# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_ph509_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1507755'
_audit_update_record             
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date             2016-09-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H20 N4 O4 Te4, C6 H6'
_chemical_formula_sum            'C34 H26 N4 O4 Te4'
_chemical_formula_weight         1064.99
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.646(3)
_cell_length_b                   17.433(2)
_cell_length_c                   10.6572(15)
_cell_angle_alpha                90
_cell_angle_beta                 95.384(2)
_cell_angle_gamma                90
_cell_volume                     3448.9(8)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    3040
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      3.02
_shelx_estimated_absorpt_T_max   0.899
_shelx_estimated_absorpt_T_min   0.509
_exptl_absorpt_coefficient_mu    3.393
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0463 before and 0.0317 after correction.
The Ratio of minimum to maximum transmission is 0.6097.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.051
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       rod
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.032
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13318
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.299
_diffrn_reflns_theta_min         3.206
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2913
_reflns_number_total             4255
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.968
_refine_diff_density_min         -1.514
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4255
_refine_ls_number_restraints     177
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0410
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+15.4489P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0917
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H11(0.068) H12(0.086) H7(0.082) H6(0.092) H14(0.081) H5(0.09)
 H10(0.07) H13(0.093) H4(0.083) H3(0.067) H17(0.112) H16(0.108) H15(0.103)
 Fixed X: H11(0.5576) H12(0.5915) H7(0.2985) H6(0.1771) H14(0.7167) H5(0.1391)
 H10(0.7257) H13(0.6705) H4(0.2212) H3(0.4291) H17(0.0213) H16(0.0444)
 H15(0.0208)
 Fixed Y: H11(0.6966) H12(0.8002) H7(0.5092) H6(0.5232) H14(0.8802) H5(0.587)
 H10(0.804) H13(0.8906) H4(0.6427) H3(0.5321) H17(0.4658) H16(0.5791)
 H15(0.6935)
 Fixed Z: H11(0.2981) H12(0.1809) H7(0.1843) H6(0.2056) H14(0.4758) H5(0.3746)
 H10(0.6851) H13(0.2694) H4(0.5267) H3(0.2724) H17(0.154) H16(0.0563)
 H15(0.1509)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Te2 Te 0.59177(2) 0.63692(2) 0.57970(4) 0.05082(12) Uani 1 1 d . U . . .
Te1 Te 0.39432(2) 0.65267(2) 0.57138(4) 0.05815(13) Uani 1 1 d . U . . .
O1 O 0.52481(19) 0.5846(2) 0.4213(4) 0.0626(10) Uani 1 1 d . U . . .
O2 O 0.6932(2) 0.6974(3) 0.8224(4) 0.0721(11) Uani 1 1 d . U . . .
N2 N 0.6675(2) 0.7125(2) 0.7012(5) 0.0570(11) Uani 1 1 d . U . . .
N1 N 0.4520(2) 0.5918(2) 0.4249(5) 0.0541(11) Uani 1 1 d . U . . .
C11 C 0.5893(3) 0.7333(3) 0.3346(6) 0.0569(13) Uani 1 1 d . U . . .
H11 H 0.5576 0.6966 0.2981 0.068 Uiso 1 1 calc R . . . .
C12 C 0.6098(3) 0.7952(3) 0.2646(7) 0.0718(17) Uani 1 1 d . U . . .
H12 H 0.5915 0.8002 0.1809 0.086 Uiso 1 1 calc R . . . .
C8 C 0.6165(2) 0.7266(3) 0.4590(6) 0.0487(12) Uani 1 1 d . U . . .
C1 C 0.3109(3) 0.6077(3) 0.4465(6) 0.0565(13) Uani 1 1 d . U . . .
C7 C 0.2833(3) 0.5355(3) 0.2530(7) 0.0683(16) Uani 1 1 d . U . . .
H7 H 0.2985 0.5092 0.1843 0.082 Uiso 1 1 calc R . . . .
C2 C 0.3340(3) 0.5669(3) 0.3442(6) 0.0586(13) Uani 1 1 d . U . . .
C6 C 0.2109(3) 0.5439(3) 0.2659(8) 0.0766(18) Uani 1 1 d . U . . .
H6 H 0.1771 0.5232 0.2056 0.092 Uiso 1 1 calc R . . . .
C9 C 0.6646(2) 0.7815(3) 0.5159(6) 0.0533(12) Uani 1 1 d . U . . .
C14 C 0.6846(3) 0.8434(3) 0.4411(7) 0.0672(16) Uani 1 1 d . U . . .
H14 H 0.7167 0.8802 0.4758 0.081 Uiso 1 1 calc R . . . .
C5 C 0.1882(3) 0.5827(4) 0.3670(7) 0.0754(17) Uani 1 1 d . U . . .
H5 H 0.1391 0.5870 0.3746 0.090 Uiso 1 1 calc R . . . .
C10 C 0.6920(3) 0.7707(3) 0.6446(6) 0.0583(13) Uani 1 1 d . U . . .
H10 H 0.7257 0.8040 0.6851 0.070 Uiso 1 1 calc R . . . .
C13 C 0.6571(3) 0.8495(3) 0.3178(8) 0.0778(18) Uani 1 1 d . U . . .
H13 H 0.6705 0.8906 0.2694 0.093 Uiso 1 1 calc R . . . .
C4 C 0.2372(3) 0.6159(3) 0.4592(7) 0.0688(16) Uani 1 1 d . U . . .
H4 H 0.2212 0.6427 0.5267 0.083 Uiso 1 1 calc R . . . .
C3 C 0.4106(3) 0.5592(3) 0.3372(6) 0.0560(13) Uani 1 1 d . U . . .
H3 H 0.4291 0.5321 0.2724 0.067 Uiso 1 1 calc R . . . .
C17 C 0.0127(4) 0.5122(4) 0.1932(7) 0.094(2) Uani 1 1 d . U . . .
H17 H 0.0213 0.4658 0.1540 0.112 Uiso 1 1 calc R . . . .
C16 C 0.0262(3) 0.5796(5) 0.1346(8) 0.090(2) Uani 1 1 d . U . . .
H16 H 0.0444 0.5791 0.0563 0.108 Uiso 1 1 calc R . . . .
C15 C 0.0128(3) 0.6474(4) 0.1912(8) 0.086(2) Uani 1 1 d . U . . .
H15 H 0.0208 0.6935 0.1509 0.103 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te2 O1 2.201(4) . ?
Te2 N2 2.250(5) . ?
Te2 C8 2.104(5) . ?
Te1 O2 2.214(4) 2_656 ?
Te1 N1 2.244(5) . ?
Te1 C1 2.102(6) . ?
O1 N1 1.368(5) . ?
O2 Te1 2.214(4) 2_656 ?
O2 N2 1.361(6) . ?
N2 C10 1.286(7) . ?
N1 C3 1.287(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(8) . ?
C11 C8 1.380(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.379(9) . ?
C8 C9 1.408(7) . ?
C1 C2 1.403(8) . ?
C1 C4 1.401(8) . ?
C7 H7 0.9300 . ?
C7 C2 1.401(8) . ?
C7 C6 1.378(8) . ?
C2 C3 1.444(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.371(10) . ?
C9 C14 1.412(8) . ?
C9 C10 1.431(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.369(10) . ?
C5 H5 0.9300 . ?
C5 C4 1.402(9) . ?
C10 H10 0.9300 . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C17 C17 1.341(15) 2 ?
C17 H17 0.9300 . ?
C17 C16 1.365(10) . ?
C16 H16 0.9300 . ?
C16 C15 1.360(10) . ?
C15 C15 1.383(16) 2 ?
C15 H15 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Te2 N2 164.59(17) . . ?
C8 Te2 O1 88.87(18) . . ?
C8 Te2 N2 75.8(2) . . ?
O2 Te1 N1 161.21(16) 2_656 . ?
C1 Te1 O2 85.3(2) . 2_656 ?
C1 Te1 N1 75.9(2) . . ?
N1 O1 Te2 115.7(3) . . ?
N2 O2 Te1 110.0(3) . 2_656 ?
O2 N2 Te2 125.4(3) . . ?
C10 N2 Te2 115.1(4) . . ?
C10 N2 O2 119.2(5) . . ?
O1 N1 Te1 127.2(3) . . ?
C3 N1 Te1 114.8(4) . . ?
C3 N1 O1 118.0(5) . . ?
C12 C11 H11 120.4 . . ?
C8 C11 H11 120.4 . . ?
C8 C11 C12 119.1(6) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.8(7) . . ?
C13 C12 H12 119.6 . . ?
C11 C8 Te2 124.6(4) . . ?
C11 C8 C9 121.2(5) . . ?
C9 C8 Te2 114.2(4) . . ?
C2 C1 Te1 114.8(4) . . ?
C4 C1 Te1 125.1(5) . . ?
C4 C1 C2 120.1(6) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C6 C7 C2 119.4(7) . . ?
C1 C2 C3 117.7(5) . . ?
C7 C2 C1 120.1(5) . . ?
C7 C2 C3 122.2(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 C7 120.5(6) . . ?
C5 C6 H6 119.7 . . ?
C8 C9 C14 117.9(6) . . ?
C8 C9 C10 118.7(5) . . ?
C14 C9 C10 123.5(5) . . ?
C9 C14 H14 119.8 . . ?
C13 C14 C9 120.4(6) . . ?
C13 C14 H14 119.8 . . ?
C6 C5 H5 119.1 . . ?
C6 C5 C4 121.7(6) . . ?
C4 C5 H5 119.1 . . ?
N2 C10 C9 116.2(5) . . ?
N2 C10 H10 121.9 . . ?
C9 C10 H10 121.9 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.5(6) . . ?
C14 C13 H13 119.7 . . ?
C1 C4 C5 118.0(7) . . ?
C1 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C3 C2 116.8(6) . . ?
N1 C3 H3 121.6 . . ?
C2 C3 H3 121.6 . . ?
C17 C17 H17 119.7 2 . ?
C17 C17 C16 120.6(5) 2 . ?
C16 C17 H17 119.7 . . ?
C17 C16 H16 120.1 . . ?
C15 C16 C17 119.7(8) . . ?
C15 C16 H16 120.1 . . ?
C16 C15 C15 119.7(5) . 2 ?
C16 C15 H15 120.2 . . ?
C15 C15 H15 120.2 2 . ?

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
Te2 O1 N1 Te1 1.4(5) . . . . ?
Te2 O1 N1 C3 -177.0(3) . . . . ?
Te2 N2 C10 C9 3.6(6) . . . . ?
Te2 C8 C9 C14 179.4(4) . . . . ?
Te2 C8 C9 C10 1.1(6) . . . . ?
Te1 O2 N2 Te2 -42.6(4) 2_656 . . . ?
Te1 O2 N2 C10 143.8(4) 2_656 . . . ?
Te1 N1 C3 C2 0.6(6) . . . . ?
Te1 C1 C2 C7 -178.7(4) . . . . ?
Te1 C1 C2 C3 1.1(6) . . . . ?
Te1 C1 C4 C5 179.6(4) . . . . ?
O1 N1 C3 C2 179.3(4) . . . . ?
O2 N2 C10 C9 177.7(4) . . . . ?
C11 C12 C13 C14 -0.2(9) . . . . ?
C11 C8 C9 C14 -0.6(7) . . . . ?
C11 C8 C9 C10 -178.8(4) . . . . ?
C12 C11 C8 Te2 -180.0(4) . . . . ?
C12 C11 C8 C9 0.0(7) . . . . ?
C8 C11 C12 C13 0.4(8) . . . . ?
C8 C9 C14 C13 0.8(8) . . . . ?
C8 C9 C10 N2 -3.2(7) . . . . ?
C1 C2 C3 N1 -1.2(7) . . . . ?
C7 C2 C3 N1 178.6(5) . . . . ?
C7 C6 C5 C4 1.0(9) . . . . ?
C2 C1 C4 C5 -0.2(8) . . . . ?
C2 C7 C6 C5 0.0(9) . . . . ?
C6 C7 C2 C1 -1.1(8) . . . . ?
C6 C7 C2 C3 179.1(5) . . . . ?
C6 C5 C4 C1 -0.9(9) . . . . ?
C9 C14 C13 C12 -0.4(9) . . . . ?
C14 C9 C10 N2 178.6(5) . . . . ?
C10 C9 C14 C13 178.9(5) . . . . ?
C4 C1 C2 C7 1.2(8) . . . . ?
C4 C1 C2 C3 -179.0(5) . . . . ?
C17 C17 C16 C15 -0.8(14) 2 . . . ?
C17 C16 C15 C15 1.4(12) . . . 2 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_twin4
_database_code_depnum_ccdc_archive 'CCDC 1530647'
_audit_update_record             
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date             2017-02-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C7 H5 N O Se'
_chemical_formula_sum            'C7 H5 N O Se'
_chemical_formula_weight         198.08
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   7.3324(9)
_cell_length_b                   8.0016(10)
_cell_length_c                   11.8324(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     694.22(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4214
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      26.60
_cell_measurement_theta_min      3.074
_shelx_estimated_absorpt_T_max   0.618
_shelx_estimated_absorpt_T_min   0.415
_exptl_absorpt_coefficient_mu    5.327
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1010 before and 0.0567 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1186 before and 0.0645 after correction.
 The Ratio of minimum to maximum transmission not present.
 The λ/2 correction factor is Not present
 
For component 3:
 wR2(int) was 0.1040 before and 0.0575 after correction.
 The Ratio of minimum to maximum transmission is 0.58.
 The λ/2 correction factor is Not present

Final HKLF 4 output contains 25696 reflections, Rint = 0.0614
 (14788 with I > 3sig(I), Rint = 0.0507)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.895
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7086
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.391
_diffrn_reflns_theta_min         3.073
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.691
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                6534
_reflns_number_total             7086
_reflns_special_details          
;
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.622
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details 
;
 Flack x determined using 665 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.017(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         7086
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0447P)²+0.1724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0876
_refine_special_details          
;
 Refined as a 3-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.399(2) 0.1669(10) 0.4343(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C3(H3)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.2854(7) 0.6462(7) 0.6773(5) 0.0113(12) Uani 1 1 d . . . . .
C4 C 0.4033(8) 0.7758(8) 0.7075(5) 0.0153(13) Uani 1 1 d . . . . .
H4 H 0.3699 0.8550 0.7636 0.018 Uiso 1 1 calc R . . . .
C5 C 0.5706(9) 0.7853(8) 0.6532(5) 0.0161(12) Uani 1 1 d . . . . .
H5 H 0.6522 0.8732 0.6721 0.019 Uiso 1 1 calc R . . . .
C6 C 0.6220(8) 0.6676(8) 0.5709(5) 0.0141(12) Uani 1 1 d . . . . .
H6 H 0.7383 0.6756 0.5360 0.017 Uiso 1 1 calc R . . . .
C7 C 0.5047(8) 0.5406(7) 0.5405(5) 0.0132(13) Uani 1 1 d . . . . .
H7 H 0.5391 0.4617 0.4845 0.016 Uiso 1 1 calc R . . . .
C2 C 0.3331(8) 0.5293(7) 0.5937(5) 0.0128(12) Uani 1 1 d . . . . .
C3 C 0.1980(7) 0.4026(9) 0.5696(5) 0.0155(12) Uani 1 1 d . . . . .
H3 H 0.2159 0.3155 0.5162 0.019 Uiso 1 1 calc R . . . .
N1 N 0.0485(7) 0.4203(6) 0.6287(4) 0.0116(9) Uani 1 1 d . . . . .
O1 O -0.0938(5) 0.3204(6) 0.6252(4) 0.0150(9) Uani 1 1 d . . . . .
Se1 Se 0.04975(7) 0.60273(7) 0.73639(5) 0.01196(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
C1 C4 1.397(8) . ?
C1 C2 1.405(8) . ?
C1 Se1 1.896(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.407(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(9) . ?
C7 H7 0.9500 . ?
C7 C2 1.410(8) . ?
C2 C3 1.446(8) . ?
C3 H3 0.9500 . ?
C3 N1 1.308(7) . ?
N1 O1 1.315(6) . ?
N1 Se1 1.938(5) . ?

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
C4 C1 C2 121.4(5) . . ?
C4 C1 Se1 127.3(5) . . ?
C2 C1 Se1 111.3(4) . . ?
C1 C4 H4 121.0 . . ?
C5 C4 C1 118.0(6) . . ?
C5 C4 H4 121.0 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.4(6) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.5(6) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C2 119.2(6) . . ?
C2 C7 H7 120.4 . . ?
C1 C2 C7 119.6(6) . . ?
C1 C2 C3 115.8(5) . . ?
C7 C2 C3 124.6(6) . . ?
C2 C3 H3 123.4 . . ?
N1 C3 C2 113.1(6) . . ?
N1 C3 H3 123.4 . . ?
C3 N1 O1 125.6(5) . . ?
C3 N1 Se1 115.4(4) . . ?
O1 N1 Se1 118.8(4) . . ?
C1 Se1 N1 84.3(2) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.399(2)
2 0.1669(10)
3 0.4343(17)

# start Validation Reply Form
_vrf_PLAT430_twin4               
;
PROBLEM: Short Inter D...A Contact Se1 .. O1 .. 2.41 Ang.
RESPONSE: The short contact is expected due to chalcogen bonding interaction
;
# end Validation Reply Form 
####################################################################### 
# 
# 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_ph462yellow_b
_database_code_depnum_ccdc_archive 'CCDC 1507754'
_audit_update_record             
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date             2016-04-21
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C28 H20 N4 O4 Te4'
_chemical_formula_sum            'C28 H20 N4 O4 Te4'
_chemical_formula_weight         986.88
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.2250(2)
_cell_length_b                   8.7915(3)
_cell_length_c                   12.1257(4)
_cell_angle_alpha                106.411(2)
_cell_angle_beta                 102.489(2)
_cell_angle_gamma                90.001(2)
_cell_volume                     719.81(4)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.13
_cell_measurement_theta_min      2.56
_shelx_estimated_absorpt_T_max   0.848
_shelx_estimated_absorpt_T_min   0.418
_exptl_absorpt_coefficient_mu    4.054
_exptl_absorpt_correction_T_max  0.8668
_exptl_absorpt_correction_T_min  0.5443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0387 before and 0.0347 after correction.
The Ratio of minimum to maximum transmission is 0.6279.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.277
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.261
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23510
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.131
_diffrn_reflns_theta_min         2.894
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4690
_reflns_number_total             5456
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.419
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.133
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         5456
_refine_ls_number_restraints     168
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0238
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0455P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0677
_refine_special_details          ?
_olex2_refinement_description    
;
1. Others
 Fixed Uiso: H10(0.027) H5(0.05) H11(0.03) H7(0.042) H12(0.034) H6(0.052)
 H4(0.038) H14(0.031) H13(0.033) H3(0.034)
 Fixed X: H10(0.0906) H5(1.3298) H11(0.4353) H7(0.949) H12(0.4628) H6(1.2286)
 H4(1.1502) H14(0.2088) H13(0.3576) H3(0.6587)
 Fixed Y: H10(0.0652) H5(0.9083) H11(0.1466) H7(0.7442) H12(-0.1266)
 H6(0.8904) H4(0.7813) H14(-0.1816) H13(-0.291) H3(0.5686)
 Fixed Z: H10(0.3377) H5(1.0058) H11(0.7877) H7(1.1519) H12(0.7426) H6(1.1719)
 H4(0.8154) H14(0.4003) H13(0.5486) H3(1.0165)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Te1 Te 0.75629(2) 0.56416(2) 0.70944(2) 0.01879(4) Uani 1 1 d . U . . .
Te2 Te 0.26463(2) 0.38930(2) 0.64186(2) 0.01942(4) Uani 1 1 d . U . . .
O2 O 0.0395(2) 0.3585(2) 0.38298(14) 0.0249(3) Uani 1 1 d . U . . .
O1 O 0.4476(2) 0.4340(2) 0.82325(14) 0.0290(4) Uani 1 1 d . U . . .
N2 N 0.1250(3) 0.2752(2) 0.45640(16) 0.0205(3) Uani 1 1 d . U . . .
N1 N 0.6125(3) 0.5218(2) 0.84477(16) 0.0216(3) Uani 1 1 d . U . . .
C9 C 0.2348(3) 0.0488(3) 0.5046(2) 0.0203(4) Uani 1 1 d . U . . .
C1 C 0.9406(3) 0.6861(3) 0.87010(19) 0.0225(4) Uani 1 1 d . U . . .
C2 C 0.8800(3) 0.6739(3) 0.9704(2) 0.0260(4) Uani 1 1 d . U . . .
C10 C 0.1395(3) 0.1236(3) 0.41785(19) 0.0223(4) Uani 1 1 d . U . . .
H10 H 0.0906 0.0652 0.3377 0.027 Uiso 1 1 calc R . . . .
C5 C 1.2148(4) 0.8487(4) 0.9962(3) 0.0416(7) Uani 1 1 d . U . . .
H5 H 1.3298 0.9083 1.0058 0.050 Uiso 1 1 calc R . . . .
C11 C 0.3903(3) 0.0810(3) 0.7091(2) 0.0252(4) Uani 1 1 d . U . . .
H11 H 0.4353 0.1466 0.7877 0.030 Uiso 1 1 calc R . . . .
C8 C 0.3071(3) 0.1478(3) 0.62006(19) 0.0198(4) Uani 1 1 d . U . . .
C7 C 0.9892(4) 0.7514(3) 1.0839(2) 0.0354(6) Uani 1 1 d . U . . .
H7 H 0.9490 0.7442 1.1519 0.042 Uiso 1 1 calc R . . . .
C12 C 0.4067(3) -0.0812(3) 0.6819(2) 0.0284(5) Uani 1 1 d . U . . .
H12 H 0.4628 -0.1266 0.7426 0.034 Uiso 1 1 calc R . . . .
C6 C 1.1547(4) 0.8377(4) 1.0954(3) 0.0433(7) Uani 1 1 d . U . . .
H6 H 1.2286 0.8904 1.1719 0.052 Uiso 1 1 calc R . . . .
C4 C 1.1085(3) 0.7732(3) 0.8828(2) 0.0317(5) Uani 1 1 d . U . . .
H4 H 1.1502 0.7813 0.8154 0.038 Uiso 1 1 calc R . . . .
C14 C 0.2550(3) -0.1150(3) 0.4785(2) 0.0258(4) Uani 1 1 d . U . . .
H14 H 0.2088 -0.1816 0.4003 0.031 Uiso 1 1 calc R . . . .
C13 C 0.3419(3) -0.1801(3) 0.5664(2) 0.0278(5) Uani 1 1 d . U . . .
H13 H 0.3576 -0.2910 0.5486 0.033 Uiso 1 1 calc R . . . .
C3 C 0.7045(3) 0.5828(3) 0.9521(2) 0.0281(5) Uani 1 1 d . U . . .
H3 H 0.6587 0.5686 1.0165 0.034 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te1 O2 2.2448(15) 2_666 ?
Te1 N1 2.2345(18) . ?
Te1 C1 2.101(2) . ?
Te2 O1 2.2347(16) . ?
Te2 N2 2.1966(18) . ?
Te2 C8 2.096(2) . ?
O2 Te1 2.2448(15) 2_666 ?
O2 N2 1.357(2) . ?
O1 N1 1.354(2) . ?
N2 C10 1.294(3) . ?
N1 C3 1.286(3) . ?
C9 C10 1.445(3) . ?
C9 C8 1.409(3) . ?
C9 C14 1.399(3) . ?
C1 C2 1.409(3) . ?
C1 C4 1.391(3) . ?
C2 C7 1.408(3) . ?
C2 C3 1.441(3) . ?
C10 H10 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C5 C4 1.396(4) . ?
C11 H11 0.9500 . ?
C11 C8 1.396(3) . ?
C11 C12 1.381(3) . ?
C7 H7 0.9500 . ?
C7 C6 1.376(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.402(4) . ?
C6 H6 0.9500 . ?
C4 H4 0.9500 . ?
C14 H14 0.9500 . ?
C14 C13 1.383(3) . ?
C13 H13 0.9500 . ?
C3 H3 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
N1 Te1 O2 164.46(7) . 2_666 ?
C1 Te1 O2 87.86(8) . 2_666 ?
C1 Te1 N1 76.61(8) . . ?
N2 Te2 O1 162.38(7) . . ?
C8 Te2 O1 86.72(8) . . ?
C8 Te2 N2 76.40(8) . . ?
N2 O2 Te1 111.60(12) . 2_666 ?
N1 O1 Te2 115.49(12) . . ?
O2 N2 Te2 122.67(14) . . ?
C10 N2 Te2 116.13(14) . . ?
C10 N2 O2 121.04(18) . . ?
O1 N1 Te1 126.29(13) . . ?
C3 N1 Te1 114.46(15) . . ?
C3 N1 O1 119.18(19) . . ?
C8 C9 C10 117.3(2) . . ?
C14 C9 C10 122.9(2) . . ?
C14 C9 C8 119.8(2) . . ?
C2 C1 Te1 113.83(16) . . ?
C4 C1 Te1 125.89(17) . . ?
C4 C1 C2 120.3(2) . . ?
C1 C2 C3 118.0(2) . . ?
C7 C2 C1 119.8(2) . . ?
C7 C2 C3 122.2(2) . . ?
N2 C10 C9 115.7(2) . . ?
N2 C10 H10 122.1 . . ?
C9 C10 H10 122.1 . . ?
C6 C5 H5 119.5 . . ?
C6 C5 C4 120.9(3) . . ?
C4 C5 H5 119.5 . . ?
C8 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C12 C11 C8 119.5(2) . . ?
C9 C8 Te2 114.28(15) . . ?
C11 C8 Te2 125.81(17) . . ?
C11 C8 C9 119.8(2) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 C2 119.4(2) . . ?
C6 C7 H7 120.3 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.2(2) . . ?
C13 C12 H12 119.4 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.7(2) . . ?
C7 C6 H6 119.7 . . ?
C1 C4 C5 118.9(2) . . ?
C1 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C9 C14 H14 119.9 . . ?
C13 C14 C9 120.1(2) . . ?
C13 C14 H14 119.9 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
N1 C3 C2 117.1(2) . . ?
N1 C3 H3 121.5 . . ?
C2 C3 H3 121.5 . . ?

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
Te1 O2 N2 Te2 89.38(14) 2_666 . . . ?
Te1 O2 N2 C10 -85.9(2) 2_666 . . . ?
Te1 N1 C3 C2 2.4(3) . . . . ?
Te1 C1 C2 C7 -179.3(2) . . . . ?
Te1 C1 C2 C3 -0.2(3) . . . . ?
Te1 C1 C4 C5 179.5(2) . . . . ?
Te2 O1 N1 Te1 -19.0(2) . . . . ?
Te2 O1 N1 C3 164.45(18) . . . . ?
Te2 N2 C10 C9 4.0(2) . . . . ?
O2 N2 C10 C9 179.54(17) . . . . ?
O1 N1 C3 C2 179.4(2) . . . . ?
C9 C14 C13 C12 1.1(3) . . . . ?
C1 C2 C7 C6 -0.3(4) . . . . ?
C1 C2 C3 N1 -1.6(4) . . . . ?
C2 C1 C4 C5 -0.3(4) . . . . ?
C2 C7 C6 C5 -0.1(5) . . . . ?
C10 C9 C8 Te2 -1.1(2) . . . . ?
C10 C9 C8 C11 176.13(19) . . . . ?
C10 C9 C14 C13 -177.8(2) . . . . ?
C11 C12 C13 C14 -1.9(4) . . . . ?
C8 C9 C10 N2 -2.0(3) . . . . ?
C8 C9 C14 C13 1.4(3) . . . . ?
C8 C11 C12 C13 0.3(3) . . . . ?
C7 C2 C3 N1 177.5(2) . . . . ?
C12 C11 C8 Te2 179.08(16) . . . . ?
C12 C11 C8 C9 2.2(3) . . . . ?
C6 C5 C4 C1 -0.1(5) . . . . ?
C4 C1 C2 C7 0.6(4) . . . . ?
C4 C1 C2 C3 179.7(2) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C14 C9 C10 N2 177.2(2) . . . . ?
C14 C9 C8 Te2 179.73(15) . . . . ?
C14 C9 C8 C11 -3.1(3) . . . . ?
C3 C2 C7 C6 -179.4(3) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ph462_2_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1507753'
_audit_update_record             
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date             2016-10-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C42 H30 N6 O6 Te6, 1.78(C H2 Cl2), 0.22(H2 O1)'
_chemical_formula_sum            'C43.78 H34 Cl3.56 N6 O6.22 Te6'
_chemical_formula_weight         1635.57
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      trigonal
_space_group_IT_number           144
_space_group_name_H-M_alt        'P 31'
_space_group_name_Hall           'P 31'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'

_cell_length_a                   14.4246(7)
_cell_length_b                   14.4246(7)
_cell_length_c                   21.3472(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3846.6(4)
_cell_formula_units_Z            3
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.255
_cell_measurement_theta_min      2.510
_shelx_estimated_absorpt_T_max   0.714
_shelx_estimated_absorpt_T_min   0.581
_exptl_absorpt_coefficient_mu    3.605
_exptl_absorpt_correction_T_max  0.7000
_exptl_absorpt_correction_T_min  0.5727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0631 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.8181.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.118
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2283
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            131669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.536
_diffrn_reflns_theta_min         2.510
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                17518
_reflns_number_total             20091
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.669
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.51(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         20091
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0264P)²+4.2435P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0686
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.49(2) 0.51(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uiso(C44) = Uiso(O44A)
4. Rigid body (RIGU) restrains
 C44, Cl4, Cl3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O44A)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
 Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(Cl3)=Sof(Cl4)=FVAR(1)
6.a Free rotating group:
 O44A(H44C,H44D)
6.b Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
6.c Aromatic/amide H refined with riding coordinates:
 C42(H42), C4(H4), C41(H41), C12(H12), C28(H28), C32(H32), C13(H13), C5(H5),
 C6(H6), C19(H19), C14(H14), C21(H21), C40(H40), C31(H31), C20(H20), C7(H7),
 C34(H34), C3(H3), C35(H35), C17(H17), C25(H25), C11(H11), C38(H38), C33(H33),
 C26(H26), C10(H10), C27(H27), C24(H24), C39(H39)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Te3 Te 0.44432(3) 0.39457(3) 0.48611(2) 0.01624(7) Uani 1 1 d . . . . .
Te5 Te 0.94027(3) 0.68766(3) 0.49258(2) 0.01785(8) Uani 1 1 d . . . . .
Te1 Te 0.66629(3) 0.90635(3) 0.48191(2) 0.01845(8) Uani 1 1 d . . . . .
Te6 Te 0.92058(3) 0.92762(3) 0.52407(2) 0.01696(7) Uani 1 1 d . . . . .
Te2 Te 0.42482(3) 0.64024(3) 0.51173(2) 0.01823(8) Uani 1 1 d . . . . .
Te4 Te 0.70577(3) 0.42082(3) 0.51580(2) 0.01794(8) Uani 1 1 d . . . . .
O6 O 0.7994(4) 0.9887(4) 0.4161(2) 0.0266(10) Uani 1 1 d . . . . .
O4 O 0.9017(4) 0.5673(4) 0.4197(2) 0.0253(9) Uani 1 1 d . . . . .
O2 O 0.3644(4) 0.4410(3) 0.41517(19) 0.0224(9) Uani 1 1 d . . . . .
O5 O 0.9902(4) 0.8740(4) 0.59676(18) 0.0228(9) Uani 1 1 d . . . . .
O1 O 0.4702(4) 0.7676(4) 0.5803(2) 0.0254(9) Uani 1 1 d . . . . .
O3 O 0.5785(3) 0.3327(4) 0.5844(2) 0.0230(9) Uani 1 1 d . . . . .
N5 N 1.0078(4) 0.7932(4) 0.5784(2) 0.0205(10) Uani 1 1 d . . . . .
N3 N 0.4820(4) 0.3237(4) 0.5702(2) 0.0197(10) Uani 1 1 d . . . . .
N1 N 0.5535(4) 0.8668(4) 0.5640(2) 0.0195(10) Uani 1 1 d . . . . .
N2 N 0.3496(4) 0.5247(4) 0.4306(2) 0.0190(9) Uani 1 1 d . . . . .
N6 N 0.8936(4) 0.9985(4) 0.4361(2) 0.0194(9) Uani 1 1 d . . . . .
N4 N 0.8176(4) 0.4682(4) 0.4327(2) 0.0192(9) Uani 1 1 d . . . . .
C29 C 1.0318(5) 0.6309(5) 0.5381(3) 0.0210(12) Uani 1 1 d . . . . .
C18 C 0.2019(5) 0.3028(5) 0.5150(3) 0.0242(12) Uani 1 1 d . . . . .
C1 C 0.7228(5) 1.0528(5) 0.5291(3) 0.0208(11) Uani 1 1 d . . . . .
C42 C 1.1710(5) 1.1086(5) 0.3894(3) 0.0260(13) Uani 1 1 d . . . . .
H42 H 1.1730 1.1400 0.3499 0.031 Uiso 1 1 calc R . . . .
C4 C 0.8080(5) 1.1511(5) 0.5093(3) 0.0247(12) Uani 1 1 d . . . . .
H4 H 0.8445 1.1564 0.4712 0.030 Uiso 1 1 calc R . . . .
C9 C 0.2745(5) 0.6333(5) 0.4128(3) 0.0210(12) Uani 1 1 d . . . . .
C41 C 1.2634(5) 1.1170(5) 0.4141(3) 0.0266(13) Uani 1 1 d . . . . .
H41 H 1.3284 1.1522 0.3911 0.032 Uiso 1 1 calc R . . . .
C15 C 0.2990(5) 0.3143(5) 0.5353(3) 0.0193(11) Uani 1 1 d . . . . .
C12 C 0.2502(6) 0.8034(6) 0.4509(4) 0.0347(17) Uani 1 1 d . . . . .
H12 H 0.2413 0.8615 0.4639 0.042 Uiso 1 1 calc R . . . .
C28 C 0.6733(6) 0.1976(5) 0.3696(3) 0.0278(13) Uani 1 1 d . . . . .
H28 H 0.7110 0.2040 0.3319 0.033 Uiso 1 1 calc R . . . .
C32 C 1.0446(5) 0.5470(5) 0.5157(3) 0.0282(14) Uani 1 1 d . . . . .
H32 H 1.0109 0.5106 0.4780 0.034 Uiso 1 1 calc R . . . .
C13 C 0.1964(6) 0.7451(6) 0.3987(3) 0.0312(15) Uani 1 1 d . . . . .
H13 H 0.1522 0.7643 0.3757 0.037 Uiso 1 1 calc R . . . .
C2 C 0.6673(5) 1.0472(5) 0.5842(3) 0.0205(11) Uani 1 1 d . . . . .
C5 C 0.8382(6) 1.2407(6) 0.5465(4) 0.0327(15) Uani 1 1 d . . . . .
H5 H 0.8974 1.3071 0.5338 0.039 Uiso 1 1 calc R . . . .
C6 C 0.7852(6) 1.2368(5) 0.6015(3) 0.0306(15) Uani 1 1 d . . . . .
H6 H 0.8071 1.2997 0.6257 0.037 Uiso 1 1 calc R . . . .
C16 C 0.3040(5) 0.2670(5) 0.5921(3) 0.0212(12) Uani 1 1 d . . . . .
C19 C 0.1125(5) 0.2473(5) 0.5529(3) 0.0276(14) Uani 1 1 d . . . . .
H19 H 0.0460 0.2387 0.5392 0.033 Uiso 1 1 calc R . . . .
C14 C 0.2062(5) 0.6588(6) 0.3795(3) 0.0289(14) Uani 1 1 d . . . . .
H14 H 0.1673 0.6173 0.3443 0.035 Uiso 1 1 calc R . . . .
C30 C 1.0822(5) 0.6853(5) 0.5934(3) 0.0234(12) Uani 1 1 d . . . . .
C21 C 0.2112(6) 0.2120(5) 0.6295(3) 0.0281(14) Uani 1 1 d . . . . .
H21 H 0.2139 0.1806 0.6681 0.034 Uiso 1 1 calc R . . . .
C40 C 1.2612(5) 1.0738(5) 0.4728(3) 0.0247(12) Uani 1 1 d . . . . .
H40 H 1.3253 1.0811 0.4900 0.030 Uiso 1 1 calc R . . . .
C8 C 0.3298(5) 0.6932(5) 0.4658(3) 0.0197(11) Uani 1 1 d . . . . .
C31 C 1.0667(5) 0.7717(5) 0.6140(3) 0.0235(12) Uani 1 1 d . . . . .
H31 H 1.0979 0.8103 0.6515 0.028 Uiso 1 1 calc R . . . .
C20 C 0.1165(5) 0.2044(5) 0.6095(3) 0.0309(15) Uani 1 1 d . . . . .
H20 H 0.0542 0.1695 0.6349 0.037 Uiso 1 1 calc R . . . .
C7 C 0.7007(6) 1.1408(5) 0.6205(3) 0.0294(14) Uani 1 1 d . . . . .
H7 H 0.6643 1.1370 0.6583 0.035 Uiso 1 1 calc R . . . .
C34 C 1.1575(6) 0.5704(6) 0.6048(3) 0.0357(17) Uani 1 1 d . . . . .
H34 H 1.2000 0.5486 0.6275 0.043 Uiso 1 1 calc R . . . .
C3 C 0.5780(5) 0.9451(5) 0.6018(3) 0.0223(12) Uani 1 1 d . . . . .
H3 H 0.5392 0.9361 0.6394 0.027 Uiso 1 1 calc R . . . .
C35 C 1.1465(6) 0.6529(6) 0.6270(3) 0.0318(15) Uani 1 1 d . . . . .
H35 H 1.1815 0.6885 0.6646 0.038 Uiso 1 1 calc R . . . .
C17 C 0.4040(5) 0.2744(5) 0.6094(3) 0.0210(11) Uani 1 1 d . . . . .
H17 H 0.4121 0.2449 0.6473 0.025 Uiso 1 1 calc R . . . .
C36 C 1.0726(5) 1.0093(5) 0.4811(3) 0.0195(11) Uani 1 1 d . . . . .
C25 C 0.5639(5) 0.1795(5) 0.4817(3) 0.0239(12) Uani 1 1 d . . . . .
H25 H 0.5265 0.1727 0.5196 0.029 Uiso 1 1 calc R . . . .
C11 C 0.3180(5) 0.7786(5) 0.4852(3) 0.0248(13) Uani 1 1 d . . . . .
H11 H 0.3550 0.8194 0.5210 0.030 Uiso 1 1 calc R . . . .
C43 C 0.7200(8) 0.7193(8) 0.6470(5) 0.076(3) Uani 1 1 d . . . A 1
H43A H 0.7212 0.7851 0.6327 0.091 Uiso 1 1 calc R . . A 1
H43B H 0.7941 0.7322 0.6446 0.091 Uiso 1 1 calc R . . A 1
C44 C 0.6308(7) 0.6019(8) 0.3582(4) 0.0339(17) Uiso 0.780(5) 1 d . U P B 1
H44A H 0.5594 0.5782 0.3767 0.041 Uiso 0.780(5) 1 calc R . P B 1
H44B H 0.6435 0.5404 0.3590 0.041 Uiso 0.780(5) 1 calc R . P B 1
C37 C 1.0740(5) 1.0538(5) 0.4225(3) 0.0200(11) Uani 1 1 d . . . . .
C38 C 0.9760(5) 1.0449(5) 0.3999(3) 0.0207(11) Uani 1 1 d . . . . .
H38 H 0.9722 1.0721 0.3601 0.025 Uiso 1 1 calc R . . . .
C33 C 1.1090(6) 0.5182(6) 0.5506(4) 0.0334(16) Uani 1 1 d . . . . .
H33 H 1.1189 0.4615 0.5363 0.040 Uiso 1 1 calc R . . . .
C23 C 0.7048(5) 0.2876(5) 0.4084(3) 0.0211(12) Uani 1 1 d . . . . .
C26 C 0.5329(6) 0.0900(5) 0.4432(4) 0.0314(15) Uani 1 1 d . . . . .
H26 H 0.4749 0.0223 0.4553 0.038 Uiso 1 1 calc R . . . .
C10 C 0.2869(5) 0.5430(5) 0.3955(3) 0.0206(11) Uani 1 1 d . . . . .
H10 H 0.2509 0.4993 0.3603 0.025 Uiso 1 1 calc R . . . .
C27 C 0.5872(6) 0.0999(5) 0.3869(3) 0.0295(14) Uani 1 1 d . . . . .
H27 H 0.5647 0.0394 0.3605 0.035 Uiso 1 1 calc R . . . .
C24 C 0.7955(5) 0.3916(5) 0.3931(3) 0.0225(12) Uani 1 1 d . . . . .
H24 H 0.8364 0.4030 0.3561 0.027 Uiso 1 1 calc R . . . .
C22 C 0.6497(5) 0.2781(5) 0.4643(3) 0.0202(11) Uani 1 1 d . . . . .
C39 C 1.1658(5) 1.0199(5) 0.5069(3) 0.0212(11) Uani 1 1 d . . . . .
H39 H 1.1648 0.9909 0.5470 0.025 Uiso 1 1 calc R . . . .
Cl3 Cl 0.7290(2) 0.7069(2) 0.40286(12) 0.0468(8) Uani 0.780(5) 1 d . U P B 1
Cl4 Cl 0.63286(19) 0.6426(2) 0.27975(11) 0.0377(7) Uani 0.780(5) 1 d . U P B 1
Cl2 Cl 0.63948(18) 0.61520(17) 0.59736(9) 0.0452(4) Uani 1 1 d . . . A 1
Cl1 Cl 0.67636(16) 0.69386(19) 0.72578(10) 0.0438(5) Uani 1 1 d . . . A 1
H18 H 0.197(5) 0.328(5) 0.478(3) 0.017(16) Uiso 1 1 d . . . C 1
O44A O 0.6823(19) 0.6154(19) 0.4084(10) 0.0339(17) Uiso 0.220(5) 1 d . . P B 2
H44C H 0.6283 0.5508 0.4124 0.051 Uiso 0.220(5) 1 d G . P B 2
H44D H 0.7365 0.6126 0.3925 0.051 Uiso 0.220(5) 1 d G . P B 2


_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
Te3 O2 2.201(4) . ?
Te3 N3 2.262(5) . ?
Te3 C15 2.099(6) . ?
Te5 O4 2.185(4) . ?
Te5 N5 2.268(5) . ?
Te5 C29 2.107(6) . ?
Te1 O6 2.189(5) . ?
Te1 N1 2.261(5) . ?
Te1 C1 2.102(6) . ?
Te6 O5 2.189(4) . ?
Te6 N6 2.264(5) . ?
Te6 C36 2.110(6) . ?
Te2 O1 2.178(4) . ?
Te2 N2 2.268(5) . ?
Te2 C8 2.114(6) . ?
Te4 O3 2.190(4) . ?
Te4 N4 2.261(5) . ?
Te4 C22 2.105(6) . ?
O6 N6 1.361(6) . ?
O4 N4 1.363(7) . ?
O2 N2 1.368(7) . ?
O5 N5 1.368(7) . ?
O1 N1 1.375(7) . ?
O3 N3 1.366(7) . ?
N5 C31 1.288(8) . ?
N3 C17 1.293(7) . ?
N1 C3 1.286(7) . ?
N2 C10 1.300(7) . ?
N6 C38 1.289(8) . ?
N4 C24 1.298(8) . ?
C29 C32 1.397(9) . ?
C29 C30 1.403(9) . ?
C18 C15 1.395(9) . ?
C18 C19 1.388(9) . ?
C18 H18 0.88(6) . ?
C1 C4 1.399(9) . ?
C1 C2 1.401(9) . ?
C42 H42 0.9500 . ?
C42 C41 1.382(10) . ?
C42 C37 1.405(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(10) . ?
C9 C14 1.404(9) . ?
C9 C8 1.405(9) . ?
C9 C10 1.447(9) . ?
C41 H41 0.9500 . ?
C41 C40 1.393(9) . ?
C15 C16 1.411(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.378(11) . ?
C12 C11 1.403(10) . ?
C28 H28 0.9500 . ?
C28 C23 1.409(8) . ?
C28 C27 1.384(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.405(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(10) . ?
C2 C7 1.416(8) . ?
C2 C3 1.440(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.371(10) . ?
C16 C21 1.413(9) . ?
C16 C17 1.440(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.370(10) . ?
C14 H14 0.9500 . ?
C30 C31 1.440(9) . ?
C30 C35 1.425(8) . ?
C21 H21 0.9500 . ?
C21 C20 1.383(10) . ?
C40 H40 0.9500 . ?
C40 C39 1.398(8) . ?
C8 C11 1.388(9) . ?
C31 H31 0.9500 . ?
C20 H20 0.9500 . ?
C7 H7 0.9500 . ?
C34 H34 0.9500 . ?
C34 C35 1.362(11) . ?
C34 C33 1.367(11) . ?
C3 H3 0.9500 . ?
C35 H35 0.9500 . ?
C17 H17 0.9500 . ?
C36 C37 1.402(8) . ?
C36 C39 1.389(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.402(9) . ?
C25 C22 1.391(9) . ?
C11 H11 0.9500 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 Cl2 1.727(10) . ?
C43 Cl1 1.769(10) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 Cl3 1.751(10) . ?
C44 Cl4 1.770(9) . ?
C37 C38 1.438(9) . ?
C38 H38 0.9500 . ?
C33 H33 0.9500 . ?
C23 C24 1.451(9) . ?
C23 C22 1.403(9) . ?
C26 H26 0.9500 . ?
C26 C27 1.402(10) . ?
C10 H10 0.9500 . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C39 H39 0.9500 . ?
O44A H44C 0.8699 . ?
O44A H44D 0.8701 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Te3 N3 164.65(18) . . ?
C15 Te3 O2 88.9(2) . . ?
C15 Te3 N3 75.7(2) . . ?
O4 Te5 N5 164.10(19) . . ?
C29 Te5 O4 88.8(2) . . ?
C29 Te5 N5 75.3(2) . . ?
O6 Te1 N1 163.62(18) . . ?
C1 Te1 O6 88.2(2) . . ?
C1 Te1 N1 75.6(2) . . ?
O5 Te6 N6 163.93(17) . . ?
C36 Te6 O5 88.5(2) . . ?
C36 Te6 N6 75.7(2) . . ?
O1 Te2 N2 164.70(19) . . ?
C8 Te2 O1 89.0(2) . . ?
C8 Te2 N2 75.7(2) . . ?
O3 Te4 N4 164.60(18) . . ?
C22 Te4 O3 88.9(2) . . ?
C22 Te4 N4 75.7(2) . . ?
N6 O6 Te1 114.5(3) . . ?
N4 O4 Te5 115.4(3) . . ?
N2 O2 Te3 116.0(3) . . ?
N5 O5 Te6 114.3(3) . . ?
N1 O1 Te2 116.4(3) . . ?
N3 O3 Te4 115.2(3) . . ?
O5 N5 Te5 127.0(4) . . ?
C31 N5 Te5 115.4(4) . . ?
C31 N5 O5 117.6(5) . . ?
O3 N3 Te3 126.7(4) . . ?
C17 N3 Te3 114.9(4) . . ?
C17 N3 O3 118.3(5) . . ?
O1 N1 Te1 127.1(3) . . ?
C3 N1 Te1 114.7(4) . . ?
C3 N1 O1 117.9(5) . . ?
O2 N2 Te2 127.2(3) . . ?
C10 N2 Te2 114.6(4) . . ?
C10 N2 O2 118.1(5) . . ?
O6 N6 Te6 126.9(4) . . ?
C38 N6 Te6 114.1(4) . . ?
C38 N6 O6 118.7(5) . . ?
O4 N4 Te4 127.1(3) . . ?
C24 N4 Te4 114.8(4) . . ?
C24 N4 O4 118.1(5) . . ?
C32 C29 Te5 123.9(5) . . ?
C32 C29 C30 121.2(6) . . ?
C30 C29 Te5 114.9(4) . . ?
C15 C18 H18 120(4) . . ?
C19 C18 C15 118.4(6) . . ?
C19 C18 H18 121(4) . . ?
C4 C1 Te1 125.2(5) . . ?
C4 C1 C2 119.9(6) . . ?
C2 C1 Te1 114.9(5) . . ?
C41 C42 H42 119.9 . . ?
C41 C42 C37 120.1(6) . . ?
C37 C42 H42 119.9 . . ?
C1 C4 H4 120.7 . . ?
C5 C4 C1 118.6(6) . . ?
C5 C4 H4 120.7 . . ?
C14 C9 C8 120.2(6) . . ?
C14 C9 C10 121.7(6) . . ?
C8 C9 C10 118.1(5) . . ?
C42 C41 H41 120.0 . . ?
C42 C41 C40 120.0(6) . . ?
C40 C41 H41 120.0 . . ?
C18 C15 Te3 125.3(5) . . ?
C18 C15 C16 120.0(6) . . ?
C16 C15 Te3 114.7(4) . . ?
C13 C12 H12 119.4 . . ?
C13 C12 C11 121.2(7) . . ?
C11 C12 H12 119.4 . . ?
C23 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C27 C28 C23 119.6(6) . . ?
C29 C32 H32 121.1 . . ?
C29 C32 C33 117.8(7) . . ?
C33 C32 H32 121.1 . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.6(6) . . ?
C14 C13 H13 119.7 . . ?
C1 C2 C7 119.5(6) . . ?
C1 C2 C3 118.1(5) . . ?
C7 C2 C3 122.4(6) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 C4 122.5(7) . . ?
C6 C5 H5 118.8 . . ?
C5 C6 H6 120.5 . . ?
C7 C6 C5 119.0(6) . . ?
C7 C6 H6 120.5 . . ?
C15 C16 C21 119.6(6) . . ?
C15 C16 C17 118.4(5) . . ?
C21 C16 C17 122.0(6) . . ?
C18 C19 H19 118.7 . . ?
C20 C19 C18 122.5(6) . . ?
C20 C19 H19 118.7 . . ?
C9 C14 H14 120.4 . . ?
C13 C14 C9 119.1(7) . . ?
C13 C14 H14 120.4 . . ?
C29 C30 C31 118.7(5) . . ?
C29 C30 C35 118.7(6) . . ?
C35 C30 C31 122.6(6) . . ?
C16 C21 H21 120.3 . . ?
C20 C21 C16 119.4(6) . . ?
C20 C21 H21 120.3 . . ?
C41 C40 H40 119.6 . . ?
C41 C40 C39 120.8(6) . . ?
C39 C40 H40 119.6 . . ?
C9 C8 Te2 115.0(4) . . ?
C11 C8 Te2 124.8(5) . . ?
C11 C8 C9 120.2(6) . . ?
N5 C31 C30 115.8(6) . . ?
N5 C31 H31 122.1 . . ?
C30 C31 H31 122.1 . . ?
C19 C20 C21 120.0(6) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.5(6) . . ?
C6 C7 H7 119.7 . . ?
C35 C34 H34 119.2 . . ?
C35 C34 C33 121.6(6) . . ?
C33 C34 H34 119.2 . . ?
N1 C3 C2 116.5(6) . . ?
N1 C3 H3 121.7 . . ?
C2 C3 H3 121.7 . . ?
C30 C35 H35 120.3 . . ?
C34 C35 C30 119.4(7) . . ?
C34 C35 H35 120.3 . . ?
N3 C17 C16 116.1(6) . . ?
N3 C17 H17 121.9 . . ?
C16 C17 H17 121.9 . . ?
C37 C36 Te6 114.7(4) . . ?
C39 C36 Te6 124.6(4) . . ?
C39 C36 C37 120.7(5) . . ?
C26 C25 H25 120.1 . . ?
C22 C25 H25 120.1 . . ?
C22 C25 C26 119.8(6) . . ?
C12 C11 H11 120.6 . . ?
C8 C11 C12 118.7(7) . . ?
C8 C11 H11 120.6 . . ?
H43A C43 H43B 107.8 . . ?
Cl2 C43 H43A 109.0 . . ?
Cl2 C43 H43B 109.0 . . ?
Cl2 C43 Cl1 112.8(5) . . ?
Cl1 C43 H43A 109.0 . . ?
Cl1 C43 H43B 109.0 . . ?
H44A C44 H44B 108.1 . . ?
Cl3 C44 H44A 109.5 . . ?
Cl3 C44 H44B 109.5 . . ?
Cl3 C44 Cl4 110.8(5) . . ?
Cl4 C44 H44A 109.5 . . ?
Cl4 C44 H44B 109.5 . . ?
C42 C37 C38 122.6(6) . . ?
C36 C37 C42 119.3(6) . . ?
C36 C37 C38 118.0(5) . . ?
N6 C38 C37 117.2(5) . . ?
N6 C38 H38 121.4 . . ?
C37 C38 H38 121.4 . . ?
C32 C33 H33 119.4 . . ?
C34 C33 C32 121.3(7) . . ?
C34 C33 H33 119.4 . . ?
C28 C23 C24 121.9(6) . . ?
C22 C23 C28 120.3(6) . . ?
C22 C23 C24 117.8(5) . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.3(6) . . ?
C27 C26 H26 119.9 . . ?
N2 C10 C9 116.6(6) . . ?
N2 C10 H10 121.7 . . ?
C9 C10 H10 121.7 . . ?
C28 C27 C26 120.2(6) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N4 C24 C23 116.4(5) . . ?
N4 C24 H24 121.8 . . ?
C23 C24 H24 121.8 . . ?
C25 C22 Te4 124.9(5) . . ?
C25 C22 C23 119.8(6) . . ?
C23 C22 Te4 115.3(4) . . ?
C40 C39 H39 120.5 . . ?
C36 C39 C40 119.0(6) . . ?
C36 C39 H39 120.5 . . ?
H44C O44A H44D 109.4 . . ?

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
Te3 O2 N2 Te2 12.6(5) . . . . ?
Te3 O2 N2 C10 -168.2(4) . . . . ?
Te3 N3 C17 C16 3.3(7) . . . . ?
Te3 C15 C16 C21 179.2(4) . . . . ?
Te3 C15 C16 C17 -2.2(7) . . . . ?
Te5 O4 N4 Te4 6.7(6) . . . . ?
Te5 O4 N4 C24 -175.5(4) . . . . ?
Te5 N5 C31 C30 1.0(7) . . . . ?
Te5 C29 C32 C33 179.3(5) . . . . ?
Te5 C29 C30 C31 0.7(7) . . . . ?
Te5 C29 C30 C35 -179.5(5) . . . . ?
Te1 O6 N6 Te6 5.5(6) . . . . ?
Te1 O6 N6 C38 179.2(4) . . . . ?
Te1 N1 C3 C2 4.7(7) . . . . ?
Te1 C1 C4 C5 -178.2(5) . . . . ?
Te1 C1 C2 C7 178.3(4) . . . . ?
Te1 C1 C2 C3 -1.3(7) . . . . ?
Te6 O5 N5 Te5 -15.0(5) . . . . ?
Te6 O5 N5 C31 167.0(4) . . . . ?
Te6 N6 C38 C37 -5.4(7) . . . . ?
Te6 C36 C37 C42 -179.1(4) . . . . ?
Te6 C36 C37 C38 3.5(7) . . . . ?
Te6 C36 C39 C40 178.4(4) . . . . ?
Te2 O1 N1 Te1 -11.3(6) . . . . ?
Te2 O1 N1 C3 175.9(4) . . . . ?
Te2 N2 C10 C9 0.2(7) . . . . ?
Te2 C8 C11 C12 -178.6(5) . . . . ?
Te4 O3 N3 Te3 -2.2(6) . . . . ?
Te4 O3 N3 C17 -178.6(4) . . . . ?
Te4 N4 C24 C23 -1.3(7) . . . . ?
O6 N6 C38 C37 -179.9(5) . . . . ?
O4 N4 C24 C23 -179.4(5) . . . . ?
O2 N2 C10 C9 -179.1(5) . . . . ?
O5 N5 C31 C30 179.3(5) . . . . ?
O1 N1 C3 C2 178.4(5) . . . . ?
O3 N3 C17 C16 -179.9(5) . . . . ?
C29 C32 C33 C34 0.0(10) . . . . ?
C29 C30 C31 N5 -1.1(9) . . . . ?
C29 C30 C35 C34 0.1(9) . . . . ?
C18 C15 C16 C21 -2.8(9) . . . . ?
C18 C15 C16 C17 175.8(6) . . . . ?
C18 C19 C20 C21 -2.5(10) . . . . ?
C1 C4 C5 C6 -1.8(10) . . . . ?
C1 C2 C7 C6 1.4(9) . . . . ?
C1 C2 C3 N1 -2.5(9) . . . . ?
C42 C41 C40 C39 1.2(9) . . . . ?
C42 C37 C38 N6 -175.7(6) . . . . ?
C4 C1 C2 C7 -2.4(9) . . . . ?
C4 C1 C2 C3 178.1(5) . . . . ?
C4 C5 C6 C7 0.9(10) . . . . ?
C9 C8 C11 C12 0.0(9) . . . . ?
C41 C42 C37 C36 1.0(9) . . . . ?
C41 C42 C37 C38 178.2(6) . . . . ?
C41 C40 C39 C36 0.4(9) . . . . ?
C15 C18 C19 C20 0.5(10) . . . . ?
C15 C16 C21 C20 0.8(9) . . . . ?
C15 C16 C17 N3 -0.9(8) . . . . ?
C12 C13 C14 C9 -2.0(10) . . . . ?
C28 C23 C24 N4 -179.2(6) . . . . ?
C28 C23 C22 Te4 -179.1(5) . . . . ?
C28 C23 C22 C25 0.3(9) . . . . ?
C32 C29 C30 C31 179.5(6) . . . . ?
C32 C29 C30 C35 -0.6(9) . . . . ?
C13 C12 C11 C8 -0.3(9) . . . . ?
C2 C1 C4 C5 2.5(9) . . . . ?
C5 C6 C7 C2 -0.7(10) . . . . ?
C16 C21 C20 C19 1.9(10) . . . . ?
C19 C18 C15 Te3 180.0(4) . . . . ?
C19 C18 C15 C16 2.1(9) . . . . ?
C14 C9 C8 Te2 178.0(4) . . . . ?
C14 C9 C8 C11 -0.6(9) . . . . ?
C14 C9 C10 N2 -178.0(6) . . . . ?
C30 C29 C32 C33 0.6(9) . . . . ?
C21 C16 C17 N3 177.7(5) . . . . ?
C8 C9 C14 C13 1.7(9) . . . . ?
C8 C9 C10 N2 -0.5(8) . . . . ?
C31 C30 C35 C34 179.9(6) . . . . ?
C7 C2 C3 N1 178.0(6) . . . . ?
C3 C2 C7 C6 -179.0(6) . . . . ?
C35 C30 C31 N5 179.0(6) . . . . ?
C35 C34 C33 C32 -0.6(11) . . . . ?
C17 C16 C21 C20 -177.8(6) . . . . ?
C36 C37 C38 N6 1.5(8) . . . . ?
C25 C26 C27 C28 1.5(10) . . . . ?
C11 C12 C13 C14 1.3(10) . . . . ?
C37 C42 C41 C40 -1.9(9) . . . . ?
C37 C36 C39 C40 -1.3(9) . . . . ?
C33 C34 C35 C30 0.5(11) . . . . ?
C23 C28 C27 C26 -1.3(10) . . . . ?
C26 C25 C22 Te4 179.2(5) . . . . ?
C26 C25 C22 C23 -0.1(9) . . . . ?
C10 C9 C14 C13 179.1(6) . . . . ?
C10 C9 C8 Te2 0.5(7) . . . . ?
C10 C9 C8 C11 -178.1(5) . . . . ?
C27 C28 C23 C24 179.1(6) . . . . ?
C27 C28 C23 C22 0.4(9) . . . . ?
C24 C23 C22 Te4 2.2(7) . . . . ?
C24 C23 C22 C25 -178.4(6) . . . . ?
C22 C25 C26 C27 -0.8(9) . . . . ?
C22 C23 C24 N4 -0.6(8) . . . . ?
C39 C36 C37 C42 0.6(9) . . . . ?
C39 C36 C37 C38 -176.8(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.49(2)
2 0.51(2)

