# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_1_plus_RT
_database_code_depnum_ccdc_archive 'CCDC 1854369'
_audit_update_record             
;
2018-07-07 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 I8 Mn2 N16 Nb'
_chemical_formula_weight         2050.88

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_H-M_alt        'I 41'
_space_group_name_Hall           'I 4bw'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'

_cell_length_a                   20.8730(7)
_cell_length_b                   20.8730(7)
_cell_length_c                   14.2157(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6193.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    43746
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.46

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_F_000             3788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    4.617
_shelx_estimated_absorpt_T_min   0.416
_shelx_estimated_absorpt_T_max   0.444
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_T_max  0.785
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            7092
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.086
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_full        25.242
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7084
_reflns_number_gt                6993
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 4-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)+(0.0534P)²+26.3894P] 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 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7084
_refine_ls_number_parameters     342
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1144
_refine_ls_wR_factor_gt          0.1141
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.002

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
Nb1 Nb 0.5000 0.5000 0.06897(14) 0.0103(2) Uani 1 2 d S T P . .
C1 C 0.4002(8) 0.5192(7) 0.0257(12) 0.027(3) Uani 1 1 d . U . . .
C2 C 0.4856(5) 0.6027(5) 0.1213(9) 0.009(2) Uani 1 1 d . . . . .
C3 C 0.4848(6) 0.4361(6) -0.0573(9) 0.014(3) Uani 1 1 d . U . . .
C4 C 0.4359(10) 0.4898(9) 0.1954(15) 0.044(5) Uani 1 1 d . . . . .
N1 N 0.3485(7) 0.5258(7) -0.0073(12) 0.035(3) Uani 1 1 d . U . . .
N2 N 0.4784(6) 0.6516(6) 0.1410(9) 0.025(3) Uani 1 1 d . U . . .
N3 N 0.4744(9) 0.4043(7) -0.1240(10) 0.040(4) Uani 1 1 d . . . . .
N4 N 0.3998(8) 0.4809(9) 0.2537(12) 0.047(5) Uani 1 1 d . . . . .
Mn1 Mn 0.25037(14) 0.52127(8) -0.0567(2) 0.0218(3) Uani 1 1 d . . . . .
N11 N 0.2138(7) 0.5137(6) 0.0977(10) 0.026(3) Uani 1 1 d . U . . .
C12 C 0.2524(9) 0.4964(13) 0.1603(12) 0.041(4) Uani 1 1 d . U . . .
H12 H 0.2951 0.4895 0.1449 0.049 Uiso 1 1 calc R U . . .
C13 C 0.2298(10) 0.4863(10) 0.2631(13) 0.043(4) Uani 1 1 d . U . . .
H13 H 0.2581 0.4732 0.3099 0.051 Uiso 1 1 calc R U . . .
C14 C 0.1713(9) 0.4967(11) 0.2806(11) 0.041(3) Uani 1 1 d . U . . .
C15 C 0.1295(11) 0.5150(13) 0.2056(15) 0.060(7) Uani 1 1 d . U . . .
H15 H 0.0860 0.5198 0.2173 0.072 Uiso 1 1 calc R U . . .
C16 C 0.1507(10) 0.5246(10) 0.1246(15) 0.044(5) Uani 1 1 d . . . . .
H16 H 0.1225 0.5402 0.0795 0.053 Uiso 1 1 calc R U . . .
I17 I 0.13848(6) 0.48633(6) 0.41895(6) 0.0420(3) Uani 1 1 d . . . . .
N21 N 0.2897(6) 0.5176(7) -0.2075(11) 0.034(4) Uani 1 1 d . U . . .
C22 C 0.2487(7) 0.4974(12) -0.2812(14) 0.038(4) Uani 1 1 d . . . . .
H22 H 0.2056 0.4912 -0.2672 0.046 Uiso 1 1 calc R U . . .
C23 C 0.2664(8) 0.4873(12) -0.3630(12) 0.047(6) Uani 1 1 d . U . . .
H23 H 0.2364 0.4755 -0.4081 0.056 Uiso 1 1 calc R U . . .
C24 C 0.3329(8) 0.4938(11) -0.3896(14) 0.043(4) Uani 1 1 d . U . . .
C25 C 0.3753(8) 0.5094(9) -0.3253(16) 0.036(4) Uani 1 1 d . U . . .
H25 H 0.4183 0.5139 -0.3408 0.043 Uiso 1 1 calc R U . . .
C26 C 0.3527(8) 0.5198(10) -0.2261(14) 0.040(5) Uani 1 1 d . U . . .
H26 H 0.3820 0.5277 -0.1782 0.048 Uiso 1 1 calc R U . . .
I27 I 0.36392(6) 0.47554(6) -0.52766(7) 0.0416(3) Uani 1 1 d . . . . .
N31 N 0.2459(10) 0.6320(7) -0.0551(16) 0.042(3) Uani 1 1 d . . . . .
C32 C 0.1903(11) 0.6626(9) -0.0568(13) 0.045(5) Uani 1 1 d . . . . .
H32 H 0.1522 0.6396 -0.0533 0.054 Uiso 1 1 calc R U . . .
C33 C 0.1889(19) 0.7298(11) -0.064(2) 0.091(11) Uani 1 1 d . . . . .
H33 H 0.1495 0.7494 -0.0742 0.110 Uiso 1 1 calc R U . . .
C34 C 0.2372(15) 0.7652(8) -0.0576(19) 0.066(8) Uani 1 1 d . . . . .
C35 C 0.2994(15) 0.7331(10) -0.0559(15) 0.062(7) Uani 1 1 d . . . . .
H35 H 0.3380 0.7553 -0.0580 0.074 Uiso 1 1 calc R U . . .
C36 C 0.2962(11) 0.6675(11) -0.0510(16) 0.053(6) Uani 1 1 d . . . . .
H36 H 0.3350 0.6461 -0.0438 0.063 Uiso 1 1 calc R U . . .
I37 I 0.2331(2) 0.86457(7) -0.0492(2) 0.1427(16) Uani 1 1 d . . . . .
N41 N 0.2544(9) 0.4100(5) -0.0578(15) 0.038(3) Uani 1 1 d . . . . .
C42 C 0.3142(11) 0.3796(10) -0.066(2) 0.064(6) Uani 1 1 d . U . . .
H42 H 0.3515 0.4039 -0.0683 0.077 Uiso 1 1 calc R U . . .
C43 C 0.3172(14) 0.3169(10) -0.0721(15) 0.069(6) Uani 1 1 d . U . . .
H43 H 0.3576 0.2994 -0.0818 0.082 Uiso 1 1 calc R U . . .
C44 C 0.2701(11) 0.2765(9) -0.0655(15) 0.055(5) Uani 1 1 d . . . . .
C45 C 0.2107(18) 0.3055(11) -0.064(2) 0.086(10) Uani 1 1 d . . . . .
H45 H 0.1735 0.2813 -0.0705 0.103 Uiso 1 1 calc R U . . .
C46 C 0.2073(10) 0.3764(8) -0.0511(14) 0.045(5) Uani 1 1 d . . . . .
H46 H 0.1680 0.3952 -0.0376 0.054 Uiso 1 1 calc R U . . .
I47 I 0.27966(14) 0.17934(7) -0.07388(16) 0.1027(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 C1 2.208(17) . ?
Nb1 C1 2.208(17) 2_665 ?
Nb1 C4 2.25(2) . ?
Nb1 C4 2.25(2) 2_665 ?
Nb1 C3 2.258(13) . ?
Nb1 C3 2.258(13) 2_665 ?
Nb1 C2 2.289(12) . ?
Nb1 C2 2.289(12) 2_665 ?
C1 N1 1.18(2) . ?
C2 N2 1.069(17) . ?
C3 N3 1.18(2) . ?
C4 N4 1.13(3) . ?
N1 Mn1 2.168(15) . ?
N2 Mn1 2.192(13) 3_655 ?
Mn1 N2 2.192(13) 8_454 ?
Mn1 N21 2.297(15) . ?
Mn1 N31 2.313(14) . ?
Mn1 N11 2.328(14) . ?
Mn1 N41 2.324(10) . ?
N11 C12 1.25(2) . ?
N11 C16 1.39(2) . ?
C12 C13 1.55(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.27(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.43(3) . ?
C14 I17 2.094(16) . ?
C15 C16 1.25(3) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
N21 C26 1.34(2) . ?
N21 C22 1.42(2) . ?
C22 C23 1.24(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.45(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.31(3) . ?
C24 I27 2.10(2) . ?
C25 C26 1.50(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
N31 C36 1.29(3) . ?
N31 C32 1.33(3) . ?
C32 C33 1.41(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.25(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.46(4) . ?
C34 I37 2.079(17) . ?
C35 C36 1.37(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N41 C46 1.21(3) . ?
N41 C42 1.40(3) . ?
C42 C43 1.31(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.30(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.38(4) . ?
C44 I47 2.04(2) . ?
C45 C46 1.49(3) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Nb1 C1 147.6(9) . 2_665 ?
C1 Nb1 C4 71.3(7) . . ?
C1 Nb1 C4 140.0(6) 2_665 . ?
C1 Nb1 C4 140.0(6) . 2_665 ?
C1 Nb1 C4 71.3(7) 2_665 2_665 ?
C4 Nb1 C4 74.1(11) . 2_665 ?
C1 Nb1 C3 75.7(5) . . ?
C1 Nb1 C3 78.7(6) 2_665 . ?
C4 Nb1 C3 119.6(5) . . ?
C4 Nb1 C3 140.7(4) 2_665 . ?
C1 Nb1 C3 78.7(6) . 2_665 ?
C1 Nb1 C3 75.7(5) 2_665 2_665 ?
C4 Nb1 C3 140.7(4) . 2_665 ?
C4 Nb1 C3 119.6(5) 2_665 2_665 ?
C3 Nb1 C3 74.7(7) . 2_665 ?
C1 Nb1 C2 78.3(4) . . ?
C1 Nb1 C2 112.6(4) 2_665 . ?
C4 Nb1 C2 75.6(6) . . ?
C4 Nb1 C2 74.3(5) 2_665 . ?
C3 Nb1 C2 142.4(5) . . ?
C3 Nb1 C2 74.0(5) 2_665 . ?
C1 Nb1 C2 112.6(4) . 2_665 ?
C1 Nb1 C2 78.3(4) 2_665 2_665 ?
C4 Nb1 C2 74.3(5) . 2_665 ?
C4 Nb1 C2 75.6(6) 2_665 2_665 ?
C3 Nb1 C2 74.0(5) . 2_665 ?
C3 Nb1 C2 142.4(5) 2_665 2_665 ?
C2 Nb1 C2 142.1(6) . 2_665 ?
N1 C1 Nb1 172.2(15) . . ?
N2 C2 Nb1 176.2(11) . . ?
N3 C3 Nb1 177.1(13) . . ?
N4 C4 Nb1 173(2) . . ?
C1 N1 Mn1 169.8(13) . . ?
C2 N2 Mn1 170.6(12) . 3_655 ?
N1 Mn1 N2 177.2(4) . 8_454 ?
N1 Mn1 N21 88.1(6) . . ?
N2 Mn1 N21 91.1(5) 8_454 . ?
N1 Mn1 N31 89.5(6) . . ?
N2 Mn1 N31 87.8(6) 8_454 . ?
N21 Mn1 N31 93.3(7) . . ?
N1 Mn1 N11 90.4(6) . . ?
N2 Mn1 N11 90.7(5) 8_454 . ?
N21 Mn1 N11 173.9(4) . . ?
N31 Mn1 N11 92.6(6) . . ?
N1 Mn1 N41 90.6(6) . . ?
N2 Mn1 N41 92.0(6) 8_454 . ?
N21 Mn1 N41 87.0(7) . . ?
N31 Mn1 N41 179.7(9) . . ?
N11 Mn1 N41 87.1(6) . . ?
C12 N11 C16 117.4(16) . . ?
C12 N11 Mn1 118.6(12) . . ?
C16 N11 Mn1 124.0(12) . . ?
N11 C12 C13 120.9(16) . . ?
N11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C14 C13 C12 117.1(17) . . ?
C14 C13 H13 121.5 . . ?
C12 C13 H13 121.4 . . ?
C13 C14 C15 119.2(17) . . ?
C13 C14 I17 118.9(14) . . ?
C15 C14 I17 121.9(15) . . ?
C16 C15 C14 121(2) . . ?
C16 C15 H15 119.5 . . ?
C14 C15 H15 119.5 . . ?
C15 C16 N11 124(2) . . ?
C15 C16 H16 117.9 . . ?
N11 C16 H16 117.9 . . ?
C26 N21 C22 117.1(15) . . ?
C26 N21 Mn1 122.2(12) . . ?
C22 N21 Mn1 119.0(10) . . ?
C23 C22 N21 124.4(15) . . ?
C23 C22 H22 117.8 . . ?
N21 C22 H22 117.8 . . ?
C22 C23 C24 121.1(17) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C25 C24 C23 119.2(18) . . ?
C25 C24 I27 119.2(12) . . ?
C23 C24 I27 121.6(14) . . ?
C24 C25 C26 118.6(15) . . ?
C24 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
N21 C26 C25 119.1(16) . . ?
N21 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C36 N31 C32 116.0(16) . . ?
C36 N31 Mn1 122.9(16) . . ?
C32 N31 Mn1 121.1(15) . . ?
N31 C32 C33 120(2) . . ?
N31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C34 C33 C32 124(3) . . ?
C34 C33 H33 117.7 . . ?
C32 C33 H33 117.8 . . ?
C33 C34 C35 116.5(17) . . ?
C33 C34 I37 124(2) . . ?
C35 C34 I37 120(2) . . ?
C36 C35 C34 114(2) . . ?
C36 C35 H35 122.8 . . ?
C34 C35 H35 122.8 . . ?
N31 C36 C35 128(2) . . ?
N31 C36 H36 116.1 . . ?
C35 C36 H36 116.1 . . ?
C46 N41 C42 117.7(16) . . ?
C46 N41 Mn1 123.3(15) . . ?
C42 N41 Mn1 119.0(13) . . ?
C43 C42 N41 120(2) . . ?
C43 C42 H42 120.1 . . ?
N41 C42 H42 120.1 . . ?
C44 C43 C42 127(3) . . ?
C44 C43 H43 116.3 . . ?
C42 C43 H43 116.3 . . ?
C43 C44 C45 113.4(19) . . ?
C43 C44 I47 124.5(18) . . ?
C45 C44 I47 121.6(15) . . ?
C44 C45 C46 119(2) . . ?
C44 C45 H45 120.7 . . ?
C46 C45 H45 120.7 . . ?
N41 C46 C45 122(2) . . ?
N41 C46 H46 119.1 . . ?
C45 C46 H46 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 N11 C12 C13 1(3) . . . . ?
Mn1 N11 C12 C13 -176.1(15) . . . . ?
N11 C12 C13 C14 0(3) . . . . ?
C12 C13 C14 C15 2(3) . . . . ?
C12 C13 C14 I17 -178.4(15) . . . . ?
C13 C14 C15 C16 -5(4) . . . . ?
I17 C14 C15 C16 176(2) . . . . ?
C14 C15 C16 N11 6(4) . . . . ?
C12 N11 C16 C15 -4(3) . . . . ?
Mn1 N11 C16 C15 173(2) . . . . ?
C26 N21 C22 C23 -7(3) . . . . ?
Mn1 N21 C22 C23 -172(2) . . . . ?
N21 C22 C23 C24 2(4) . . . . ?
C22 C23 C24 C25 1(4) . . . . ?
C22 C23 C24 I27 179(2) . . . . ?
C23 C24 C25 C26 0(3) . . . . ?
I27 C24 C25 C26 -177.7(15) . . . . ?
C22 N21 C26 C25 8(3) . . . . ?
Mn1 N21 C26 C25 172.8(13) . . . . ?
C24 C25 C26 N21 -5(3) . . . . ?
C36 N31 C32 C33 7(4) . . . . ?
Mn1 N31 C32 C33 -175(2) . . . . ?
N31 C32 C33 C34 -9(5) . . . . ?
C32 C33 C34 C35 9(5) . . . . ?
C32 C33 C34 I37 -171(2) . . . . ?
C33 C34 C35 C36 -7(4) . . . . ?
I37 C34 C35 C36 172.9(18) . . . . ?
C32 N31 C36 C35 -6(4) . . . . ?
Mn1 N31 C36 C35 175.3(19) . . . . ?
C34 C35 C36 N31 6(4) . . . . ?
C46 N41 C42 C43 3(4) . . . . ?
Mn1 N41 C42 C43 -177(2) . . . . ?
N41 C42 C43 C44 -4(4) . . . . ?
C42 C43 C44 C45 8(4) . . . . ?
C42 C43 C44 I47 -179(2) . . . . ?
C43 C44 C45 C46 -12(4) . . . . ?
I47 C44 C45 C46 175.9(18) . . . . ?
C42 N41 C46 C45 -8(4) . . . . ?
Mn1 N41 C46 C45 172(2) . . . . ?
C44 C45 C46 N41 12(4) . . . . ?

_refine_diff_density_max         2.131
_refine_diff_density_min         -1.657
_refine_diff_density_rms         0.150


_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_1_minus_RT
_database_code_depnum_ccdc_archive 'CCDC 1854373'
_audit_update_record             
;
2018-07-07 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 I8 Mn2 N16 Nb'
_chemical_formula_weight         2050.88

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_H-M_alt        'I 41'
_space_group_name_Hall           'I 4bw'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'

_cell_length_a                   20.8811(9)
_cell_length_b                   20.8811(9)
_cell_length_c                   14.2190(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6199.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    43344
_cell_measurement_theta_min      3.09
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.197
_exptl_crystal_F_000             3788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    4.613
_shelx_estimated_absorpt_T_min   0.417
_shelx_estimated_absorpt_T_max   0.459
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.155
_exptl_absorpt_correction_T_max  0.158
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            47965
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.085
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_full        25.242
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6964
_reflns_number_gt                6834
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 4-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)+(0.0625P)²+29.9208P] 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 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6964
_refine_ls_number_parameters     342
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0445
_refine_ls_wR_factor_ref         0.1099
_refine_ls_wR_factor_gt          0.1094
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.088
_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
Nb1 Nb 0.5000 0.0000 0.93074(14) 0.01119(19) Uani 1 2 d S T P . .
C1 C 0.6005(10) -0.0192(7) 0.9757(12) 0.035(4) Uani 1 1 d . . . . .
C2 C 0.4856(6) 0.1018(5) 0.8799(9) 0.014(3) Uani 1 1 d . . . . .
C3 C 0.5158(8) 0.0650(7) 1.0588(12) 0.029(4) Uani 1 1 d . . . . .
C4 C 0.5638(8) 0.0112(8) 0.8047(11) 0.032(4) Uani 1 1 d . U . . .
N1 N 0.6521(5) -0.0250(6) 1.0068(11) 0.031(3) Uani 1 1 d . . . . .
N2 N 0.4783(7) 0.1518(7) 0.8593(9) 0.037(4) Uani 1 1 d . . . . .
N3 N 0.5252(9) 0.0963(7) 1.1234(11) 0.044(4) Uani 1 1 d . . . . .
N4 N 0.5994(8) 0.0192(9) 0.7452(11) 0.049(5) Uani 1 1 d . U . . .
Mn1 Mn 0.74933(13) -0.02117(8) 1.0570(2) 0.0227(3) Uani 1 1 d . . . . .
N11 N 0.7846(7) -0.0138(6) 0.9026(10) 0.030(3) Uani 1 1 d . U . . .
C12 C 0.8496(9) -0.0235(9) 0.8768(15) 0.039(4) Uani 1 1 d . . . . .
H12 H 0.8773 -0.0392 0.9224 0.047 Uiso 1 1 calc R U . . .
C13 C 0.8730(10) -0.0120(11) 0.7943(17) 0.053(6) Uani 1 1 d . U . . .
H13 H 0.9168 -0.0136 0.7830 0.064 Uiso 1 1 calc R U . . .
C14 C 0.8277(10) 0.0037(9) 0.7201(10) 0.040(4) Uani 1 1 d . U . . .
C15 C 0.7701(7) 0.0139(9) 0.7391(11) 0.036(4) Uani 1 1 d . U . . .
H15 H 0.7416 0.0270 0.6926 0.044 Uiso 1 1 calc R U . . .
C16 C 0.7481(9) 0.0046(13) 0.8387(10) 0.045(4) Uani 1 1 d . U . . .
H16 H 0.7054 0.0129 0.8532 0.054 Uiso 1 1 calc R U . . .
I17 I 0.86151(6) 0.01340(6) 0.58103(6) 0.0428(3) Uani 1 1 d . . . . .
N21 N 0.7083(6) -0.0170(7) 1.2082(9) 0.030(3) Uani 1 1 d . . . . .
C22 C 0.7513(7) 0.0011(11) 1.2811(15) 0.040(4) Uani 1 1 d . . . . .
H22 H 0.7943 0.0057 1.2657 0.048 Uiso 1 1 calc R U . . .
C23 C 0.7352(10) 0.0114(13) 1.3645(15) 0.057(7) Uani 1 1 d . . . . .
H23 H 0.7652 0.0225 1.4099 0.069 Uiso 1 1 calc R U . . .
C24 C 0.6661(7) 0.0049(12) 1.3882(15) 0.048(5) Uani 1 1 d . . . . .
C25 C 0.6262(8) -0.0110(12) 1.3263(15) 0.051(6) Uani 1 1 d . . . . .
H25 H 0.5834 -0.0170 1.3419 0.061 Uiso 1 1 calc R U . . .
C26 C 0.6482(10) -0.0203(11) 1.2274(13) 0.048(6) Uani 1 1 d . . . . .
H26 H 0.6187 -0.0284 1.1800 0.057 Uiso 1 1 calc R U . . .
I27 I 0.63612(6) 0.02454(6) 1.52764(6) 0.0426(3) Uani 1 1 d . . . . .
N31 N 0.7569(7) -0.1314(7) 1.0538(14) 0.038(3) Uani 1 1 d . . . . .
C32 C 0.8095(11) -0.1631(9) 1.0568(16) 0.051(5) Uani 1 1 d . . . . .
H32 H 0.8479 -0.1406 1.0550 0.062 Uiso 1 1 calc R U . . .
C33 C 0.812(2) -0.2294(11) 1.063(2) 0.107(14) Uani 1 1 d . . . . .
H33 H 0.8514 -0.2488 1.0706 0.128 Uiso 1 1 calc R U . . .
C34 C 0.7619(15) -0.2657(9) 1.0583(18) 0.069(8) Uani 1 1 d . . . . .
C35 C 0.7003(13) -0.2335(10) 1.0538(14) 0.058(6) Uani 1 1 d . . . . .
H35 H 0.6616 -0.2555 1.0524 0.070 Uiso 1 1 calc R U . . .
C36 C 0.7042(11) -0.1683(11) 1.0516(14) 0.051(5) Uani 1 1 d . . . . .
H36 H 0.6653 -0.1466 1.0482 0.062 Uiso 1 1 calc R U . . .
I37 I 0.76853(19) -0.36444(7) 1.0493(2) 0.1345(15) Uani 1 1 d . . . . .
N41 N 0.7463(10) 0.0900(5) 1.0564(15) 0.042(3) Uani 1 1 d . . . . .
I47 I 0.72022(14) 0.32080(7) 1.07408(16) 0.1033(8) Uani 1 1 d . . . . .
C46 C 0.6852(12) 0.1200(10) 1.066(2) 0.063(7) Uani 1 1 d . . . . .
H46 H 0.6480 0.0956 1.0689 0.076 Uiso 1 1 calc R U . . .
C42 C 0.7937(11) 0.1229(8) 1.0515(17) 0.054(5) Uani 1 1 d . . . . .
H42 H 0.8333 0.1040 1.0405 0.064 Uiso 1 1 calc R U . . .
C44 C 0.7305(12) 0.2237(11) 1.0659(17) 0.065(6) Uani 1 1 d . . . . .
C43 C 0.7888(14) 0.1940(12) 1.063(2) 0.076(8) Uani 1 1 d . . . . .
H43 H 0.8259 0.2183 1.0685 0.091 Uiso 1 1 calc R U . . .
C45 C 0.6825(13) 0.1843(11) 1.0692(16) 0.071(7) Uani 1 1 d . . . . .
H45 H 0.6420 0.2024 1.0746 0.085 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
Nb1 C1 2.230(19) 2_655 ?
Nb1 C1 2.230(19) . ?
Nb1 C4 2.245(16) 2_655 ?
Nb1 C4 2.245(16) . ?
Nb1 C2 2.266(12) 2_655 ?
Nb1 C2 2.266(12) . ?
Nb1 C3 2.295(16) 2_655 ?
Nb1 C3 2.295(16) . ?
C1 N1 1.17(2) . ?
C2 N2 1.094(19) . ?
C3 N3 1.14(2) . ?
C4 N4 1.14(2) . ?
N1 Mn1 2.154(12) . ?
N2 Mn1 2.195(15) 8_554 ?
Mn1 N2 2.195(15) 3_645 ?
Mn1 N31 2.307(14) . ?
Mn1 N21 2.316(12) . ?
Mn1 N11 2.321(15) . ?
Mn1 N41 2.323(10) . ?
N11 C16 1.25(2) . ?
N11 C12 1.42(2) . ?
C12 C13 1.29(3) . ?
C12 H12 0.9300 . ?
C13 C14 1.45(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.25(3) . ?
C14 I17 2.109(16) . ?
C15 C16 1.50(2) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
N21 C26 1.29(2) . ?
N21 C22 1.42(2) . ?
C22 C23 1.25(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.49(2) . ?
C23 H23 0.9300 . ?
C24 C25 1.26(3) . ?
C24 I27 2.12(2) . ?
C25 C26 1.49(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
N31 C32 1.28(2) . ?
N31 C36 1.34(3) . ?
C32 C33 1.39(3) . ?
C32 H32 0.9300 . ?
C33 C34 1.29(5) . ?
C33 H33 0.9300 . ?
C34 C35 1.45(4) . ?
C34 I37 2.071(18) . ?
C35 C36 1.36(3) . ?
C35 H35 0.9300 . ?
C36 H36 0.9300 . ?
N41 C42 1.21(3) . ?
N41 C46 1.43(3) . ?
I47 C44 2.04(2) . ?
C46 C45 1.34(3) . ?
C46 H46 0.9300 . ?
C42 C43 1.50(3) . ?
C42 H42 0.9300 . ?
C44 C45 1.30(4) . ?
C44 C43 1.37(4) . ?
C43 H43 0.9300 . ?
C45 H45 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Nb1 C1 146.7(9) 2_655 . ?
C1 Nb1 C4 71.9(6) 2_655 2_655 ?
C1 Nb1 C4 140.2(6) . 2_655 ?
C1 Nb1 C4 140.2(6) 2_655 . ?
C1 Nb1 C4 71.9(6) . . ?
C4 Nb1 C4 74.0(9) 2_655 . ?
C1 Nb1 C2 112.7(4) 2_655 2_655 ?
C1 Nb1 C2 78.3(4) . 2_655 ?
C4 Nb1 C2 74.1(5) 2_655 2_655 ?
C4 Nb1 C2 76.4(5) . 2_655 ?
C1 Nb1 C2 78.3(4) 2_655 . ?
C1 Nb1 C2 112.7(4) . . ?
C4 Nb1 C2 76.4(5) 2_655 . ?
C4 Nb1 C2 74.1(5) . . ?
C2 Nb1 C2 142.8(6) 2_655 . ?
C1 Nb1 C3 75.1(6) 2_655 2_655 ?
C1 Nb1 C3 78.5(6) . 2_655 ?
C4 Nb1 C3 119.1(5) 2_655 2_655 ?
C4 Nb1 C3 141.3(4) . 2_655 ?
C2 Nb1 C3 73.6(5) 2_655 2_655 ?
C2 Nb1 C3 142.1(5) . 2_655 ?
C1 Nb1 C3 78.5(6) 2_655 . ?
C1 Nb1 C3 75.1(6) . . ?
C4 Nb1 C3 141.3(4) 2_655 . ?
C4 Nb1 C3 119.1(5) . . ?
C2 Nb1 C3 142.1(5) 2_655 . ?
C2 Nb1 C3 73.6(5) . . ?
C3 Nb1 C3 75.0(8) 2_655 . ?
N1 C1 Nb1 173.1(15) . . ?
N2 C2 Nb1 177.0(11) . . ?
N3 C3 Nb1 178.0(15) . . ?
N4 C4 Nb1 174.7(17) . . ?
C1 N1 Mn1 171.5(12) . . ?
C2 N2 Mn1 170.8(12) . 8_554 ?
N1 Mn1 N2 177.6(4) . 3_645 ?
N1 Mn1 N31 91.2(5) . . ?
N2 Mn1 N31 86.4(6) 3_645 . ?
N1 Mn1 N21 87.8(5) . . ?
N2 Mn1 N21 91.9(5) 3_645 . ?
N31 Mn1 N21 94.6(6) . . ?
N1 Mn1 N11 89.3(5) . . ?
N2 Mn1 N11 91.3(5) 3_645 . ?
N31 Mn1 N11 91.4(6) . . ?
N21 Mn1 N11 173.3(5) . . ?
N1 Mn1 N41 90.6(6) . . ?
N2 Mn1 N41 91.8(6) 3_645 . ?
N31 Mn1 N41 177.2(7) . . ?
N21 Mn1 N41 87.5(7) . . ?
N11 Mn1 N41 86.5(7) . . ?
C16 N11 C12 116.0(16) . . ?
C16 N11 Mn1 121.1(12) . . ?
C12 N11 Mn1 122.6(12) . . ?
C13 C12 N11 125(2) . . ?
C13 C12 H12 117.6 . . ?
N11 C12 H12 117.6 . . ?
C12 C13 C14 117.1(19) . . ?
C12 C13 H13 121.5 . . ?
C14 C13 H13 121.5 . . ?
C15 C14 C13 120.4(16) . . ?
C15 C14 I17 120.5(12) . . ?
C13 C14 I17 119.0(15) . . ?
C14 C15 C16 118.5(15) . . ?
C14 C15 H15 120.8 . . ?
C16 C15 H15 120.8 . . ?
N11 C16 C15 122.7(17) . . ?
N11 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C26 N21 C22 118.3(14) . . ?
C26 N21 Mn1 123.8(11) . . ?
C22 N21 Mn1 117.0(10) . . ?
C23 C22 N21 124.5(16) . . ?
C23 C22 H22 117.7 . . ?
N21 C22 H22 117.7 . . ?
C22 C23 C24 117.4(19) . . ?
C22 C23 H23 121.3 . . ?
C24 C23 H23 121.3 . . ?
C25 C24 C23 120.5(18) . . ?
C25 C24 I27 120.7(12) . . ?
C23 C24 I27 118.7(15) . . ?
C24 C25 C26 119.3(16) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
N21 C26 C25 119.6(16) . . ?
N21 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C32 N31 C36 113.9(16) . . ?
C32 N31 Mn1 124.9(13) . . ?
C36 N31 Mn1 121.1(15) . . ?
N31 C32 C33 123(3) . . ?
N31 C32 H32 118.5 . . ?
C33 C32 H32 118.5 . . ?
C34 C33 C32 124(3) . . ?
C34 C33 H33 118.0 . . ?
C32 C33 H33 118.0 . . ?
C33 C34 C35 116.4(17) . . ?
C33 C34 I37 122(2) . . ?
C35 C34 I37 121(2) . . ?
C36 C35 C34 114(2) . . ?
C36 C35 H35 122.9 . . ?
C34 C35 H35 122.9 . . ?
N31 C36 C35 128(2) . . ?
N31 C36 H36 115.8 . . ?
C35 C36 H36 115.8 . . ?
C42 N41 C46 119.2(15) . . ?
C42 N41 Mn1 123.2(15) . . ?
C46 N41 Mn1 117.5(13) . . ?
C45 C46 N41 119(2) . . ?
C45 C46 H46 120.7 . . ?
N41 C46 H46 120.7 . . ?
N41 C42 C43 120(2) . . ?
N41 C42 H42 119.9 . . ?
C43 C42 H42 119.9 . . ?
C45 C44 C43 114(2) . . ?
C45 C44 I47 123.2(19) . . ?
C43 C44 I47 123.1(16) . . ?
C44 C43 C42 121(2) . . ?
C44 C43 H43 119.5 . . ?
C42 C43 H43 119.5 . . ?
C44 C45 C46 127(2) . . ?
C44 C45 H45 116.6 . . ?
C46 C45 H45 116.6 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 N11 C12 C13 3(3) . . . . ?
Mn1 N11 C12 C13 -170.7(17) . . . . ?
N11 C12 C13 C14 -9(3) . . . . ?
C12 C13 C14 C15 9(3) . . . . ?
C12 C13 C14 I17 -173.6(16) . . . . ?
C13 C14 C15 C16 -5(3) . . . . ?
I17 C14 C15 C16 178.4(15) . . . . ?
C12 N11 C16 C15 2(3) . . . . ?
Mn1 N11 C16 C15 176.1(15) . . . . ?
C14 C15 C16 N11 -1(3) . . . . ?
C26 N21 C22 C23 4(3) . . . . ?
Mn1 N21 C22 C23 173(2) . . . . ?
N21 C22 C23 C24 -1(4) . . . . ?
C22 C23 C24 C25 1(4) . . . . ?
C22 C23 C24 I27 -178(2) . . . . ?
C23 C24 C25 C26 -3(4) . . . . ?
I27 C24 C25 C26 176.0(18) . . . . ?
C22 N21 C26 C25 -6(3) . . . . ?
Mn1 N21 C26 C25 -174.2(16) . . . . ?
C24 C25 C26 N21 6(4) . . . . ?
C36 N31 C32 C33 -4(4) . . . . ?
Mn1 N31 C32 C33 174(2) . . . . ?
N31 C32 C33 C34 6(5) . . . . ?
C32 C33 C34 C35 -5(5) . . . . ?
C32 C33 C34 I37 171(2) . . . . ?
C33 C34 C35 C36 2(4) . . . . ?
I37 C34 C35 C36 -174.0(16) . . . . ?
C32 N31 C36 C35 1(3) . . . . ?
Mn1 N31 C36 C35 -176.8(17) . . . . ?
C34 C35 C36 N31 0(3) . . . . ?
C42 N41 C46 C45 -1(4) . . . . ?
Mn1 N41 C46 C45 177(2) . . . . ?
C46 N41 C42 C43 5(4) . . . . ?
Mn1 N41 C42 C43 -172.6(19) . . . . ?
C45 C44 C43 C42 8(4) . . . . ?
I47 C44 C43 C42 -176(2) . . . . ?
N41 C42 C43 C44 -9(4) . . . . ?
C43 C44 C45 C46 -3(4) . . . . ?
I47 C44 C45 C46 -179(2) . . . . ?
N41 C46 C45 C44 -1(4) . . . . ?

_refine_diff_density_max         2.008
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.146


_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_2_LT
_database_code_depnum_ccdc_archive 'CCDC 1854374'
_audit_update_record             
;
2018-07-07 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Cl8 Mn2 N16 Nb'
_chemical_formula_weight         1319.28

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.7697(5)
_cell_length_b                   26.2046(9)
_cell_length_c                   31.9937(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11544.3(7)
_cell_formula_units_Z            8
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    40409
_cell_measurement_theta_min      3.11
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             5272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.112
_exptl_absorpt_coefficient_mu    1.045
_shelx_estimated_absorpt_T_min   0.833
_shelx_estimated_absorpt_T_max   0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            44534
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_theta_min         3.110
_diffrn_reflns_theta_max         27.480
_diffrn_reflns_theta_full        25.242
_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 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3310
_reflns_number_gt                3225
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0071P)²+69.5749P] 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         3310
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0453
_refine_ls_wR_factor_ref         0.0702
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.417
_refine_ls_restrained_S_all      1.417
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.42399(17) 0.42089(9) 0.42923(7) 0.0124(5) Uani 1 1 d . . . . .
C2 C 0.50391(18) 0.32925(9) 0.39811(7) 0.0144(5) Uani 1 1 d . . . . .
C3 C 0.5090(2) 0.38810(10) 0.54134(9) 0.0222(6) Uani 1 1 d . . . . .
H3 H 0.5132 0.3798 0.5125 0.027 Uiso 1 1 calc R U . . .
C4 C 0.5079(2) 0.34859(10) 0.56981(9) 0.0244(6) Uani 1 1 d . . . . .
H4 H 0.5116 0.3141 0.5609 0.029 Uiso 1 1 calc R U . . .
C5 C 0.50111(19) 0.36080(10) 0.61187(9) 0.0226(6) Uani 1 1 d . . . . .
C6 C 0.49660(19) 0.41125(10) 0.62402(9) 0.0229(5) Uani 1 1 d . . . . .
H6 H 0.4926 0.4203 0.6527 0.027 Uiso 1 1 calc R U . . .
C7 C 0.49816(19) 0.44841(10) 0.59298(8) 0.0205(5) Uani 1 1 d . . . . .
H7 H 0.4945 0.4832 0.6012 0.025 Uiso 1 1 calc R U . . .
C8 C 0.26944(18) 0.51154(9) 0.49258(8) 0.0178(5) Uani 1 1 d . . . . .
H8 H 0.2842 0.4964 0.4664 0.021 Uiso 1 1 calc R U . . .
C9 C 0.17282(19) 0.52155(10) 0.50188(8) 0.0205(5) Uani 1 1 d . . . . .
H9 H 0.1226 0.5136 0.4826 0.025 Uiso 1 1 calc R U . . .
C10 C 0.15201(18) 0.54341(9) 0.54020(8) 0.0170(5) Uani 1 1 d . . . . .
C11 C 0.22639(19) 0.55467(10) 0.56787(8) 0.0200(5) Uani 1 1 d . . . . .
H11 H 0.2133 0.5694 0.5944 0.024 Uiso 1 1 calc R U . . .
C12 C 0.32073(19) 0.54375(10) 0.55549(8) 0.0190(5) Uani 1 1 d . . . . .
H12 H 0.3722 0.5520 0.5741 0.023 Uiso 1 1 calc R U . . .
Cl3 Cl 0.03298(5) 0.55613(3) 0.55424(2) 0.02427(15) Uani 1 1 d . . . . .
Cl4 Cl 0.49824(6) 0.31232(3) 0.64848(2) 0.03348(18) Uani 1 1 d . . . . .
Mn1 Mn 0.5000 0.5000 0.5000 0.01251(12) Uani 1 2 d S . P . .
N1 N 0.44782(15) 0.44529(8) 0.45729(7) 0.0168(4) Uani 1 1 d . . . . .
N2 N 0.56758(16) 0.30463(9) 0.40964(7) 0.0237(5) Uani 1 1 d . . . . .
N3 N 0.50451(15) 0.43768(8) 0.55200(7) 0.0178(4) Uani 1 1 d . . . . .
N4 N 0.34305(15) 0.52213(8) 0.51862(6) 0.0155(4) Uani 1 1 d . . . . .
Nb1 Nb 0.3750 0.3750 0.3750 0.00746(9) Uani 1 4 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
C1 N1 1.150(3) . ?
C1 Nb1 2.216(2) . ?
C2 N2 1.149(3) . ?
C2 Nb1 2.266(2) . ?
C3 N3 1.345(3) . ?
C3 C4 1.379(4) . ?
C4 C5 1.386(4) . ?
C5 C6 1.379(4) . ?
C5 Cl4 1.728(3) . ?
C6 C7 1.391(4) . ?
C7 N3 1.344(3) . ?
C8 N4 1.341(3) . ?
C8 C9 1.388(4) . ?
C9 C10 1.383(4) . ?
C10 C11 1.386(4) . ?
C10 Cl3 1.732(2) . ?
C11 C12 1.388(4) . ?
C12 N4 1.344(3) . ?
Mn1 N1 2.107(2) 17_666 ?
Mn1 N1 2.107(2) . ?
Mn1 N4 2.315(2) . ?
Mn1 N4 2.316(2) 17_666 ?
Mn1 N3 2.332(2) 17_666 ?
Mn1 N3 2.332(2) . ?
Nb1 C1 2.216(2) 7 ?
Nb1 C1 2.216(2) 12 ?
Nb1 C1 2.216(2) 14 ?
Nb1 C2 2.266(2) 12 ?
Nb1 C2 2.266(2) 7 ?
Nb1 C2 2.266(2) 14 ?

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
N1 C1 Nb1 178.7(2) . . ?
N2 C2 Nb1 177.8(2) . . ?
N3 C3 C4 123.9(3) . . ?
C3 C4 C5 117.9(2) . . ?
C6 C5 C4 119.9(2) . . ?
C6 C5 Cl4 120.8(2) . . ?
C4 C5 Cl4 119.3(2) . . ?
C5 C6 C7 118.0(3) . . ?
N3 C7 C6 123.5(2) . . ?
N4 C8 C9 123.5(2) . . ?
C10 C9 C8 117.8(2) . . ?
C9 C10 C11 120.1(2) . . ?
C9 C10 Cl3 120.4(2) . . ?
C11 C10 Cl3 119.52(19) . . ?
C10 C11 C12 117.8(2) . . ?
N4 C12 C11 123.5(2) . . ?
N1 Mn1 N1 180.00(9) 17_666 . ?
N1 Mn1 N4 88.91(8) 17_666 . ?
N1 Mn1 N4 91.09(8) . . ?
N1 Mn1 N4 91.09(8) 17_666 17_666 ?
N1 Mn1 N4 88.91(8) . 17_666 ?
N4 Mn1 N4 180.0 . 17_666 ?
N1 Mn1 N3 89.73(8) 17_666 17_666 ?
N1 Mn1 N3 90.27(8) . 17_666 ?
N4 Mn1 N3 89.04(7) . 17_666 ?
N4 Mn1 N3 90.96(7) 17_666 17_666 ?
N1 Mn1 N3 90.27(8) 17_666 . ?
N1 Mn1 N3 89.73(8) . . ?
N4 Mn1 N3 90.96(7) . . ?
N4 Mn1 N3 89.04(7) 17_666 . ?
N3 Mn1 N3 180.0 17_666 . ?
C1 N1 Mn1 169.1(2) . . ?
C7 N3 C3 116.9(2) . . ?
C7 N3 Mn1 123.22(17) . . ?
C3 N3 Mn1 119.79(17) . . ?
C8 N4 C12 117.4(2) . . ?
C8 N4 Mn1 119.59(16) . . ?
C12 N4 Mn1 123.01(17) . . ?
C1 Nb1 C1 144.56(12) . 7 ?
C1 Nb1 C1 114.28(12) . 12 ?
C1 Nb1 C1 76.95(12) 7 12 ?
C1 Nb1 C1 76.95(12) . 14 ?
C1 Nb1 C1 114.28(12) 7 14 ?
C1 Nb1 C1 144.56(12) 12 14 ?
C1 Nb1 C2 141.35(8) . 12 ?
C1 Nb1 C2 72.30(8) 7 12 ?
C1 Nb1 C2 78.06(8) 12 12 ?
C1 Nb1 C2 74.33(8) 14 12 ?
C1 Nb1 C2 74.33(8) . 7 ?
C1 Nb1 C2 78.06(8) 7 7 ?
C1 Nb1 C2 72.30(8) 12 7 ?
C1 Nb1 C2 141.35(8) 14 7 ?
C2 Nb1 C2 141.92(11) 12 7 ?
C1 Nb1 C2 72.30(8) . 14 ?
C1 Nb1 C2 141.35(8) 7 14 ?
C1 Nb1 C2 74.33(8) 12 14 ?
C1 Nb1 C2 78.06(8) 14 14 ?
C2 Nb1 C2 76.86(12) 12 14 ?
C2 Nb1 C2 116.11(12) 7 14 ?
C1 Nb1 C2 78.07(8) . . ?
C1 Nb1 C2 74.33(8) 7 . ?
C1 Nb1 C2 141.35(8) 12 . ?
C1 Nb1 C2 72.30(8) 14 . ?
C2 Nb1 C2 116.12(12) 12 . ?
C2 Nb1 C2 76.86(12) 7 . ?
C2 Nb1 C2 141.92(11) 14 . ?

_refine_diff_density_max         0.476
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.071


_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_1_plus_LT
_database_code_depnum_ccdc_archive 'CCDC 1854372'
_audit_update_record             
;
2018-07-07 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 I8 Mn2 N16 Nb'
_chemical_formula_weight         2050.88

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'
I I -0.4742 1.8119 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_H-M_alt        'I 41'
_space_group_name_Hall           'I 4bw'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-y, x+1/2, z+1/4'
'y+1/2, -x, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1, z+1'
'-y+1/2, x+1, z+3/4'
'y+1, -x+1/2, z+5/4'

_cell_length_a                   20.7954(7)
_cell_length_b                   20.7954(7)
_cell_length_c                   14.1103(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6102.0(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    49497
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.232
_exptl_crystal_F_000             3788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.210
_exptl_absorpt_coefficient_mu    4.687
_shelx_estimated_absorpt_T_min   0.412
_shelx_estimated_absorpt_T_max   0.439
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.134
_exptl_absorpt_correction_T_max  0.140
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            48185
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.098
_diffrn_reflns_theta_max         27.472
_diffrn_reflns_theta_full        25.242
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6988
_reflns_number_gt                6985
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 4-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)+(0.0287P)²+25.7657P] 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 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6988
_refine_ls_number_parameters     342
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0218
_refine_ls_R_factor_gt           0.0217
_refine_ls_wR_factor_ref         0.0526
_refine_ls_wR_factor_gt          0.0526
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Nb1 Nb 0.5000 0.0000 0.37367(7) 0.00375(15) Uani 1 2 d S T P . .
C1 C 0.6006(3) 0.0149(4) 0.4231(5) 0.0073(14) Uani 1 1 d . . . . .
C2 C 0.4790(4) -0.1003(4) 0.3252(6) 0.0098(15) Uani 1 1 d . . . . .
C3 C 0.5147(4) -0.0674(4) 0.4999(6) 0.0150(18) Uani 1 1 d . . . . .
C4 C 0.5648(4) -0.0163(4) 0.2466(6) 0.0108(16) Uani 1 1 d . U . . .
N1 N 0.6532(3) 0.0218(3) 0.4470(5) 0.0111(14) Uani 1 1 d . . . . .
N2 N 0.4681(3) -0.1519(3) 0.3000(5) 0.0119(14) Uani 1 1 d . . . . .
N3 N 0.5254(4) -0.0987(4) 0.5617(6) 0.0200(17) Uani 1 1 d . . . . .
N4 N 0.5978(4) -0.0247(4) 0.1818(5) 0.0167(15) Uani 1 1 d . U . . .
Mn1 Mn 0.75083(6) 0.02460(5) 0.49758(11) 0.00761(19) Uani 1 1 d . . . . .
N11 N 0.7901(3) 0.0185(3) 0.3456(5) 0.0123(14) Uani 1 1 d . . . . .
C12 C 0.7494(4) 0.0003(4) 0.2756(6) 0.0143(16) Uani 1 1 d . . . . .
H12 H 0.7047 -0.0017 0.2898 0.017 Uiso 1 1 calc R U . . .
C13 C 0.7687(4) -0.0156(4) 0.1857(6) 0.0125(16) Uani 1 1 d . . . . .
H13 H 0.7383 -0.0297 0.1398 0.015 Uiso 1 1 calc R U . . .
C14 C 0.8332(4) -0.0107(4) 0.1630(6) 0.0141(16) Uani 1 1 d . . . . .
C15 C 0.8761(4) 0.0087(5) 0.2328(7) 0.0191(18) Uani 1 1 d . . . . .
H15 H 0.9207 0.0124 0.2193 0.023 Uiso 1 1 calc R U . . .
C16 C 0.8528(4) 0.0225(4) 0.3219(7) 0.0173(18) Uani 1 1 d . . . . .
H16 H 0.8825 0.0356 0.3693 0.021 Uiso 1 1 calc R U . . .
I17 I 0.86553(3) -0.03025(3) 0.02542(3) 0.01279(10) Uani 1 1 d . . . . .
N21 N 0.7127(4) 0.0165(3) 0.6507(5) 0.0118(13) Uani 1 1 d . . . . .
C22 C 0.7533(4) -0.0052(4) 0.7170(6) 0.0155(17) Uani 1 1 d . . . . .
H22 H 0.7966 -0.0143 0.7002 0.019 Uiso 1 1 calc R U . . .
C23 C 0.7330(5) -0.0147(5) 0.8119(7) 0.0185(18) Uani 1 1 d . . . . .
H23 H 0.7623 -0.0302 0.8582 0.022 Uiso 1 1 calc R U . . .
C24 C 0.6705(4) -0.0011(4) 0.8357(6) 0.0118(15) Uani 1 1 d . . . . .
C25 C 0.6285(4) 0.0197(4) 0.7663(7) 0.0144(17) Uani 1 1 d . . . . .
H25 H 0.5846 0.0281 0.7808 0.017 Uiso 1 1 calc R U . . .
C26 C 0.6518(4) 0.0283(4) 0.6743(6) 0.0134(17) Uani 1 1 d . . . . .
H26 H 0.6231 0.0431 0.6267 0.016 Uiso 1 1 calc R U . . .
I27 I 0.63884(2) -0.01369(3) 0.97535(3) 0.01337(10) Uani 1 1 d . . . . .
N31 N 0.7423(3) 0.1353(3) 0.4963(6) 0.0119(13) Uani 1 1 d . . . . .
C32 C 0.6871(4) 0.1647(4) 0.4948(6) 0.0162(17) Uani 1 1 d . . . . .
H32 H 0.6492 0.1393 0.4917 0.019 Uiso 1 1 calc R U . . .
C33 C 0.6799(6) 0.2324(4) 0.4975(6) 0.026(2) Uani 1 1 d . . . . .
H33 H 0.6387 0.2520 0.4971 0.031 Uiso 1 1 calc R U . . .
C34 C 0.7356(6) 0.2689(4) 0.5007(7) 0.026(2) Uani 1 1 d . . . . .
C35 C 0.7952(5) 0.2390(5) 0.5022(7) 0.023(2) Uani 1 1 d . . . . .
H35 H 0.8337 0.2635 0.5046 0.028 Uiso 1 1 calc R U . . .
C36 C 0.7973(4) 0.1726(4) 0.5001(6) 0.0148(17) Uani 1 1 d . . . . .
H36 H 0.8380 0.1519 0.5013 0.018 Uiso 1 1 calc R U . . .
I37 I 0.72641(4) 0.36927(3) 0.50677(5) 0.03768(19) Uani 1 1 d . . . . .
N41 N 0.7577(3) -0.0864(3) 0.4957(6) 0.0132(13) Uani 1 1 d . . . . .
C42 C 0.7053(5) -0.1246(5) 0.5013(7) 0.022(2) Uani 1 1 d . . . . .
H42 H 0.6641 -0.1060 0.5109 0.027 Uiso 1 1 calc R U . . .
C43 C 0.7113(5) -0.1913(5) 0.4928(7) 0.026(2) Uani 1 1 d . . . . .
H43 H 0.6738 -0.2174 0.4922 0.031 Uiso 1 1 calc R U . . .
C44 C 0.7715(4) -0.2199(4) 0.4854(7) 0.0212(18) Uani 1 1 d . . . . .
C45 C 0.8241(4) -0.1796(4) 0.4834(7) 0.0229(19) Uani 1 1 d . . . . .
H45 H 0.8664 -0.1967 0.4794 0.028 Uiso 1 1 calc R U . . .
C46 C 0.8144(5) -0.1138(4) 0.4873(8) 0.023(2) Uani 1 1 d . . . . .
H46 H 0.8510 -0.0866 0.4837 0.028 Uiso 1 1 calc R U . . .
I47 I 0.78441(4) -0.31862(3) 0.47466(5) 0.02771(15) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 C1 2.227(7) 6_544 ?
Nb1 C1 2.227(7) . ?
Nb1 C2 2.238(8) . ?
Nb1 C2 2.238(8) 6_544 ?
Nb1 C4 2.269(8) 6_544 ?
Nb1 C4 2.269(8) . ?
Nb1 C3 2.287(9) . ?
Nb1 C3 2.287(9) 6_544 ?
C1 N1 1.154(10) . ?
C2 N2 1.152(11) . ?
C3 N3 1.111(12) . ?
C4 N4 1.157(11) . ?
N1 Mn1 2.153(7) . ?
N2 Mn1 2.160(7) 7_534 ?
Mn1 N2 2.160(7) 8_554 ?
Mn1 N11 2.298(7) . ?
Mn1 N21 2.307(7) . ?
Mn1 N31 2.308(7) . ?
Mn1 N41 2.313(6) . ?
N11 C16 1.348(11) . ?
N11 C12 1.355(11) . ?
C12 C13 1.372(13) . ?
C13 C14 1.382(12) . ?
C14 C15 1.388(13) . ?
C14 I17 2.095(8) . ?
C15 C16 1.379(14) . ?
N21 C26 1.333(11) . ?
N21 C22 1.339(12) . ?
C22 C23 1.417(13) . ?
C23 C24 1.373(13) . ?
C24 C25 1.382(11) . ?
C24 I27 2.094(8) . ?
C25 C26 1.397(12) . ?
N31 C32 1.303(10) . ?
N31 C36 1.383(11) . ?
C32 C33 1.416(12) . ?
C33 C34 1.386(16) . ?
C34 C35 1.388(15) . ?
C34 I37 2.097(9) . ?
C35 C36 1.380(13) . ?
N41 C46 1.314(11) . ?
N41 C42 1.352(12) . ?
C42 C43 1.397(14) . ?
C43 C44 1.391(13) . ?
C44 C45 1.379(14) . ?
C44 I47 2.076(9) . ?
C45 C46 1.386(12) . ?

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
C1 Nb1 C1 143.5(4) 6_544 . ?
C1 Nb1 C2 77.4(3) 6_544 . ?
C1 Nb1 C2 114.2(3) . . ?
C1 Nb1 C2 114.2(3) 6_544 6_544 ?
C1 Nb1 C2 77.4(3) . 6_544 ?
C2 Nb1 C2 144.4(4) . 6_544 ?
C1 Nb1 C4 73.2(3) 6_544 6_544 ?
C1 Nb1 C4 141.7(3) . 6_544 ?
C2 Nb1 C4 77.4(3) . 6_544 ?
C2 Nb1 C4 74.7(3) 6_544 6_544 ?
C1 Nb1 C4 141.7(3) 6_544 . ?
C1 Nb1 C4 73.2(3) . . ?
C2 Nb1 C4 74.7(3) . . ?
C2 Nb1 C4 77.4(3) 6_544 . ?
C4 Nb1 C4 75.6(4) 6_544 . ?
C1 Nb1 C3 78.2(3) 6_544 . ?
C1 Nb1 C3 73.5(3) . . ?
C2 Nb1 C3 72.1(3) . . ?
C2 Nb1 C3 141.6(3) 6_544 . ?
C4 Nb1 C3 141.8(2) 6_544 . ?
C4 Nb1 C3 116.4(3) . . ?
C1 Nb1 C3 73.5(3) 6_544 6_544 ?
C1 Nb1 C3 78.2(3) . 6_544 ?
C2 Nb1 C3 141.6(3) . 6_544 ?
C2 Nb1 C3 72.1(3) 6_544 6_544 ?
C4 Nb1 C3 116.4(3) 6_544 6_544 ?
C4 Nb1 C3 141.8(2) . 6_544 ?
C3 Nb1 C3 77.7(4) . 6_544 ?
N1 C1 Nb1 178.4(7) . . ?
N2 C2 Nb1 179.8(8) . . ?
N3 C3 Nb1 175.8(7) . . ?
N4 C4 Nb1 179.8(8) . . ?
C1 N1 Mn1 174.1(7) . . ?
C2 N2 Mn1 164.5(6) . 7_534 ?
N1 Mn1 N2 177.4(3) . 8_554 ?
N1 Mn1 N11 91.4(3) . . ?
N2 Mn1 N11 89.5(3) 8_554 . ?
N1 Mn1 N21 89.1(3) . . ?
N2 Mn1 N21 90.4(3) 8_554 . ?
N11 Mn1 N21 172.6(2) . . ?
N1 Mn1 N31 87.3(3) . . ?
N2 Mn1 N31 90.2(2) 8_554 . ?
N11 Mn1 N31 94.3(3) . . ?
N21 Mn1 N31 93.1(3) . . ?
N1 Mn1 N41 91.6(3) . . ?
N2 Mn1 N41 90.9(3) 8_554 . ?
N11 Mn1 N41 85.0(3) . . ?
N21 Mn1 N41 87.6(3) . . ?
N31 Mn1 N41 178.6(3) . . ?
C16 N11 C12 116.2(7) . . ?
C16 N11 Mn1 124.8(6) . . ?
C12 N11 Mn1 118.2(5) . . ?
N11 C12 C13 124.0(7) . . ?
C12 C13 C14 118.7(8) . . ?
C13 C14 C15 118.8(8) . . ?
C13 C14 I17 120.8(7) . . ?
C15 C14 I17 120.4(6) . . ?
C16 C15 C14 118.8(8) . . ?
N11 C16 C15 123.6(8) . . ?
C26 N21 C22 119.1(8) . . ?
C26 N21 Mn1 123.2(6) . . ?
C22 N21 Mn1 117.6(6) . . ?
N21 C22 C23 121.3(8) . . ?
C24 C23 C22 119.0(9) . . ?
C23 C24 C25 119.3(8) . . ?
C23 C24 I27 120.2(6) . . ?
C25 C24 I27 120.5(6) . . ?
C24 C25 C26 118.6(8) . . ?
N21 C26 C25 122.6(8) . . ?
C32 N31 C36 117.7(7) . . ?
C32 N31 Mn1 122.5(6) . . ?
C36 N31 Mn1 119.8(5) . . ?
N31 C32 C33 124.1(9) . . ?
C34 C33 C32 117.2(9) . . ?
C33 C34 C35 120.1(8) . . ?
C33 C34 I37 118.0(7) . . ?
C35 C34 I37 121.9(8) . . ?
C36 C35 C34 118.4(9) . . ?
C35 C36 N31 122.5(8) . . ?
C46 N41 C42 118.3(7) . . ?
C46 N41 Mn1 119.3(6) . . ?
C42 N41 Mn1 122.4(6) . . ?
N41 C42 C43 120.4(9) . . ?
C44 C43 C42 120.8(9) . . ?
C45 C44 C43 117.1(8) . . ?
C45 C44 I47 119.8(6) . . ?
C43 C44 I47 123.1(7) . . ?
C44 C45 C46 118.9(8) . . ?
N41 C46 C45 124.3(8) . . ?

_refine_diff_density_max         1.571
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.112


_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_2_RT
_database_code_depnum_ccdc_archive 'CCDC 1854371'
_audit_update_record             
;
2018-07-07 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 Cl8 Mn2 N16 Nb'
_chemical_formula_weight         1319.28

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_H-M_alt        'F d d d'
_space_group_name_Hall           '-F 2uv 2vw'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'

_cell_length_a                   13.9379(3)
_cell_length_b                   26.6853(5)
_cell_length_c                   31.5931(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     11750.6(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    37235
_cell_measurement_theta_min      3.00
_cell_measurement_theta_max      27.48

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_F_000             5272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.112
_exptl_absorpt_coefficient_mu    1.027
_shelx_estimated_absorpt_T_min   0.835
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            45659
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         3.053
_diffrn_reflns_theta_max         27.479
_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             3378
_reflns_number_gt                3226
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0275P)²+56.7682P] 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         3378
_refine_ls_number_parameters     172
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0589
_refine_ls_wR_factor_ref         0.1080
_refine_ls_wR_factor_gt          0.1058
_refine_ls_goodness_of_fit_ref   1.368
_refine_ls_restrained_S_all      1.368
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4236(2) 0.42118(12) 0.42946(10) 0.0322(7) Uani 1 1 d . . . . .
C2 C 0.5031(2) 0.33131(14) 0.39907(10) 0.0375(7) Uani 1 1 d . . . . .
C3 C 0.5084(3) 0.39004(16) 0.54314(16) 0.0669(12) Uani 1 1 d . . . . .
H3 H 0.5123 0.3814 0.5147 0.080 Uiso 1 1 calc R U . . .
C4 C 0.5071(4) 0.35228(18) 0.5723(2) 0.0798(15) Uani 1 1 d . . . . .
H4 H 0.5103 0.3189 0.5639 0.096 Uiso 1 1 calc R U . . .
C5 C 0.5012(3) 0.3647(2) 0.61420(19) 0.0745(15) Uani 1 1 d . . . . .
C6 C 0.4968(3) 0.4137(2) 0.62597(17) 0.0745(13) Uani 1 1 d . . . . .
H6 H 0.4930 0.4228 0.6543 0.089 Uiso 1 1 calc R U . . .
C7 C 0.4982(3) 0.44947(18) 0.59446(15) 0.0631(11) Uani 1 1 d . . . . .
H7 H 0.4948 0.4830 0.6024 0.076 Uiso 1 1 calc R U . . .
C8 C 0.2721(3) 0.50947(16) 0.49311(13) 0.0539(10) Uani 1 1 d . . . . .
H8 H 0.2866 0.4939 0.4675 0.065 Uiso 1 1 calc R U . . .
C9 C 0.1768(3) 0.51886(17) 0.50251(14) 0.0596(11) Uani 1 1 d . . . . .
H9 H 0.1283 0.5093 0.4840 0.071 Uiso 1 1 calc R U . . .
C10 C 0.1558(3) 0.54259(15) 0.53991(14) 0.0539(10) Uani 1 1 d . . . . .
C11 C 0.2286(3) 0.55600(18) 0.56673(15) 0.0629(12) Uani 1 1 d . . . . .
H11 H 0.2159 0.5722 0.5922 0.076 Uiso 1 1 calc R U . . .
C12 C 0.3217(3) 0.54478(16) 0.55482(14) 0.0584(11) Uani 1 1 d . . . . .
H12 H 0.3714 0.5540 0.5729 0.070 Uiso 1 1 calc R U . . .
Cl3 Cl 0.03788(8) 0.55522(5) 0.55373(5) 0.0829(4) Uani 1 1 d . . . . .
Cl4 Cl 0.49833(13) 0.31768(7) 0.65177(7) 0.1256(7) Uani 1 1 d . . . . .
Mn1 Mn 0.5000 0.5000 0.5000 0.0384(2) Uani 1 2 d S . P . .
N1 N 0.4481(2) 0.44572(12) 0.45690(10) 0.0482(8) Uani 1 1 d . . . . .
N2 N 0.5667(2) 0.30827(15) 0.41083(11) 0.0650(10) Uani 1 1 d . . . . .
N3 N 0.5041(2) 0.43877(12) 0.55314(11) 0.0514(8) Uani 1 1 d . . . . .
N4 N 0.3441(2) 0.52157(12) 0.51889(10) 0.0451(7) Uani 1 1 d . . . . .
Nb1 Nb 0.3750 0.3750 0.3750 0.01926(13) Uani 1 4 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
C1 N1 1.139(4) . ?
C1 Nb1 2.222(3) . ?
C2 N2 1.140(4) . ?
C2 Nb1 2.264(3) . ?
C3 N3 1.340(5) . ?
C3 C4 1.366(7) . ?
C4 C5 1.366(8) . ?
C5 C6 1.362(7) . ?
C5 Cl4 1.728(5) . ?
C6 C7 1.378(7) . ?
C7 N3 1.339(5) . ?
C8 N4 1.332(5) . ?
C8 C9 1.384(5) . ?
C9 C10 1.372(6) . ?
C10 C11 1.369(6) . ?
C10 Cl3 1.734(4) . ?
C11 C12 1.384(6) . ?
C12 N4 1.330(5) . ?
Mn1 N1 2.115(3) . ?
Mn1 N1 2.115(3) 17_666 ?
Mn1 N4 2.326(3) 17_666 ?
Mn1 N4 2.326(3) . ?
Mn1 N3 2.343(3) . ?
Mn1 N3 2.344(3) 17_666 ?
Nb1 C1 2.222(3) 7 ?
Nb1 C1 2.222(3) 12 ?
Nb1 C1 2.222(3) 14 ?
Nb1 C2 2.264(3) 12 ?
Nb1 C2 2.264(3) 7 ?
Nb1 C2 2.264(3) 14 ?

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
N1 C1 Nb1 178.6(3) . . ?
N2 C2 Nb1 178.3(4) . . ?
N3 C3 C4 123.8(5) . . ?
C5 C4 C3 118.4(5) . . ?
C6 C5 C4 120.0(5) . . ?
C6 C5 Cl4 120.6(5) . . ?
C4 C5 Cl4 119.4(4) . . ?
C5 C6 C7 117.8(5) . . ?
N3 C7 C6 123.9(5) . . ?
N4 C8 C9 123.2(4) . . ?
C10 C9 C8 118.2(4) . . ?
C9 C10 C11 119.7(4) . . ?
C9 C10 Cl3 120.5(3) . . ?
C11 C10 Cl3 119.7(3) . . ?
C10 C11 C12 118.0(4) . . ?
N4 C12 C11 123.5(4) . . ?
N1 Mn1 N1 180.0 . 17_666 ?
N1 Mn1 N4 89.13(11) . 17_666 ?
N1 Mn1 N4 90.87(11) 17_666 17_666 ?
N1 Mn1 N4 90.86(11) . . ?
N1 Mn1 N4 89.14(11) 17_666 . ?
N4 Mn1 N4 180.00(14) 17_666 . ?
N1 Mn1 N3 89.55(12) . . ?
N1 Mn1 N3 90.44(12) 17_666 . ?
N4 Mn1 N3 89.32(11) 17_666 . ?
N4 Mn1 N3 90.67(11) . . ?
N1 Mn1 N3 90.45(12) . 17_666 ?
N1 Mn1 N3 89.56(12) 17_666 17_666 ?
N4 Mn1 N3 90.68(11) 17_666 17_666 ?
N4 Mn1 N3 89.33(11) . 17_666 ?
N3 Mn1 N3 180.0 . 17_666 ?
C1 N1 Mn1 170.5(3) . . ?
C3 N3 C7 116.1(4) . . ?
C3 N3 Mn1 120.6(3) . . ?
C7 N3 Mn1 123.3(3) . . ?
C12 N4 C8 117.3(3) . . ?
C12 N4 Mn1 123.5(3) . . ?
C8 N4 Mn1 119.1(2) . . ?
C1 Nb1 C1 78.50(16) 7 12 ?
C1 Nb1 C1 112.64(17) 7 14 ?
C1 Nb1 C1 144.53(16) 12 14 ?
C1 Nb1 C1 144.53(16) 7 . ?
C1 Nb1 C1 112.64(17) 12 . ?
C1 Nb1 C1 78.50(16) 14 . ?
C1 Nb1 C2 72.23(12) 7 12 ?
C1 Nb1 C2 77.60(12) 12 12 ?
C1 Nb1 C2 74.58(11) 14 12 ?
C1 Nb1 C2 141.80(11) . 12 ?
C1 Nb1 C2 77.60(12) 7 7 ?
C1 Nb1 C2 72.23(12) 12 7 ?
C1 Nb1 C2 141.79(11) 14 7 ?
C1 Nb1 C2 74.58(11) . 7 ?
C2 Nb1 C2 140.77(16) 12 7 ?
C1 Nb1 C2 141.79(11) 7 14 ?
C1 Nb1 C2 74.58(11) 12 14 ?
C1 Nb1 C2 77.60(12) 14 14 ?
C1 Nb1 C2 72.23(12) . 14 ?
C2 Nb1 C2 75.86(18) 12 14 ?
C2 Nb1 C2 118.02(19) 7 14 ?
C1 Nb1 C2 74.59(11) 7 . ?
C1 Nb1 C2 141.80(11) 12 . ?
C1 Nb1 C2 72.22(12) 14 . ?
C1 Nb1 C2 77.60(12) . . ?
C2 Nb1 C2 118.02(19) 12 . ?
C2 Nb1 C2 75.86(18) 7 . ?
C2 Nb1 C2 140.76(16) 14 . ?

_refine_diff_density_max         0.487
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.059


_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_1_minus_LT
_database_code_depnum_ccdc_archive 'CCDC 1854370'
_audit_update_record             
;
2018-07-07 deposited with the CCDC.
2018-09-24 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H32 I8 Mn2 N16 Nb'
_chemical_formula_weight         2050.88

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_H-M_alt        'I 41'
_space_group_name_Hall           'I 4bw'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x+1/2, z+1/4'
'y, -x+1/2, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'y+1/2, -x+1, z+3/4'

_cell_length_a                   20.792(2)
_cell_length_b                   20.792(2)
_cell_length_c                   14.1122(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6100.8(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    90(2)
_cell_measurement_reflns_used    45416
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_F_000             3788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.688
_shelx_estimated_absorpt_T_min   0.503
_shelx_estimated_absorpt_T_max   0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.305
_exptl_absorpt_correction_T_max  0.381
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      90(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            46794
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.098
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_full        25.242
_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 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6889
_reflns_number_gt                6881
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.923
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 4-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)+(0.0250P)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 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6889
_refine_ls_number_parameters     342
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0652
_refine_ls_wR_factor_gt          0.0651
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.5000 0.0000 0.93071(8) 0.00385(19) Uani 1 2 d S T P . .
C1 C 0.6005(4) -0.0217(4) 0.9794(6) 0.0087(17) Uani 1 1 d . . . . .
C2 C 0.5146(4) -0.1007(4) 0.8820(6) 0.0057(16) Uani 1 1 d . . . . .
C3 C 0.5165(5) 0.0659(4) 1.0582(6) 0.0120(19) Uani 1 1 d . . . . .
C4 C 0.5671(4) 0.0141(4) 0.8040(6) 0.0129(18) Uani 1 1 d . U . . .
N1 N 0.6518(4) -0.0322(3) 1.0047(5) 0.0085(15) Uani 1 1 d . . . . .
N2 N 0.5219(4) -0.1528(3) 0.8583(5) 0.0113(16) Uani 1 1 d . . . . .
N3 N 0.5245(4) 0.0975(4) 1.1215(6) 0.0149(17) Uani 1 1 d . . . . .
N4 N 0.5988(4) 0.0259(4) 0.7425(6) 0.0200(18) Uani 1 1 d . U . . .
Mn1 Mn 0.74904(7) -0.02451(6) 1.05666(11) 0.0079(2) Uani 1 1 d . . . . .
N11 N 0.7870(4) -0.0173(4) 0.9038(5) 0.0122(16) Uani 1 1 d . . . . .
C12 C 0.7470(5) 0.0055(5) 0.8369(7) 0.0143(19) Uani 1 1 d . . . . .
H12 H 0.7040 0.0158 0.8538 0.017 Uiso 1 1 calc R U . . .
C13 C 0.7669(5) 0.0143(5) 0.7430(7) 0.016(2) Uani 1 1 d . U . . .
H13 H 0.7376 0.0293 0.6963 0.019 Uiso 1 1 calc R U . . .
C14 C 0.8298(4) 0.0008(5) 0.7198(6) 0.0119(17) Uani 1 1 d . U . . .
C15 C 0.8719(4) -0.0197(4) 0.7885(7) 0.0118(17) Uani 1 1 d . U . . .
H15 H 0.9158 -0.0279 0.7741 0.014 Uiso 1 1 calc R U . . .
C16 C 0.8483(5) -0.0280(4) 0.8792(7) 0.0138(19) Uani 1 1 d . U . . .
H16 H 0.8773 -0.0421 0.9270 0.017 Uiso 1 1 calc R U . . .
I17 I 0.86113(3) 0.01359(3) 0.57902(4) 0.01345(12) Uani 1 1 d . . . . .
N21 N 0.7092(4) -0.0186(4) 1.2093(5) 0.0137(17) Uani 1 1 d . . . . .
C22 C 0.7505(4) -0.0005(5) 1.2784(7) 0.0135(18) Uani 1 1 d . U . . .
H22 H 0.7950 0.0013 1.2636 0.016 Uiso 1 1 calc R U . . .
C23 C 0.7318(4) 0.0153(5) 1.3692(7) 0.0128(19) Uani 1 1 d . . . . .
H23 H 0.7623 0.0285 1.4153 0.015 Uiso 1 1 calc R U . . .
C24 C 0.6665(5) 0.0114(5) 1.3910(7) 0.015(2) Uani 1 1 d . . . . .
C25 C 0.6247(5) -0.0081(5) 1.3218(7) 0.019(2) Uani 1 1 d . . . . .
H25 H 0.5801 -0.0117 1.3353 0.022 Uiso 1 1 calc R U . . .
C26 C 0.6479(4) -0.0226(5) 1.2312(7) 0.017(2) Uani 1 1 d . . . . .
H26 H 0.6182 -0.0358 1.1838 0.021 Uiso 1 1 calc R U . . .
I27 I 0.63445(3) 0.03027(3) 1.52886(3) 0.01286(12) Uani 1 1 d . . . . .
N31 N 0.7581(4) -0.1352(4) 1.0581(6) 0.0118(15) Uani 1 1 d . . . . .
C32 C 0.8132(5) -0.1647(4) 1.0591(6) 0.0147(19) Uani 1 1 d . . . . .
H32 H 0.8510 -0.1391 1.0609 0.018 Uiso 1 1 calc R U . . .
C33 C 0.8207(6) -0.2316(5) 1.0577(7) 0.029(3) Uani 1 1 d . . . . .
H33 H 0.8620 -0.2510 1.0601 0.034 Uiso 1 1 calc R U . . .
C34 C 0.7647(6) -0.2687(5) 1.0528(8) 0.024(2) Uani 1 1 d . . . . .
C35 C 0.7044(6) -0.2386(5) 1.0525(7) 0.023(2) Uani 1 1 d . . . . .
H35 H 0.6657 -0.2629 1.0512 0.028 Uiso 1 1 calc R U . . .
C36 C 0.7035(5) -0.1724(4) 1.0542(7) 0.0138(19) Uani 1 1 d . . . . .
H36 H 0.6630 -0.1512 1.0527 0.017 Uiso 1 1 calc R U . . .
I37 I 0.77354(5) -0.36917(3) 1.04743(6) 0.0379(2) Uani 1 1 d . . . . .
N41 N 0.7425(4) 0.0859(3) 1.0589(6) 0.0127(15) Uani 1 1 d . . . . .
C42 C 0.6870(5) 0.1140(5) 1.0657(8) 0.023(2) Uani 1 1 d . . . . .
H42 H 0.6502 0.0869 1.0676 0.027 Uiso 1 1 calc R U . . .
C43 C 0.6762(5) 0.1800(5) 1.0707(8) 0.021(2) Uani 1 1 d . . . . .
H43 H 0.6339 0.1970 1.0752 0.025 Uiso 1 1 calc R U . . .
C44 C 0.7286(5) 0.2197(5) 1.0688(7) 0.020(2) Uani 1 1 d . . . . .
C45 C 0.7888(6) 0.1914(5) 1.0616(7) 0.024(2) Uani 1 1 d . . . . .
H45 H 0.8263 0.2174 1.0624 0.029 Uiso 1 1 calc R U . . .
C46 C 0.7942(5) 0.1250(5) 1.0532(7) 0.021(2) Uani 1 1 d . . . . .
H46 H 0.8355 0.1066 1.0431 0.025 Uiso 1 1 calc R U . . .
I47 I 0.71551(4) 0.31868(3) 1.07953(5) 0.02750(17) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 C2 2.223(8) 2_655 ?
Nb1 C2 2.224(8) . ?
Nb1 C1 2.246(9) 2_655 ?
Nb1 C1 2.246(9) . ?
Nb1 C3 2.287(9) 2_655 ?
Nb1 C3 2.287(9) . ?
Nb1 C4 2.287(9) 2_655 ?
Nb1 C4 2.287(9) . ?
C1 N1 1.146(11) . ?
C2 N2 1.146(11) . ?
C3 N3 1.122(12) . ?
C4 N4 1.118(12) . ?
N1 Mn1 2.156(7) . ?
N2 Mn1 2.167(8) 7_534 ?
Mn1 N2 2.167(8) 4_655 ?
Mn1 N41 2.301(7) . ?
Mn1 N11 2.301(8) . ?
Mn1 N31 2.310(8) . ?
Mn1 N21 2.311(8) . ?
N11 C16 1.340(12) . ?
N11 C12 1.344(12) . ?
C12 C13 1.399(14) . ?
C12 H12 0.9500 . ?
C13 C14 1.378(14) . ?
C13 H13 0.9500 . ?
C14 C15 1.373(13) . ?
C14 I17 2.107(9) . ?
C15 C16 1.382(13) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
N21 C26 1.315(12) . ?
N21 C22 1.352(12) . ?
C22 C23 1.378(13) . ?
C22 H22 0.9500 . ?
C23 C24 1.394(13) . ?
C23 H23 0.9500 . ?
C24 C25 1.368(14) . ?
C24 I27 2.094(9) . ?
C25 C26 1.400(15) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
N31 C32 1.300(11) . ?
N31 C36 1.374(12) . ?
C32 C33 1.400(13) . ?
C32 H32 0.9500 . ?
C33 C34 1.397(17) . ?
C33 H33 0.9500 . ?
C34 C35 1.401(15) . ?
C34 I37 2.099(10) . ?
C35 C36 1.377(14) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
N41 C42 1.297(13) . ?
N41 C46 1.350(13) . ?
C42 C43 1.394(13) . ?
C42 H42 0.9500 . ?
C43 C44 1.366(14) . ?
C43 H43 0.9500 . ?
C44 C45 1.385(15) . ?
C44 I47 2.082(10) . ?
C45 C46 1.390(15) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Nb1 C2 144.0(4) 2_655 . ?
C2 Nb1 C1 77.2(3) 2_655 2_655 ?
C2 Nb1 C1 114.3(3) . 2_655 ?
C2 Nb1 C1 114.3(3) 2_655 . ?
C2 Nb1 C1 77.2(3) . . ?
C1 Nb1 C1 144.3(4) 2_655 . ?
C2 Nb1 C3 141.9(3) 2_655 2_655 ?
C2 Nb1 C3 72.5(3) . 2_655 ?
C1 Nb1 C3 74.9(3) 2_655 2_655 ?
C1 Nb1 C3 77.2(3) . 2_655 ?
C2 Nb1 C3 72.5(3) 2_655 . ?
C2 Nb1 C3 141.9(3) . . ?
C1 Nb1 C3 77.2(3) 2_655 . ?
C1 Nb1 C3 74.9(3) . . ?
C3 Nb1 C3 76.3(4) 2_655 . ?
C2 Nb1 C4 78.2(3) 2_655 2_655 ?
C2 Nb1 C4 73.8(3) . 2_655 ?
C1 Nb1 C4 72.4(3) 2_655 2_655 ?
C1 Nb1 C4 141.4(3) . 2_655 ?
C3 Nb1 C4 116.5(3) 2_655 2_655 ?
C3 Nb1 C4 141.6(3) . 2_655 ?
C2 Nb1 C4 73.8(3) 2_655 . ?
C2 Nb1 C4 78.2(3) . . ?
C1 Nb1 C4 141.4(3) 2_655 . ?
C1 Nb1 C4 72.4(3) . . ?
C3 Nb1 C4 141.6(3) 2_655 . ?
C3 Nb1 C4 116.5(3) . . ?
C4 Nb1 C4 77.1(5) 2_655 . ?
N1 C1 Nb1 179.4(8) . . ?
N2 C2 Nb1 179.0(8) . . ?
N3 C3 Nb1 179.0(8) . . ?
N4 C4 Nb1 174.8(8) . . ?
C1 N1 Mn1 164.6(7) . . ?
C2 N2 Mn1 173.4(7) . 7_534 ?
N1 Mn1 N2 177.1(3) . 4_655 ?
N1 Mn1 N41 91.4(3) . . ?
N2 Mn1 N41 91.5(3) 4_655 . ?
N1 Mn1 N11 90.4(3) . . ?
N2 Mn1 N11 89.5(3) 4_655 . ?
N41 Mn1 N11 88.2(3) . . ?
N1 Mn1 N31 90.3(3) . . ?
N2 Mn1 N31 86.9(3) 4_655 . ?
N41 Mn1 N31 178.2(3) . . ?
N11 Mn1 N31 92.6(3) . . ?
N1 Mn1 N21 89.2(3) . . ?
N2 Mn1 N21 91.3(3) 4_655 . ?
N41 Mn1 N21 85.0(3) . . ?
N11 Mn1 N21 173.1(3) . . ?
N31 Mn1 N21 94.3(3) . . ?
C16 N11 C12 117.7(8) . . ?
C16 N11 Mn1 123.9(7) . . ?
C12 N11 Mn1 118.0(6) . . ?
N11 C12 C13 121.9(9) . . ?
N11 C12 H12 119.1 . . ?
C13 C12 H12 119.1 . . ?
C14 C13 C12 118.6(10) . . ?
C14 C13 H13 120.7 . . ?
C12 C13 H13 120.7 . . ?
C13 C14 C15 120.0(9) . . ?
C13 C14 I17 119.5(7) . . ?
C15 C14 I17 120.5(7) . . ?
C16 C15 C14 117.8(9) . . ?
C16 C15 H15 121.1 . . ?
C14 C15 H15 121.1 . . ?
N11 C16 C15 123.8(9) . . ?
N11 C16 H16 118.1 . . ?
C15 C16 H16 118.1 . . ?
C26 N21 C22 117.6(8) . . ?
C26 N21 Mn1 124.3(6) . . ?
C22 N21 Mn1 117.4(6) . . ?
N21 C22 C23 123.9(8) . . ?
N21 C22 H22 118.1 . . ?
C23 C22 H22 118.1 . . ?
C22 C23 C24 117.8(9) . . ?
C22 C23 H23 121.1 . . ?
C24 C23 H23 121.1 . . ?
C25 C24 C23 118.6(9) . . ?
C25 C24 I27 121.0(8) . . ?
C23 C24 I27 120.3(7) . . ?
C24 C25 C26 119.8(9) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
N21 C26 C25 122.3(9) . . ?
N21 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C32 N31 C36 117.7(8) . . ?
C32 N31 Mn1 122.8(6) . . ?
C36 N31 Mn1 119.5(6) . . ?
N31 C32 C33 124.5(10) . . ?
N31 C32 H32 117.8 . . ?
C33 C32 H32 117.8 . . ?
C34 C33 C32 117.2(11) . . ?
C34 C33 H33 121.4 . . ?
C32 C33 H33 121.4 . . ?
C33 C34 C35 119.9(9) . . ?
C33 C34 I37 118.6(8) . . ?
C35 C34 I37 121.5(8) . . ?
C36 C35 C34 117.3(9) . . ?
C36 C35 H35 121.4 . . ?
C34 C35 H35 121.4 . . ?
C35 C36 N31 123.4(9) . . ?
C35 C36 H36 118.3 . . ?
N31 C36 H36 118.3 . . ?
C42 N41 C46 116.3(8) . . ?
C42 N41 Mn1 120.1(6) . . ?
C46 N41 Mn1 123.6(6) . . ?
N41 C42 C43 126.1(9) . . ?
N41 C42 H42 116.9 . . ?
C43 C42 H42 116.9 . . ?
C44 C43 C42 117.7(9) . . ?
C44 C43 H43 121.1 . . ?
C42 C43 H43 121.1 . . ?
C43 C44 C45 117.8(9) . . ?
C43 C44 I47 119.4(7) . . ?
C45 C44 I47 122.9(7) . . ?
C44 C45 C46 120.1(10) . . ?
C44 C45 H45 120.0 . . ?
C46 C45 H45 120.0 . . ?
N41 C46 C45 121.9(10) . . ?
N41 C46 H46 119.1 . . ?
C45 C46 H46 119.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C16 N11 C12 C13 3.8(14) . . . . ?
Mn1 N11 C12 C13 177.0(7) . . . . ?
N11 C12 C13 C14 -1.8(15) . . . . ?
C12 C13 C14 C15 -1.2(15) . . . . ?
C12 C13 C14 I17 -180.0(7) . . . . ?
C13 C14 C15 C16 2.0(14) . . . . ?
I17 C14 C15 C16 -179.2(7) . . . . ?
C12 N11 C16 C15 -3.0(14) . . . . ?
Mn1 N11 C16 C15 -175.8(7) . . . . ?
C14 C15 C16 N11 0.1(15) . . . . ?
C26 N21 C22 C23 -1.7(15) . . . . ?
Mn1 N21 C22 C23 168.9(8) . . . . ?
N21 C22 C23 C24 1.2(15) . . . . ?
C22 C23 C24 C25 0.1(14) . . . . ?
C22 C23 C24 I27 177.0(7) . . . . ?
C23 C24 C25 C26 -0.8(15) . . . . ?
I27 C24 C25 C26 -177.7(8) . . . . ?
C22 N21 C26 C25 0.9(15) . . . . ?
Mn1 N21 C26 C25 -169.0(8) . . . . ?
C24 C25 C26 N21 0.3(16) . . . . ?
C36 N31 C32 C33 -0.8(15) . . . . ?
Mn1 N31 C32 C33 -178.4(8) . . . . ?
N31 C32 C33 C34 1.5(16) . . . . ?
C32 C33 C34 C35 -2.0(16) . . . . ?
C32 C33 C34 I37 178.6(8) . . . . ?
C33 C34 C35 C36 2.0(16) . . . . ?
I37 C34 C35 C36 -178.7(8) . . . . ?
C34 C35 C36 N31 -1.3(15) . . . . ?
C32 N31 C36 C35 0.7(15) . . . . ?
Mn1 N31 C36 C35 178.4(8) . . . . ?
C46 N41 C42 C43 -2.1(17) . . . . ?
Mn1 N41 C42 C43 178.0(9) . . . . ?
N41 C42 C43 C44 -0.5(18) . . . . ?
C42 C43 C44 C45 0.4(16) . . . . ?
C42 C43 C44 I47 -178.4(8) . . . . ?
C43 C44 C45 C46 2.3(16) . . . . ?
I47 C44 C45 C46 -179.0(8) . . . . ?
C42 N41 C46 C45 4.9(15) . . . . ?
Mn1 N41 C46 C45 -175.3(8) . . . . ?
C44 C45 C46 N41 -5.1(16) . . . . ?

_refine_diff_density_max         0.964
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.140


_exptl_crystal_preparation       'Magnetic properties'
