O2 Na2 Mn1 31.41(17) 3_565 3_565 ?
O2 Na2 Mn1 81.8(2) 2_665 3_565 ?
O3 Na2 Mn1 96.70(17) 3_565 3_565 ?
O3 Na2 Mn1 118.15(18) 2_665 3_565 ?
O3 Na2 Mn1 152.1(2) . 3_565 ?
O7 Na2 Mn1 33.17(6) . 3_565 ?
O2 Na2 Mn1 81.8(2) . 2_665 ?
O2 Na2 Mn1 85.0(2) 3_565 2_665 ?
O2 Na2 Mn1 31.40(17) 2_665 2_665 ?
O3 Na2 Mn1 152.1(2) 3_565 2_665 ?
O3 Na2 Mn1 96.70(17) 2_665 2_665 ?
O3 Na2 Mn1 118.15(18) . 2_665 ?
O7 Na2 Mn1 33.17(6) . 2_665 ?
Mn1 Na2 Mn1 56.56(10) 3_565 2_665 ?
O2 Na2 Mn1 31.41(17) . . ?
O2 Na2 Mn1 81.8(2) 3_565 . ?
O2 Na2 Mn1 85.0(2) 2_665 . ?
O3 Na2 Mn1 118.15(18) 3_565 . ?
O3 Na2 Mn1 152.1(2) 2_665 . ?
O3 Na2 Mn1 96.70(17) . . ?
O7 Na2 Mn1 33.17(6) . . ?
Mn1 Na2 Mn1 56.56(10) 3_565 . ?
Mn1 Na2 Mn1 56.56(10) 2_665 . ?
C1 O1 Mn1 111.4(5) . . ?
C1 O1 Gd1 121.2(5) . . ?
Mn1 O1 Gd1 124.1(3) . . ?
C15 O2 Mn1 128.5(6) . . ?
C15 O2 Na2 120.3(5) . . ?
Mn1 O2 Na2 109.1(3) . . ?
C14 O3 C16 114.3(7) . . ?
C14 O3 Na2 119.3(5) . . ?
C16 O3 Na2 126.4(6) . . ?
C17 O4 Mn2 115.2(5) . . ?
C17 O4 Gd1 133.3(5) . . ?
Mn2 O4 Gd1 111.5(3) . . ?
C31 O5 Mn2 124.8(5) . . ?
C31 O5 Na1 119.8(5) . . ?
Mn2 O5 Na1 111.6(3) . . ?
C30 O6 C32 117.5(8) . . ?
C30 O6 Na1 117.9(5) . . ?
C32 O6 Na1 124.4(7) . . ?
Mn1 O7 Mn1 119.84(4) 3_565 . ?
Mn1 O7 Mn1 119.84(4) 3_565 2_665 ?
Mn1 O7 Mn1 119.83(4) . 2_665 ?
Mn1 O7 Na2 92.3(3) 3_565 . ?
Mn1 O7 Na2 92.3(3) . . ?
Mn1 O7 Na2 92.3(3) 2_665 . ?
Mn2 O8 Mn2 119.10(11) 3_565 2_665 ?
Mn2 O8 Mn2 119.10(11) 3_565 . ?
Mn2 O8 Mn2 119.10(11) 2_665 . ?
Mn2 O8 Gd1 95.5(3) 3_565 . ?
Mn2 O8 Gd1 95.5(3) 2_665 . ?
Mn2 O8 Gd1 95.5(3) . . ?
C9 N1 C2 121.7(7) . . ?
C9 N1 Mn1 124.1(6) . . ?
C2 N1 Mn1 113.6(5) . . ?
C25 N2 C18 125.6(7) . . ?
C25 N2 Mn2 126.5(6) . . ?
C18 N2 Mn2 107.8(5) . . ?
O1 C1 C2 109.0(7) . . ?
O1 C1 H1A 109.9 . . ?
C2 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
C2 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N1 C2 C3 117.7(8) . . ?
N1 C2 C1 105.4(7) . . ?
C3 C2 C1 111.7(8) . . ?
N1 C2 H2 107.2 . . ?
C3 C2 H2 107.2 . . ?
C1 C2 H2 107.2 . . ?
C4 C3 C8 117.4(12) . . ?
C4 C3 C2 123.8(12) . . ?
C8 C3 C2 118.8(11) . . ?
C5 C4 C3 127.7(15) . . ?
C5 C4 H4 116.1 . . ?
C3 C4 H4 116.1 . . ?
C6 C5 C4 117.2(15) . . ?
C6 C5 H5 121.4 . . ?
C4 C5 H5 121.4 . . ?
C5 C6 C7 123.3(14) . . ?
C5 C6 H6 118.4 . . ?
C7 C6 H6 118.4 . . ?
C6 C7 C8 122.4(13) . . ?
C6 C7 H7 118.8 . . ?
C8 C7 H7 118.8 . . ?
C3 C8 C7 111.8(11) . . ?
C3 C8 H8A 109.3 . . ?
C7 C8 H8A 109.3 . . ?
C3 C8 H8B 109.3 . . ?
C7 C8 H8B 109.3 . . ?
H8A C8 H8B 107.9 . . ?
N1 C9 C10 127.8(8) . . ?
N1 C9 H9 116.1 . . ?
C10 C9 H9 116.1 . . ?
C15 C10 C11 119.4(8) . . ?
C15 C10 C9 122.8(8) . . ?
C11 C10 C9 117.8(8) . . ?
C12 C11 C10 119.5(9) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C13 C12 C11 120.0(10) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 121.5(10) . . ?
C12 C13 H13 119.3 . . ?
C14 C13 H13 119.3 . . ?
C13 C14 C15 122.4(9) . . ?
C13 C14 O3 125.2(8) . . ?
C15 C14 O3 112.3(8) . . ?
O2 C15 C10 122.9(8) . . ?
O2 C15 C14 119.8(8) . . ?
C10 C15 C14 117.2(8) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C18 106.8(7) . . ?
O4 C17 H17A 110.4 . . ?
C18 C17 H17A 110.4 . . ?
O4 C17 H17B 110.4 . . ?
C18 C17 H17B 110.4 . . ?
H17A C17 H17B 108.6 . . ?
N2 C18 C17 103.9(7) . . ?
N2 C18 C19 114.3(7) . . ?
C17 C18 C19 116.7(7) . . ?
N2 C18 H18 107.1 . . ?
C17 C18 H18 107.1 . . ?
C19 C18 H18 107.1 . . ?
C20 C19 C24 118.7(9) . . ?
C20 C19 C18 122.8(9) . . ?
C24 C19 C18 118.4(9) . . ?
C21 C20 C19 117.2(11) . . ?
C21 C20 H20 121.4 . . ?
C19 C20 H20 121.4 . . ?
C22 C21 C20 121.3(13) . . ?
C22 C21 H21 119.3 . . ?
C20 C21 H21 119.3 . . ?
C21 C22 C23 125.9(13) . . ?
C21 C22 H22 117.0 . . ?
C23 C22 H22 117.0 . . ?
C22 C23 C24 116.9(12) . . ?
C22 C23 H23 121.5 . . ?
C24 C23 H23 121.5 . . ?
C23 C24 C19 119.9(11) . . ?
C23 C24 H24 120.1 . . ?
C19 C24 H24 120.1 . . ?
N2 C25 C26 125.4(8) . . ?
N2 C25 H25 117.3 . . ?
C26 C25 H25 117.3 . . ?
C27 C26 C31 119.6(8) . . ?
C27 C26 C25 119.0(8) . . ?
C31 C26 C25 121.3(8) . . ?
C28 C27 C26 121.2(8) . . ?
C28 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
C29 C28 C27 119.9(8) . . ?
C29 C28 H28 120.1 . . ?
C27 C28 H28 120.1 . . ?
C28 C29 C30 120.1(9) . . ?
C28 C29 H29 120.0 . . ?
C30 C29 H29 120.0 . . ?
C29 C30 O6 123.8(8) . . ?
C29 C30 C31 122.0(9) . . ?
O6 C30 C31 114.2(8) . . ?
O5 C31 C30 119.2(8) . . ?
O5 C31 C26 123.7(7) . . ?
C30 C31 C26 117.1(8) . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Mn1 Cl1 Mn1 75.79(8) 2_665 . ?
Mn2 Cl2 Mn2 79.08(8) 2_665 . ?

_refine_diff_density_max         0.923
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.086



_exptl_crystal_recrystallization_method 
'Methanol/Acetonitrile layered with diethylether'
_exptl_crystal_preparation       ', Magnetic properties,chirality'
####################################################################### 
# 
# 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_mo_i06ub84_0m_a_sq_da
_database_code_depnum_ccdc_archive 'CCDC 1983655'
loop_
_audit_author_name
_audit_author_address
'Merce Font-Bardia'
;Departament de Mineralogia Cristallografia i Diposits Minerals Universitat de Barcelona
Spain
;
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C96 H90 Cl6 Mn6 N6 Na2 O20 Tb, 3(C H4 O), 4(H2 O)'
_chemical_formula_sum            'C99 H110 Cl6 Mn6 N6 Na2 O27 Tb'
_chemical_formula_weight         2563.16

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'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.4240(8)
_cell_length_b                   19.4240(8)
_cell_length_c                   28.5924(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9342.4(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3081
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      25.49

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_F_000             3903
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    1.349
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6659
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4258
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.524
_diffrn_reflns_theta_max         26.383
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4258
_reflns_number_gt                2698
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Data were apparently pre-merged, so _diffrn_reflns_number
 etc. will have to be added later.
 
 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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0673P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4258
_refine_ls_number_parameters     192
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0465
_refine_ls_wR_factor_ref         0.1269
_refine_ls_wR_factor_gt          0.1229
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.947
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 206 13 ' '
2 0.333 0.667 0.667 207 13 ' '
3 0.667 0.333 0.333 207 13 ' '
_platon_squeeze_details          ?

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 0.6667 0.3333 0.3333 0.03243(19) Uani 1 6 d S TU P . .
Na1 Na 0.6667 0.3333 0.53974(9) 0.0244(7) Uani 1 3 d S T P . .
Mn1 Mn 0.76949(4) 0.42604(4) 0.43895(2) 0.02132(18) Uani 1 1 d . . . . .
Cl1 Cl 0.68717(7) 0.49821(7) 0.43930(4) 0.0305(3) Uani 1 1 d . . . . .
N1 N 0.8768(2) 0.5210(2) 0.43183(13) 0.0412(11) Uani 1 1 d . . . . .
O1 O 0.77103(16) 0.43200(16) 0.37263(10) 0.0232(6) Uani 1 1 d . U . . .
O2 O 0.78182(16) 0.42860(17) 0.50467(10) 0.0244(7) Uani 1 1 d . . . . .
O3 O 0.78008(18) 0.37521(19) 0.58694(12) 0.0416(9) Uani 1 1 d . U . . .
O4 O 0.6667 0.3333 0.43788(16) 0.0180(10) Uani 1 3 d S T P . .
C1 C 0.8242(3) 0.5095(3) 0.35570(17) 0.0390(12) Uani 1 1 d . . . . .
H1A H 0.7999 0.5423 0.3589 0.047 Uiso 1 1 calc R U . . .
H1B H 0.8343 0.5065 0.3227 0.047 Uiso 1 1 calc R U . . .
C2 C 0.8987(3) 0.5458(4) 0.38081(18) 0.0577(16) Uani 1 1 d . U . . .
H2 H 0.9298 0.5222 0.3694 0.069 Uiso 1 1 calc R U . . .
C3 C 0.9477(4) 0.6348(5) 0.3736(3) 0.0807(11) Uani 1 1 d . U . . .
C4 C 1.0095(4) 0.6620(4) 0.3449(2) 0.0807(11) Uani 1 1 d . . . . .
H4 H 1.0210 0.6263 0.3301 0.097 Uiso 1 1 calc R U . . .
C5 C 1.0578(4) 0.7438(4) 0.3367(2) 0.0807(11) Uani 1 1 d . . . . .
H5 H 1.1009 0.7622 0.3165 0.097 Uiso 1 1 calc R U . . .
C6 C 1.0410(4) 0.7963(5) 0.3586(2) 0.0807(11) Uani 1 1 d . . . . .
H6 H 1.0735 0.8506 0.3536 0.097 Uiso 1 1 calc R U . . .
C7 C 0.9817(4) 0.7720(4) 0.3858(2) 0.0807(11) Uani 1 1 d . . . . .
H7 H 0.9703 0.8082 0.4001 0.097 Uiso 1 1 calc R U . . .
C8 C 0.9318(4) 0.6877(4) 0.3944(2) 0.0807(11) Uani 1 1 d . . . . .
H8 H 0.8884 0.6699 0.4144 0.097 Uiso 1 1 calc R U . . .
C9 C 0.9299(3) 0.5545(3) 0.46384(18) 0.0470(15) Uani 1 1 d . . . . .
H9 H 0.9779 0.5987 0.4553 0.056 Uiso 1 1 calc R U . . .
C10 C 0.9208(3) 0.5293(3) 0.51122(15) 0.0289(11) Uani 1 1 d . . . . .
C11 C 0.9868(3) 0.5693(3) 0.54020(16) 0.0361(12) Uani 1 1 d . . . . .
H11 H 1.0327 0.6128 0.5287 0.043 Uiso 1 1 calc R U . . .
C12 C 0.9850(3) 0.5452(3) 0.58575(17) 0.0433(14) Uani 1 1 d . . . . .
H12 H 1.0296 0.5716 0.6048 0.052 Uiso 1 1 calc R U . . .
C13 C 0.9167(3) 0.4820(3) 0.60249(16) 0.0394(13) Uani 1 1 d . . . . .
H13 H 0.9153 0.4663 0.6334 0.047 Uiso 1 1 calc R U . . .
C14 C 0.8497(3) 0.4406(3) 0.57507(14) 0.0252(9) Uani 1 1 d . U . . .
C15 C 0.8494(3) 0.4655(3) 0.52879(15) 0.0265(10) Uani 1 1 d . . . . .
C16 C 0.7833(3) 0.3393(3) 0.63319(16) 0.0515(16) Uani 1 1 d . . . . .
H16A H 0.7317 0.2950 0.6403 0.077 Uiso 1 1 calc R U . . .
H16B H 0.7990 0.3786 0.6574 0.077 Uiso 1 1 calc R U . . .
H16C H 0.8212 0.3214 0.6313 0.077 Uiso 1 1 calc R U . . .
O4W O 1.1271(12) 0.6640(12) 0.2236(7) 0.082 Uiso 0.25 1 d . U P . .
O3W O 0.8495(10) 0.3323(10) 0.7406(5) 0.056 Uiso 0.25 1 d . U P . .
O2W O 0.6667 0.3333 0.7489(5) 0.070 Uiso 0.4999 3 d S U P . .
O1W O 0.8259(6) 0.2158(6) 0.5485(3) 0.080 Uiso 0.5 1 d . U P . .
H1WO H 0.8226 0.1918 0.5243 0.096 Uiso 0.5 1 calc R U P . .
C1W C 0.8696(6) 0.2914(6) 0.5415(3) 0.041 Uiso 0.5 1 d . U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O1 2.271(3) 18_545 ?
Tb1 O1 2.271(3) . ?
Tb1 O1 2.271(3) 3_665 ?
Tb1 O1 2.271(3) 2_655 ?
Tb1 O1 2.272(3) 16_655 ?
Tb1 O1 2.272(3) 17 ?
Tb1 Mn1 3.5713(6) . ?
Tb1 Mn1 3.5713(6) 3_665 ?
Tb1 Mn1 3.5713(6) 2_655 ?
Tb1 Mn1 3.5713(6) 18_545 ?
Tb1 Mn1 3.5714(6) 16_655 ?
Tb1 Mn1 3.5714(6) 17 ?
Na1 O2 2.301(3) 2_655 ?
Na1 O2 2.301(3) . ?
Na1 O2 2.301(3) 3_665 ?
Na1 O3 2.354(3) 3_665 ?
Na1 O3 2.354(3) 2_655 ?
Na1 O3 2.355(3) . ?
Na1 O4 2.912(5) . ?
Na1 Mn1 3.455(2) 3_665 ?
Na1 Mn1 3.455(2) 2_655 ?
Na1 Mn1 3.455(2) . ?
Mn1 O2 1.892(3) . ?
Mn1 O1 1.899(3) . ?
Mn1 O4 1.9068(6) . ?
Mn1 N1 1.986(4) . ?
Mn1 Cl1 2.6007(13) . ?
Mn1 Cl1 2.6949(13) 3_665 ?
Cl1 Mn1 2.6948(13) 2_655 ?
N1 C9 1.286(6) . ?
N1 C2 1.529(6) . ?
O1 C1 1.418(5) . ?
O2 C15 1.331(5) . ?
O3 C14 1.356(5) . ?
O3 C16 1.511(5) . ?
O4 Mn1 1.9068(6) 3_665 ?
O4 Mn1 1.9068(6) 2_655 ?
C1 C2 1.444(7) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.514(9) . ?
C2 H2 0.9800 . ?
C3 C4 1.327(10) . ?
C3 C8 1.350(11) . ?
C4 C5 1.404(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.369(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.269(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.447(9) . ?
C7 H7 0.9300 . ?
C8 H8 0.9300 . ?
C9 C10 1.421(6) . ?
C9 H9 0.9300 . ?
C10 C11 1.392(6) . ?
C10 C15 1.411(6) . ?
C11 C12 1.378(6) . ?
C11 H11 0.9300 . ?
C12 C13 1.366(7) . ?
C12 H12 0.9300 . ?
C13 C14 1.382(6) . ?
C13 H13 0.9300 . ?
C14 C15 1.410(6) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O4W O3W 1.109(19) 10_766 ?
O3W O4W 1.109(19) 10_766 ?
O1W C1W 1.293(13) . ?
O1W H1WO 0.8200 . ?

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 O1 82.36(9) 18_545 . ?
O1 Tb1 O1 180.0 18_545 3_665 ?
O1 Tb1 O1 97.65(9) . 3_665 ?
O1 Tb1 O1 82.36(9) 18_545 2_655 ?
O1 Tb1 O1 97.65(9) . 2_655 ?
O1 Tb1 O1 97.65(9) 3_665 2_655 ?
O1 Tb1 O1 97.65(9) 18_545 16_655 ?
O1 Tb1 O1 180.0 . 16_655 ?
O1 Tb1 O1 82.35(9) 3_665 16_655 ?
O1 Tb1 O1 82.36(9) 2_655 16_655 ?
O1 Tb1 O1 97.64(9) 18_545 17 ?
O1 Tb1 O1 82.35(9) . 17 ?
O1 Tb1 O1 82.35(9) 3_665 17 ?
O1 Tb1 O1 180.00(14) 2_655 17 ?
O1 Tb1 O1 97.64(9) 16_655 17 ?
O1 Tb1 Mn1 101.70(7) 18_545 . ?
O1 Tb1 Mn1 28.14(7) . . ?
O1 Tb1 Mn1 78.30(7) 3_665 . ?
O1 Tb1 Mn1 80.21(7) 2_655 . ?
O1 Tb1 Mn1 151.86(7) 16_655 . ?
O1 Tb1 Mn1 99.79(7) 17 . ?
O1 Tb1 Mn1 151.87(7) 18_545 3_665 ?
O1 Tb1 Mn1 80.21(7) . 3_665 ?
O1 Tb1 Mn1 28.14(7) 3_665 3_665 ?
O1 Tb1 Mn1 78.30(7) 2_655 3_665 ?
O1 Tb1 Mn1 99.79(7) 16_655 3_665 ?
O1 Tb1 Mn1 101.70(7) 17 3_665 ?
Mn1 Tb1 Mn1 55.076(16) . 3_665 ?
O1 Tb1 Mn1 99.79(7) 18_545 2_655 ?
O1 Tb1 Mn1 78.30(7) . 2_655 ?
O1 Tb1 Mn1 80.21(7) 3_665 2_655 ?
O1 Tb1 Mn1 28.14(7) 2_655 2_655 ?
O1 Tb1 Mn1 101.71(7) 16_655 2_655 ?
O1 Tb1 Mn1 151.86(7) 17 2_655 ?
Mn1 Tb1 Mn1 55.076(16) . 2_655 ?
Mn1 Tb1 Mn1 55.075(16) 3_665 2_655 ?
O1 Tb1 Mn1 28.14(7) 18_545 18_545 ?
O1 Tb1 Mn1 99.79(7) . 18_545 ?
O1 Tb1 Mn1 151.86(7) 3_665 18_545 ?
O1 Tb1 Mn1 101.70(7) 2_655 18_545 ?
O1 Tb1 Mn1 80.21(7) 16_655 18_545 ?
O1 Tb1 Mn1 78.30(7) 17 18_545 ?
Mn1 Tb1 Mn1 124.925(16) . 18_545 ?
Mn1 Tb1 Mn1 180.0 3_665 18_545 ?
Mn1 Tb1 Mn1 124.926(16) 2_655 18_545 ?
O1 Tb1 Mn1 78.30(7) 18_545 16_655 ?
O1 Tb1 Mn1 151.86(7) . 16_655 ?
O1 Tb1 Mn1 101.70(7) 3_665 16_655 ?
O1 Tb1 Mn1 99.79(7) 2_655 16_655 ?
O1 Tb1 Mn1 28.14(7) 16_655 16_655 ?
O1 Tb1 Mn1 80.21(7) 17 16_655 ?
Mn1 Tb1 Mn1 180.0 . 16_655 ?
Mn1 Tb1 Mn1 124.924(16) 3_665 16_655 ?
Mn1 Tb1 Mn1 124.926(16) 2_655 16_655 ?
Mn1 Tb1 Mn1 55.075(16) 18_545 16_655 ?
O1 Tb1 Mn1 80.21(7) 18_545 17 ?
O1 Tb1 Mn1 101.70(7) . 17 ?
O1 Tb1 Mn1 99.79(7) 3_665 17 ?
O1 Tb1 Mn1 151.86(7) 2_655 17 ?
O1 Tb1 Mn1 78.29(7) 16_655 17 ?
O1 Tb1 Mn1 28.14(7) 17 17 ?
Mn1 Tb1 Mn1 124.924(16) . 17 ?
Mn1 Tb1 Mn1 124.924(16) 3_665 17 ?
Mn1 Tb1 Mn1 180.0 2_655 17 ?
Mn1 Tb1 Mn1 55.074(16) 18_545 17 ?
Mn1 Tb1 Mn1 55.074(16) 16_655 17 ?
O2 Na1 O2 102.42(11) 2_655 . ?
O2 Na1 O2 102.42(11) 2_655 3_665 ?
O2 Na1 O2 102.42(11) . 3_665 ?
O2 Na1 O3 105.00(11) 2_655 3_665 ?
O2 Na1 O3 152.12(12) . 3_665 ?
O2 Na1 O3 66.83(11) 3_665 3_665 ?
O2 Na1 O3 66.83(10) 2_655 2_655 ?
O2 Na1 O3 105.00(11) . 2_655 ?
O2 Na1 O3 152.12(12) 3_665 2_655 ?
O3 Na1 O3 90.42(14) 3_665 2_655 ?
O2 Na1 O3 152.12(12) 2_655 . ?
O2 Na1 O3 66.83(11) . . ?
O2 Na1 O3 105.00(11) 3_665 . ?
O3 Na1 O3 90.42(14) 3_665 . ?
O3 Na1 O3 90.42(14) 2_655 . ?
O2 Na1 O4 64.16(9) 2_655 . ?
O2 Na1 O4 64.16(9) . . ?
O2 Na1 O4 64.17(9) 3_665 . ?
O3 Na1 O4 124.97(10) 3_665 . ?
O3 Na1 O4 124.97(10) 2_655 . ?
O3 Na1 O4 124.97(10) . . ?
O2 Na1 Mn1 85.15(10) 2_655 3_665 ?
O2 Na1 Mn1 81.54(10) . 3_665 ?
O2 Na1 Mn1 30.83(8) 3_665 3_665 ?
O3 Na1 Mn1 95.79(9) 3_665 3_665 ?
O3 Na1 Mn1 151.95(10) 2_655 3_665 ?
O3 Na1 Mn1 116.79(10) . 3_665 ?
O4 Na1 Mn1 33.49(3) . 3_665 ?
O2 Na1 Mn1 30.82(8) 2_655 2_655 ?
O2 Na1 Mn1 85.15(10) . 2_655 ?
O2 Na1 Mn1 81.54(10) 3_665 2_655 ?
O3 Na1 Mn1 116.79(10) 3_665 2_655 ?
O3 Na1 Mn1 95.79(9) 2_655 2_655 ?
O3 Na1 Mn1 151.95(10) . 2_655 ?
O4 Na1 Mn1 33.49(3) . 2_655 ?
Mn1 Na1 Mn1 57.09(4) 3_665 2_655 ?
O2 Na1 Mn1 81.54(10) 2_655 . ?
O2 Na1 Mn1 30.82(8) . . ?
O2 Na1 Mn1 85.15(10) 3_665 . ?
O3 Na1 Mn1 151.95(10) 3_665 . ?
O3 Na1 Mn1 116.79(10) 2_655 . ?
O3 Na1 Mn1 95.79(9) . . ?
O4 Na1 Mn1 33.49(3) . . ?
Mn1 Na1 Mn1 57.09(4) 3_665 . ?
Mn1 Na1 Mn1 57.09(4) 2_655 . ?
O2 Mn1 O1 172.87(13) . . ?
O2 Mn1 O4 95.72(16) . . ?
O1 Mn1 O4 91.08(16) . . ?
O2 Mn1 N1 90.98(14) . . ?
O1 Mn1 N1 82.17(14) . . ?
O4 Mn1 N1 173.13(17) . . ?
O2 Mn1 Cl1 94.92(9) . . ?
O1 Mn1 Cl1 88.07(9) . . ?
O4 Mn1 Cl1 82.71(3) . . ?
N1 Mn1 Cl1 98.22(14) . . ?
O2 Mn1 Cl1 86.11(9) . 3_665 ?
O1 Mn1 Cl1 92.95(9) . 3_665 ?
O4 Mn1 Cl1 80.16(3) . 3_665 ?
N1 Mn1 Cl1 98.87(14) . 3_665 ?
Cl1 Mn1 Cl1 162.86(4) . 3_665 ?
O2 Mn1 Na1 38.54(9) . . ?
O1 Mn1 Na1 148.42(9) . . ?
O4 Mn1 Na1 57.43(14) . . ?
N1 Mn1 Na1 129.37(11) . . ?
Cl1 Mn1 Na1 85.80(3) . . ?
Cl1 Mn1 Na1 84.41(3) 3_665 . ?
O2 Mn1 Tb1 152.21(9) . . ?
O1 Mn1 Tb1 34.33(8) . . ?
O4 Mn1 Tb1 56.82(14) . . ?
N1 Mn1 Tb1 116.38(11) . . ?
Cl1 Mn1 Tb1 86.31(3) . . ?
Cl1 Mn1 Tb1 84.95(3) 3_665 . ?
Na1 Mn1 Tb1 114.25(3) . . ?
Mn1 Cl1 Mn1 77.14(4) . 2_655 ?
C9 N1 C2 119.5(4) . . ?
C9 N1 Mn1 127.0(3) . . ?
C2 N1 Mn1 112.9(3) . . ?
C1 O1 Mn1 112.7(3) . . ?
C1 O1 Tb1 126.6(3) . . ?
Mn1 O1 Tb1 117.53(13) . . ?
C15 O2 Mn1 127.4(3) . . ?
C15 O2 Na1 120.5(3) . . ?
Mn1 O2 Na1 110.63(14) . . ?
C14 O3 C16 113.6(3) . . ?
C14 O3 Na1 120.2(3) . . ?
C16 O3 Na1 126.1(3) . . ?
Mn1 O4 Mn1 119.975(8) 3_665 2_655 ?
Mn1 O4 Mn1 119.976(8) 3_665 . ?
Mn1 O4 Mn1 119.974(8) 2_655 . ?
Mn1 O4 Na1 89.08(14) 3_665 . ?
Mn1 O4 Na1 89.08(14) 2_655 . ?
Mn1 O4 Na1 89.08(14) . . ?
O1 C1 C2 111.7(4) . . ?
O1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
O1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C1 C2 C3 113.3(5) . . ?
C1 C2 N1 105.5(4) . . ?
C3 C2 N1 114.0(5) . . ?
C1 C2 H2 107.9 . . ?
C3 C2 H2 107.9 . . ?
N1 C2 H2 107.9 . . ?
C4 C3 C8 118.4(8) . . ?
C4 C3 C2 117.7(8) . . ?
C8 C3 C2 123.9(7) . . ?
C3 C4 C5 120.9(9) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
C6 C5 C4 119.6(8) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C7 C6 C5 121.0(8) . . ?
C7 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C6 C7 C8 119.6(9) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C3 C8 C7 120.5(8) . . ?
C3 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
N1 C9 C10 125.0(5) . . ?
N1 C9 H9 117.5 . . ?
C10 C9 H9 117.5 . . ?
C11 C10 C15 120.3(4) . . ?
C11 C10 C9 116.9(4) . . ?
C15 C10 C9 122.7(4) . . ?
C12 C11 C10 120.9(4) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C13 C12 C11 119.0(5) . . ?
C13 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C12 C13 C14 122.2(4) . . ?
C12 C13 H13 118.9 . . ?
C14 C13 H13 118.9 . . ?
O3 C14 C13 127.6(4) . . ?
O3 C14 C15 112.5(4) . . ?
C13 C14 C15 119.8(4) . . ?
O2 C15 C14 118.3(4) . . ?
O2 C15 C10 124.0(4) . . ?
C14 C15 C10 117.7(4) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1W O1W H1WO 109.5 . . ?

_refine_diff_density_max         1.520
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.105



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/ACN/diethylether'
####################################################################### 
# 
# 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_mo_i06ub53_0m_b_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1983654'
loop_
_audit_author_name
_audit_author_address
'Merce Font-Bardia'
;Departament de Mineralogia Cristallografia i Diposits Minerals Universitat de Barcelona
Spain
;
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C96 H90 Cl6 Mn6 N6 Na2 O20 Tb, 7(H2 O)'
_chemical_formula_sum            'C96 H104 Cl6 Mn6 N6 Na2 O27 Tb'
_chemical_formula_weight         2521.09

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'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   19.5854(10)
_cell_length_b                   19.5854(10)
_cell_length_c                   28.5183(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9473.7(11)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9968
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      24.42

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_F_000             3831
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.086
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.078
_exptl_absorpt_coefficient_mu    1.329
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6164
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19397
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         2.506
_diffrn_reflns_theta_max         24.421
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.902
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.902
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_point_group_measured_fraction_full 0.876
_reflns_number_total             6709
_reflns_number_gt                6430
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.941
_reflns_Friedel_fraction_max     0.932
_reflns_Friedel_fraction_full    0.849

_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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
 Upon completion of the refinement, PLATON (spek, 1991) was used 
 to verify the correctness of the structure and a new space group 
 was suggested ( R3) But the molecule was chiral and chiral 
 molecules are incompatible with an inversion centre, 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1402P)²+86.4074P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
 At the end of refinement, large voids remained in 
 the structure containing only diffuse electron 
 density that could not be modelled satisfactorily. 
 These voids were thus analyzed and taken into account 
 by PLATON/SQUEEZE, occupying a total of 1311.7 Å3 (main voids 
 volumes are 437 Å3 ), resulting in a significant improvement 
 both in R1 and wR2 factors. 
 The derived figures (electro/volumes) would reasonably 
 account for a number of diffuse small solvent molecules, 
 e.g water or methanol
;
_refine_ls_abs_structure_Flack   0.06(2)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         6709
_refine_ls_number_parameters     322
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0625
_refine_ls_wR_factor_ref         0.1883
_refine_ls_wR_factor_gt          0.1844
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 0.313 431 74 ' '
2 0.000 0.000 0.646 433 75 ' '
3 0.667 0.333 -0.021 428 75 ' '
_platon_squeeze_details          ?

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 0.6667 0.3333 0.47843(3) 0.0174(3) Uani 1 3 d S T P . .
Mn1 Mn 0.57863(10) 0.34841(10) 0.59110(6) 0.0129(4) Uani 1 1 d . . . . .
Mn2 Mn 0.66689(10) 0.43150(10) 0.37753(6) 0.0126(4) Uani 1 1 d . . . . .
Cl2 Cl 0.82052(16) 0.48414(16) 0.37674(10) 0.0185(6) Uani 1 1 d . . . . .
Na1 Na 0.6667 0.3333 0.6923(3) 0.0168(16) Uani 1 3 d S T P . .
Na2 Na 0.6667 0.3333 0.2751(3) 0.0138(15) Uani 1 3 d S T P . .
O1 O 0.5741(4) 0.3419(5) 0.5254(3) 0.0138(16) Uani 1 1 d . . . . .
O2 O 0.5752(5) 0.3582(5) 0.6562(3) 0.0156(17) Uani 1 1 d . . . . .
O3 O 0.6276(6) 0.4050(5) 0.7422(3) 0.024(2) Uani 1 1 d . . . . .
O4 O 0.6669(4) 0.4377(4) 0.4441(3) 0.0139(16) Uani 1 1 d . . . . .
O5 O 0.6737(5) 0.4429(5) 0.3118(3) 0.0158(17) Uani 1 1 d . . . . .
O6 O 0.7355(5) 0.4481(5) 0.2282(3) 0.024(2) Uani 1 1 d . . . . .
O7 O 0.6667 0.3333 0.5939(5) 0.014(3) Uani 1 3 d S T P . .
O8 O 0.6667 0.3333 0.3824(5) 0.020(3) Uani 1 3 d S T P . .
N1 N 0.4891(5) 0.3678(6) 0.5828(4) 0.016(2) Uani 1 1 d . . . . .
N2 N 0.6533(6) 0.5251(5) 0.3816(3) 0.015(2) Uani 1 1 d . . . . .
C1 C 0.4968(7) 0.3173(7) 0.5079(4) 0.016(2) Uani 1 1 d . . . . .
H1A H 0.4622 0.2601 0.5133 0.019 Uiso 1 1 calc R U . . .
H1B H 0.4992 0.3272 0.4737 0.019 Uiso 1 1 calc R U . . .
C2 C 0.4637(7) 0.3623(7) 0.5325(4) 0.017(2) Uani 1 1 d . . . . .
H2 H 0.4902 0.4169 0.5193 0.021 Uiso 1 1 calc R U . . .
C3 C 0.3767(4) 0.3258(6) 0.5241(4) 0.0488(18) Uani 1 1 d G . . . .
C4 C 0.3502(5) 0.3589(5) 0.4907(4) 0.0488(18) Uani 1 1 d G . . . .
H4 H 0.3868 0.4055 0.4746 0.059 Uiso 1 1 calc R U . . .
C5 C 0.2702(6) 0.3240(6) 0.4809(4) 0.0488(18) Uani 1 1 d G . . . .
H5 H 0.2521 0.3466 0.4581 0.059 Uiso 1 1 calc R U . . .
C6 C 0.2166(4) 0.2558(6) 0.5045(4) 0.0488(18) Uani 1 1 d G . . . .
H6 H 0.1619 0.2319 0.4978 0.059 Uiso 1 1 calc R U . . .
C7 C 0.2431(5) 0.2226(5) 0.5378(4) 0.0488(18) Uani 1 1 d G . . . .
H7 H 0.2065 0.1761 0.5539 0.059 Uiso 1 1 calc R U . . .
C8 C 0.3232(6) 0.2576(6) 0.5476(3) 0.0488(18) Uani 1 1 d G . . . .
H8 H 0.3413 0.2350 0.5704 0.059 Uiso 1 1 calc R U . . .
C9 C 0.4588(7) 0.3904(7) 0.6154(4) 0.019(2) Uani 1 1 d . . . . .
H9 H 0.4171 0.3992 0.6064 0.023 Uiso 1 1 calc R U . . .
C10 C 0.4814(5) 0.4034(5) 0.6632(2) 0.022(3) Uani 1 1 d G . . . .
C11 C 0.4455(4) 0.4349(5) 0.6909(3) 0.027(3) Uani 1 1 d G . . . .
H11 H 0.4043 0.4416 0.6784 0.033 Uiso 1 1 calc R U . . .
C12 C 0.4699(5) 0.4565(5) 0.7370(3) 0.030(3) Uani 1 1 d G . . . .
H12 H 0.4454 0.4780 0.7560 0.037 Uiso 1 1 calc R U . . .
C13 C 0.5302(5) 0.4467(5) 0.7553(2) 0.027(3) Uani 1 1 d G . . . .
H13 H 0.5469 0.4615 0.7868 0.032 Uiso 1 1 calc R U . . .
C14 C 0.5661(4) 0.4152(5) 0.7276(2) 0.017(2) Uani 1 1 d G . . . .
C15 C 0.5417(4) 0.3936(5) 0.6815(2) 0.020(3) Uani 1 1 d G . . . .
C16 C 0.6656(10) 0.4452(10) 0.7851(5) 0.038(2) Uani 1 1 d . . . . .
H16A H 0.7204 0.4568 0.7852 0.057 Uiso 1 1 calc R U . . .
H16B H 0.6377 0.4115 0.8120 0.057 Uiso 1 1 calc R U . . .
H16C H 0.6645 0.4945 0.7874 0.057 Uiso 1 1 calc R U . . .
C17 C 0.6635(8) 0.5055(7) 0.4626(4) 0.021(3) Uani 1 1 d . . . . .
H17A H 0.7174 0.5514 0.4659 0.026 Uiso 1 1 calc R U . . .
H17B H 0.6378 0.4930 0.4938 0.026 Uiso 1 1 calc R U . . .
C18 C 0.6168(7) 0.5239(7) 0.4285(4) 0.018(2) Uani 1 1 d . . . . .
H18 H 0.5621 0.4775 0.4283 0.021 Uiso 1 1 calc R U . . .
C19 C 0.6096(6) 0.5963(5) 0.4390(4) 0.0406(15) Uani 1 1 d G . . . .
C20 C 0.5430(5) 0.5963(5) 0.4223(3) 0.0406(15) Uani 1 1 d G . . . .
H20 H 0.5056 0.5535 0.4038 0.049 Uiso 1 1 calc R U . . .
C21 C 0.5311(5) 0.6590(5) 0.4325(4) 0.0406(15) Uani 1 1 d G . . . .
H21 H 0.4856 0.6591 0.4210 0.049 Uiso 1 1 calc R U . . .
C22 C 0.5859(6) 0.7217(4) 0.4594(4) 0.0406(15) Uani 1 1 d G . . . .
H22 H 0.5778 0.7646 0.4664 0.049 Uiso 1 1 calc R U . . .
C23 C 0.6525(5) 0.7217(5) 0.4762(4) 0.0406(15) Uani 1 1 d G . . . .
H23 H 0.6899 0.7645 0.4947 0.049 Uiso 1 1 calc R U . . .
C24 C 0.6644(5) 0.6589(5) 0.4660(4) 0.0406(15) Uani 1 1 d G . . . .
H24 H 0.7099 0.6589 0.4775 0.049 Uiso 1 1 calc R U . . .
C25 C 0.6752(7) 0.5792(7) 0.3523(4) 0.021(3) Uani 1 1 d . . . . .
H25 H 0.6714 0.6240 0.3608 0.026 Uiso 1 1 calc R U . . .
C26 C 0.7060(5) 0.5789(4) 0.3063(2) 0.020(3) Uani 1 1 d G . . . .
C27 C 0.7347(5) 0.6471(3) 0.2795(3) 0.022(3) Uani 1 1 d G . . . .
H27 H 0.7341 0.6919 0.2918 0.026 Uiso 1 1 calc R U . . .
C28 C 0.7641(5) 0.6497(3) 0.2348(2) 0.022(3) Uani 1 1 d G . . . .
H28 H 0.7837 0.6963 0.2165 0.027 Uiso 1 1 calc R U . . .
C29 C 0.7648(5) 0.5841(4) 0.2168(2) 0.028(3) Uani 1 1 d G . . . .
H29 H 0.7849 0.5859 0.1863 0.033 Uiso 1 1 calc R U . . .
C30 C 0.7362(5) 0.5159(3) 0.2436(2) 0.017(2) Uani 1 1 d G . . . .
C31 C 0.7068(4) 0.5133(3) 0.2883(2) 0.015(2) Uani 1 1 d G . . . .
C32 C 0.7739(10) 0.4525(10) 0.1855(5) 0.038(2) Uani 1 1 d . . . . .
H32A H 0.7540 0.4730 0.1609 0.057 Uiso 1 1 calc R U . . .
H32B H 0.7635 0.3998 0.1767 0.057 Uiso 1 1 calc R U . . .
H32C H 0.8308 0.4877 0.1892 0.057 Uiso 1 1 calc R U . . .
Cl1 Cl 0.69287(17) 0.50040(16) 0.59082(10) 0.0188(6) Uani 1 1 d . . . . .
O1W O 0.1182(19) 0.269(2) 0.3660(10) 0.072(4) Uani 0.5 1 d . . P . .
O2W O 0.501(2) 0.440(2) 0.2677(10) 0.072(4) Uani 0.5 1 d . . P . .
O3W O 0.5485(19) 0.680(2) 0.2447(10) 0.072(4) Uani 0.5 1 d . . P . .
O5W O 0.3333 0.6667 0.4069(6) 0.028(3) Uani 1 3 d S T P . .
O4W O 0.3331(19) 0.499(2) 0.4037(10) 0.072(4) Uani 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O4 2.264(7) 2_655 ?
Tb1 O4 2.264(7) . ?
Tb1 O4 2.264(7) 3_665 ?
Tb1 O1 2.327(8) . ?
Tb1 O1 2.327(8) 2_655 ?
Tb1 O1 2.327(8) 3_665 ?
Tb1 O8 2.738(16) . ?
Tb1 Mn2 3.4594(18) . ?
Tb1 Mn2 3.4594(18) 3_665 ?
Tb1 Mn2 3.4594(18) 2_655 ?
Mn1 O2 1.871(8) . ?
Mn1 O1 1.878(8) . ?
Mn1 O7 1.8908(18) . ?
Mn1 N1 1.985(9) . ?
Mn1 Cl1 2.645(3) 2_655 ?
Mn1 Cl1 2.685(3) . ?
Mn1 Na1 3.449(7) . ?
Mn2 O5 1.886(8) . ?
Mn2 O4 1.903(8) . ?
Mn2 O8 1.926(2) . ?
Mn2 N2 1.982(9) . ?
Mn2 Cl2 2.590(3) 2_655 ?
Mn2 Cl2 2.649(3) . ?
Mn2 Na2 3.495(7) . ?
Cl2 Mn2 2.590(3) 3_665 ?
Na1 O2 2.320(9) 2_655 ?
Na1 O2 2.320(9) 3_665 ?
Na1 O2 2.320(9) . ?
Na1 O3 2.376(10) 3_665 ?
Na1 O3 2.376(10) 2_655 ?
Na1 O3 2.376(10) . ?
Na1 O7 2.806(16) . ?
Na1 Mn1 3.449(7) 3_665 ?
Na1 Mn1 3.449(7) 2_655 ?
Na2 O5 2.329(9) 3_665 ?
Na2 O5 2.329(9) 2_655 ?
Na2 O5 2.329(9) . ?
Na2 O6 2.373(10) . ?
Na2 O6 2.373(10) 3_665 ?
Na2 O6 2.373(10) 2_655 ?
Na2 Mn2 3.495(7) 3_665 ?
Na2 Mn2 3.495(7) 2_655 ?
O1 C1 1.428(14) . ?
O2 C15 1.373(9) . ?
O3 C14 1.381(10) . ?
O3 C16 1.446(17) . ?
O4 C17 1.462(14) . ?
O5 C31 1.369(9) . ?
O6 C30 1.393(10) . ?
O6 C32 1.411(17) . ?
O7 Mn1 1.8908(18) 3_665 ?
O7 Mn1 1.8909(18) 2_655 ?
O8 Mn2 1.926(2) 3_665 ?
O8 Mn2 1.926(2) 2_655 ?
N1 C9 1.296(15) . ?
N1 C2 1.503(14) . ?
N2 C25 1.245(16) . ?
N2 C18 1.513(14) . ?
C1 C2 1.504(16) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.502(13) . ?
C2 H2 1.0000 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 C8 1.3900 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.416(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9500 . ?
C12 C13 1.3900 . ?
C12 H12 0.9500 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.497(17) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.522(12) . ?
C18 H18 1.0000 . ?
C19 C20 1.3900 . ?
C19 C24 1.3900 . ?
C20 C21 1.3900 . ?
C20 H20 0.9500 . ?
C21 C22 1.3900 . ?
C21 H21 0.9500 . ?
C22 C23 1.3900 . ?
C22 H22 0.9500 . ?
C23 C24 1.3900 . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.445(13) . ?
C25 H25 0.9500 . ?
C26 C27 1.3900 . ?
C26 C31 1.3900 . ?
C27 C28 1.3900 . ?
C27 H27 0.9500 . ?
C28 C29 1.3900 . ?
C28 H28 0.9500 . ?
C29 C30 1.3900 . ?
C29 H29 0.9500 . ?
C30 C31 1.3900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
Cl1 Mn1 2.645(3) 3_665 ?

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
O4 Tb1 O4 102.7(3) 2_655 . ?
O4 Tb1 O4 102.7(3) 2_655 3_665 ?
O4 Tb1 O4 102.7(3) . 3_665 ?
O4 Tb1 O1 85.9(3) 2_655 . ?
O4 Tb1 O1 80.4(3) . . ?
O4 Tb1 O1 169.8(3) 3_665 . ?
O4 Tb1 O1 80.4(3) 2_655 2_655 ?
O4 Tb1 O1 169.8(3) . 2_655 ?
O4 Tb1 O1 85.9(3) 3_665 2_655 ?
O1 Tb1 O1 90.2(3) . 2_655 ?
O4 Tb1 O1 169.8(3) 2_655 3_665 ?
O4 Tb1 O1 85.9(3) . 3_665 ?
O4 Tb1 O1 80.4(3) 3_665 3_665 ?
O1 Tb1 O1 90.2(3) . 3_665 ?
O1 Tb1 O1 90.2(3) 2_655 3_665 ?
O4 Tb1 O8 64.4(2) 2_655 . ?
O4 Tb1 O8 64.4(2) . . ?
O4 Tb1 O8 64.4(2) 3_665 . ?
O1 Tb1 O8 125.1(2) . . ?
O1 Tb1 O8 125.1(2) 2_655 . ?
O1 Tb1 O8 125.1(2) 3_665 . ?
O4 Tb1 Mn2 83.7(2) 2_655 . ?
O4 Tb1 Mn2 30.7(2) . . ?
O4 Tb1 Mn2 83.7(2) 3_665 . ?
O1 Tb1 Mn2 102.9(2) . . ?
O1 Tb1 Mn2 158.6(2) 2_655 . ?
O1 Tb1 Mn2 106.35(19) 3_665 . ?
O8 Tb1 Mn2 33.72(3) . . ?
O4 Tb1 Mn2 83.7(2) 2_655 3_665 ?
O4 Tb1 Mn2 83.7(2) . 3_665 ?
O4 Tb1 Mn2 30.7(2) 3_665 3_665 ?
O1 Tb1 Mn2 158.6(2) . 3_665 ?
O1 Tb1 Mn2 106.35(19) 2_655 3_665 ?
O1 Tb1 Mn2 102.9(2) 3_665 3_665 ?
O8 Tb1 Mn2 33.72(3) . 3_665 ?
Mn2 Tb1 Mn2 57.47(5) . 3_665 ?
O4 Tb1 Mn2 30.7(2) 2_655 2_655 ?
O4 Tb1 Mn2 83.7(2) . 2_655 ?
O4 Tb1 Mn2 83.7(2) 3_665 2_655 ?
O1 Tb1 Mn2 106.35(19) . 2_655 ?
O1 Tb1 Mn2 102.9(2) 2_655 2_655 ?
O1 Tb1 Mn2 158.6(2) 3_665 2_655 ?
O8 Tb1 Mn2 33.72(3) . 2_655 ?
Mn2 Tb1 Mn2 57.47(5) . 2_655 ?
Mn2 Tb1 Mn2 57.47(5) 3_665 2_655 ?
O2 Mn1 O1 173.9(3) . . ?
O2 Mn1 O7 93.3(5) . . ?
O1 Mn1 O7 92.7(5) . . ?
O2 Mn1 N1 91.0(4) . . ?
O1 Mn1 N1 82.9(4) . . ?
O7 Mn1 N1 175.2(5) . . ?
O2 Mn1 Cl1 95.2(3) . 2_655 ?
O1 Mn1 Cl1 86.5(3) . 2_655 ?
O7 Mn1 Cl1 82.69(8) . 2_655 ?
N1 Mn1 Cl1 99.0(3) . 2_655 ?
O2 Mn1 Cl1 86.7(3) . . ?
O1 Mn1 Cl1 93.3(3) . . ?
O7 Mn1 Cl1 81.59(8) . . ?
N1 Mn1 Cl1 96.5(3) . . ?
Cl1 Mn1 Cl1 164.25(10) 2_655 . ?
O2 Mn1 Na1 39.1(2) . . ?
O1 Mn1 Na1 147.0(2) . . ?
O7 Mn1 Na1 54.4(4) . . ?
N1 Mn1 Na1 130.0(3) . . ?
Cl1 Mn1 Na1 86.14(8) 2_655 . ?
Cl1 Mn1 Na1 85.54(8) . . ?
O5 Mn2 O4 170.9(3) . . ?
O5 Mn2 O8 99.0(5) . . ?
O4 Mn2 O8 89.5(5) . . ?
O5 Mn2 N2 89.0(4) . . ?
O4 Mn2 N2 83.1(3) . . ?
O8 Mn2 N2 169.9(5) . . ?
O5 Mn2 Cl2 93.7(3) . 2_655 ?
O4 Mn2 Cl2 91.0(2) . 2_655 ?
O8 Mn2 Cl2 81.42(8) . 2_655 ?
N2 Mn2 Cl2 91.9(3) . 2_655 ?
O5 Mn2 Cl2 86.9(3) . . ?
O4 Mn2 Cl2 91.2(2) . . ?
O8 Mn2 Cl2 79.88(8) . . ?
N2 Mn2 Cl2 107.0(3) . . ?
Cl2 Mn2 Cl2 161.15(10) 2_655 . ?
O5 Mn2 Tb1 150.9(2) . . ?
O4 Mn2 Tb1 37.4(2) . . ?
O8 Mn2 Tb1 52.1(5) . . ?
N2 Mn2 Tb1 120.1(3) . . ?
Cl2 Mn2 Tb1 85.64(8) 2_655 . ?
Cl2 Mn2 Tb1 84.78(8) . . ?
O5 Mn2 Na2 38.3(3) . . ?
O4 Mn2 Na2 150.3(2) . . ?
O8 Mn2 Na2 60.8(5) . . ?
N2 Mn2 Na2 126.4(3) . . ?
Cl2 Mn2 Na2 84.85(8) 2_655 . ?
Cl2 Mn2 Na2 84.01(7) . . ?
Tb1 Mn2 Na2 112.95(8) . . ?
Mn2 Cl2 Mn2 78.82(10) 3_665 . ?
O2 Na1 O2 101.8(3) 2_655 3_665 ?
O2 Na1 O2 101.8(3) 2_655 . ?
O2 Na1 O2 101.8(3) 3_665 . ?
O2 Na1 O3 106.9(3) 2_655 3_665 ?
O2 Na1 O3 68.3(3) 3_665 3_665 ?
O2 Na1 O3 150.9(3) . 3_665 ?
O2 Na1 O3 68.3(3) 2_655 2_655 ?
O2 Na1 O3 150.9(3) 3_665 2_655 ?
O2 Na1 O3 106.9(3) . 2_655 ?
O3 Na1 O3 87.9(4) 3_665 2_655 ?
O2 Na1 O3 150.9(3) 2_655 . ?
O2 Na1 O3 106.9(3) 3_665 . ?
O2 Na1 O3 68.3(3) . . ?
O3 Na1 O3 87.9(4) 3_665 . ?
O3 Na1 O3 87.9(4) 2_655 . ?
O2 Na1 O7 63.7(3) 2_655 . ?
O2 Na1 O7 63.7(3) 3_665 . ?
O2 Na1 O7 63.7(3) . . ?
O3 Na1 O7 126.8(3) 3_665 . ?
O3 Na1 O7 126.8(3) 2_655 . ?
O3 Na1 O7 126.8(3) . . ?
O2 Na1 Mn1 81.1(3) 2_655 . ?
O2 Na1 Mn1 84.4(3) 3_665 . ?
O2 Na1 Mn1 30.6(2) . . ?
O3 Na1 Mn1 152.6(3) 3_665 . ?
O3 Na1 Mn1 119.1(2) 2_655 . ?
O3 Na1 Mn1 97.4(2) . . ?
O7 Na1 Mn1 33.21(8) . . ?
O2 Na1 Mn1 84.4(3) 2_655 3_665 ?
O2 Na1 Mn1 30.6(2) 3_665 3_665 ?
O2 Na1 Mn1 81.1(3) . 3_665 ?
O3 Na1 Mn1 97.4(2) 3_665 3_665 ?
O3 Na1 Mn1 152.6(3) 2_655 3_665 ?
O3 Na1 Mn1 119.1(2) . 3_665 ?
O7 Na1 Mn1 33.21(8) . 3_665 ?
Mn1 Na1 Mn1 56.64(13) . 3_665 ?
O2 Na1 Mn1 30.6(2) 2_655 2_655 ?
O2 Na1 Mn1 81.1(3) 3_665 2_655 ?
O2 Na1 Mn1 84.4(3) . 2_655 ?
O3 Na1 Mn1 119.1(2) 3_665 2_655 ?
O3 Na1 Mn1 97.4(2) 2_655 2_655 ?
O3 Na1 Mn1 152.6(3) . 2_655 ?
O7 Na1 Mn1 33.21(8) . 2_655 ?
Mn1 Na1 Mn1 56.64(13) . 2_655 ?
Mn1 Na1 Mn1 56.63(13) 3_665 2_655 ?
O5 Na2 O5 101.4(3) 3_665 2_655 ?
O5 Na2 O5 101.4(3) 3_665 . ?
O5 Na2 O5 101.4(3) 2_655 . ?
O5 Na2 O6 102.1(3) 3_665 . ?
O5 Na2 O6 155.9(3) 2_655 . ?
O5 Na2 O6 68.7(3) . . ?
O5 Na2 O6 68.7(3) 3_665 3_665 ?
O5 Na2 O6 102.1(3) 2_655 3_665 ?
O5 Na2 O6 155.9(3) . 3_665 ?
O6 Na2 O6 91.3(4) . 3_665 ?
O5 Na2 O6 155.9(3) 3_665 2_655 ?
O5 Na2 O6 68.7(3) 2_655 2_655 ?
O5 Na2 O6 102.1(3) . 2_655 ?
O6 Na2 O6 91.3(4) . 2_655 ?
O6 Na2 O6 91.3(4) 3_665 2_655 ?
O5 Na2 Mn2 83.9(3) 3_665 . ?
O5 Na2 Mn2 81.2(3) 2_655 . ?
O5 Na2 Mn2 30.1(2) . . ?
O6 Na2 Mn2 96.1(2) . . ?
O6 Na2 Mn2 152.5(3) 3_665 . ?
O6 Na2 Mn2 114.8(2) 2_655 . ?
O5 Na2 Mn2 30.1(2) 3_665 3_665 ?
O5 Na2 Mn2 83.9(3) 2_655 3_665 ?
O5 Na2 Mn2 81.2(3) . 3_665 ?
O6 Na2 Mn2 114.8(2) . 3_665 ?
O6 Na2 Mn2 96.1(2) 3_665 3_665 ?
O6 Na2 Mn2 152.5(3) 2_655 3_665 ?
Mn2 Na2 Mn2 56.82(12) . 3_665 ?
O5 Na2 Mn2 81.2(3) 3_665 2_655 ?
O5 Na2 Mn2 30.1(2) 2_655 2_655 ?
O5 Na2 Mn2 83.9(3) . 2_655 ?
O6 Na2 Mn2 152.5(3) . 2_655 ?
O6 Na2 Mn2 114.8(2) 3_665 2_655 ?
O6 Na2 Mn2 96.1(2) 2_655 2_655 ?
Mn2 Na2 Mn2 56.82(12) . 2_655 ?
Mn2 Na2 Mn2 56.82(12) 3_665 2_655 ?
C1 O1 Mn1 112.2(7) . . ?
C1 O1 Tb1 120.5(6) . . ?
Mn1 O1 Tb1 124.5(4) . . ?
C15 O2 Mn1 128.7(6) . . ?
C15 O2 Na1 119.1(6) . . ?
Mn1 O2 Na1 110.3(4) . . ?
C14 O3 C16 115.1(9) . . ?
C14 O3 Na1 117.9(6) . . ?
C16 O3 Na1 126.8(8) . . ?
C17 O4 Mn2 114.8(7) . . ?
C17 O4 Tb1 133.2(7) . . ?
Mn2 O4 Tb1 112.0(4) . . ?
C31 O5 Mn2 125.1(6) . . ?
C31 O5 Na2 119.3(6) . . ?
Mn2 O5 Na2 111.6(4) . . ?
C30 O6 C32 117.6(9) . . ?
C30 O6 Na2 117.0(6) . . ?
C32 O6 Na2 125.3(8) . . ?
Mn1 O7 Mn1 119.83(7) 3_665 . ?
Mn1 O7 Mn1 119.82(7) 3_665 2_655 ?
Mn1 O7 Mn1 119.82(7) . 2_655 ?
Mn1 O7 Na1 92.4(4) 3_665 . ?
Mn1 O7 Na1 92.4(4) . . ?
Mn1 O7 Na1 92.4(4) 2_655 . ?
Mn2 O8 Mn2 119.48(12) . 3_665 ?
Mn2 O8 Mn2 119.48(12) . 2_655 ?
Mn2 O8 Mn2 119.48(12) 3_665 2_655 ?
Mn2 O8 Tb1 94.2(5) . . ?
Mn2 O8 Tb1 94.2(5) 3_665 . ?
Mn2 O8 Tb1 94.2(5) 2_655 . ?
C9 N1 C2 121.2(9) . . ?
C9 N1 Mn1 125.4(8) . . ?
C2 N1 Mn1 113.1(7) . . ?
C25 N2 C18 124.4(10) . . ?
C25 N2 Mn2 126.9(8) . . ?
C18 N2 Mn2 108.6(7) . . ?
O1 C1 C2 109.5(9) . . ?
O1 C1 H1A 109.8 . . ?
C2 C1 H1A 109.8 . . ?
O1 C1 H1B 109.8 . . ?
C2 C1 H1B 109.8 . . ?
H1A C1 H1B 108.2 . . ?
C3 C2 N1 116.3(9) . . ?
C3 C2 C1 111.4(9) . . ?
N1 C2 C1 105.3(9) . . ?
C3 C2 H2 107.9 . . ?
N1 C2 H2 107.9 . . ?
C1 C2 H2 107.9 . . ?
C4 C3 C8 120.0 . . ?
C4 C3 C2 119.1(8) . . ?
C8 C3 C2 120.8(8) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C7 C6 C5 120.0 . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C6 C7 C8 120.0 . . ?
C6 C7 H7 120.0 . . ?
C8 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 H8 120.0 . . ?
C3 C8 H8 120.0 . . ?
N1 C9 C10 126.7(10) . . ?
N1 C9 H9 116.7 . . ?
C10 C9 H9 116.7 . . ?
C11 C10 C15 120.0 . . ?
C11 C10 C9 116.5(7) . . ?
C15 C10 C9 123.2(7) . . ?
C10 C11 C12 120.0 . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C13 C12 C11 120.0 . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
O3 C14 C13 124.4(6) . . ?
O3 C14 C15 115.6(6) . . ?
C13 C14 C15 120.0 . . ?
O2 C15 C14 118.2(6) . . ?
O2 C15 C10 121.7(6) . . ?
C14 C15 C10 120.0 . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C18 107.2(9) . . ?
O4 C17 H17A 110.3 . . ?
C18 C17 H17A 110.3 . . ?
O4 C17 H17B 110.3 . . ?
C18 C17 H17B 110.3 . . ?
H17A C17 H17B 108.5 . . ?
C17 C18 N2 103.7(9) . . ?
C17 C18 C19 116.6(10) . . ?
N2 C18 C19 115.1(9) . . ?
C17 C18 H18 107.0 . . ?
N2 C18 H18 107.0 . . ?
C19 C18 H18 107.0 . . ?
C20 C19 C24 120.0 . . ?
C20 C19 C18 117.1(7) . . ?
C24 C19 C18 122.8(7) . . ?
C21 C20 C19 120.0 . . ?
C21 C20 H20 120.0 . . ?
C19 C20 H20 120.0 . . ?
C22 C21 C20 120.0 . . ?
C22 C21 H21 120.0 . . ?
C20 C21 H21 120.0 . . ?
C23 C22 C21 120.0 . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C19 120.0 . . ?
C23 C24 H24 120.0 . . ?
C19 C24 H24 120.0 . . ?
N2 C25 C26 124.9(10) . . ?
N2 C25 H25 117.6 . . ?
C26 C25 H25 117.6 . . ?
C27 C26 C31 120.0 . . ?
C27 C26 C25 117.6(6) . . ?
C31 C26 C25 122.4(6) . . ?
C26 C27 C28 120.0 . . ?
C26 C27 H27 120.0 . . ?
C28 C27 H27 120.0 . . ?
C29 C28 C27 120.0 . . ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 120.0 . . ?
C29 C30 O6 123.3(6) . . ?
C31 C30 O6 116.7(6) . . ?
O5 C31 C30 117.7(6) . . ?
O5 C31 C26 122.1(6) . . ?
C30 C31 C26 120.0 . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
Mn1 Cl1 Mn1 75.75(10) 3_665 . ?

_refine_diff_density_max         2.469
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.197



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/ACN/diethylether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_mo_i06ub117_01_aa_sq_s
_database_code_depnum_ccdc_archive 'CCDC 1983657'
loop_
_audit_author_name
_audit_author_address
'Merce Font-Bardia'
;Departament de Mineralogia Cristallografia i Diposits Minerals Universitat de Barcelona
Spain
;
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C96 H93 Br6 Mn6 N6 Na2 O20 Tb, Br, 3(O) [+ solvent]'
_chemical_formula_sum            'C96 H99 Br7 Mn6 N6 Na2 O23 Tb'
_chemical_formula_weight         2798.72

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'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   19.9312(3)
_cell_length_b                   19.9312(3)
_cell_length_c                   28.8052(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9909.9(4)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6102
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_F_000             4149
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    3.263
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14655
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.464
_diffrn_reflns_theta_max         25.023
_diffrn_reflns_theta_full        25.023
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             7725
_reflns_number_gt                6888
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.983
_reflns_Friedel_fraction_max     0.982
_reflns_Friedel_fraction_full    0.982

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_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)+(0.0413P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2981 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(8)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         7725
_refine_ls_number_parameters     435
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0363
_refine_ls_wR_factor_ref         0.0895
_refine_ls_wR_factor_gt          0.0869
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_restrained_S_all      1.008
_refine_ls_shift/su_max          0.024
_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 0.666667 0.333333 0.52900(2) 0.01598(17) Uani 1 3 d S T P . .
Na1 Na 0.666667 0.333333 0.74126(19) 0.0175(12) Uani 1 3 d S T P . .
N1 N 0.6258(4) 0.5026(4) 0.6328(2) 0.0144(14) Uani 1 1 d . . . . .
O1 O 0.6547(3) 0.4214(3) 0.57594(18) 0.0105(11) Uani 1 1 d . . . . .
C1 C 0.6776(5) 0.4975(5) 0.5578(3) 0.024(2) Uani 1 1 d . . . . .
H1A H 0.667926 0.494788 0.523987 0.028 Uiso 1 1 calc R U . . .
H1B H 0.733488 0.533233 0.563416 0.028 Uiso 1 1 calc R U . . .
Mn1 Mn 0.64837(7) 0.41770(7) 0.64109(4) 0.0121(3) Uani 1 1 d . U . . .
Br1 Br 0.80931(5) 0.50946(5) 0.64288(3) 0.0219(2) Uani 1 1 d . U . . .
Na2 Na 0.666667 0.333333 0.3263(2) 0.0231(13) Uani 1 3 d S T P . .
N2 N 0.8656(4) 0.5239(4) 0.4329(2) 0.0131(14) Uani 1 1 d . . . . .
O2 O 0.6381(3) 0.4209(3) 0.70644(19) 0.0165(12) Uani 1 1 d . . . . .
C2 C 0.6298(5) 0.5261(5) 0.5828(3) 0.0168(17) Uani 1 1 d . . . . .
H2 H 0.576146 0.497827 0.569743 0.020 Uiso 1 1 calc R U . . .
Br2 Br 0.82593(6) 0.33757(6) 0.42566(3) 0.0326(2) Uani 1 1 d . U . . .
Mn2 Mn 0.76260(6) 0.43049(6) 0.42738(4) 0.0116(3) Uani 1 1 d . U . . .
O6 O 0.7127(4) 0.4462(4) 0.2798(2) 0.0365(17) Uani 1 1 d . . . . .
C6 C 0.7277(9) 0.7679(8) 0.5511(5) 0.065(4) Uani 1 1 d . U . . .
H6 H 0.749995 0.820869 0.542610 0.078 Uiso 1 1 calc R U . . .
C5 C 0.6588(9) 0.7138(8) 0.5301(4) 0.053(3) Uani 1 1 d . . . . .
H5 H 0.633043 0.730069 0.509052 0.063 Uiso 1 1 calc R U . . .
O5 O 0.7671(3) 0.4412(3) 0.3627(2) 0.0175(13) Uani 1 1 d . . . . .
C4 C 0.6276(6) 0.6345(6) 0.5403(3) 0.033(2) Uani 1 1 d . . . . .
H4 H 0.582898 0.596393 0.524477 0.040 Uiso 1 1 calc R U . . .
O4 O 0.7677(3) 0.4348(3) 0.49359(19) 0.0135(12) Uani 1 1 d . . . . .
C3 C 0.6631(6) 0.6130(5) 0.5738(3) 0.027(2) Uani 1 1 d . . . . .
O3 O 0.5941(4) 0.3709(4) 0.7898(2) 0.0298(15) Uani 1 1 d . . . . .
C7 C 0.7658(7) 0.7468(7) 0.5846(4) 0.049(3) Uani 1 1 d . U . . .
H7 H 0.812986 0.784127 0.598653 0.059 Uiso 1 1 calc R U . . .
O7 O 0.666667 0.333333 0.6446(3) 0.010(2) Uani 1 3 d S T P . .
C8 C 0.7301(6) 0.6679(6) 0.5961(4) 0.036(2) Uani 1 1 d . . . . .
H8 H 0.752247 0.651639 0.619586 0.044 Uiso 1 1 calc R U . . .
O8 O 0.666667 0.333333 0.4319(4) 0.018(2) Uani 1 3 d S T P . .
C9 C 0.6066(5) 0.5349(5) 0.6651(3) 0.0175(18) Uani 1 1 d . . . . .
H9 H 0.601924 0.578311 0.656308 0.021 Uiso 1 1 calc R U . . .
C10 C 0.5916(5) 0.5118(5) 0.7124(3) 0.0213(19) Uani 1 1 d . . . . .
C11 C 0.5597(5) 0.5466(6) 0.7394(3) 0.030(2) Uani 1 1 d . . . . .
H11 H 0.548492 0.584085 0.727035 0.036 Uiso 1 1 calc R U . . .
Br3 Br 0.666667 0.333333 0.07330(10) 0.0772(7) Uani 1 3 d S T P . .
C12 C 0.5444(6) 0.5224(6) 0.7876(4) 0.040(3) Uani 1 1 d . . . . .
H12 H 0.526688 0.547677 0.808020 0.048 Uiso 1 1 calc R U . . .
C16 C 0.5593(9) 0.3366(8) 0.8355(4) 0.062(4) Uani 1 1 d . . . . .
H16A H 0.504899 0.323324 0.835918 0.092 Uiso 1 1 calc R U . . .
H16B H 0.587582 0.374175 0.860176 0.092 Uiso 1 1 calc R U . . .
H16C H 0.562608 0.289706 0.840632 0.092 Uiso 1 1 calc R U . . .
C15 C 0.6049(5) 0.4531(5) 0.7298(3) 0.0181(18) Uani 1 1 d . . . . .
C14 C 0.5827(5) 0.4294(5) 0.7761(3) 0.022(2) Uani 1 1 d . . . . .
C13 C 0.5545(6) 0.4659(6) 0.8037(3) 0.031(2) Uani 1 1 d . . . . .
H13 H 0.542019 0.450274 0.835138 0.037 Uiso 1 1 calc R U . . .
C17 C 0.8325(5) 0.5017(5) 0.5114(3) 0.0164(18) Uani 1 1 d . . . . .
H17A H 0.845396 0.491118 0.542736 0.020 Uiso 1 1 calc R U . . .
H17B H 0.820953 0.544446 0.513828 0.020 Uiso 1 1 calc R U . . .
C18 C 0.8998(5) 0.5243(5) 0.4790(3) 0.023(2) Uani 1 1 d . . . . .
H18 H 0.910317 0.480239 0.478778 0.028 Uiso 1 1 calc R U . . .
C19 C 0.9766(5) 0.5972(5) 0.4903(3) 0.029(2) Uani 1 1 d . . . . .
C20 C 0.9799(6) 0.6544(6) 0.5162(4) 0.043(3) Uani 1 1 d . . . . .
H20 H 0.933187 0.652052 0.525857 0.051 Uiso 1 1 calc R U . . .
O1W O 0.5674(11) 0.2903(13) 0.9306(7) 0.086(7) Uani 0.5 1 d . . P . .
C21 C 1.0517(8) 0.7183(7) 0.5295(5) 0.062(3) Uani 1 1 d . U . . .
H21 H 1.052779 0.756256 0.549932 0.074 Uiso 1 1 calc R U . . .
C22 C 1.1153(10) 0.7256(9) 0.5144(6) 0.072(4) Uani 1 1 d . U . . .
H22 H 1.162483 0.770924 0.522438 0.086 Uiso 1 1 calc R U . . .
C23 C 1.1182(8) 0.6750(10) 0.4891(6) 0.082(5) Uani 1 1 d . U . . .
H23 H 1.167335 0.682519 0.480093 0.099 Uiso 1 1 calc R U . . .
C24 C 1.0449(6) 0.6019(7) 0.4727(4) 0.052(3) Uani 1 1 d . U . . .
H24A H 1.043135 0.601792 0.438332 0.062 Uiso 1 1 calc R U . . .
H24B H 1.047325 0.555677 0.482687 0.062 Uiso 1 1 calc R U . . .
C25 C 0.9009(5) 0.5787(5) 0.4021(3) 0.0218(19) Uani 1 1 d . . . . .
H25 H 0.949588 0.622221 0.409902 0.026 Uiso 1 1 calc R U . . .
C26 C 0.8687(5) 0.5760(5) 0.3561(3) 0.0211(19) Uani 1 1 d . . . . .
C27 C 0.9070(5) 0.6421(5) 0.3280(3) 0.029(2) Uani 1 1 d . . . . .
H27 H 0.950557 0.686962 0.340299 0.035 Uiso 1 1 calc R U . . .
C28 C 0.8842(6) 0.6441(6) 0.2842(3) 0.028(2) Uani 1 1 d . . . . .
H28 H 0.912499 0.689153 0.265643 0.033 Uiso 1 1 calc R U . . .
C29 C 0.8204(6) 0.5810(6) 0.2667(3) 0.030(2) Uani 1 1 d . . . . .
H29 H 0.803348 0.582760 0.236126 0.037 Uiso 1 1 calc R U . . .
C30 C 0.7789(5) 0.5125(5) 0.2936(3) 0.0218(19) Uani 1 1 d . . . . .
O2W O 0.9400(14) 0.4386(16) 0.3155(7) 0.108(9) Uani 0.5 1 d . . P . .
C31 C 0.8041(5) 0.5086(5) 0.3383(3) 0.0181(18) Uani 1 1 d . . . . .
C32 C 0.6894(9) 0.4540(8) 0.2346(5) 0.068(4) Uani 1 1 d . . . . .
H32A H 0.725959 0.454271 0.211789 0.102 Uiso 1 1 calc R U . . .
H32B H 0.688571 0.502655 0.232538 0.102 Uiso 1 1 calc R U . . .
H32C H 0.637435 0.410392 0.228300 0.102 Uiso 1 1 calc R 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 O4 2.262(5) 3_665 ?
Tb1 O4 2.262(5) . ?
Tb1 O4 2.262(5) 2_655 ?
Tb1 O1 2.320(5) 3_665 ?
Tb1 O1 2.320(5) 2_655 ?
Tb1 O1 2.320(5) . ?
Tb1 O8 2.798(10) . ?
Tb1 Mn2 3.5031(13) 3_665 ?
Tb1 Mn2 3.5031(13) 2_655 ?
Tb1 Mn2 3.5031(13) . ?
Na1 O2 2.317(6) . ?
Na1 O2 2.317(6) 3_665 ?
Na1 O2 2.317(6) 2_655 ?
Na1 O3 2.385(7) . ?
Na1 O3 2.385(7) 3_665 ?
Na1 O3 2.385(7) 2_655 ?
Na1 O7 2.786(10) . ?
Na1 Mn1 3.450(5) 2_655 ?
Na1 Mn1 3.450(5) 3_665 ?
Na1 Mn1 3.450(5) . ?
N1 C9 1.294(10) . ?
N1 C2 1.507(10) . ?
N1 Mn1 1.969(6) . ?
O1 C1 1.446(10) . ?
O1 Mn1 1.880(5) . ?
C1 C2 1.512(11) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
Mn1 O7 1.8931(12) . ?
Mn1 O2 1.898(6) . ?
Mn1 Br1 2.7875(15) . ?
Mn1 Br1 2.8331(15) 2_655 ?
Na2 O5 2.329(6) 2_655 ?
Na2 O5 2.329(6) . ?
Na2 O5 2.329(6) 3_665 ?
Na2 O6 2.375(8) 3_665 ?
Na2 O6 2.375(8) . ?
Na2 O6 2.375(8) 2_655 ?
Na2 Mn2 3.489(5) . ?
Na2 Mn2 3.490(5) 3_665 ?
Na2 Mn2 3.490(5) 2_655 ?
N2 C25 1.307(10) . ?
N2 C18 1.491(10) . ?
N2 Mn2 1.970(6) . ?
O2 C15 1.315(10) . ?
C2 C3 1.536(11) . ?
C2 H2 1.0000 . ?
Br2 Mn2 2.7135(15) . ?
Br2 Mn2 2.7608(15) 3_665 ?
Mn2 O5 1.873(6) . ?
Mn2 O4 1.909(6) . ?
Mn2 O8 1.9286(13) . ?
O6 C30 1.379(11) . ?
O6 C32 1.415(13) . ?
C6 C5 1.39(2) . ?
C6 C7 1.416(18) . ?
C6 H6 0.9500 . ?
C5 C4 1.410(15) . ?
C5 H5 0.9500 . ?
O5 C31 1.360(10) . ?
C4 C3 1.385(13) . ?
C4 H4 0.9500 . ?
O4 C17 1.409(9) . ?
C3 C8 1.389(14) . ?
O3 C14 1.353(11) . ?
O3 C16 1.487(13) . ?
C7 C8 1.404(15) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.422(12) . ?
C9 H9 0.9500 . ?
C10 C11 1.390(12) . ?
C10 C15 1.414(12) . ?
C11 C12 1.450(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.323(15) . ?
C12 H12 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C15 C14 1.409(12) . ?
C14 C13 1.374(13) . ?
C13 H13 0.9500 . ?
C17 C18 1.506(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.528(12) . ?
C18 H18 1.0000 . ?
C19 C20 1.337(14) . ?
C19 C24 1.410(15) . ?
C20 C21 1.412(16) . ?
C20 H20 0.9500 . ?
C21 C22 1.28(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.27(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.533(18) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.462(12) . ?
C25 H25 0.9500 . ?
C26 C27 1.402(12) . ?
C26 C31 1.411(12) . ?
C27 C28 1.350(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.362(14) . ?
C28 H28 0.9500 . ?
C29 C30 1.422(13) . ?
C29 H29 0.9500 . ?
C30 C31 1.398(12) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Tb1 O4 101.24(17) 3_665 . ?
O4 Tb1 O4 101.24(17) 3_665 2_655 ?
O4 Tb1 O4 101.24(17) . 2_655 ?
O4 Tb1 O1 88.21(19) 3_665 3_665 ?
O4 Tb1 O1 80.55(18) . 3_665 ?
O4 Tb1 O1 169.8(2) 2_655 3_665 ?
O4 Tb1 O1 80.55(18) 3_665 2_655 ?
O4 Tb1 O1 169.8(2) . 2_655 ?
O4 Tb1 O1 88.21(19) 2_655 2_655 ?
O1 Tb1 O1 89.46(18) 3_665 2_655 ?
O4 Tb1 O1 169.8(2) 3_665 . ?
O4 Tb1 O1 88.21(19) . . ?
O4 Tb1 O1 80.54(18) 2_655 . ?
O1 Tb1 O1 89.46(18) 3_665 . ?
O1 Tb1 O1 89.46(18) 2_655 . ?
O4 Tb1 O8 63.19(14) 3_665 . ?
O4 Tb1 O8 63.19(14) . . ?
O4 Tb1 O8 63.19(14) 2_655 . ?
O1 Tb1 O8 125.65(13) 3_665 . ?
O1 Tb1 O8 125.65(13) 2_655 . ?
O1 Tb1 O8 125.64(13) . . ?
O4 Tb1 Mn2 29.87(14) 3_665 3_665 ?
O4 Tb1 Mn2 82.24(14) . 3_665 ?
O4 Tb1 Mn2 82.62(14) 2_655 3_665 ?
O1 Tb1 Mn2 107.63(13) 3_665 3_665 ?
O1 Tb1 Mn2 103.11(13) 2_655 3_665 ?
O1 Tb1 Mn2 158.62(13) . 3_665 ?
O8 Tb1 Mn2 33.321(19) . 3_665 ?
O4 Tb1 Mn2 82.24(14) 3_665 2_655 ?
O4 Tb1 Mn2 82.61(14) . 2_655 ?
O4 Tb1 Mn2 29.87(14) 2_655 2_655 ?
O1 Tb1 Mn2 158.62(13) 3_665 2_655 ?
O1 Tb1 Mn2 107.63(13) 2_655 2_655 ?
O1 Tb1 Mn2 103.11(13) . 2_655 ?
O8 Tb1 Mn2 33.321(19) . 2_655 ?
Mn2 Tb1 Mn2 56.81(3) 3_665 2_655 ?
O4 Tb1 Mn2 82.61(14) 3_665 . ?
O4 Tb1 Mn2 29.87(14) . . ?
O4 Tb1 Mn2 82.24(14) 2_655 . ?
O1 Tb1 Mn2 103.11(13) 3_665 . ?
O1 Tb1 Mn2 158.62(13) 2_655 . ?
O1 Tb1 Mn2 107.63(13) . . ?
O8 Tb1 Mn2 33.320(19) . . ?
Mn2 Tb1 Mn2 56.81(3) 3_665 . ?
Mn2 Tb1 Mn2 56.81(3) 2_655 . ?
O2 Na1 O2 102.6(2) . 3_665 ?
O2 Na1 O2 102.6(2) . 2_655 ?
O2 Na1 O2 102.6(2) 3_665 2_655 ?
O2 Na1 O3 66.5(2) . . ?
O2 Na1 O3 149.8(2) 3_665 . ?
O2 Na1 O3 107.2(2) 2_655 . ?
O2 Na1 O3 107.2(2) . 3_665 ?
O2 Na1 O3 66.5(2) 3_665 3_665 ?
O2 Na1 O3 149.8(2) 2_655 3_665 ?
O3 Na1 O3 89.1(3) . 3_665 ?
O2 Na1 O3 149.8(2) . 2_655 ?
O2 Na1 O3 107.2(2) 3_665 2_655 ?
O2 Na1 O3 66.5(2) 2_655 2_655 ?
O3 Na1 O3 89.1(3) . 2_655 ?
O3 Na1 O3 89.1(3) 3_665 2_655 ?
O2 Na1 O7 64.35(18) . . ?
O2 Na1 O7 64.35(18) 3_665 . ?
O2 Na1 O7 64.35(18) 2_655 . ?
O3 Na1 O7 125.88(19) . . ?
O3 Na1 O7 125.89(19) 3_665 . ?
O3 Na1 O7 125.89(19) 2_655 . ?
O2 Na1 Mn1 81.61(19) . 2_655 ?
O2 Na1 Mn1 85.1(2) 3_665 2_655 ?
O2 Na1 Mn1 31.25(16) 2_655 2_655 ?
O3 Na1 Mn1 118.96(17) . 2_655 ?
O3 Na1 Mn1 151.38(19) 3_665 2_655 ?
O3 Na1 Mn1 96.25(17) 2_655 2_655 ?
O7 Na1 Mn1 33.23(5) . 2_655 ?
O2 Na1 Mn1 85.1(2) . 3_665 ?
O2 Na1 Mn1 31.25(16) 3_665 3_665 ?
O2 Na1 Mn1 81.61(19) 2_655 3_665 ?
O3 Na1 Mn1 151.38(19) . 3_665 ?
O3 Na1 Mn1 96.25(17) 3_665 3_665 ?
O3 Na1 Mn1 118.96(17) 2_655 3_665 ?
O7 Na1 Mn1 33.23(5) . 3_665 ?
Mn1 Na1 Mn1 56.67(9) 2_655 3_665 ?
O2 Na1 Mn1 31.25(16) . . ?
O2 Na1 Mn1 81.61(19) 3_665 . ?
O2 Na1 Mn1 85.1(2) 2_655 . ?
O3 Na1 Mn1 96.25(16) . . ?
O3 Na1 Mn1 118.96(17) 3_665 . ?
O3 Na1 Mn1 151.38(19) 2_655 . ?
O7 Na1 Mn1 33.23(5) . . ?
Mn1 Na1 Mn1 56.67(9) 2_655 . ?
Mn1 Na1 Mn1 56.67(9) 3_665 . ?
C9 N1 C2 121.1(7) . . ?
C9 N1 Mn1 126.4(6) . . ?
C2 N1 Mn1 112.5(5) . . ?
C1 O1 Mn1 112.4(5) . . ?
C1 O1 Tb1 119.1(5) . . ?
Mn1 O1 Tb1 125.6(2) . . ?
O1 C1 C2 107.2(7) . . ?
O1 C1 H1A 110.3 . . ?
C2 C1 H1A 110.3 . . ?
O1 C1 H1B 110.3 . . ?
C2 C1 H1B 110.3 . . ?
H1A C1 H1B 108.5 . . ?
O1 Mn1 O7 92.8(3) . . ?
O1 Mn1 O2 174.3(2) . . ?
O7 Mn1 O2 92.8(3) . . ?
O1 Mn1 N1 83.4(2) . . ?
O7 Mn1 N1 175.7(3) . . ?
O2 Mn1 N1 90.9(3) . . ?
O1 Mn1 Br1 87.70(17) . . ?
O7 Mn1 Br1 84.96(4) . . ?
O2 Mn1 Br1 93.90(18) . . ?
N1 Mn1 Br1 96.93(19) . . ?
O1 Mn1 Br1 94.35(17) . 2_655 ?
O7 Mn1 Br1 83.67(4) . 2_655 ?
O2 Mn1 Br1 85.16(17) . 2_655 ?
N1 Mn1 Br1 94.52(19) . 2_655 ?
Br1 Mn1 Br1 168.53(5) . 2_655 ?
O1 Mn1 Na1 146.37(16) . . ?
O7 Mn1 Na1 53.7(3) . . ?
O2 Mn1 Na1 39.30(17) . . ?
N1 Mn1 Na1 130.1(2) . . ?
Br1 Mn1 Na1 86.38(3) . . ?
Br1 Mn1 Na1 85.69(4) 2_655 . ?
Mn1 Br1 Mn1 71.26(5) . 3_665 ?
O5 Na2 O5 101.4(2) 2_655 . ?
O5 Na2 O5 101.4(2) 2_655 3_665 ?
O5 Na2 O5 101.4(2) . 3_665 ?
O5 Na2 O6 155.2(2) 2_655 3_665 ?
O5 Na2 O6 102.8(2) . 3_665 ?
O5 Na2 O6 68.4(2) 3_665 3_665 ?
O5 Na2 O6 102.8(2) 2_655 . ?
O5 Na2 O6 68.4(2) . . ?
O5 Na2 O6 155.2(2) 3_665 . ?
O6 Na2 O6 91.2(3) 3_665 . ?
O5 Na2 O6 68.4(2) 2_655 2_655 ?
O5 Na2 O6 155.2(2) . 2_655 ?
O5 Na2 O6 102.8(2) 3_665 2_655 ?
O6 Na2 O6 91.2(3) 3_665 2_655 ?
O6 Na2 O6 91.2(3) . 2_655 ?
O5 Na2 Mn2 83.8(2) 2_655 . ?
O5 Na2 Mn2 29.89(16) . . ?
O5 Na2 Mn2 81.3(2) 3_665 . ?
O6 Na2 Mn2 115.33(19) 3_665 . ?
O6 Na2 Mn2 95.76(18) . . ?
O6 Na2 Mn2 152.3(2) 2_655 . ?
O5 Na2 Mn2 81.3(2) 2_655 3_665 ?
O5 Na2 Mn2 83.8(2) . 3_665 ?
O5 Na2 Mn2 29.90(16) 3_665 3_665 ?
O6 Na2 Mn2 95.75(18) 3_665 3_665 ?
O6 Na2 Mn2 152.3(2) . 3_665 ?
O6 Na2 Mn2 115.33(19) 2_655 3_665 ?
Mn2 Na2 Mn2 57.05(9) . 3_665 ?
O5 Na2 Mn2 29.89(16) 2_655 2_655 ?
O5 Na2 Mn2 81.3(2) . 2_655 ?
O5 Na2 Mn2 83.8(2) 3_665 2_655 ?
O6 Na2 Mn2 152.3(2) 3_665 2_655 ?
O6 Na2 Mn2 115.33(19) . 2_655 ?
O6 Na2 Mn2 95.75(18) 2_655 2_655 ?
Mn2 Na2 Mn2 57.05(9) . 2_655 ?
Mn2 Na2 Mn2 57.05(9) 3_665 2_655 ?
C25 N2 C18 123.1(7) . . ?
C25 N2 Mn2 127.3(6) . . ?
C18 N2 Mn2 109.6(5) . . ?
C15 O2 Mn1 127.8(5) . . ?
C15 O2 Na1 121.3(5) . . ?
Mn1 O2 Na1 109.4(3) . . ?
N1 C2 C1 106.5(6) . . ?
N1 C2 C3 115.9(7) . . ?
C1 C2 C3 110.3(7) . . ?
N1 C2 H2 108.0 . . ?
C1 C2 H2 108.0 . . ?
C3 C2 H2 108.0 . . ?
Mn2 Br2 Mn2 75.01(5) . 3_665 ?
O5 Mn2 O4 172.0(2) . . ?
O5 Mn2 O8 98.5(3) . . ?
O4 Mn2 O8 89.0(3) . . ?
O5 Mn2 N2 90.2(2) . . ?
O4 Mn2 N2 82.5(2) . . ?
O8 Mn2 N2 169.9(3) . . ?
O5 Mn2 Br2 92.72(17) . . ?
O4 Mn2 Br2 90.93(16) . . ?
O8 Mn2 Br2 83.22(5) . . ?
N2 Mn2 Br2 91.52(19) . . ?
O5 Mn2 Br2 86.44(17) . 2_655 ?
O4 Mn2 Br2 91.89(16) . 2_655 ?
O8 Mn2 Br2 81.94(4) . 2_655 ?
N2 Mn2 Br2 103.62(19) . 2_655 ?
Br2 Mn2 Br2 164.84(5) . 2_655 ?
O5 Mn2 Na2 38.30(18) . . ?
O4 Mn2 Na2 149.36(17) . . ?
O8 Mn2 Na2 60.4(3) . . ?
N2 Mn2 Na2 127.92(19) . . ?
Br2 Mn2 Na2 85.34(4) . . ?
Br2 Mn2 Na2 84.65(4) 2_655 . ?
O5 Mn2 Tb1 151.23(17) . . ?
O4 Mn2 Tb1 36.15(16) . . ?
O8 Mn2 Tb1 52.8(3) . . ?
N2 Mn2 Tb1 118.53(18) . . ?
Br2 Mn2 Tb1 87.11(4) . . ?
Br2 Mn2 Tb1 86.40(4) 2_655 . ?
Na2 Mn2 Tb1 113.21(6) . . ?
C30 O6 C32 111.8(8) . . ?
C30 O6 Na2 118.4(5) . . ?
C32 O6 Na2 129.0(7) . . ?
C5 C6 C7 122.3(12) . . ?
C5 C6 H6 118.8 . . ?
C7 C6 H6 118.8 . . ?
C6 C5 C4 119.3(12) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C31 O5 Mn2 126.7(5) . . ?
C31 O5 Na2 118.1(5) . . ?
Mn2 O5 Na2 111.8(3) . . ?
C3 C4 C5 119.0(11) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C17 O4 Mn2 114.1(5) . . ?
C17 O4 Tb1 131.8(5) . . ?
Mn2 O4 Tb1 114.0(3) . . ?
C4 C3 C8 121.0(9) . . ?
C4 C3 C2 117.8(9) . . ?
C8 C3 C2 120.9(8) . . ?
C14 O3 C16 114.4(8) . . ?
C14 O3 Na1 119.3(5) . . ?
C16 O3 Na1 126.3(6) . . ?
C8 C7 C6 116.5(11) . . ?
C8 C7 H7 121.7 . . ?
C6 C7 H7 121.7 . . ?
Mn1 O7 Mn1 119.72(5) . 3_665 ?
Mn1 O7 Mn1 119.73(5) . 2_655 ?
Mn1 O7 Mn1 119.72(5) 3_665 2_655 ?
Mn1 O7 Na1 93.0(3) . . ?
Mn1 O7 Na1 93.0(3) 3_665 . ?
Mn1 O7 Na1 93.0(3) 2_655 . ?
C3 C8 C7 121.6(10) . . ?
C3 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
Mn2 O8 Mn2 119.56(7) . 3_665 ?
Mn2 O8 Mn2 119.56(7) . 2_655 ?
Mn2 O8 Mn2 119.56(7) 3_665 2_655 ?
Mn2 O8 Tb1 93.8(3) . . ?
Mn2 O8 Tb1 93.8(3) 3_665 . ?
Mn2 O8 Tb1 93.8(3) 2_655 . ?
N1 C9 C10 126.5(8) . . ?
N1 C9 H9 116.8 . . ?
C10 C9 H9 116.8 . . ?
C11 C10 C15 122.4(8) . . ?
C11 C10 C9 116.7(8) . . ?
C15 C10 C9 120.8(8) . . ?
C10 C11 C12 116.2(9) . . ?
C10 C11 H11 121.9 . . ?
C12 C11 H11 121.9 . . ?
C13 C12 C11 121.5(9) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O2 C15 C14 118.0(8) . . ?
O2 C15 C10 124.8(8) . . ?
C14 C15 C10 117.2(8) . . ?
O3 C14 C13 125.3(8) . . ?
O3 C14 C15 113.9(8) . . ?
C13 C14 C15 120.8(9) . . ?
C12 C13 C14 121.7(10) . . ?
C12 C13 H13 119.2 . . ?
C14 C13 H13 119.2 . . ?
O4 C17 C18 108.4(6) . . ?
O4 C17 H17A 110.0 . . ?
C18 C17 H17A 110.0 . . ?
O4 C17 H17B 110.0 . . ?
C18 C17 H17B 110.0 . . ?
H17A C17 H17B 108.4 . . ?
N2 C18 C17 102.3(6) . . ?
N2 C18 C19 115.7(7) . . ?
C17 C18 C19 118.1(8) . . ?
N2 C18 H18 106.6 . . ?
C17 C18 H18 106.6 . . ?
C19 C18 H18 106.6 . . ?
C20 C19 C24 120.6(10) . . ?
C20 C19 C18 121.9(9) . . ?
C24 C19 C18 117.5(9) . . ?
C19 C20 C21 121.0(12) . . ?
C19 C20 H20 119.5 . . ?
C21 C20 H20 119.5 . . ?
C22 C21 C20 120.8(15) . . ?
C22 C21 H21 119.6 . . ?
C20 C21 H21 119.6 . . ?
C23 C22 C21 122.7(16) . . ?
C23 C22 H22 118.6 . . ?
C21 C22 H22 118.6 . . ?
C22 C23 C24 122.2(16) . . ?
C22 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
C19 C24 C23 112.5(12) . . ?
C19 C24 H24A 109.1 . . ?
C23 C24 H24A 109.1 . . ?
C19 C24 H24B 109.1 . . ?
C23 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
N2 C25 C26 122.8(8) . . ?
N2 C25 H25 118.6 . . ?
C26 C25 H25 118.6 . . ?
C27 C26 C31 119.7(8) . . ?
C27 C26 C25 117.6(8) . . ?
C31 C26 C25 122.6(7) . . ?
C28 C27 C26 122.3(9) . . ?
C28 C27 H27 118.9 . . ?
C26 C27 H27 118.9 . . ?
C27 C28 C29 119.4(9) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C28 C29 C30 120.7(9) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
O6 C30 C31 114.3(8) . . ?
O6 C30 C29 125.4(8) . . ?
C31 C30 C29 120.3(8) . . ?
O5 C31 C30 119.8(8) . . ?
O5 C31 C26 122.6(7) . . ?
C30 C31 C26 117.6(8) . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_refine_diff_density_max         1.722
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.106



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/ACN/diethylether'
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_mo_I06UB207_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1555188'
_audit_update_record             
;
2017-06-09 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C96 H90 Cl6 Gd Mn6 N6 Na2 O20, 4.5(C H4 O), H2 O'
_chemical_formula_sum            'C100.50 H110 Cl6 Gd Mn6 N6 Na2 O25.50'
_chemical_formula_weight         2555.51

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'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   19.4486(6)
_cell_length_b                   19.4486(6)
_cell_length_c                   28.7046(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9402.8(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6102
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      25.00

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_F_000             3891
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.045
_exptl_absorpt_coefficient_mu    1.305
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17967
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.094
_diffrn_reflns_theta_max         26.399
_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             4296
_reflns_number_gt                2997
_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    'XT-2014 (Sheldrick 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_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)+(0.1248P)²+138.4071P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4296
_refine_ls_number_parameters     223
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1052
_refine_ls_R_factor_gt           0.0692
_refine_ls_wR_factor_ref         0.2255
_refine_ls_wR_factor_gt          0.2011
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Gd1 Gd 0.6667 0.3333 0.3333 0.0318(3) Uani 1 6 d S T P . .
Na1 Na 0.6667 0.3333 0.53972(16) 0.0234(10) Uani 1 3 d S T P . .
Cl1 Cl 0.68695(11) 0.49775(10) 0.43943(6) 0.0269(4) Uani 1 1 d . . . . .
Mn1 Mn 0.76957(5) 0.42593(6) 0.43899(3) 0.0177(3) Uani 1 1 d . . . . .
O1 O 0.7713(2) 0.4323(3) 0.37315(15) 0.0183(9) Uani 1 1 d . . . . .
O2 O 0.7820(3) 0.4283(3) 0.50448(16) 0.0236(10) Uani 1 1 d . . . . .
O3 O 0.7797(3) 0.3758(3) 0.58841(17) 0.0301(12) Uani 1 1 d . . . . .
O4 O 0.6667 0.3333 0.4377(3) 0.0188(16) Uani 1 3 d S T P . .
N1 N 0.8766(4) 0.5203(4) 0.4315(2) 0.0387(17) Uani 1 1 d . . . . .
C1 C 0.8246(5) 0.5094(5) 0.3566(3) 0.0345(18) Uani 1 1 d . . . . .
H1A H 0.8004 0.5434 0.3603 0.041 Uiso 1 1 calc R U . . .
H1B H 0.8343 0.5067 0.3229 0.041 Uiso 1 1 calc R U . . .
C2 C 0.8993(5) 0.5447(6) 0.3813(3) 0.050(2) Uani 1 1 d . . . . .
H2 H 0.9313 0.5210 0.3696 0.060 Uiso 1 1 calc R U . . .
C3 C 0.9467(4) 0.6342(3) 0.3747(2) 0.063(3) Uani 1 1 d G . . . .
C4 C 1.0109(4) 0.6601(4) 0.3446(2) 0.071(4) Uani 1 1 d G . . . .
H4 H 1.0216 0.6228 0.3299 0.085 Uiso 1 1 calc R U . . .
C5 C 1.0594(3) 0.7408(5) 0.3360(3) 0.090(5) Uani 1 1 d G . . . .
H5 H 1.1033 0.7585 0.3154 0.107 Uiso 1 1 calc R U . . .
C6 C 1.0437(5) 0.7955(3) 0.3575(3) 0.088(5) Uani 1 1 d G . . . .
H6 H 1.0768 0.8506 0.3516 0.105 Uiso 1 1 calc R U . . .
C7 C 0.9794(6) 0.7695(5) 0.3876(3) 0.097(5) Uani 1 1 d G . . . .
H7 H 0.9687 0.8069 0.4023 0.117 Uiso 1 1 calc R U . . .
C8 C 0.9309(4) 0.6889(5) 0.3962(2) 0.073(4) Uani 1 1 d G . . . .
H8 H 0.8870 0.6711 0.4168 0.088 Uiso 1 1 calc R U . . .
C9 C 0.9301(5) 0.5536(5) 0.4638(3) 0.043(2) Uani 1 1 d . . . . .
H9 H 0.9798 0.5975 0.4550 0.052 Uiso 1 1 calc R U . . .
C10 C 0.9202(4) 0.5295(4) 0.5111(2) 0.0296(16) Uani 1 1 d . . . . .
C11 C 0.9871(4) 0.5694(5) 0.5400(3) 0.0359(18) Uani 1 1 d . . . . .
H11 H 1.0344 0.6129 0.5281 0.043 Uiso 1 1 calc R U . . .
C12 C 0.9844(5) 0.5458(5) 0.5853(3) 0.0391(19) Uani 1 1 d . . . . .
H12 H 1.0293 0.5738 0.6050 0.047 Uiso 1 1 calc R U . . .
C13 C 0.9162(5) 0.4812(5) 0.6023(3) 0.0379(19) Uani 1 1 d . . . . .
H13 H 0.9150 0.4643 0.6334 0.046 Uiso 1 1 calc R U . . .
C14 C 0.8495(4) 0.4408(4) 0.5745(2) 0.0247(15) Uani 1 1 d . . . . .
C15 C 0.8495(4) 0.4656(4) 0.5286(2) 0.0212(14) Uani 1 1 d . . . . .
C16 C 0.7834(6) 0.3418(6) 0.6324(3) 0.051(2) Uani 1 1 d . . . . .
H16A H 0.7325 0.2935 0.6383 0.076 Uiso 1 1 calc R U . . .
H16B H 0.7944 0.3802 0.6574 0.076 Uiso 1 1 calc R U . . .
H16C H 0.8258 0.3285 0.6313 0.076 Uiso 1 1 calc R U . . .
O1W O 0.7765(12) 0.6029(9) 0.5512(5) 0.081(4) Uani 0.5 1 d D . P . .
H1OW H 0.7269 0.5811 0.5492 0.097 Uiso 0.5 1 calc R U P . .
C1W C 0.8103(16) 0.6407(13) 0.5097(6) 0.081(4) Uani 0.5 1 d D . P . .
H1WA H 0.7785 0.6075 0.4836 0.097 Uiso 0.5 1 calc R U P . .
H1WB H 0.8644 0.6494 0.5074 0.097 Uiso 0.5 1 calc R U P . .
H1WC H 0.8120 0.6919 0.5086 0.097 Uiso 0.5 1 calc R U P . .
O2W O 0.850(2) 0.3332(16) 0.7372(11) 0.075(8) Uani 0.25 1 d D . P . .
H2OW H 0.8898 0.3614 0.7205 0.089 Uiso 0.25 1 calc R U P . .
C2W C 0.873(3) 0.338(2) 0.7833(12) 0.075(8) Uani 0.25 1 d D . P . .
H2WA H 0.8986 0.3052 0.7875 0.112 Uiso 0.25 1 calc R U P . .
H2WB H 0.8270 0.3180 0.8036 0.112 Uiso 0.25 1 calc R U P . .
H2WC H 0.9115 0.3930 0.7911 0.112 Uiso 0.25 1 calc R U P . .
O3W O 0.6667 0.3333 0.7456(10) 0.125(15) Uani 0.5 3 d S T P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.287(4) . ?
Gd1 O1 2.287(4) 18_545 ?
Gd1 O1 2.287(4) 3_665 ?
Gd1 O1 2.287(4) 2_655 ?
Gd1 O1 2.287(4) 16_655 ?
Gd1 O1 2.288(4) 17 ?
Gd1 Mn1 3.5835(9) 2_655 ?
Gd1 Mn1 3.5836(9) 3_665 ?
Gd1 Mn1 3.5836(9) 17 ?
Gd1 Mn1 3.5836(9) 16_655 ?
Gd1 Mn1 3.5836(9) 18_545 ?
Gd1 Mn1 3.5836(9) . ?
Na1 O2 2.306(5) . ?
Na1 O2 2.306(5) 3_665 ?
Na1 O2 2.306(5) 2_655 ?
Na1 O3 2.378(5) . ?
Na1 O3 2.378(5) 3_665 ?
Na1 O3 2.378(5) 2_655 ?
Na1 O4 2.928(9) . ?
Na1 Mn1 3.465(4) . ?
Na1 Mn1 3.465(4) 2_655 ?
Na1 Mn1 3.465(4) 3_665 ?
Cl1 Mn1 2.6033(19) . ?
Cl1 Mn1 2.688(2) 2_655 ?
Mn1 O2 1.893(5) . ?
Mn1 O1 1.893(4) . ?
Mn1 O4 1.9093(9) . ?
Mn1 N1 1.982(6) . ?
Mn1 Cl1 2.687(2) 3_665 ?
O1 C1 1.413(8) . ?
O2 C15 1.334(8) . ?
O3 C14 1.373(9) . ?
O3 C16 1.443(9) . ?
O4 Mn1 1.9092(9) 2_655 ?
O4 Mn1 1.9094(9) 3_665 ?
N1 C9 1.298(10) . ?
N1 C2 1.512(11) . ?
C1 C2 1.445(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.520(11) . ?
C2 H2 1.0000 . ?
C3 C4 1.3900 . ?
C3 C8 1.3900 . ?
C4 C5 1.3900 . ?
C4 H4 0.9500 . ?
C5 C6 1.3900 . ?
C5 H5 0.9500 . ?
C6 C7 1.3900 . ?
C6 H6 0.9500 . ?
C7 C8 1.3900 . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.418(11) . ?
C9 H9 0.9500 . ?
C10 C11 1.404(10) . ?
C10 C15 1.407(10) . ?
C11 C12 1.372(11) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(12) . ?
C12 H12 0.9500 . ?
C13 C14 1.385(10) . ?
C13 H13 0.9500 . ?
C14 C15 1.402(9) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1W C1W 1.381(10) . ?
O1W H1OW 0.8400 . ?
C1W H1WA 0.9800 . ?
C1W H1WB 0.9800 . ?
C1W H1WC 0.9800 . ?
O2W C2W 1.388(10) . ?
O2W H2OW 0.8400 . ?
C2W H2WA 0.9800 . ?
C2W H2WB 0.9800 . ?
C2W H2WC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O1 82.79(14) . 18_545 ?
O1 Gd1 O1 97.21(14) . 3_665 ?
O1 Gd1 O1 180.0 18_545 3_665 ?
O1 Gd1 O1 97.21(14) . 2_655 ?
O1 Gd1 O1 82.79(14) 18_545 2_655 ?
O1 Gd1 O1 97.21(14) 3_665 2_655 ?
O1 Gd1 O1 180.0 . 16_655 ?
O1 Gd1 O1 97.21(14) 18_545 16_655 ?
O1 Gd1 O1 82.79(14) 3_665 16_655 ?
O1 Gd1 O1 82.79(14) 2_655 16_655 ?
O1 Gd1 O1 82.79(14) . 17 ?
O1 Gd1 O1 97.21(14) 18_545 17 ?
O1 Gd1 O1 82.79(14) 3_665 17 ?
O1 Gd1 O1 180.0(2) 2_655 17 ?
O1 Gd1 O1 97.21(14) 16_655 17 ?
O1 Gd1 Mn1 77.91(11) . 2_655 ?
O1 Gd1 Mn1 100.09(11) 18_545 2_655 ?
O1 Gd1 Mn1 79.91(11) 3_665 2_655 ?
O1 Gd1 Mn1 27.89(11) 2_655 2_655 ?
O1 Gd1 Mn1 102.09(11) 16_655 2_655 ?
O1 Gd1 Mn1 152.11(11) 17 2_655 ?
O1 Gd1 Mn1 79.91(11) . 3_665 ?
O1 Gd1 Mn1 152.11(11) 18_545 3_665 ?
O1 Gd1 Mn1 27.89(11) 3_665 3_665 ?
O1 Gd1 Mn1 77.91(11) 2_655 3_665 ?
O1 Gd1 Mn1 100.09(11) 16_655 3_665 ?
O1 Gd1 Mn1 102.09(11) 17 3_665 ?
Mn1 Gd1 Mn1 54.95(2) 2_655 3_665 ?
O1 Gd1 Mn1 102.09(11) . 17 ?
O1 Gd1 Mn1 79.91(11) 18_545 17 ?
O1 Gd1 Mn1 100.09(11) 3_665 17 ?
O1 Gd1 Mn1 152.11(11) 2_655 17 ?
O1 Gd1 Mn1 77.91(11) 16_655 17 ?
O1 Gd1 Mn1 27.89(11) 17 17 ?
Mn1 Gd1 Mn1 180.0 2_655 17 ?
Mn1 Gd1 Mn1 125.05(2) 3_665 17 ?
O1 Gd1 Mn1 152.11(11) . 16_655 ?
O1 Gd1 Mn1 77.91(11) 18_545 16_655 ?
O1 Gd1 Mn1 102.09(11) 3_665 16_655 ?
O1 Gd1 Mn1 100.09(11) 2_655 16_655 ?
O1 Gd1 Mn1 27.89(11) 16_655 16_655 ?
O1 Gd1 Mn1 79.91(11) 17 16_655 ?
Mn1 Gd1 Mn1 125.05(2) 2_655 16_655 ?
Mn1 Gd1 Mn1 125.05(2) 3_665 16_655 ?
Mn1 Gd1 Mn1 54.95(2) 17 16_655 ?
O1 Gd1 Mn1 100.09(11) . 18_545 ?
O1 Gd1 Mn1 27.89(11) 18_545 18_545 ?
O1 Gd1 Mn1 152.11(11) 3_665 18_545 ?
O1 Gd1 Mn1 102.09(11) 2_655 18_545 ?
O1 Gd1 Mn1 79.91(11) 16_655 18_545 ?
O1 Gd1 Mn1 77.91(11) 17 18_545 ?
Mn1 Gd1 Mn1 125.06(2) 2_655 18_545 ?
Mn1 Gd1 Mn1 180.0 3_665 18_545 ?
Mn1 Gd1 Mn1 54.95(2) 17 18_545 ?
Mn1 Gd1 Mn1 54.95(2) 16_655 18_545 ?
O1 Gd1 Mn1 27.89(11) . . ?
O1 Gd1 Mn1 102.09(11) 18_545 . ?
O1 Gd1 Mn1 77.91(11) 3_665 . ?
O1 Gd1 Mn1 79.91(11) 2_655 . ?
O1 Gd1 Mn1 152.11(11) 16_655 . ?
O1 Gd1 Mn1 100.09(11) 17 . ?
Mn1 Gd1 Mn1 54.95(2) 2_655 . ?
Mn1 Gd1 Mn1 54.95(2) 3_665 . ?
Mn1 Gd1 Mn1 125.05(2) 17 . ?
Mn1 Gd1 Mn1 180.00(6) 16_655 . ?
Mn1 Gd1 Mn1 125.05(2) 18_545 . ?
O2 Na1 O2 102.21(18) . 3_665 ?
O2 Na1 O2 102.21(18) . 2_655 ?
O2 Na1 O2 102.21(18) 3_665 2_655 ?
O2 Na1 O3 67.66(17) . . ?
O2 Na1 O3 105.93(18) 3_665 . ?
O2 Na1 O3 151.51(19) 2_655 . ?
O2 Na1 O3 151.51(19) . 3_665 ?
O2 Na1 O3 67.66(16) 3_665 3_665 ?
O2 Na1 O3 105.93(18) 2_655 3_665 ?
O3 Na1 O3 89.0(2) . 3_665 ?
O2 Na1 O3 105.94(18) . 2_655 ?
O2 Na1 O3 151.51(19) 3_665 2_655 ?
O2 Na1 O3 67.66(16) 2_655 2_655 ?
O3 Na1 O3 89.0(2) . 2_655 ?
O3 Na1 O3 89.0(2) 3_665 2_655 ?
O2 Na1 O4 63.99(15) . . ?
O2 Na1 O4 63.99(15) 3_665 . ?
O2 Na1 O4 63.99(15) 2_655 . ?
O3 Na1 O4 126.00(15) . . ?
O3 Na1 O4 126.00(15) 3_665 . ?
O3 Na1 O4 126.00(15) 2_655 . ?
O2 Na1 Mn1 30.71(13) . . ?
O2 Na1 Mn1 85.01(16) 3_665 . ?
O2 Na1 Mn1 81.30(16) 2_655 . ?
O3 Na1 Mn1 96.70(13) . . ?
O3 Na1 Mn1 152.58(15) 3_665 . ?
O3 Na1 Mn1 117.86(14) 2_655 . ?
O4 Na1 Mn1 33.43(4) . . ?
O2 Na1 Mn1 85.01(16) . 2_655 ?
O2 Na1 Mn1 81.30(16) 3_665 2_655 ?
O2 Na1 Mn1 30.71(13) 2_655 2_655 ?
O3 Na1 Mn1 152.58(16) . 2_655 ?
O3 Na1 Mn1 117.86(14) 3_665 2_655 ?
O3 Na1 Mn1 96.70(13) 2_655 2_655 ?
O4 Na1 Mn1 33.43(4) . 2_655 ?
Mn1 Na1 Mn1 57.00(7) . 2_655 ?
O2 Na1 Mn1 81.30(16) . 3_665 ?
O2 Na1 Mn1 30.71(13) 3_665 3_665 ?
O2 Na1 Mn1 85.02(16) 2_655 3_665 ?
O3 Na1 Mn1 117.86(14) . 3_665 ?
O3 Na1 Mn1 96.70(13) 3_665 3_665 ?
O3 Na1 Mn1 152.58(15) 2_655 3_665 ?
O4 Na1 Mn1 33.43(4) . 3_665 ?
Mn1 Na1 Mn1 57.00(7) . 3_665 ?
Mn1 Na1 Mn1 57.00(7) 2_655 3_665 ?
Mn1 Cl1 Mn1 77.33(6) . 2_655 ?
O2 Mn1 O1 172.7(2) . . ?
O2 Mn1 O4 95.9(3) . . ?
O1 Mn1 O4 91.0(3) . . ?
O2 Mn1 N1 91.3(2) . . ?
O1 Mn1 N1 81.7(2) . . ?
O4 Mn1 N1 172.6(3) . . ?
O2 Mn1 Cl1 95.03(15) . . ?
O1 Mn1 Cl1 88.01(14) . . ?
O4 Mn1 Cl1 82.48(5) . . ?
N1 Mn1 Cl1 98.5(2) . . ?
O2 Mn1 Cl1 85.90(15) . 3_665 ?
O1 Mn1 Cl1 93.17(14) . 3_665 ?
O4 Mn1 Cl1 80.20(5) . 3_665 ?
N1 Mn1 Cl1 98.8(2) . 3_665 ?
Cl1 Mn1 Cl1 162.65(6) . 3_665 ?
O2 Mn1 Na1 38.48(14) . . ?
O1 Mn1 Na1 148.61(14) . . ?
O4 Mn1 Na1 57.7(2) . . ?
N1 Mn1 Na1 129.6(2) . . ?
Cl1 Mn1 Na1 85.63(5) . . ?
Cl1 Mn1 Na1 84.39(4) 3_665 . ?
O2 Mn1 Gd1 152.24(14) . . ?
O1 Mn1 Gd1 34.41(13) . . ?
O4 Mn1 Gd1 56.7(2) . . ?
N1 Mn1 Gd1 115.97(19) . . ?
Cl1 Mn1 Gd1 86.23(4) . . ?
Cl1 Mn1 Gd1 85.02(4) 3_665 . ?
Na1 Mn1 Gd1 114.38(5) . . ?
C1 O1 Mn1 112.6(4) . . ?
C1 O1 Gd1 126.6(4) . . ?
Mn1 O1 Gd1 117.7(2) . . ?
C15 O2 Mn1 127.4(4) . . ?
C15 O2 Na1 120.4(4) . . ?
Mn1 O2 Na1 110.8(2) . . ?
C14 O3 C16 115.1(6) . . ?
C14 O3 Na1 117.7(4) . . ?
C16 O3 Na1 127.2(5) . . ?
Mn1 O4 Mn1 119.964(18) 2_655 . ?
Mn1 O4 Mn1 119.963(18) 2_655 3_665 ?
Mn1 O4 Mn1 119.961(17) . 3_665 ?
Mn1 O4 Na1 88.9(2) 2_655 . ?
Mn1 O4 Na1 88.9(2) . . ?
Mn1 O4 Na1 88.9(2) 3_665 . ?
C9 N1 C2 119.2(7) . . ?
C9 N1 Mn1 126.4(5) . . ?
C2 N1 Mn1 113.6(5) . . ?
O1 C1 C2 111.6(7) . . ?
O1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
O1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C1 C2 N1 104.7(7) . . ?
C1 C2 C3 111.9(7) . . ?
N1 C2 C3 113.1(7) . . ?
C1 C2 H2 109.0 . . ?
N1 C2 H2 109.0 . . ?
C3 C2 H2 109.0 . . ?
C4 C3 C8 120.0 . . ?
C4 C3 C2 114.4(7) . . ?
C8 C3 C2 125.6(7) . . ?
C5 C4 C3 120.0 . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C7 120.0 . . ?
C5 C6 H6 120.0 . . ?
C7 C6 H6 120.0 . . ?
C8 C7 C6 120.0 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C3 120.0 . . ?
C7 C8 H8 120.0 . . ?
C3 C8 H8 120.0 . . ?
N1 C9 C10 125.2(7) . . ?
N1 C9 H9 117.4 . . ?
C10 C9 H9 117.4 . . ?
C11 C10 C15 120.2(7) . . ?
C11 C10 C9 116.6(7) . . ?
C15 C10 C9 123.0(6) . . ?
C12 C11 C10 120.4(7) . . ?
C12 C11 H11 119.8 . . ?
C10 C11 H11 119.8 . . ?
C11 C12 C13 119.8(7) . . ?
C11 C12 H12 120.1 . . ?
C13 C12 H12 120.1 . . ?
C12 C13 C14 121.0(7) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
O3 C14 C13 124.7(7) . . ?
O3 C14 C15 114.9(6) . . ?
C13 C14 C15 120.4(7) . . ?
O2 C15 C14 118.0(6) . . ?
O2 C15 C10 123.9(6) . . ?
C14 C15 C10 118.1(6) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1W O1W H1OW 109.5 . . ?
O1W C1W H1WA 109.5 . . ?
O1W C1W H1WB 109.5 . . ?
H1WA C1W H1WB 109.5 . . ?
O1W C1W H1WC 109.5 . . ?
H1WA C1W H1WC 109.5 . . ?
H1WB C1W H1WC 109.5 . . ?
C2W O2W H2OW 109.5 . . ?
O2W C2W H2WA 109.5 . . ?
O2W C2W H2WB 109.5 . . ?
H2WA C2W H2WB 109.5 . . ?
O2W C2W H2WC 109.5 . . ?
H2WA C2W H2WC 109.5 . . ?
H2WB C2W H2WC 109.5 . . ?

_refine_diff_density_max         2.303
_refine_diff_density_min         -1.067
_refine_diff_density_rms         0.175

_shelxl_version_number           2012-9

####################################################################### 
# 
# 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_mo_i06ub94_0m_b_sq_d
_database_code_depnum_ccdc_archive 'CCDC 1983656'
loop_
_audit_author_name
_audit_author_address
'Merce Font-Bardia'
;Departament de Mineralogia Cristallografia i Diposits Minerals Universitat de Barcelona
Spain
;
_audit_update_record             
;
2020-02-12 deposited with the CCDC.	2020-03-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C96 H90 Cl6 Mn6 N6 Na2 O20 Tb, 6.50(H2 O),3(C H4 O)'
_chemical_formula_sum            'C99 H115 Cl6 Mn6 N6 Na2 O29.50 Tb'
_chemical_formula_weight         2608.20

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'
Mn Mn 0.3368 0.7283 '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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_H-M_alt        'R 3 :H'
_space_group_name_Hall           'R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'

_cell_length_a                   19.5945(5)
_cell_length_b                   19.5945(5)
_cell_length_c                   28.3967(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     9442.1(5)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9152
_cell_measurement_theta_min      2.51
_cell_measurement_theta_max      26.34

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_F_000             3978
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.125
_exptl_absorpt_coefficient_mu    1.338
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6585
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   microfocus
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26515
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_theta_min         2.079
_diffrn_reflns_theta_max         26.434
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             8375
_reflns_number_gt                7577
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_max     0.933
_reflns_Friedel_fraction_full    0.942

_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. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_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-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0779P)²+30.0030P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.019(18)
_chemical_absolute_configuration rm
_refine_ls_number_reflns         8375
_refine_ls_number_parameters     452
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1394
_refine_ls_wR_factor_gt          0.1355
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_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
Tb1 Tb 0.3333 0.6667 0.49456(2) 0.01195(18) Uani 1 3 d S T P . .
Mn1 Mn 0.24503(8) 0.56378(8) 0.60754(5) 0.0116(3) Uani 1 1 d . . . . .
Mn2 Mn 0.33329(8) 0.56843(8) 0.39330(5) 0.0112(3) Uani 1 1 d . . . . .
Cl1 Cl 0.35803(13) 0.52543(13) 0.60720(8) 0.0166(5) Uani 1 1 d . . . . .
Cl2 Cl 0.48639(13) 0.66868(13) 0.39241(8) 0.0161(5) Uani 1 1 d . . . . .
Na1 Na 0.3333 0.6667 0.7091(2) 0.0160(14) Uani 1 3 d S T P . .
Na2 Na 0.3333 0.6667 0.2906(2) 0.0141(13) Uani 1 3 d S T P . .
O1 O 0.2402(4) 0.5661(4) 0.5407(2) 0.0140(14) Uani 1 1 d . . . . .
O2 O 0.2412(4) 0.5502(4) 0.6740(2) 0.0135(14) Uani 1 1 d . . . . .
O3 O 0.2945(4) 0.5558(4) 0.7594(2) 0.0210(15) Uani 1 1 d . . . . .
O4 O 0.3332(4) 0.5612(4) 0.4603(2) 0.0131(13) Uani 1 1 d . . . . .
O5 O 0.3408(4) 0.5651(4) 0.3271(2) 0.0150(14) Uani 1 1 d . . . . .
O6 O 0.4018(4) 0.6206(4) 0.2440(2) 0.0224(16) Uani 1 1 d . . . . .
O7 O 0.3333 0.6667 0.6101(4) 0.011(2) Uani 1 3 d S T P . .
O8 O 0.3333 0.6667 0.3999(4) 0.014(2) Uani 1 3 d S T P . .
N1 N 0.1550(4) 0.4551(4) 0.5990(3) 0.0148(15) Uani 1 1 d . . . . .
N2 N 0.3198(4) 0.4616(4) 0.3978(3) 0.0125(15) Uani 1 1 d . . . . .
C1 C 0.1629(6) 0.5140(5) 0.5241(3) 0.015(2) Uani 1 1 d . . . . .
H1A H 0.1644 0.5060 0.4897 0.018 Uiso 1 1 calc R U . . .
H1B H 0.1289 0.5371 0.5298 0.018 Uiso 1 1 calc R U . . .
C2 C 0.1292(6) 0.4348(5) 0.5496(3) 0.0184(19) Uani 1 1 d . . . . .
H2 H 0.1557 0.4067 0.5364 0.022 Uiso 1 1 calc R U . . .
C3 C 0.0413(6) 0.3833(6) 0.5409(4) 0.030(3) Uani 1 1 d . . . . .
C4 C 0.0147(8) 0.3248(7) 0.5083(5) 0.044(4) Uani 1 1 d . . . . .
H4 H 0.0514 0.3146 0.4926 0.052 Uiso 1 1 calc R U . . .
C5 C -0.0641(12) 0.2800(10) 0.4975(7) 0.069(6) Uani 1 1 d . . . . .
H5 H -0.0813 0.2405 0.4739 0.083 Uiso 1 1 calc R U . . .
C6 C -0.1164(12) 0.2927(10) 0.5207(7) 0.077(7) Uani 1 1 d . . . . .
H6 H -0.1711 0.2602 0.5146 0.092 Uiso 1 1 calc R U . . .
C7 C -0.0910(9) 0.3526(11) 0.5531(7) 0.073(6) Uani 1 1 d . . . . .
H7 H -0.1280 0.3635 0.5680 0.088 Uiso 1 1 calc R U . . .
C8 C -0.0116(7) 0.3973(8) 0.5642(5) 0.046(3) Uani 1 1 d . . . . .
H8 H 0.0058 0.4372 0.5877 0.056 Uiso 1 1 calc R U . . .
C9 C 0.1244(6) 0.4017(6) 0.6317(3) 0.019(2) Uani 1 1 d . . . . .
H9 H 0.0816 0.3518 0.6229 0.023 Uiso 1 1 calc R U . . .
C10 C 0.1492(6) 0.4112(6) 0.6798(3) 0.018(2) Uani 1 1 d . . . . .
C11 C 0.1137(7) 0.3448(6) 0.7087(4) 0.029(2) Uani 1 1 d . . . . .
H11 H 0.0726 0.2965 0.6964 0.035 Uiso 1 1 calc R U . . .
C12 C 0.1370(7) 0.3479(6) 0.7546(4) 0.030(3) Uani 1 1 d . . . . .
H12 H 0.1117 0.3026 0.7742 0.036 Uiso 1 1 calc R U . . .
C13 C 0.2326(6) 0.4837(6) 0.7442(3) 0.019(2) Uani 1 1 d . . . . .
C14 C 0.1970(7) 0.4169(6) 0.7716(4) 0.025(2) Uani 1 1 d . . . . .
H14 H 0.2147 0.4190 0.8030 0.030 Uiso 1 1 calc R U . . .
C15 C 0.2084(5) 0.4837(6) 0.6978(3) 0.0146(19) Uani 1 1 d . . . . .
C16 C 0.3304(8) 0.5537(8) 0.8036(4) 0.041(3) Uani 1 1 d . . . . .
H16A H 0.3324 0.5049 0.8055 0.061 Uiso 1 1 calc R U . . .
H16B H 0.2990 0.5560 0.8298 0.061 Uiso 1 1 calc R U . . .
H16C H 0.3839 0.5990 0.8053 0.061 Uiso 1 1 calc R U . . .
C17 C 0.3286(6) 0.4915(5) 0.4790(3) 0.0155(19) Uani 1 1 d . . . . .
H17A H 0.3019 0.4787 0.5100 0.019 Uiso 1 1 calc R U . . .
H17B H 0.3821 0.4991 0.4832 0.019 Uiso 1 1 calc R U . . .
C18 C 0.2818(6) 0.4253(5) 0.4440(3) 0.0157(18) Uani 1 1 d . . . . .
H18 H 0.2270 0.4168 0.4432 0.019 Uiso 1 1 calc R U . . .
C19 C 0.2753(6) 0.3462(6) 0.4548(4) 0.022(2) Uani 1 1 d . . . . .
C20 C 0.3288(7) 0.3377(7) 0.4810(4) 0.029(3) Uani 1 1 d . . . . .
H20 H 0.3751 0.3828 0.4922 0.035 Uiso 1 1 calc R U . . .
C21 C 0.3153(8) 0.2630(8) 0.4912(5) 0.044(4) Uani 1 1 d . . . . .
H21 H 0.3510 0.2567 0.5108 0.053 Uiso 1 1 calc R U . . .
C22 C 0.2515(9) 0.1989(8) 0.4735(6) 0.049(4) Uani 1 1 d . . . . .
H22 H 0.2448 0.1483 0.4797 0.058 Uiso 1 1 calc R U . . .
C23 C 0.1976(8) 0.2043(7) 0.4475(5) 0.040(3) Uani 1 1 d . . . . .
H23 H 0.1528 0.1580 0.4362 0.048 Uiso 1 1 calc R U . . .
C24 C 0.2077(7) 0.2786(6) 0.4372(4) 0.033(3) Uani 1 1 d . . . . .
H24 H 0.1699 0.2835 0.4187 0.039 Uiso 1 1 calc R U . . .
C25 C 0.3408(5) 0.4288(5) 0.3669(3) 0.0176(19) Uani 1 1 d . . . . .
H25 H 0.3342 0.3786 0.3745 0.021 Uiso 1 1 calc R U . . .
C26 C 0.3735(6) 0.4609(5) 0.3217(3) 0.0156(19) Uani 1 1 d . . . . .
C27 C 0.4028(6) 0.4222(6) 0.2945(4) 0.021(2) Uani 1 1 d . . . . .
H27 H 0.4026 0.3769 0.3066 0.025 Uiso 1 1 calc R U . . .
C28 C 0.4322(6) 0.4497(6) 0.2501(3) 0.020(2) Uani 1 1 d . . . . .
H28 H 0.4524 0.4232 0.2316 0.024 Uiso 1 1 calc R U . . .
C29 C 0.4324(7) 0.5156(7) 0.2322(4) 0.026(2) Uani 1 1 d . . . . .
H29 H 0.4518 0.5336 0.2013 0.032 Uiso 1 1 calc R U . . .
C30 C 0.4046(6) 0.5551(6) 0.2590(3) 0.017(2) Uani 1 1 d . . . . .
C31 C 0.3722(5) 0.5278(5) 0.3037(3) 0.0126(18) Uani 1 1 d . . . . .
C32 C 0.4422(8) 0.6575(8) 0.2005(4) 0.036(3) Uani 1 1 d . . . . .
H32A H 0.4217 0.6186 0.1750 0.054 Uiso 1 1 calc R U . . .
H32B H 0.4988 0.6775 0.2042 0.054 Uiso 1 1 calc R U . . .
H32C H 0.4333 0.7012 0.1929 0.054 Uiso 1 1 calc R U . . .
O1W O 0.4445(13) 0.5113(13) 0.7155(6) 0.059(3) Uani 0.5 1 d D . P . .
C1W C 0.4713(18) 0.4977(19) 0.6731(8) 0.059(3) Uani 0.5 1 d D . P . .
O2W O 0.1709(13) 0.3829(13) 0.2860(7) 0.059(3) Uani 0.5 1 d D . P . .
C2W C 0.1277(18) 0.4212(18) 0.2884(10) 0.059(3) Uani 0.5 1 d D . P . .
O3W O 0.826(2) 0.824(2) 0.4243(12) 0.111(5) Uani 0.5 1 d . . P . .
O3W' O 0.804(2) 0.801(2) 0.3889(12) 0.111(5) Uani 0.5 1 d . . P . .
O4W O 1.0000 1.0000 0.4134(10) 0.111(5) Uani 1 3 d S T P . .
O6W O 0.470(2) 0.355(2) 0.5806(11) 0.111(5) Uani 0.5 1 d . . P . .
O5W O -0.284(3) 0.343(3) 0.5906(16) 0.111(5) Uani 0.3333 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Tb1 O4 2.282(6) 2_665 ?
Tb1 O4 2.282(6) . ?
Tb1 O4 2.282(6) 3_565 ?
Tb1 O1 2.310(6) 3_565 ?
Tb1 O1 2.310(6) . ?
Tb1 O1 2.310(6) 2_665 ?
Tb1 O8 2.688(11) . ?
Tb1 Mn2 3.4601(14) . ?
Tb1 Mn2 3.4602(14) 3_565 ?
Tb1 Mn2 3.4602(14) 2_665 ?
Mn1 O7 1.8908(14) . ?
Mn1 O2 1.901(6) . ?
Mn1 O1 1.901(6) . ?
Mn1 N1 1.987(7) . ?
Mn1 Cl1 2.644(3) 3_565 ?
Mn1 Cl1 2.670(3) . ?
Mn1 Na1 3.449(6) . ?
Mn2 O5 1.890(7) . ?
Mn2 O4 1.908(6) . ?
Mn2 O8 1.9336(17) . ?
Mn2 N2 1.979(7) . ?
Mn2 Cl2 2.594(3) 3_565 ?
Mn2 Cl2 2.639(3) . ?
Mn2 Na2 3.494(5) . ?
Cl1 Mn1 2.644(3) 2_665 ?
Cl2 Mn2 2.594(3) 2_665 ?
Na1 O2 2.312(7) 3_565 ?
Na1 O2 2.313(7) . ?
Na1 O2 2.313(7) 2_665 ?
Na1 O3 2.383(8) 3_565 ?
Na1 O3 2.383(8) 2_665 ?
Na1 O3 2.383(8) . ?
Na1 O7 2.812(12) . ?
Na1 Mn1 3.449(6) 3_565 ?
Na1 Mn1 3.449(6) 2_665 ?
Na2 O5 2.311(7) 3_565 ?
Na2 O5 2.311(7) 2_665 ?
Na2 O5 2.311(7) . ?
Na2 O6 2.362(8) 3_565 ?
Na2 O6 2.362(8) 2_665 ?
Na2 O6 2.362(8) . ?
Na2 Mn2 3.494(5) 3_565 ?
Na2 Mn2 3.494(5) 2_665 ?
O1 C1 1.419(11) . ?
O2 C15 1.316(11) . ?
O3 C13 1.392(13) . ?
O3 C16 1.449(13) . ?
O4 C17 1.426(11) . ?
O5 C31 1.345(11) . ?
O6 C30 1.379(12) . ?
O6 C32 1.449(12) . ?
O7 Mn1 1.8908(14) 3_565 ?
O7 Mn1 1.8908(14) 2_665 ?
O8 Mn2 1.9336(17) 3_565 ?
O8 Mn2 1.9336(18) 2_665 ?
N1 C9 1.299(12) . ?
N1 C2 1.478(11) . ?
N2 C25 1.271(12) . ?
N2 C18 1.500(11) . ?
C1 C2 1.531(13) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.519(13) . ?
C2 H2 1.0000 . ?
C3 C4 1.358(17) . ?
C3 C8 1.368(19) . ?
C4 C5 1.38(2) . ?
C4 H4 0.9500 . ?
C5 C6 1.34(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.38(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(19) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.430(13) . ?
C9 H9 0.9500 . ?
C10 C11 1.395(14) . ?
C10 C15 1.406(14) . ?
C11 C12 1.373(15) . ?
C11 H11 0.9500 . ?
C12 C14 1.363(16) . ?
C12 H12 0.9500 . ?
C13 C14 1.376(14) . ?
C13 C15 1.400(13) . ?
C14 H14 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.524(13) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C19 1.522(13) . ?
C18 H18 1.0000 . ?
C19 C20 1.364(15) . ?
C19 C24 1.416(16) . ?
C20 C21 1.382(16) . ?
C20 H20 0.9500 . ?
C21 C22 1.35(2) . ?
C21 H21 0.9500 . ?
C22 C23 1.33(2) . ?
C22 H22 0.9500 . ?
C23 C24 1.400(16) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.432(13) . ?
C25 H25 0.9500 . ?
C26 C27 1.391(13) . ?
C26 C31 1.418(13) . ?
C27 C28 1.380(14) . ?
C27 H27 0.9500 . ?
C28 C29 1.385(15) . ?
C28 H28 0.9500 . ?
C29 C30 1.380(14) . ?
C29 H29 0.9500 . ?
C30 C31 1.398(13) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
O1W C1W 1.390(14) . ?
O2W C2W 1.384(14) . ?
O3W O3W' 1.10(4) . ?
O5W O5W 1.53(7) 3_455 ?
O5W O5W 1.53(7) 2_565 ?

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
O4 Tb1 O4 103.16(19) 2_665 . ?
O4 Tb1 O4 103.16(19) 2_665 3_565 ?
O4 Tb1 O4 103.16(19) . 3_565 ?
O4 Tb1 O1 85.1(2) 2_665 3_565 ?
O4 Tb1 O1 170.1(2) . 3_565 ?
O4 Tb1 O1 80.0(2) 3_565 3_565 ?
O4 Tb1 O1 170.1(2) 2_665 . ?
O4 Tb1 O1 80.0(2) . . ?
O4 Tb1 O1 85.1(2) 3_565 . ?
O1 Tb1 O1 91.0(2) 3_565 . ?
O4 Tb1 O1 80.0(2) 2_665 2_665 ?
O4 Tb1 O1 85.1(2) . 2_665 ?
O4 Tb1 O1 170.1(2) 3_565 2_665 ?
O1 Tb1 O1 91.0(2) 3_565 2_665 ?
O1 Tb1 O1 91.0(2) . 2_665 ?
O4 Tb1 O8 64.78(16) 2_665 . ?
O4 Tb1 O8 64.78(16) . . ?
O4 Tb1 O8 64.78(16) 3_565 . ?
O1 Tb1 O8 124.57(15) 3_565 . ?
O1 Tb1 O8 124.58(16) . . ?
O1 Tb1 O8 124.57(16) 2_665 . ?
O4 Tb1 Mn2 84.10(16) 2_665 . ?
O4 Tb1 Mn2 30.99(16) . . ?
O4 Tb1 Mn2 84.14(16) 3_565 . ?
O1 Tb1 Mn2 158.21(16) 3_565 . ?
O1 Tb1 Mn2 102.50(16) . . ?
O1 Tb1 Mn2 105.66(15) 2_665 . ?
O8 Tb1 Mn2 33.79(2) . . ?
O4 Tb1 Mn2 84.13(16) 2_665 3_565 ?
O4 Tb1 Mn2 84.10(16) . 3_565 ?
O4 Tb1 Mn2 30.99(16) 3_565 3_565 ?
O1 Tb1 Mn2 102.50(16) 3_565 3_565 ?
O1 Tb1 Mn2 105.66(15) . 3_565 ?
O1 Tb1 Mn2 158.21(16) 2_665 3_565 ?
O8 Tb1 Mn2 33.79(2) . 3_565 ?
Mn2 Tb1 Mn2 57.59(4) . 3_565 ?
O4 Tb1 Mn2 30.99(16) 2_665 2_665 ?
O4 Tb1 Mn2 84.14(16) . 2_665 ?
O4 Tb1 Mn2 84.10(16) 3_565 2_665 ?
O1 Tb1 Mn2 105.66(16) 3_565 2_665 ?
O1 Tb1 Mn2 158.21(16) . 2_665 ?
O1 Tb1 Mn2 102.50(16) 2_665 2_665 ?
O8 Tb1 Mn2 33.79(2) . 2_665 ?
Mn2 Tb1 Mn2 57.59(4) . 2_665 ?
Mn2 Tb1 Mn2 57.59(4) 3_565 2_665 ?
O7 Mn1 O2 93.6(4) . . ?
O7 Mn1 O1 92.5(4) . . ?
O2 Mn1 O1 173.9(3) . . ?
O7 Mn1 N1 174.9(4) . . ?
O2 Mn1 N1 91.1(3) . . ?
O1 Mn1 N1 82.9(3) . . ?
O7 Mn1 Cl1 82.37(7) . 3_565 ?
O2 Mn1 Cl1 95.2(2) . 3_565 ?
O1 Mn1 Cl1 86.2(2) . 3_565 ?
N1 Mn1 Cl1 99.3(2) . 3_565 ?
O7 Mn1 Cl1 81.64(7) . . ?
O2 Mn1 Cl1 86.8(2) . . ?
O1 Mn1 Cl1 93.5(2) . . ?
N1 Mn1 Cl1 96.6(2) . . ?
Cl1 Mn1 Cl1 163.98(8) 3_565 . ?
O7 Mn1 Na1 54.6(3) . . ?
O2 Mn1 Na1 39.2(2) . . ?
O1 Mn1 Na1 146.9(2) . . ?
N1 Mn1 Na1 130.2(2) . . ?
Cl1 Mn1 Na1 86.00(6) 3_565 . ?
Cl1 Mn1 Na1 85.60(6) . . ?
O5 Mn2 O4 170.8(3) . . ?
O5 Mn2 O8 99.7(4) . . ?
O4 Mn2 O8 88.7(4) . . ?
O5 Mn2 N2 90.0(3) . . ?
O4 Mn2 N2 82.1(3) . . ?
O8 Mn2 N2 168.6(4) . . ?
O5 Mn2 Cl2 93.9(2) . 3_565 ?
O4 Mn2 Cl2 91.2(2) . 3_565 ?
O8 Mn2 Cl2 81.13(7) . 3_565 ?
N2 Mn2 Cl2 92.3(2) . 3_565 ?
O5 Mn2 Cl2 86.4(2) . . ?
O4 Mn2 Cl2 91.3(2) . . ?
O8 Mn2 Cl2 79.94(7) . . ?
N2 Mn2 Cl2 106.8(2) . . ?
Cl2 Mn2 Cl2 160.85(9) 3_565 . ?
O5 Mn2 Tb1 150.2(2) . . ?
O4 Mn2 Tb1 38.00(19) . . ?
O8 Mn2 Tb1 50.7(3) . . ?
N2 Mn2 Tb1 119.8(2) . . ?
Cl2 Mn2 Tb1 85.49(6) 3_565 . ?
Cl2 Mn2 Tb1 84.83(6) . . ?
O5 Mn2 Na2 37.8(2) . . ?
O4 Mn2 Na2 150.8(2) . . ?
O8 Mn2 Na2 62.1(3) . . ?
N2 Mn2 Na2 126.9(2) . . ?
Cl2 Mn2 Na2 84.61(6) 3_565 . ?
Cl2 Mn2 Na2 83.97(6) . . ?
Tb1 Mn2 Na2 112.79(7) . . ?
Mn1 Cl1 Mn1 76.01(8) 2_665 . ?
Mn2 Cl2 Mn2 79.12(9) 2_665 . ?
O2 Na1 O2 102.7(3) 3_565 . ?
O2 Na1 O2 102.7(3) 3_565 2_665 ?
O2 Na1 O2 102.7(3) . 2_665 ?
O2 Na1 O3 67.8(2) 3_565 3_565 ?
O2 Na1 O3 106.2(3) . 3_565 ?
O2 Na1 O3 150.9(3) 2_665 3_565 ?
O2 Na1 O3 106.2(3) 3_565 2_665 ?
O2 Na1 O3 150.9(3) . 2_665 ?
O2 Na1 O3 67.8(2) 2_665 2_665 ?
O3 Na1 O3 87.9(3) 3_565 2_665 ?
O2 Na1 O3 150.9(3) 3_565 . ?
O2 Na1 O3 67.8(2) . . ?
O2 Na1 O3 106.2(2) 2_665 . ?
O3 Na1 O3 87.9(3) 3_565 . ?
O3 Na1 O3 87.9(3) 2_665 . ?
O2 Na1 O7 64.4(2) 3_565 . ?
O2 Na1 O7 64.4(2) . . ?
O2 Na1 O7 64.4(2) 2_665 . ?
O3 Na1 O7 126.7(2) 3_565 . ?
O3 Na1 O7 126.7(2) 2_665 . ?
O3 Na1 O7 126.7(2) . . ?
O2 Na1 Mn1 31.31(18) 3_565 3_565 ?
O2 Na1 Mn1 85.1(2) . 3_565 ?
O2 Na1 Mn1 81.7(2) 2_665 3_565 ?
O3 Na1 Mn1 97.43(18) 3_565 3_565 ?
O3 Na1 Mn1 118.88(19) 2_665 3_565 ?
O3 Na1 Mn1 152.8(2) . 3_565 ?
O7 Na1 Mn1 33.22(6) . 3_565 ?
O2 Na1 Mn1 85.1(2) 3_565 2_665 ?
O2 Na1 Mn1 81.7(2) . 2_665 ?
O2 Na1 Mn1 31.31(18) 2_665 2_665 ?
O3 Na1 Mn1 152.8(2) 3_565 2_665 ?
O3 Na1 Mn1 97.43(18) 2_665 2_665 ?
O3 Na1 Mn1 118.88(19) . 2_665 ?
O7 Na1 Mn1 33.22(6) . 2_665 ?
Mn1 Na1 Mn1 56.65(10) 3_565 2_665 ?
O2 Na1 Mn1 81.7(2) 3_565 . ?
O2 Na1 Mn1 31.31(18) . . ?
O2 Na1 Mn1 85.1(2) 2_665 . ?
O3 Na1 Mn1 118.9(2) 3_565 . ?
O3 Na1 Mn1 152.8(2) 2_665 . ?
O3 Na1 Mn1 97.44(18) . . ?
O7 Na1 Mn1 33.22(6) . . ?
Mn1 Na1 Mn1 56.65(10) 3_565 . ?
Mn1 Na1 Mn1 56.65(10) 2_665 . ?
O5 Na2 O5 101.5(3) 3_565 2_665 ?
O5 Na2 O5 101.5(3) 3_565 . ?
O5 Na2 O5 101.5(3) 2_665 . ?
O5 Na2 O6 68.3(2) 3_565 3_565 ?
O5 Na2 O6 155.6(3) 2_665 3_565 ?
O5 Na2 O6 102.3(2) . 3_565 ?
O5 Na2 O6 102.3(2) 3_565 2_665 ?
O5 Na2 O6 68.3(2) 2_665 2_665 ?
O5 Na2 O6 155.6(3) . 2_665 ?
O6 Na2 O6 91.7(3) 3_565 2_665 ?
O5 Na2 O6 155.6(3) 3_565 . ?
O5 Na2 O6 102.3(2) 2_665 . ?
O5 Na2 O6 68.3(2) . . ?
O6 Na2 O6 91.7(3) 3_565 . ?
O6 Na2 O6 91.7(3) 2_665 . ?
O5 Na2 Mn2 30.07(18) 3_565 3_565 ?
O5 Na2 Mn2 81.1(2) 2_665 3_565 ?
O5 Na2 Mn2 84.1(2) . 3_565 ?
O6 Na2 Mn2 95.79(18) 3_565 3_565 ?
O6 Na2 Mn2 114.6(2) 2_665 3_565 ?
O6 Na2 Mn2 152.4(2) . 3_565 ?
O5 Na2 Mn2 84.1(2) 3_565 2_665 ?
O5 Na2 Mn2 30.07(18) 2_665 2_665 ?
O5 Na2 Mn2 81.1(2) . 2_665 ?
O6 Na2 Mn2 152.4(2) 3_565 2_665 ?
O6 Na2 Mn2 95.79(18) 2_665 2_665 ?
O6 Na2 Mn2 114.6(2) . 2_665 ?
Mn2 Na2 Mn2 56.98(10) 3_565 2_665 ?
O5 Na2 Mn2 81.1(2) 3_565 . ?
O5 Na2 Mn2 84.1(2) 2_665 . ?
O5 Na2 Mn2 30.07(18) . . ?
O6 Na2 Mn2 114.6(2) 3_565 . ?
O6 Na2 Mn2 152.4(2) 2_665 . ?
O6 Na2 Mn2 95.79(18) . . ?
Mn2 Na2 Mn2 56.98(10) 3_565 . ?
Mn2 Na2 Mn2 56.98(10) 2_665 . ?
C1 O1 Mn1 111.3(5) . . ?
C1 O1 Tb1 121.9(5) . . ?
Mn1 O1 Tb1 124.0(3) . . ?
C15 O2 Mn1 128.0(6) . . ?
C15 O2 Na1 120.6(6) . . ?
Mn1 O2 Na1 109.5(3) . . ?
C13 O3 C16 115.4(8) . . ?
C13 O3 Na1 117.3(6) . . ?
C16 O3 Na1 127.2(7) . . ?
C17 O4 Mn2 116.1(5) . . ?
C17 O4 Tb1 132.8(5) . . ?
Mn2 O4 Tb1 111.0(3) . . ?
C31 O5 Mn2 125.1(6) . . ?
C31 O5 Na2 119.4(6) . . ?
Mn2 O5 Na2 112.2(3) . . ?
C30 O6 C32 117.6(8) . . ?
C30 O6 Na2 118.4(6) . . ?
C32 O6 Na2 124.0(6) . . ?
Mn1 O7 Mn1 119.85(4) 3_565 . ?
Mn1 O7 Mn1 119.85(4) 3_565 2_665 ?
Mn1 O7 Mn1 119.85(4) . 2_665 ?
Mn1 O7 Na1 92.2(3) 3_565 . ?
Mn1 O7 Na1 92.2(3) . . ?
Mn1 O7 Na1 92.2(3) 2_665 . ?
Mn2 O8 Mn2 119.07(11) . 3_565 ?
Mn2 O8 Mn2 119.07(11) . 2_665 ?
Mn2 O8 Mn2 119.07(11) 3_565 2_665 ?
Mn2 O8 Tb1 95.6(3) . . ?
Mn2 O8 Tb1 95.6(3) 3_565 . ?
Mn2 O8 Tb1 95.6(3) 2_665 . ?
C9 N1 C2 120.3(8) . . ?
C9 N1 Mn1 125.6(7) . . ?
C2 N1 Mn1 113.8(6) . . ?
C25 N2 C18 125.0(7) . . ?
C25 N2 Mn2 125.8(6) . . ?
C18 N2 Mn2 109.2(5) . . ?
O1 C1 C2 109.6(7) . . ?
O1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
O1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N1 C2 C3 117.0(8) . . ?
N1 C2 C1 105.2(7) . . ?
C3 C2 C1 111.6(8) . . ?
N1 C2 H2 107.6 . . ?
C3 C2 H2 107.6 . . ?
C1 C2 H2 107.6 . . ?
C4 C3 C8 119.3(12) . . ?
C4 C3 C2 120.0(12) . . ?
C8 C3 C2 120.6(10) . . ?
C3 C4 C5 121.7(17) . . ?
C3 C4 H4 119.2 . . ?
C5 C4 H4 119.2 . . ?
C6 C5 C4 119.3(17) . . ?
C6 C5 H5 120.3 . . ?
C4 C5 H5 120.3 . . ?
C5 C6 C7 120.2(16) . . ?
C5 C6 H6 119.9 . . ?
C7 C6 H6 119.9 . . ?
C6 C7 C8 120.3(18) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C3 C8 C7 119.1(15) . . ?
C3 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
N1 C9 C10 125.9(9) . . ?
N1 C9 H9 117.0 . . ?
C10 C9 H9 117.0 . . ?
C11 C10 C15 120.2(9) . . ?
C11 C10 C9 117.5(9) . . ?
C15 C10 C9 122.3(9) . . ?
C12 C11 C10 121.1(10) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C14 C12 C11 118.9(10) . . ?
C14 C12 H12 120.5 . . ?
C11 C12 H12 120.5 . . ?
C14 C13 O3 124.0(9) . . ?
C14 C13 C15 121.5(10) . . ?
O3 C13 C15 114.5(9) . . ?
C12 C14 C13 121.3(10) . . ?
C12 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
O2 C15 C13 119.1(9) . . ?
O2 C15 C10 124.1(9) . . ?
C13 C15 C10 116.8(9) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O4 C17 C18 107.1(7) . . ?
O4 C17 H17A 110.3 . . ?
C18 C17 H17A 110.3 . . ?
O4 C17 H17B 110.3 . . ?
C18 C17 H17B 110.3 . . ?
H17A C17 H17B 108.5 . . ?
N2 C18 C19 115.2(7) . . ?
N2 C18 C17 102.9(7) . . ?
C19 C18 C17 116.4(8) . . ?
N2 C18 H18 107.3 . . ?
C19 C18 H18 107.3 . . ?
C17 C18 H18 107.3 . . ?
C20 C19 C24 119.7(10) . . ?
C20 C19 C18 123.8(10) . . ?
C24 C19 C18 116.5(10) . . ?
C19 C20 C21 119.5(12) . . ?
C19 C20 H20 120.3 . . ?
C21 C20 H20 120.3 . . ?
C22 C21 C20 120.3(14) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 122.3(13) . . ?
C23 C22 H22 118.9 . . ?
C21 C22 H22 118.9 . . ?
C22 C23 C24 119.5(13) . . ?
C22 C23 H23 120.2 . . ?
C24 C23 H23 120.2 . . ?
C23 C24 C19 118.6(12) . . ?
C23 C24 H24 120.7 . . ?
C19 C24 H24 120.7 . . ?
N2 C25 C26 125.7(8) . . ?
N2 C25 H25 117.2 . . ?
C26 C25 H25 117.2 . . ?
C27 C26 C31 120.3(9) . . ?
C27 C26 C25 118.3(9) . . ?
C31 C26 C25 121.3(8) . . ?
C28 C27 C26 120.1(9) . . ?
C28 C27 H27 120.0 . . ?
C26 C27 H27 120.0 . . ?
C27 C28 C29 120.3(9) . . ?
C27 C28 H28 119.9 . . ?
C29 C28 H28 119.9 . . ?
C30 C29 C28 120.2(10) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
O6 C30 C29 124.2(9) . . ?
O6 C30 C31 114.7(8) . . ?
C29 C30 C31 121.1(9) . . ?
O5 C31 C30 118.8(9) . . ?
O5 C31 C26 123.3(8) . . ?
C30 C31 C26 117.9(8) . . ?
O6 C32 H32A 109.5 . . ?
O6 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
O6 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O5W O5W O5W 59.998(14) 3_455 2_565 ?

_refine_diff_density_max         1.846
_refine_diff_density_min         -0.579
_refine_diff_density_rms         0.143



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: methanol/ACN/diethylether'
_exptl_crystal_preparation       'Magnetic properties'
