# 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_TcOTePh
_database_code_depnum_ccdc_archive 'CCDC 1536445'
_audit_update_record             
;
2017-03-07 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;



_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
 Tetrabutylammoniumtetra(phenyltelurolato)oxidotechnetate(V)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H20 O Tc Te4 1-, C16 H36 N1 1+, C H2 Cl2'
_chemical_formula_sum            'C41 H58 Cl2 N1 O1 Tc1 Te4'
_chemical_formula_weight         1260.18

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'
Tc Tc -1.4390 0.7593 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+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                   15.907(2)
_cell_length_b                   18.392(2)
_cell_length_c                   16.246(2)
_cell_angle_alpha                90
_cell_angle_beta                 90.350(10)
_cell_angle_gamma                90
_cell_volume                     4752.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    15908
_cell_measurement_theta_min      3.34
_cell_measurement_theta_max      29.09

_exptl_crystal_description       block
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_F_000             2416
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.851
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_T_max  0.8045
_exptl_absorpt_process_details   
;
P. Coppens in "Crystallographic Computing" ed F.R Ahmed, S.R. Hall 
and C.P.Huber, Copenhagen, Munksgaard, (1979) pp 255-270
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            22751
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.346
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5191
_reflns_number_gt                3175
_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       'STOE X-AREA'
_computing_cell_refinement       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0733P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5191
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0464
_refine_ls_wR_factor_ref         0.1320
_refine_ls_wR_factor_gt          0.1127
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_restrained_S_all      0.930
_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
Cl1 Cl 0.0763(5) 0.4140(4) 0.7166(8) 0.365(6) Uani 1 1 d . . . . .
C50 C 0.0000 0.3613(12) 0.7500 0.228(16) Uani 1 2 d S T P . .
H50A H 0.0204 0.3305 0.7942 0.274 Uiso 0.5 1 calc R U P . .
H50B H -0.0204 0.3305 0.7058 0.274 Uiso 0.5 1 calc R U P . .
Tc1 Tc 0.0000 0.12402(4) 0.7500 0.0445(2) Uani 1 2 d S T P . .
O1 O 0.0000 0.0337(3) 0.7500 0.0628(18) Uani 1 2 d S T P . .
Te1 Te 0.03807(3) 0.16921(3) 0.90138(3) 0.06058(18) Uani 1 1 d . . . . .
Te2 Te -0.15213(3) 0.17352(3) 0.78670(3) 0.05484(16) Uani 1 1 d . . . . .
C11 C -0.0708(4) 0.1492(4) 0.9754(3) 0.0466(16) Uani 1 1 d . . . . .
C12 C -0.0850(5) 0.0794(4) 1.0027(5) 0.0636(19) Uani 1 1 d . . . . .
H12 H -0.0507 0.0417 0.9847 0.076 Uiso 1 1 calc R U . . .
C13 C -0.1492(6) 0.0648(5) 1.0564(5) 0.083(3) Uani 1 1 d . . . . .
H13 H -0.1584 0.0174 1.0740 0.100 Uiso 1 1 calc R U . . .
C14 C -0.1997(5) 0.1196(6) 1.0839(5) 0.079(3) Uani 1 1 d . . . . .
H14 H -0.2424 0.1096 1.1210 0.095 Uiso 1 1 calc R U . . .
C15 C -0.1874(5) 0.1887(5) 1.0572(5) 0.070(2) Uani 1 1 d . . . . .
H15 H -0.2227 0.2257 1.0752 0.084 Uiso 1 1 calc R U . . .
C16 C -0.1225(4) 0.2043(5) 1.0033(4) 0.0574(18) Uani 1 1 d . . . . .
H16 H -0.1137 0.2519 0.9860 0.069 Uiso 1 1 calc R U . . .
C21 C -0.2299(4) 0.1573(4) 0.6795(4) 0.0469(16) Uani 1 1 d . . . . .
C22 C -0.2637(4) 0.0894(4) 0.6661(4) 0.0568(18) Uani 1 1 d . . . . .
H22 H -0.2486 0.0510 0.7004 0.068 Uiso 1 1 calc R U . . .
C23 C -0.3201(5) 0.0776(5) 0.6016(5) 0.070(2) Uani 1 1 d . . . . .
H23 H -0.3423 0.0315 0.5928 0.084 Uiso 1 1 calc R U . . .
C24 C -0.3429(5) 0.1340(5) 0.5510(5) 0.069(2) Uani 1 1 d . . . . .
H24 H -0.3803 0.1262 0.5077 0.083 Uiso 1 1 calc R U . . .
C25 C -0.3103(4) 0.2021(5) 0.5647(5) 0.065(2) Uani 1 1 d . . . . .
H25 H -0.3258 0.2403 0.5303 0.078 Uiso 1 1 calc R U . . .
C26 C -0.2542(4) 0.2147(4) 0.6297(4) 0.0548(17) Uani 1 1 d . . . . .
H26 H -0.2334 0.2612 0.6393 0.066 Uiso 1 1 calc R U . . .
N1 N 0.5000 0.7416(4) 0.2500 0.0445(17) Uani 1 2 d S T P . .
C31 C 0.4286(4) 0.7883(4) 0.2163(4) 0.0481(15) Uani 1 1 d . . . . .
H31A H 0.4025 0.8136 0.2619 0.058 Uiso 1 1 calc R U . . .
H31B H 0.3865 0.7566 0.1921 0.058 Uiso 1 1 calc R U . . .
C32 C 0.4546(4) 0.8445(4) 0.1519(4) 0.0528(17) Uani 1 1 d . . . . .
H32A H 0.4979 0.8758 0.1749 0.063 Uiso 1 1 calc R U . . .
H32B H 0.4780 0.8197 0.1045 0.063 Uiso 1 1 calc R U . . .
C33 C 0.3805(5) 0.8901(4) 0.1250(5) 0.067(2) Uani 1 1 d . . . . .
H33A H 0.3360 0.8585 0.1052 0.081 Uiso 1 1 calc R U . . .
H33B H 0.3592 0.9169 0.1719 0.081 Uiso 1 1 calc R U . . .
C34 C 0.4038(6) 0.9430(6) 0.0578(6) 0.096(3) Uani 1 1 d . . . . .
H34A H 0.3553 0.9710 0.0424 0.144 Uiso 1 1 calc R U . . .
H34B H 0.4471 0.9751 0.0776 0.144 Uiso 1 1 calc R U . . .
H34C H 0.4239 0.9167 0.0109 0.144 Uiso 1 1 calc R U . . .
C41 C 0.5335(4) 0.6941(4) 0.1807(4) 0.0487(15) Uani 1 1 d . . . . .
H41A H 0.4864 0.6681 0.1566 0.058 Uiso 1 1 calc R U . . .
H41B H 0.5558 0.7259 0.1385 0.058 Uiso 1 1 calc R U . . .
C42 C 0.6002(4) 0.6396(4) 0.2030(4) 0.0502(16) Uani 1 1 d . . . . .
H42A H 0.5786 0.6066 0.2443 0.060 Uiso 1 1 calc R U . . .
H42B H 0.6484 0.6647 0.2265 0.060 Uiso 1 1 calc R U . . .
C43 C 0.6277(5) 0.5965(4) 0.1282(5) 0.066(2) Uani 1 1 d . . . . .
H43A H 0.5806 0.5679 0.1084 0.080 Uiso 1 1 calc R U . . .
H43B H 0.6432 0.6302 0.0849 0.080 Uiso 1 1 calc R U . . .
C44 C 0.7005(6) 0.5467(5) 0.1450(6) 0.088(3) Uani 1 1 d . . . . .
H44A H 0.7148 0.5212 0.0955 0.132 Uiso 1 1 calc R U . . .
H44B H 0.7479 0.5747 0.1634 0.132 Uiso 1 1 calc R U . . .
H44C H 0.6853 0.5124 0.1869 0.132 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
Cl1 C50 1.647(14) . ?
C50 Cl1 1.647(14) 2_556 ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
Tc1 O1 1.662(6) . ?
Tc1 Te2 2.6566(6) . ?
Tc1 Te2 2.6567(6) 2_556 ?
Tc1 Te1 2.6622(6) . ?
Tc1 Te1 2.6623(6) 2_556 ?
Te1 C11 2.146(6) . ?
Te2 C21 2.151(7) . ?
C11 C12 1.378(10) . ?
C11 C16 1.384(9) . ?
C12 C13 1.373(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.365(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.356(12) . ?
C14 H14 0.9300 . ?
C15 C16 1.389(10) . ?
C15 H15 0.9300 . ?
C16 H16 0.9300 . ?
C21 C22 1.376(10) . ?
C21 C26 1.386(9) . ?
C22 C23 1.393(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.370(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.373(12) . ?
C24 H24 0.9300 . ?
C25 C26 1.398(10) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
N1 C41 1.522(7) . ?
N1 C41 1.522(7) 2_655 ?
N1 C31 1.523(7) 2_655 ?
N1 C31 1.523(7) . ?
C31 C32 1.530(9) . ?
C31 H31A 0.9700 . ?
C31 H31B 0.9700 . ?
C32 C33 1.510(9) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 C34 1.509(11) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C41 C42 1.504(9) . ?
C41 H41A 0.9700 . ?
C41 H41B 0.9700 . ?
C42 C43 1.518(9) . ?
C42 H42A 0.9700 . ?
C42 H42B 0.9700 . ?
C43 C44 1.500(11) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?

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
Cl1 C50 Cl1 108.0(13) . 2_556 ?
Cl1 C50 H50A 110.1 . . ?
Cl1 C50 H50A 110.1 2_556 . ?
Cl1 C50 H50B 110.1 . . ?
Cl1 C50 H50B 110.1 2_556 . ?
H50A C50 H50B 108.4 . . ?
O1 Tc1 Te2 110.04(2) . . ?
O1 Tc1 Te2 110.04(2) . 2_556 ?
Te2 Tc1 Te2 139.92(4) . 2_556 ?
O1 Tc1 Te1 108.19(2) . . ?
Te2 Tc1 Te1 83.573(19) . . ?
Te2 Tc1 Te1 84.146(19) 2_556 . ?
O1 Tc1 Te1 108.19(2) . 2_556 ?
Te2 Tc1 Te1 84.146(19) . 2_556 ?
Te2 Tc1 Te1 83.572(19) 2_556 2_556 ?
Te1 Tc1 Te1 143.62(4) . 2_556 ?
C11 Te1 Tc1 106.50(16) . . ?
C21 Te2 Tc1 106.92(15) . . ?
C12 C11 C16 118.5(6) . . ?
C12 C11 Te1 118.4(5) . . ?
C16 C11 Te1 122.8(5) . . ?
C13 C12 C11 120.7(8) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.3(8) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 120.1(7) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C16 120.3(7) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C11 C16 C15 120.1(8) . . ?
C11 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C22 C21 C26 119.5(6) . . ?
C22 C21 Te2 118.5(5) . . ?
C26 C21 Te2 121.6(5) . . ?
C21 C22 C23 120.6(7) . . ?
C21 C22 H22 119.7 . . ?
C23 C22 H22 119.7 . . ?
C24 C23 C22 120.0(8) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C23 C24 C25 119.7(8) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C25 C26 120.8(8) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C21 C26 C25 119.3(7) . . ?
C21 C26 H26 120.4 . . ?
C25 C26 H26 120.4 . . ?
C41 N1 C41 110.1(7) . 2_655 ?
C41 N1 C31 109.0(3) . 2_655 ?
C41 N1 C31 108.7(4) 2_655 2_655 ?
C41 N1 C31 108.7(4) . . ?
C41 N1 C31 109.0(3) 2_655 . ?
C31 N1 C31 111.3(7) 2_655 . ?
N1 C31 C32 115.0(4) . . ?
N1 C31 H31A 108.5 . . ?
C32 C31 H31A 108.5 . . ?
N1 C31 H31B 108.5 . . ?
C32 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
C33 C32 C31 111.1(5) . . ?
C33 C32 H32A 109.4 . . ?
C31 C32 H32A 109.4 . . ?
C33 C32 H32B 109.4 . . ?
C31 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
C34 C33 C32 111.9(6) . . ?
C34 C33 H33A 109.2 . . ?
C32 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 C41 N1 117.0(5) . . ?
C42 C41 H41A 108.0 . . ?
N1 C41 H41A 108.0 . . ?
C42 C41 H41B 108.0 . . ?
N1 C41 H41B 108.0 . . ?
H41A C41 H41B 107.3 . . ?
C41 C42 C43 111.2(6) . . ?
C41 C42 H42A 109.4 . . ?
C43 C42 H42A 109.4 . . ?
C41 C42 H42B 109.4 . . ?
C43 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C44 C43 C42 113.5(7) . . ?
C44 C43 H43A 108.9 . . ?
C42 C43 H43A 108.9 . . ?
C44 C43 H43B 108.9 . . ?
C42 C43 H43B 108.9 . . ?
H43A C43 H43B 107.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

_refine_diff_density_max         0.841
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.138

####################################################################### 
# 
# 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_TcOSePh4
_database_code_depnum_ccdc_archive 'CCDC 1536444'
_audit_update_record             
;
2017-03-07 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
'tetrabutylammonium tetra(phenylselenolato)oxidotechnetate(V) CH2Cl2 solvate'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'N C16 H36 1+, C24 H20 O Se4 Tc 1-, C H2 Cl2'
_chemical_formula_sum            'C41 H58 Cl2 N O Se4 Tc'
_chemical_formula_weight         1065.62

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'
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'
Tc Tc -1.4390 0.7593 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+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                   15.4526(8)
_cell_length_b                   18.3197(11)
_cell_length_c                   15.7324(8)
_cell_angle_alpha                90
_cell_angle_beta                 90.029(2)
_cell_angle_gamma                90
_cell_volume                     4453.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9471
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      32.08

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_F_000             2128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.743
_shelx_estimated_absorpt_T_min   0.212
_shelx_estimated_absorpt_T_max   0.521
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.0308
_exptl_absorpt_correction_T_max  0.0716
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'BRUKER APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            29773
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.573
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4392
_reflns_number_gt                3900
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'BRUKER APEX-II CCD'
_computing_cell_refinement       SAINT
_computing_data_reduction        SAINT
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_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)+(0.0393P)²+29.5737P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4392
_refine_ls_number_parameters     228
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0349
_refine_ls_wR_factor_ref         0.0907
_refine_ls_wR_factor_gt          0.0867
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_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
Tc Tc 0.500000 0.36760(2) 0.750000 0.02036(11) Uani 1 2 d S T P . .
Se1 Se 0.35277(2) 0.32268(2) 0.71742(2) 0.02373(11) Uani 1 1 d . . . . .
Se2 Se 0.53310(2) 0.32287(2) 0.60506(2) 0.02404(11) Uani 1 1 d . . . . .
O1 O 0.500000 0.4579(2) 0.750000 0.0293(8) Uani 1 2 d S T P . .
Cl1 Cl 0.08521(17) 0.58882(16) 0.7776(3) 0.1773(17) Uani 1 1 d . . . . .
N1 N 0.500000 0.7408(2) 0.750000 0.0184(8) Uani 1 2 d S T P . .
C21 C 0.4348(2) 0.3455(2) 0.5342(2) 0.0216(7) Uani 1 1 d . . . . .
C11 C 0.2802(2) 0.3404(2) 0.8154(2) 0.0224(7) Uani 1 1 d . . . . .
C12 C 0.2512(2) 0.2840(2) 0.8673(2) 0.0240(7) Uani 1 1 d . . . . .
H12 H 0.271063 0.235575 0.858061 0.029 Uiso 1 1 calc R U . . .
C22 C 0.3791(2) 0.2927(2) 0.5025(2) 0.0265(8) Uani 1 1 d . . . . .
H22 H 0.384991 0.243364 0.520061 0.032 Uiso 1 1 calc R U . . .
C32 C 0.3993(2) 0.6371(2) 0.7008(2) 0.0225(7) Uani 1 1 d . . . . .
H32A H 0.349962 0.661372 0.729197 0.027 Uiso 1 1 calc R U . . .
H32B H 0.424206 0.600946 0.740638 0.027 Uiso 1 1 calc R U . . .
C16 C 0.2497(2) 0.4108(2) 0.8294(2) 0.0266(8) Uani 1 1 d . . . . .
H16 H 0.269059 0.449626 0.794166 0.032 Uiso 1 1 calc R U . . .
C13 C 0.1931(2) 0.2987(2) 0.9328(2) 0.0264(8) Uani 1 1 d . . . . .
H13 H 0.173799 0.260089 0.968378 0.032 Uiso 1 1 calc R U . . .
C26 C 0.4243(3) 0.4174(2) 0.5081(2) 0.0296(8) Uani 1 1 d . . . . .
H26 H 0.461445 0.454016 0.530367 0.035 Uiso 1 1 calc R U . . .
C31 C 0.4674(2) 0.69339(19) 0.6774(2) 0.0205(7) Uani 1 1 d . . . . .
H31A H 0.443160 0.725710 0.632973 0.025 Uiso 1 1 calc R U . . .
H31B H 0.517536 0.667575 0.652271 0.025 Uiso 1 1 calc R U . . .
C23 C 0.3144(3) 0.3121(3) 0.4450(2) 0.0352(10) Uani 1 1 d . . . . .
H23 H 0.275965 0.275956 0.423915 0.042 Uiso 1 1 calc R U . . .
C14 C 0.1633(2) 0.3685(2) 0.9463(2) 0.0297(9) Uani 1 1 d . . . . .
H14 H 0.123740 0.378064 0.991207 0.036 Uiso 1 1 calc R U . . .
C15 C 0.1912(3) 0.4249(2) 0.8941(2) 0.0305(8) Uani 1 1 d . . . . .
H15 H 0.170288 0.473137 0.902800 0.037 Uiso 1 1 calc R U . . .
C33 C 0.3680(3) 0.5985(2) 0.6201(2) 0.0279(8) Uani 1 1 d . . . . .
H33A H 0.341976 0.634927 0.581251 0.033 Uiso 1 1 calc R U . . .
H33B H 0.418220 0.576366 0.590733 0.033 Uiso 1 1 calc R U . . .
C41 C 0.5735(2) 0.7883(2) 0.7172(2) 0.0211(7) Uani 1 1 d . . . . .
H41A H 0.599929 0.814292 0.765894 0.025 Uiso 1 1 calc R U . . .
H41B H 0.618504 0.756319 0.692273 0.025 Uiso 1 1 calc R U . . .
C42 C 0.5468(2) 0.8442(2) 0.6509(2) 0.0243(8) Uani 1 1 d . . . . .
H42A H 0.501540 0.876451 0.675011 0.029 Uiso 1 1 calc R U . . .
H42B H 0.521797 0.818801 0.601104 0.029 Uiso 1 1 calc R U . . .
C24 C 0.3060(3) 0.3834(3) 0.4184(3) 0.0399(11) Uani 1 1 d . . . . .
H24 H 0.262540 0.396053 0.378344 0.048 Uiso 1 1 calc R U . . .
C25 C 0.3608(3) 0.4366(3) 0.4501(3) 0.0395(10) Uani 1 1 d . . . . .
H25 H 0.354826 0.485853 0.432248 0.047 Uiso 1 1 calc R U . . .
C34 C 0.3017(3) 0.5394(2) 0.6388(3) 0.0352(9) Uani 1 1 d . . . . .
H34A H 0.283670 0.516266 0.585478 0.053 Uiso 1 1 calc R U . . .
H34B H 0.327543 0.502544 0.676247 0.053 Uiso 1 1 calc R U . . .
H34C H 0.251299 0.561105 0.666766 0.053 Uiso 1 1 calc R U . . .
C43 C 0.6236(3) 0.8904(2) 0.6224(3) 0.0331(9) Uani 1 1 d . . . . .
H43A H 0.647058 0.917557 0.671751 0.040 Uiso 1 1 calc R U . . .
H43B H 0.669809 0.858136 0.600438 0.040 Uiso 1 1 calc R U . . .
C50 C 0.000000 0.6457(4) 0.750000 0.0519(18) Uani 1 2 d S T P . .
H50A H -0.016262 0.677174 0.798559 0.062 Uiso 0.5 1 calc R U P . .
H50B H 0.016262 0.677174 0.701440 0.062 Uiso 0.5 1 calc R U P . .
C44 C 0.5969(3) 0.9439(3) 0.5538(3) 0.0495(13) Uani 1 1 d . . . . .
H44A H 0.647129 0.972909 0.536518 0.074 Uiso 1 1 calc R U . . .
H44B H 0.574468 0.916974 0.504677 0.074 Uiso 1 1 calc R U . . .
H44C H 0.551746 0.976319 0.575898 0.074 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
Tc O1 1.655(4) . ?
Tc Se1 2.4727(4) 2_656 ?
Tc Se1 2.4728(4) . ?
Tc Se2 2.4765(4) 2_656 ?
Tc Se2 2.4766(4) . ?
Se1 C11 1.934(3) . ?
Se2 C21 1.929(3) . ?
Cl1 C50 1.734(5) . ?
N1 C31 1.520(4) . ?
N1 C31 1.520(4) 2_656 ?
N1 C41 1.523(4) . ?
N1 C41 1.523(4) 2_656 ?
C21 C22 1.388(5) . ?
C21 C26 1.388(6) . ?
C11 C12 1.390(5) . ?
C11 C16 1.391(5) . ?
C12 C13 1.394(5) . ?
C12 H12 0.9500 . ?
C22 C23 1.394(6) . ?
C22 H22 0.9500 . ?
C32 C31 1.518(5) . ?
C32 C33 1.532(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C16 C15 1.386(5) . ?
C16 H16 0.9500 . ?
C13 C14 1.376(6) . ?
C13 H13 0.9500 . ?
C26 C25 1.386(6) . ?
C26 H26 0.9500 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C23 C24 1.377(7) . ?
C23 H23 0.9500 . ?
C14 C15 1.389(6) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C33 C34 1.519(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C41 C42 1.519(5) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 C43 1.525(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C24 C25 1.383(7) . ?
C24 H24 0.9500 . ?
C25 H25 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C43 C44 1.515(6) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Tc Se1 109.438(13) . 2_656 ?
O1 Tc Se1 109.438(13) . . ?
Se1 Tc Se1 141.12(3) 2_656 . ?
O1 Tc Se2 109.318(13) . 2_656 ?
Se1 Tc Se2 83.657(13) 2_656 2_656 ?
Se1 Tc Se2 83.701(13) . 2_656 ?
O1 Tc Se2 109.319(13) . . ?
Se1 Tc Se2 83.703(13) 2_656 . ?
Se1 Tc Se2 83.657(13) . . ?
Se2 Tc Se2 141.36(3) 2_656 . ?
C11 Se1 Tc 108.21(10) . . ?
C21 Se2 Tc 107.33(10) . . ?
C31 N1 C31 110.3(4) . 2_656 ?
C31 N1 C41 108.59(19) . . ?
C31 N1 C41 109.56(19) 2_656 . ?
C31 N1 C41 109.56(19) . 2_656 ?
C31 N1 C41 108.59(19) 2_656 2_656 ?
C41 N1 C41 110.2(4) . 2_656 ?
C22 C21 C26 118.8(3) . . ?
C22 C21 Se2 123.1(3) . . ?
C26 C21 Se2 117.8(3) . . ?
C12 C11 C16 119.1(3) . . ?
C12 C11 Se1 122.0(3) . . ?
C16 C11 Se1 118.6(3) . . ?
C11 C12 C13 119.9(4) . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C21 C22 C23 120.0(4) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C31 C32 C33 109.4(3) . . ?
C31 C32 H32A 109.8 . . ?
C33 C32 H32A 109.8 . . ?
C31 C32 H32B 109.8 . . ?
C33 C32 H32B 109.8 . . ?
H32A C32 H32B 108.2 . . ?
C15 C16 C11 120.7(4) . . ?
C15 C16 H16 119.7 . . ?
C11 C16 H16 119.7 . . ?
C14 C13 C12 120.6(4) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C25 C26 C21 121.2(4) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
C32 C31 N1 115.8(3) . . ?
C32 C31 H31A 108.3 . . ?
N1 C31 H31A 108.3 . . ?
C32 C31 H31B 108.3 . . ?
N1 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
C24 C23 C22 120.4(4) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C13 C14 C15 119.7(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C16 C15 C14 119.9(4) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C34 C33 C32 112.4(3) . . ?
C34 C33 H33A 109.1 . . ?
C32 C33 H33A 109.1 . . ?
C34 C33 H33B 109.1 . . ?
C32 C33 H33B 109.1 . . ?
H33A C33 H33B 107.9 . . ?
C42 C41 N1 114.6(3) . . ?
C42 C41 H41A 108.6 . . ?
N1 C41 H41A 108.6 . . ?
C42 C41 H41B 108.6 . . ?
N1 C41 H41B 108.6 . . ?
H41A C41 H41B 107.6 . . ?
C41 C42 C43 111.3(3) . . ?
C41 C42 H42A 109.4 . . ?
C43 C42 H42A 109.4 . . ?
C41 C42 H42B 109.4 . . ?
C43 C42 H42B 109.4 . . ?
H42A C42 H42B 108.0 . . ?
C23 C24 C25 120.1(4) . . ?
C23 C24 H24 120.0 . . ?
C25 C24 H24 120.0 . . ?
C24 C25 C26 119.4(4) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 H25 120.3 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C44 C43 C42 110.9(3) . . ?
C44 C43 H43A 109.5 . . ?
C42 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
Cl1 C50 Cl1 106.2(5) 2_556 . ?
Cl1 C50 H50A 110.5 2_556 . ?
Cl1 C50 H50A 110.5 . . ?
Cl1 C50 H50B 110.5 2_556 . ?
Cl1 C50 H50B 110.5 . . ?
H50A C50 H50B 108.7 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?

_refine_diff_density_max         2.604
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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_TcSePh_AN
_database_code_depnum_ccdc_archive 'CCDC 1536446'
_audit_update_record             
;
2017-03-07 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
 Acetonitriletriphenylphosphinetris(2,6-dimetylphenylselenolato)technetium(III)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C44 H45 N P Se3 Tc'
_chemical_formula_sum            'C44 H45 N P Se3 Tc'
_chemical_formula_weight         953.66

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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   10.7142(6)
_cell_length_b                   11.2883(7)
_cell_length_c                   18.3014(12)
_cell_angle_alpha                86.201(2)
_cell_angle_beta                 79.812(2)
_cell_angle_gamma                68.285(2)
_cell_volume                     2024.0(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9836
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.91

_exptl_crystal_description       block
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_F_000             952
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    3.124
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7071
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS 2014/2 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            52493
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.246
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9680
_reflns_number_gt                8125
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0268P)²+4.1826P] 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         9680
_refine_ls_number_parameters     452
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0679
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_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
Tc1 Tc 0.71448(2) 0.56307(2) 0.25223(2) 0.00875(6) Uani 1 1 d . . . . .
Se2 Se 0.62795(3) 0.44407(3) 0.34538(2) 0.01280(7) Uani 1 1 d . . . . .
Se1 Se 0.88234(3) 0.63919(3) 0.27839(2) 0.01368(7) Uani 1 1 d . . . . .
Se3 Se 0.64509(3) 0.58606(3) 0.13410(2) 0.01285(7) Uani 1 1 d . . . . .
P1 P 0.89260(7) 0.37511(7) 0.20897(4) 0.01058(14) Uani 1 1 d . . . . .
N1 N 0.5596(2) 0.7376(2) 0.28652(13) 0.0120(5) Uani 1 1 d . . . . .
C51 C 1.0500(3) 0.3945(3) 0.16126(16) 0.0129(6) Uani 1 1 d . . . . .
C24 C 0.3994(3) 0.6446(3) 0.43262(16) 0.0140(6) Uani 1 1 d . . . . .
C23 C 0.4378(3) 0.5466(3) 0.38000(16) 0.0146(6) Uani 1 1 d . . . . .
C41 C 0.8604(3) 0.2842(3) 0.13925(16) 0.0126(6) Uani 1 1 d . . . . .
C56 C 1.0408(3) 0.4846(3) 0.10454(17) 0.0182(6) Uani 1 1 d . . . . .
H56 H 0.9539 0.5380 0.0939 0.022 Uiso 1 1 calc R U . . .
C25 C 0.5025(3) 0.6691(3) 0.46921(16) 0.0163(6) Uani 1 1 d . . . . .
H25A H 0.5939 0.6092 0.4499 0.024 Uiso 1 1 calc R U . . .
H25B H 0.4983 0.7567 0.4586 0.024 Uiso 1 1 calc R U . . .
H25C H 0.4826 0.6576 0.5230 0.024 Uiso 1 1 calc R U . . .
C11 C 0.7959(3) 0.7785(3) 0.34948(17) 0.0153(6) Uani 1 1 d . . . . .
C62 C 0.9530(3) 0.2531(3) 0.27927(16) 0.0133(6) Uani 1 1 d . . . . .
C14 C 0.7873(3) 0.7488(3) 0.42551(17) 0.0162(6) Uani 1 1 d . . . . .
C16 C 0.7242(3) 0.8500(3) 0.47665(18) 0.0208(7) Uani 1 1 d . . . . .
H16 H 0.7153 0.8320 0.5284 0.025 Uiso 1 1 calc R U . . .
C31 C 0.5165(3) 0.7581(3) 0.12515(16) 0.0148(6) Uani 1 1 d . . . . .
C1 C 0.4815(3) 0.8372(3) 0.30039(16) 0.0152(6) Uani 1 1 d . . . . .
C37 C 0.5669(3) 0.8527(3) 0.09589(16) 0.0186(6) Uani 1 1 d . . . . .
C42 C 0.9549(3) 0.2324(3) 0.07584(17) 0.0185(6) Uani 1 1 d . . . . .
H42 H 1.0409 0.2416 0.0681 0.022 Uiso 1 1 calc R U . . .
C52 C 1.1782(3) 0.3198(3) 0.17753(17) 0.0180(6) Uani 1 1 d . . . . .
H52 H 1.1865 0.2591 0.2166 0.022 Uiso 1 1 calc R U . . .
C54 C 1.2848(3) 0.4215(3) 0.07956(18) 0.0243(7) Uani 1 1 d . . . . .
H54 H 1.3647 0.4299 0.0516 0.029 Uiso 1 1 calc R U . . .
C15 C 0.8419(3) 0.6146(3) 0.45432(17) 0.0185(6) Uani 1 1 d . . . . .
H15A H 0.8253 0.6157 0.5087 0.028 Uiso 1 1 calc R U . . .
H15B H 0.7960 0.5641 0.4367 0.028 Uiso 1 1 calc R U . . .
H15C H 0.9401 0.5766 0.4363 0.028 Uiso 1 1 calc R U . . .
C12 C 0.7470(3) 0.9058(3) 0.32501(18) 0.0194(6) Uani 1 1 d . . . . .
C55 C 1.1573(3) 0.4972(3) 0.06339(18) 0.0237(7) Uani 1 1 d . . . . .
H55 H 1.1497 0.5577 0.0242 0.028 Uiso 1 1 calc R U . . .
C22 C 0.3393(3) 0.5194(3) 0.35088(17) 0.0206(7) Uani 1 1 d . . . . .
C38 C 0.7165(4) 0.8228(3) 0.06849(19) 0.0256(7) Uani 1 1 d . . . . .
H38A H 0.7672 0.7320 0.0762 0.038 Uiso 1 1 calc R U . . .
H38B H 0.7305 0.8429 0.0155 0.038 Uiso 1 1 calc R U . . .
H38C H 0.7491 0.8740 0.0960 0.038 Uiso 1 1 calc R U . . .
C26 C 0.2613(3) 0.7189(3) 0.45150(18) 0.0215(7) Uani 1 1 d . . . . .
H26 H 0.2336 0.7852 0.4871 0.026 Uiso 1 1 calc R U . . .
C33 C 0.3760(3) 0.7862(3) 0.14774(17) 0.0193(6) Uani 1 1 d . . . . .
C46 C 0.7362(3) 0.2676(3) 0.14968(18) 0.0185(6) Uani 1 1 d . . . . .
H46 H 0.6710 0.3017 0.1927 0.022 Uiso 1 1 calc R U . . .
C17 C 0.6750(3) 0.9746(3) 0.4529(2) 0.0272(8) Uani 1 1 d . . . . .
H17 H 0.6327 1.0416 0.4882 0.033 Uiso 1 1 calc R U . . .
C27 C 0.2031(3) 0.5973(4) 0.37024(18) 0.0269(8) Uani 1 1 d . . . . .
H27 H 0.1357 0.5813 0.3494 0.032 Uiso 1 1 calc R U . . .
C61 C 0.9663(3) 0.1262(3) 0.27285(19) 0.0212(7) Uani 1 1 d . . . . .
H61 H 0.9474 0.0988 0.2294 0.025 Uiso 1 1 calc R U . . .
C63 C 0.9825(3) 0.2906(3) 0.34310(17) 0.0224(7) Uani 1 1 d . . . . .
H63 H 0.9735 0.3766 0.3484 0.027 Uiso 1 1 calc R U . . .
C53 C 1.2944(3) 0.3343(3) 0.13638(18) 0.0225(7) Uani 1 1 d . . . . .
H53 H 1.3815 0.2831 0.1478 0.027 Uiso 1 1 calc R U . . .
C44 C 0.7998(4) 0.1530(3) 0.03447(19) 0.0244(7) Uani 1 1 d . . . . .
H44 H 0.7781 0.1099 -0.0014 0.029 Uiso 1 1 calc R U . . .
C43 C 0.9239(4) 0.1673(3) 0.02383(18) 0.0231(7) Uani 1 1 d . . . . .
H43 H 0.9888 0.1326 -0.0192 0.028 Uiso 1 1 calc R U . . .
C45 C 0.7067(3) 0.2020(3) 0.09815(19) 0.0243(7) Uani 1 1 d . . . . .
H45 H 0.6219 0.1904 0.1064 0.029 Uiso 1 1 calc R U . . .
C2 C 0.3831(4) 0.9656(3) 0.3183(2) 0.0297(8) Uani 1 1 d . . . . .
H2A H 0.3189 0.9628 0.3631 0.044 Uiso 1 1 calc R U . . .
H2B H 0.3333 0.9993 0.2768 0.044 Uiso 1 1 calc R U . . .
H2C H 0.4312 1.0209 0.3270 0.044 Uiso 1 1 calc R U . . .
C28 C 0.1642(3) 0.6973(4) 0.41905(19) 0.0259(8) Uani 1 1 d . . . . .
H28 H 0.0711 0.7512 0.4304 0.031 Uiso 1 1 calc R U . . .
C18 C 0.6869(4) 1.0029(3) 0.3779(2) 0.0255(7) Uani 1 1 d . . . . .
H18 H 0.6540 1.0893 0.3622 0.031 Uiso 1 1 calc R U . . .
C34 C 0.2880(4) 0.9116(3) 0.14031(18) 0.0268(8) Uani 1 1 d . . . . .
H34 H 0.1927 0.9326 0.1547 0.032 Uiso 1 1 calc R U . . .
C36 C 0.4743(4) 0.9770(3) 0.09063(18) 0.0272(8) Uani 1 1 d . . . . .
H36 H 0.5066 1.0427 0.0717 0.033 Uiso 1 1 calc R U . . .
C66 C 1.0070(3) 0.0393(4) 0.3298(2) 0.0291(8) Uani 1 1 d . . . . .
H66 H 1.0146 -0.0466 0.3254 0.035 Uiso 1 1 calc R U . . .
C32 C 0.3211(4) 0.6860(4) 0.1797(2) 0.0303(8) Uani 1 1 d . . . . .
H32A H 0.3966 0.6040 0.1808 0.045 Uiso 1 1 calc R U . . .
H32B H 0.2725 0.7100 0.2303 0.045 Uiso 1 1 calc R U . . .
H32C H 0.2584 0.6784 0.1489 0.045 Uiso 1 1 calc R U . . .
C21 C 0.3763(4) 0.4083(4) 0.2991(2) 0.0347(9) Uani 1 1 d . . . . .
H21A H 0.4752 0.3630 0.2909 0.052 Uiso 1 1 calc R U . . .
H21B H 0.3313 0.3500 0.3213 0.052 Uiso 1 1 calc R U . . .
H21C H 0.3463 0.4399 0.2516 0.052 Uiso 1 1 calc R U . . .
C64 C 1.0250(3) 0.2031(4) 0.39916(18) 0.0291(8) Uani 1 1 d . . . . .
H64 H 1.0463 0.2293 0.4421 0.035 Uiso 1 1 calc R U . . .
C13 C 0.7569(4) 0.9392(3) 0.2437(2) 0.0291(8) Uani 1 1 d . . . . .
H13A H 0.8013 0.8610 0.2142 0.044 Uiso 1 1 calc R U . . .
H13B H 0.6653 0.9845 0.2319 0.044 Uiso 1 1 calc R U . . .
H13C H 0.8106 0.9939 0.2322 0.044 Uiso 1 1 calc R U . . .
C35 C 0.3362(4) 1.0057(3) 0.11259(19) 0.0323(9) Uani 1 1 d . . . . .
H35 H 0.2743 1.0906 0.1085 0.039 Uiso 1 1 calc R U . . .
C65 C 1.0363(3) 0.0781(4) 0.39245(19) 0.0296(8) Uani 1 1 d . . . . .
H65 H 1.0643 0.0188 0.4311 0.035 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
Tc1 N1 2.099(2) . ?
Tc1 P1 2.3372(8) . ?
Tc1 Se2 2.3726(4) . ?
Tc1 Se3 2.3760(4) . ?
Tc1 Se1 2.3884(4) . ?
Se2 C23 1.946(3) . ?
Se1 C11 1.947(3) . ?
Se3 C31 1.938(3) . ?
P1 C62 1.836(3) . ?
P1 C51 1.838(3) . ?
P1 C41 1.841(3) . ?
N1 C1 1.138(4) . ?
C51 C52 1.393(4) . ?
C51 C56 1.394(4) . ?
C24 C26 1.397(4) . ?
C24 C23 1.409(4) . ?
C24 C25 1.503(4) . ?
C23 C22 1.397(4) . ?
C41 C46 1.390(4) . ?
C41 C42 1.396(4) . ?
C56 C55 1.389(4) . ?
C56 H56 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C11 C14 1.405(4) . ?
C11 C12 1.407(4) . ?
C62 C63 1.393(4) . ?
C62 C61 1.397(4) . ?
C14 C16 1.408(4) . ?
C14 C15 1.504(4) . ?
C16 C17 1.378(5) . ?
C16 H16 0.9500 . ?
C31 C37 1.402(4) . ?
C31 C33 1.408(4) . ?
C1 C2 1.459(4) . ?
C37 C36 1.396(5) . ?
C37 C38 1.508(5) . ?
C42 C43 1.393(4) . ?
C42 H42 0.9500 . ?
C52 C53 1.396(4) . ?
C52 H52 0.9500 . ?
C54 C53 1.374(5) . ?
C54 C55 1.389(5) . ?
C54 H54 0.9500 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C12 C18 1.397(5) . ?
C12 C13 1.505(5) . ?
C55 H55 0.9500 . ?
C22 C27 1.392(5) . ?
C22 C21 1.511(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C26 C28 1.386(5) . ?
C26 H26 0.9500 . ?
C33 C34 1.394(5) . ?
C33 C32 1.501(5) . ?
C46 C45 1.381(4) . ?
C46 H46 0.9500 . ?
C17 C18 1.382(5) . ?
C17 H17 0.9500 . ?
C27 C28 1.378(5) . ?
C27 H27 0.9500 . ?
C61 C66 1.396(5) . ?
C61 H61 0.9500 . ?
C63 C64 1.390(5) . ?
C63 H63 0.9500 . ?
C53 H53 0.9500 . ?
C44 C43 1.377(5) . ?
C44 C45 1.388(5) . ?
C44 H44 0.9500 . ?
C43 H43 0.9500 . ?
C45 H45 0.9500 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C28 H28 0.9500 . ?
C18 H18 0.9500 . ?
C34 C35 1.375(6) . ?
C34 H34 0.9500 . ?
C36 C35 1.381(6) . ?
C36 H36 0.9500 . ?
C66 C65 1.379(5) . ?
C66 H66 0.9500 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C64 C65 1.383(6) . ?
C64 H64 0.9500 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C35 H35 0.9500 . ?
C65 H65 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 Tc1 P1 176.73(7) . . ?
N1 Tc1 Se2 93.75(6) . . ?
P1 Tc1 Se2 89.52(2) . . ?
N1 Tc1 Se3 90.37(6) . . ?
P1 Tc1 Se3 88.21(2) . . ?
Se2 Tc1 Se3 118.759(14) . . ?
N1 Tc1 Se1 90.59(7) . . ?
P1 Tc1 Se1 87.72(2) . . ?
Se2 Tc1 Se1 118.175(14) . . ?
Se3 Tc1 Se1 122.852(14) . . ?
C23 Se2 Tc1 107.48(9) . . ?
C11 Se1 Tc1 109.08(8) . . ?
C31 Se3 Tc1 108.79(8) . . ?
C62 P1 C51 102.98(13) . . ?
C62 P1 C41 102.24(13) . . ?
C51 P1 C41 101.00(13) . . ?
C62 P1 Tc1 116.17(9) . . ?
C51 P1 Tc1 115.60(10) . . ?
C41 P1 Tc1 116.59(10) . . ?
C1 N1 Tc1 173.9(2) . . ?
C52 C51 C56 118.7(3) . . ?
C52 C51 P1 122.8(2) . . ?
C56 C51 P1 118.5(2) . . ?
C26 C24 C23 118.4(3) . . ?
C26 C24 C25 119.8(3) . . ?
C23 C24 C25 121.7(3) . . ?
C22 C23 C24 120.7(3) . . ?
C22 C23 Se2 117.5(2) . . ?
C24 C23 Se2 121.8(2) . . ?
C46 C41 C42 118.5(3) . . ?
C46 C41 P1 118.7(2) . . ?
C42 C41 P1 122.8(2) . . ?
C55 C56 C51 120.8(3) . . ?
C55 C56 H56 119.6 . . ?
C51 C56 H56 119.6 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C14 C11 C12 121.1(3) . . ?
C14 C11 Se1 118.3(2) . . ?
C12 C11 Se1 120.6(2) . . ?
C63 C62 C61 118.7(3) . . ?
C63 C62 P1 118.0(2) . . ?
C61 C62 P1 123.2(2) . . ?
C11 C14 C16 118.0(3) . . ?
C11 C14 C15 123.0(3) . . ?
C16 C14 C15 119.0(3) . . ?
C17 C16 C14 121.0(3) . . ?
C17 C16 H16 119.5 . . ?
C14 C16 H16 119.5 . . ?
C37 C31 C33 121.3(3) . . ?
C37 C31 Se3 118.5(2) . . ?
C33 C31 Se3 120.2(2) . . ?
N1 C1 C2 179.1(3) . . ?
C36 C37 C31 118.4(3) . . ?
C36 C37 C38 119.7(3) . . ?
C31 C37 C38 121.9(3) . . ?
C43 C42 C41 120.5(3) . . ?
C43 C42 H42 119.8 . . ?
C41 C42 H42 119.8 . . ?
C51 C52 C53 120.0(3) . . ?
C51 C52 H52 120.0 . . ?
C53 C52 H52 120.0 . . ?
C53 C54 C55 119.4(3) . . ?
C53 C54 H54 120.3 . . ?
C55 C54 H54 120.3 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 C12 C11 118.7(3) . . ?
C18 C12 C13 119.6(3) . . ?
C11 C12 C13 121.7(3) . . ?
C56 C55 C54 120.0(3) . . ?
C56 C55 H55 120.0 . . ?
C54 C55 H55 120.0 . . ?
C27 C22 C23 118.8(3) . . ?
C27 C22 C21 119.2(3) . . ?
C23 C22 C21 122.0(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C28 C26 C24 120.9(3) . . ?
C28 C26 H26 119.6 . . ?
C24 C26 H26 119.6 . . ?
C34 C33 C31 117.8(3) . . ?
C34 C33 C32 120.4(3) . . ?
C31 C33 C32 121.8(3) . . ?
C45 C46 C41 120.7(3) . . ?
C45 C46 H46 119.7 . . ?
C41 C46 H46 119.7 . . ?
C16 C17 C18 120.4(3) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C28 C27 C22 121.3(3) . . ?
C28 C27 H27 119.4 . . ?
C22 C27 H27 119.4 . . ?
C66 C61 C62 120.4(3) . . ?
C66 C61 H61 119.8 . . ?
C62 C61 H61 119.8 . . ?
C64 C63 C62 120.6(3) . . ?
C64 C63 H63 119.7 . . ?
C62 C63 H63 119.7 . . ?
C54 C53 C52 121.0(3) . . ?
C54 C53 H53 119.5 . . ?
C52 C53 H53 119.5 . . ?
C43 C44 C45 119.4(3) . . ?
C43 C44 H44 120.3 . . ?
C45 C44 H44 120.3 . . ?
C44 C43 C42 120.4(3) . . ?
C44 C43 H43 119.8 . . ?
C42 C43 H43 119.8 . . ?
C46 C45 C44 120.6(3) . . ?
C46 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C27 C28 C26 119.8(3) . . ?
C27 C28 H28 120.1 . . ?
C26 C28 H28 120.1 . . ?
C17 C18 C12 120.7(3) . . ?
C17 C18 H18 119.7 . . ?
C12 C18 H18 119.7 . . ?
C35 C34 C33 121.5(3) . . ?
C35 C34 H34 119.3 . . ?
C33 C34 H34 119.3 . . ?
C35 C36 C37 120.7(3) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C65 C66 C61 120.0(3) . . ?
C65 C66 H66 120.0 . . ?
C61 C66 H66 120.0 . . ?
C33 C32 H32A 109.5 . . ?
C33 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C33 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C65 C64 C63 120.1(3) . . ?
C65 C64 H64 120.0 . . ?
C63 C64 H64 120.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C66 C65 C64 120.2(3) . . ?
C66 C65 H65 119.9 . . ?
C64 C65 H65 119.9 . . ?

_refine_diff_density_max         0.792
_refine_diff_density_min         -0.740
_refine_diff_density_rms         0.108

####################################################################### 
# 
# 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_TcTePh_AN
_database_code_depnum_ccdc_archive 'CCDC 1536447'
_audit_update_record             
;
2017-03-07 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT910_TcTePh_AN           
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min).
RESPONSE: IPDS data
;
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
 Acetonitriletriphenylphosphinetris(2,4,6-trimetylphenyltelurolato)technetium(III)
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C47 H51 N P Tc Te3'
_chemical_formula_sum            'C47 H51 N P Tc Te3'
_chemical_formula_weight         1141.66

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tc Tc -1.4390 0.7593 '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'

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

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

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

_cell_length_a                   11.3440(6)
_cell_length_b                   18.5139(10)
_cell_length_c                   21.8268(12)
_cell_angle_alpha                87.249(2)
_cell_angle_beta                 83.169(2)
_cell_angle_gamma                89.829(2)
_cell_volume                     4546.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    499
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      15.70
_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_F_000             2216
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    2.270
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6811
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_process_details   'SADABS 2014/2 (Sheldrick, 2014)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            135937
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.248
_diffrn_reflns_theta_max         26.453
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             18689
_reflns_number_gt                14663
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-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)+(0.0176P)²+63.4613P] 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         18689
_refine_ls_number_parameters     933
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0621
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.110
_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
C41 C 0.3343(6) 0.7969(4) 0.2675(3) 0.0125(15) Uani 1 1 d . . . . .
C61 C 0.5490(7) 0.7834(4) 0.3234(3) 0.0116(15) Uani 1 1 d . . . . .
C51 C 0.4233(6) 0.6562(4) 0.2960(3) 0.0124(15) Uani 1 1 d . . . . .
C62 C 0.4916(7) 0.8298(4) 0.3663(3) 0.0133(15) Uani 1 1 d . . . . .
H62 H 0.4117 0.8405 0.3653 0.016 Uiso 1 1 calc R U . . .
C3 C 0.8112(7) 0.2485(4) 0.4786(4) 0.0142(16) Uani 1 1 d . . . . .
C101 C 1.1829(6) 0.1958(4) 0.2321(3) 0.0122(15) Uani 1 1 d . . . . .
C121 C 0.9587(6) 0.1899(4) 0.1820(3) 0.0115(15) Uani 1 1 d . . . . .
C92 C 0.9215(6) 0.0821(4) 0.5060(3) 0.0091(14) Uani 1 1 d . U . . .
C93 C 0.8418(6) 0.0536(4) 0.5548(3) 0.0104(14) Uani 1 1 d . U . . .
H93 H 0.8588 0.0583 0.5950 0.012 Uiso 1 1 calc R U . . .
C123 C 0.8563(8) 0.0824(5) 0.1596(4) 0.028(2) Uani 1 1 d . . . . .
H123 H 0.8324 0.0350 0.1701 0.034 Uiso 1 1 calc R U . . .
C111 C 1.0691(6) 0.3274(4) 0.1987(3) 0.0132(15) Uani 1 1 d . . . . .
C91 C 0.8959(6) 0.0752(4) 0.4451(3) 0.0098(14) Uani 1 1 d . U . . .
C113 C 1.0000(7) 0.4471(4) 0.1704(4) 0.0196(10) Uani 1 1 d . . . . .
H113 H 0.9380 0.4800 0.1694 0.024 Uiso 1 1 calc R U . . .
C122 C 0.9173(8) 0.1195(4) 0.1988(4) 0.0225(18) Uani 1 1 d . . . . .
H122 H 0.9313 0.0980 0.2366 0.027 Uiso 1 1 calc R U . . .
C114 C 1.1134(7) 0.4667(4) 0.1452(4) 0.0196(10) Uani 1 1 d . U . . .
H114 H 1.1282 0.5129 0.1272 0.024 Uiso 1 1 calc R U . . .
C115 C 1.1821(7) 0.3479(4) 0.1727(4) 0.0196(10) Uani 1 1 d . . . . .
H115 H 1.2437 0.3146 0.1723 0.024 Uiso 1 1 calc R U . . .
C112 C 0.9788(7) 0.3782(4) 0.1971(4) 0.0175(17) Uani 1 1 d . . . . .
H112 H 0.9023 0.3657 0.2145 0.021 Uiso 1 1 calc R U . . .
C53 C 0.3782(7) 0.5705(4) 0.3835(4) 0.0191(17) Uani 1 1 d . . . . .
H53 H 0.3779 0.5587 0.4254 0.023 Uiso 1 1 calc R U . . .
C52 C 0.4239(7) 0.6373(4) 0.3583(4) 0.0162(16) Uani 1 1 d . . . . .
H52 H 0.4552 0.6693 0.3837 0.019 Uiso 1 1 calc R U . . .
C54 C 0.3336(7) 0.5225(4) 0.3453(4) 0.0235(19) Uani 1 1 d . . . . .
H54 H 0.3032 0.4782 0.3616 0.028 Uiso 1 1 calc R U . . .
C21 C 0.4222(6) 0.7104(4) 0.0269(3) 0.0098(14) Uani 1 1 d . . . . .
C102 C 1.2224(7) 0.1455(4) 0.1882(4) 0.0204(18) Uani 1 1 d . . . . .
H102 H 1.1716 0.1312 0.1605 0.024 Uiso 1 1 calc R U . . .
C75 C 0.4962(6) 0.2904(4) 0.4596(4) 0.0144(16) Uani 1 1 d . . . . .
H75 H 0.4606 0.2624 0.4932 0.017 Uiso 1 1 calc R U . . .
C94 C 0.7588(7) 0.0286(4) 0.3703(4) 0.0170(17) Uani 1 1 d . . . . .
H94A H 0.8196 0.0494 0.3403 0.026 Uiso 1 1 calc R U . . .
H94B H 0.7526 -0.0223 0.3644 0.026 Uiso 1 1 calc R U . . .
H94C H 0.6843 0.0515 0.3653 0.026 Uiso 1 1 calc R U . . .
C71 C 0.6742(7) 0.4227(4) 0.3107(4) 0.0211(18) Uani 1 1 d . . . . .
H71A H 0.6541 0.4721 0.3187 0.032 Uiso 1 1 calc R U . . .
H71B H 0.7584 0.4164 0.3097 0.032 Uiso 1 1 calc R U . . .
H71C H 0.6502 0.4110 0.2716 0.032 Uiso 1 1 calc R U . . .
C74 C 0.5613(6) 0.2563(4) 0.4121(4) 0.0135(16) Uani 1 1 d . . . . .
C31 C 0.8259(6) 0.5956(4) 0.0633(4) 0.0137(15) Uani 1 1 d . U . . .
C76 C 0.4816(7) 0.3655(4) 0.4593(4) 0.0174(17) Uani 1 1 d . . . . .
C34 C 1.0437(7) 0.6529(4) 0.0844(4) 0.0157(16) Uani 1 1 d . . . . .
H34 H 1.1161 0.6724 0.0912 0.019 Uiso 1 1 calc R U . . .
C72 C 0.6113(6) 0.3737(4) 0.3609(3) 0.0123(15) Uani 1 1 d . . . . .
C96 C 0.7122(7) 0.0133(4) 0.4849(4) 0.0142(16) Uani 1 1 d . . . . .
H96 H 0.6415 -0.0085 0.4779 0.017 Uiso 1 1 calc R U . . .
C13 C 0.6957(7) 0.9854(4) 0.0088(4) 0.0171(10) Uani 1 1 d . U . . .
H13 H 0.6423 1.0147 -0.0100 0.020 Uiso 1 1 calc R U . . .
C33 C 0.9476(7) 0.6544(4) 0.1308(3) 0.0160(16) Uani 1 1 d . . . . .
C32 C 0.8379(6) 0.6256(4) 0.1194(4) 0.0136(15) Uani 1 1 d . . . . .
C11 C 0.7418(7) 0.9109(4) 0.0956(4) 0.0171(10) Uani 1 1 d . U . . .
C97 C 1.0318(7) 0.1196(4) 0.5204(4) 0.0192(17) Uani 1 1 d . . . . .
H97A H 1.0777 0.1363 0.4825 0.029 Uiso 1 1 calc R U . . .
H97B H 1.0100 0.1602 0.5451 0.029 Uiso 1 1 calc R U . . .
H97C H 1.0783 0.0864 0.5426 0.029 Uiso 1 1 calc R U . . .
C73 C 0.6220(6) 0.2978(4) 0.3627(4) 0.0137(15) Uani 1 1 d . . . . .
C1 C 0.7137(7) 0.7538(4) 0.0244(4) 0.0163(17) Uani 1 1 d . . . . .
C42 C 0.2249(7) 0.7663(5) 0.2902(4) 0.0219(18) Uani 1 1 d . . . . .
H42 H 0.2205 0.7179 0.3039 0.026 Uiso 1 1 calc R U . . .
C95 C 0.7902(6) 0.0399(4) 0.4342(3) 0.0110(15) Uani 1 1 d . . . . .
C35 C 1.0331(6) 0.6228(4) 0.0282(4) 0.0140(15) Uani 1 1 d . U . . .
C12 C 0.6618(7) 0.9558(4) 0.0668(4) 0.0171(10) Uani 1 1 d . U . . .
C27 C 0.3972(7) 0.5814(4) 0.0726(4) 0.0164(16) Uani 1 1 d . . . . .
H27A H 0.3848 0.6063 0.1104 0.025 Uiso 1 1 calc R U . . .
H27B H 0.3268 0.5548 0.0675 0.025 Uiso 1 1 calc R U . . .
H27C H 0.4626 0.5486 0.0741 0.025 Uiso 1 1 calc R U . . .
C23 C 0.4453(6) 0.6111(4) -0.0409(4) 0.0167(17) Uani 1 1 d . . . . .
H23 H 0.4484 0.5615 -0.0459 0.020 Uiso 1 1 calc R U . . .
C81 C 1.0205(6) 0.3698(4) 0.4510(3) 0.0128(15) Uani 1 1 d . U . . .
C104 C 1.3755(7) 0.1874(5) 0.2695(4) 0.0239(19) Uani 1 1 d . . . . .
H104 H 1.4282 0.2014 0.2963 0.029 Uiso 1 1 calc R U . . .
C84 C 0.9324(6) 0.4138(4) 0.4803(4) 0.0132(15) Uani 1 1 d . . . . .
C103 C 1.2626(7) 0.2152(4) 0.2735(4) 0.0183(17) Uani 1 1 d . . . . .
H103 H 1.2383 0.2473 0.3040 0.022 Uiso 1 1 calc R U . . .
C82 C 1.0997(7) 0.3329(4) 0.4862(4) 0.0169(16) Uani 1 1 d . U . . .
C43 C 0.3373(8) 0.8692(4) 0.2483(4) 0.0204(18) Uani 1 1 d . . . . .
H43 H 0.4097 0.8901 0.2325 0.025 Uiso 1 1 calc R U . . .
C24 C 0.4616(6) 0.6571(4) -0.0926(4) 0.0177(17) Uani 1 1 d . . . . .
C25 C 0.4605(7) 0.7314(4) -0.0840(4) 0.0193(17) Uani 1 1 d . . . . .
H25 H 0.4731 0.7634 -0.1184 0.023 Uiso 1 1 calc R U . . .
C44 C 0.2365(8) 0.9113(5) 0.2519(4) 0.028(2) Uani 1 1 d . . . . .
H44 H 0.2412 0.9601 0.2395 0.033 Uiso 1 1 calc R U . . .
C14 C 0.5409(7) 0.9739(4) 0.0996(4) 0.0236(19) Uani 1 1 d . . . . .
H14A H 0.5301 0.9492 0.1395 0.035 Uiso 1 1 calc R U . . .
H14B H 0.5356 1.0251 0.1043 0.035 Uiso 1 1 calc R U . . .
H14C H 0.4804 0.9590 0.0756 0.035 Uiso 1 1 calc R U . . .
C22 C 0.4243(6) 0.6358(4) 0.0187(4) 0.0124(15) Uani 1 1 d . . . . .
C36 C 0.9252(6) 0.5940(4) 0.0184(3) 0.0120(14) Uani 1 1 d . U . . .
H36 H 0.9181 0.5729 -0.0188 0.014 Uiso 1 1 calc R U . . .
C124 C 0.9356(7) 0.2214(4) 0.1263(4) 0.0168(16) Uani 1 1 d . . . . .
H124 H 0.9648 0.2675 0.1144 0.020 Uiso 1 1 calc R U . . .
C16 C 0.8844(8) 0.9296(5) 0.0054(4) 0.026(2) Uani 1 1 d . . . . .
H16 H 0.9594 0.9211 -0.0151 0.031 Uiso 1 1 calc R U . . .
C77 C 0.5415(7) 0.4061(4) 0.4099(4) 0.0191(17) Uani 1 1 d . . . . .
H77 H 0.5353 0.4562 0.4093 0.023 Uiso 1 1 calc R U . . .
C26 C 0.4410(7) 0.7589(4) -0.0252(4) 0.0184(17) Uani 1 1 d . . . . .
C98 C 0.7378(7) 0.0186(4) 0.5453(4) 0.0166(17) Uani 1 1 d . . . . .
C85 C 0.8404(7) 0.4497(4) 0.4460(4) 0.0226(18) Uani 1 1 d . . . . .
H85A H 0.8552 0.4394 0.4031 0.034 Uiso 1 1 calc R U . . .
H85B H 0.7632 0.4319 0.4626 0.034 Uiso 1 1 calc R U . . .
H85C H 0.8435 0.5011 0.4501 0.034 Uiso 1 1 calc R U . . .
C56 C 0.3338(7) 0.5400(4) 0.2834(4) 0.0223(18) Uani 1 1 d . . . . .
H56 H 0.3033 0.5075 0.2580 0.027 Uiso 1 1 calc R U . . .
C55 C 0.3793(7) 0.6057(4) 0.2587(4) 0.0200(18) Uani 1 1 d . . . . .
H55 H 0.3807 0.6166 0.2165 0.024 Uiso 1 1 calc R U . . .
C15 C 0.8540(7) 0.8970(4) 0.0644(4) 0.0206(18) Uani 1 1 d . . . . .
C83 C 1.1949(7) 0.2836(4) 0.4564(4) 0.0235(19) Uani 1 1 d . . . . .
H83A H 1.1894 0.2829 0.4129 0.035 Uiso 1 1 calc R U . . .
H83B H 1.2718 0.3012 0.4629 0.035 Uiso 1 1 calc R U . . .
H83C H 1.1838 0.2355 0.4747 0.035 Uiso 1 1 calc R U . . .
C37 C 0.9661(8) 0.6858(5) 0.1920(4) 0.0241(19) Uani 1 1 d . . . . .
H37A H 0.8931 0.6833 0.2192 0.036 Uiso 1 1 calc R U . . .
H37B H 1.0261 0.6586 0.2104 0.036 Uiso 1 1 calc R U . . .
H37C H 0.9910 0.7353 0.1850 0.036 Uiso 1 1 calc R U . . .
C17 C 0.8075(8) 0.9735(4) -0.0234(4) 0.0216(18) Uani 1 1 d . . . . .
C64 C 0.6720(7) 0.8446(4) 0.4127(4) 0.0159(16) Uani 1 1 d . . . . .
H64 H 0.7125 0.8647 0.4424 0.019 Uiso 1 1 calc R U . . .
C65 C 0.7302(7) 0.7987(4) 0.3705(4) 0.0191(17) Uani 1 1 d . . . . .
H65 H 0.8104 0.7887 0.3714 0.023 Uiso 1 1 calc R U . . .
C87 C 1.0057(8) 0.3865(5) 0.5797(4) 0.0224(18) Uani 1 1 d . . . . .
C79 C 0.4020(7) 0.4015(5) 0.5089(4) 0.0246(19) Uani 1 1 d . . . . .
H79A H 0.3682 0.3655 0.5390 0.037 Uiso 1 1 calc R U . . .
H79B H 0.4475 0.4353 0.5285 0.037 Uiso 1 1 calc R U . . .
H79C H 0.3396 0.4266 0.4908 0.037 Uiso 1 1 calc R U . . .
C63 C 0.5532(7) 0.8600(4) 0.4101(4) 0.0183(17) Uani 1 1 d . . . . .
H63 H 0.5142 0.8910 0.4380 0.022 Uiso 1 1 calc R U . . .
C116 C 1.2047(7) 0.4175(4) 0.1470(4) 0.0209(18) Uani 1 1 d . . . . .
H116 H 1.2816 0.4308 0.1310 0.025 Uiso 1 1 calc R U . . .
C88 C 0.9275(7) 0.4219(4) 0.5433(4) 0.0192(17) Uani 1 1 d . . . . .
H88 H 0.8698 0.4520 0.5622 0.023 Uiso 1 1 calc R U . . .
C86 C 1.0905(8) 0.3423(4) 0.5486(4) 0.0231(18) Uani 1 1 d . U . . .
H86 H 1.1437 0.3179 0.5714 0.028 Uiso 1 1 calc R U . . .
C66 C 0.6691(7) 0.7679(4) 0.3271(3) 0.0164(16) Uani 1 1 d . . . . .
H66 H 0.7084 0.7363 0.2998 0.020 Uiso 1 1 calc R U . . .
C99 C 0.6565(7) -0.0148(4) 0.5992(4) 0.0225(19) Uani 1 1 d . . . . .
H99A H 0.5894 -0.0365 0.5842 0.034 Uiso 1 1 calc R U . . .
H99B H 0.6989 -0.0510 0.6206 0.034 Uiso 1 1 calc R U . . .
H99C H 0.6295 0.0221 0.6270 0.034 Uiso 1 1 calc R U . . .
C78 C 0.5687(7) 0.1746(4) 0.4149(4) 0.0189(17) Uani 1 1 d . . . . .
H78A H 0.6168 0.1590 0.3788 0.028 Uiso 1 1 calc R U . . .
H78B H 0.6035 0.1584 0.4511 0.028 Uiso 1 1 calc R U . . .
H78C H 0.4904 0.1545 0.4166 0.028 Uiso 1 1 calc R U . . .
C126 C 0.8683(7) 0.1848(5) 0.0873(4) 0.0227(18) Uani 1 1 d . . . . .
H126 H 0.8498 0.2072 0.0506 0.027 Uiso 1 1 calc R U . . .
C38 C 0.7099(7) 0.5651(4) 0.0488(4) 0.0217(18) Uani 1 1 d . . . . .
H38A H 0.7202 0.5472 0.0080 0.033 Uiso 1 1 calc R U . . .
H38B H 0.6848 0.5264 0.0782 0.033 Uiso 1 1 calc R U . . .
H38C H 0.6508 0.6024 0.0509 0.033 Uiso 1 1 calc R U . . .
C29 C 0.4409(9) 0.8403(4) -0.0186(4) 0.029(2) Uani 1 1 d . . . . .
H29A H 0.4264 0.8506 0.0243 0.043 Uiso 1 1 calc R U . . .
H29B H 0.5165 0.8599 -0.0359 0.043 Uiso 1 1 calc R U . . .
H29C H 0.3796 0.8617 -0.0402 0.043 Uiso 1 1 calc R U . . .
C105 C 1.3348(8) 0.1168(5) 0.1853(4) 0.028(2) Uani 1 1 d . . . . .
H105 H 1.3591 0.0831 0.1562 0.033 Uiso 1 1 calc R U . . .
C39 C 1.1379(7) 0.6187(5) -0.0212(4) 0.0228(18) Uani 1 1 d . . . . .
H39A H 1.2058 0.6410 -0.0075 0.034 Uiso 1 1 calc R U . . .
H39B H 1.1552 0.5690 -0.0291 0.034 Uiso 1 1 calc R U . . .
H39C H 1.1193 0.6436 -0.0585 0.034 Uiso 1 1 calc R U . . .
C4 C 0.7662(8) 0.2513(5) 0.5441(4) 0.0251(19) Uani 1 1 d . . . . .
H4A H 0.8088 0.2173 0.5677 0.038 Uiso 1 1 calc R U . . .
H4B H 0.6832 0.2392 0.5499 0.038 Uiso 1 1 calc R U . . .
H4C H 0.7770 0.2992 0.5576 0.038 Uiso 1 1 calc R U . . .
C18 C 0.9414(7) 0.8461(5) 0.0915(4) 0.026(2) Uani 1 1 d . . . . .
H18A H 1.0148 0.8466 0.0646 0.039 Uiso 1 1 calc R U . . .
H18B H 0.9092 0.7980 0.0957 0.039 Uiso 1 1 calc R U . . .
H18C H 0.9556 0.8617 0.1313 0.039 Uiso 1 1 calc R U . . .
C45 C 0.1218(7) 0.8079(5) 0.2924(4) 0.029(2) Uani 1 1 d . . . . .
H45 H 0.0488 0.7866 0.3064 0.034 Uiso 1 1 calc R U . . .
C125 C 0.8300(7) 0.1150(5) 0.1043(4) 0.026(2) Uani 1 1 d . . . . .
H125 H 0.7866 0.0900 0.0786 0.031 Uiso 1 1 calc R U . . .
C28 C 0.4725(8) 0.6300(5) -0.1570(4) 0.030(2) Uani 1 1 d . . . . .
H28A H 0.4833 0.6703 -0.1865 0.044 Uiso 1 1 calc R U . . .
H28B H 0.5396 0.5983 -0.1629 0.044 Uiso 1 1 calc R U . . .
H28C H 0.4016 0.6042 -0.1627 0.044 Uiso 1 1 calc R U . . .
C46 C 0.1267(8) 0.8793(5) 0.2744(4) 0.030(2) Uani 1 1 d . . . . .
H46 H 0.0578 0.9069 0.2770 0.036 Uiso 1 1 calc R U . . .
C2 C 0.7721(9) 0.7560(5) -0.0391(4) 0.032(2) Uani 1 1 d . . . . .
H2A H 0.8504 0.7760 -0.0403 0.049 Uiso 1 1 calc R U . . .
H2B H 0.7267 0.7855 -0.0650 0.049 Uiso 1 1 calc R U . . .
H2C H 0.7776 0.7079 -0.0537 0.049 Uiso 1 1 calc R U . . .
C19 C 0.8411(10) 1.0090(5) -0.0867(4) 0.037(2) Uani 1 1 d . . . . .
H19A H 0.9235 1.0002 -0.0998 0.056 Uiso 1 1 calc R U . . .
H19B H 0.8277 1.0601 -0.0851 0.056 Uiso 1 1 calc R U . . .
H19C H 0.7935 0.9892 -0.1154 0.056 Uiso 1 1 calc R U . . .
C106 C 1.4100(8) 0.1378(5) 0.2249(4) 0.030(2) Uani 1 1 d . . . . .
H106 H 1.4863 0.1187 0.2221 0.037 Uiso 1 1 calc R U . . .
C89 C 1.0009(8) 0.3961(5) 0.6479(4) 0.032(2) Uani 1 1 d . . . . .
H89A H 0.9372 0.4282 0.6609 0.048 Uiso 1 1 calc R U . . .
H89B H 0.9878 0.3500 0.6697 0.048 Uiso 1 1 calc R U . . .
H89C H 1.0747 0.4161 0.6567 0.048 Uiso 1 1 calc R U . . .
Te4 Te 0.73696(4) 0.24953(3) 0.29124(2) 0.01159(11) Uani 1 1 d . . . . .
Te5 Te 1.03991(4) 0.35925(2) 0.35278(2) 0.01106(11) Uani 1 1 d . . . . .
Te6 Te 1.01395(4) 0.11573(2) 0.36694(2) 0.01129(11) Uani 1 1 d . . . . .
Tc2 Tc 0.93342(5) 0.24097(3) 0.33750(3) 0.00732(12) Uani 1 1 d . . . . .
P2 P 1.03456(16) 0.23795(10) 0.23875(8) 0.0085(4) Uani 1 1 d . . . . .
N2 N 0.8495(5) 0.2453(3) 0.4274(3) 0.0116(13) Uani 1 1 d . . . . .
Te2 Te 0.38230(4) 0.74881(3) 0.11828(2) 0.01311(11) Uani 1 1 d . . . . .
Te1 Te 0.68601(4) 0.86373(3) 0.18596(2) 0.01370(11) Uani 1 1 d . . . . .
Te3 Te 0.68717(5) 0.62999(3) 0.18965(2) 0.01462(11) Uani 1 1 d . . . . .
Tc1 Tc 0.58134(5) 0.74751(3) 0.16354(3) 0.00889(13) Uani 1 1 d . . . . .
P1 P 0.47427(17) 0.74515(10) 0.26155(9) 0.0114(4) Uani 1 1 d . . . . .
N1 N 0.6695(6) 0.7519(3) 0.0741(3) 0.0149(14) 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
C41 C43 1.382(11) . ?
C41 C42 1.392(11) . ?
C41 P1 1.847(7) . ?
C61 C66 1.401(10) . ?
C61 C62 1.403(10) . ?
C61 P1 1.847(7) . ?
C51 C52 1.390(11) . ?
C51 C55 1.398(11) . ?
C51 P1 1.843(7) . ?
C62 C63 1.388(11) . ?
C3 N2 1.153(10) . ?
C3 C4 1.464(11) . ?
C101 C102 1.403(11) . ?
C101 C103 1.412(11) . ?
C101 P2 1.846(7) . ?
C121 C124 1.376(11) . ?
C121 C122 1.403(11) . ?
C121 P2 1.853(7) . ?
C92 C93 1.396(10) . ?
C92 C91 1.407(10) . ?
C92 C97 1.505(10) . ?
C93 C98 1.390(10) . ?
C123 C122 1.373(12) . ?
C123 C125 1.388(13) . ?
C111 C115 1.385(11) . ?
C111 C112 1.391(11) . ?
C111 P2 1.856(7) . ?
C91 C95 1.418(10) . ?
C91 Te6 2.145(7) . ?
C113 C114 1.379(11) . ?
C113 C112 1.386(11) . ?
C114 C116 1.381(11) . ?
C115 C116 1.393(11) . ?
C53 C54 1.384(12) . ?
C53 C52 1.403(11) . ?
C54 C56 1.373(12) . ?
C21 C22 1.400(10) . ?
C21 C26 1.410(10) . ?
C21 Te2 2.147(7) . ?
C102 C105 1.375(12) . ?
C75 C74 1.377(11) . ?
C75 C76 1.399(11) . ?
C94 C95 1.505(10) . ?
C71 C72 1.502(11) . ?
C74 C73 1.404(11) . ?
C74 C78 1.514(10) . ?
C31 C32 1.389(11) . ?
C31 C36 1.404(10) . ?
C31 C38 1.508(10) . ?
C76 C77 1.392(11) . ?
C76 C79 1.505(11) . ?
C34 C35 1.390(11) . ?
C34 C33 1.399(11) . ?
C72 C73 1.410(10) . ?
C72 C77 1.411(11) . ?
C96 C98 1.391(11) . ?
C96 C95 1.402(10) . ?
C13 C12 1.369(11) . ?
C13 C17 1.397(12) . ?
C33 C32 1.409(11) . ?
C33 C37 1.519(10) . ?
C32 Te3 2.160(7) . ?
C11 C15 1.400(12) . ?
C11 C12 1.411(11) . ?
C11 Te1 2.142(8) . ?
C73 Te4 2.139(7) . ?
C1 N1 1.139(10) . ?
C1 C2 1.463(11) . ?
C42 C45 1.396(12) . ?
C35 C36 1.380(10) . ?
C35 C39 1.511(11) . ?
C12 C14 1.514(12) . ?
C27 C22 1.516(10) . ?
C23 C24 1.376(11) . ?
C23 C22 1.394(11) . ?
C81 C84 1.401(11) . ?
C81 C82 1.406(10) . ?
C81 Te5 2.147(8) . ?
C104 C103 1.373(11) . ?
C104 C106 1.393(13) . ?
C84 C88 1.384(11) . ?
C84 C85 1.494(11) . ?
C82 C86 1.373(12) . ?
C82 C83 1.519(11) . ?
C43 C44 1.378(12) . ?
C24 C25 1.397(11) . ?
C24 C28 1.506(11) . ?
C25 C26 1.398(11) . ?
C44 C46 1.405(13) . ?
C124 C126 1.408(11) . ?
C16 C17 1.377(12) . ?
C16 C15 1.401(11) . ?
C26 C29 1.519(10) . ?
C98 C99 1.514(11) . ?
C56 C55 1.384(11) . ?
C15 C18 1.516(11) . ?
C17 C19 1.507(12) . ?
C64 C63 1.383(11) . ?
C64 C65 1.391(11) . ?
C65 C66 1.383(11) . ?
C87 C86 1.396(12) . ?
C87 C88 1.400(12) . ?
C87 C89 1.503(12) . ?
C126 C125 1.383(12) . ?
C105 C106 1.354(13) . ?
C45 C46 1.361(13) . ?
Te4 Tc2 2.5553(8) . ?
Te5 Tc2 2.5590(7) . ?
Te6 Tc2 2.5705(7) . ?
Tc2 N2 2.082(6) . ?
Tc2 P2 2.3212(19) . ?
Te2 Tc1 2.5695(8) . ?
Te1 Tc1 2.5561(8) . ?
Te3 Tc1 2.5550(8) . ?
Tc1 N1 2.082(6) . ?
Tc1 P1 2.3297(19) . ?

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
C43 C41 C42 118.1(7) . . ?
C43 C41 P1 119.0(6) . . ?
C42 C41 P1 122.9(6) . . ?
C66 C61 C62 117.8(7) . . ?
C66 C61 P1 119.5(6) . . ?
C62 C61 P1 122.7(6) . . ?
C52 C51 C55 118.0(7) . . ?
C52 C51 P1 122.7(6) . . ?
C55 C51 P1 119.3(6) . . ?
C63 C62 C61 120.5(7) . . ?
N2 C3 C4 178.1(9) . . ?
C102 C101 C103 117.4(7) . . ?
C102 C101 P2 124.3(6) . . ?
C103 C101 P2 118.3(6) . . ?
C124 C121 C122 119.2(7) . . ?
C124 C121 P2 123.0(6) . . ?
C122 C121 P2 117.7(6) . . ?
C93 C92 C91 119.0(6) . . ?
C93 C92 C97 118.9(7) . . ?
C91 C92 C97 122.1(6) . . ?
C98 C93 C92 122.3(7) . . ?
C122 C123 C125 120.5(8) . . ?
C115 C111 C112 117.7(7) . . ?
C115 C111 P2 123.3(6) . . ?
C112 C111 P2 118.9(6) . . ?
C92 C91 C95 119.7(6) . . ?
C92 C91 Te6 121.8(5) . . ?
C95 C91 Te6 118.5(5) . . ?
C114 C113 C112 119.8(8) . . ?
C123 C122 C121 120.2(8) . . ?
C113 C114 C116 119.6(7) . . ?
C111 C115 C116 121.0(8) . . ?
C113 C112 C111 121.7(8) . . ?
C54 C53 C52 119.3(8) . . ?
C51 C52 C53 121.0(7) . . ?
C56 C54 C53 120.5(7) . . ?
C22 C21 C26 119.6(7) . . ?
C22 C21 Te2 119.2(5) . . ?
C26 C21 Te2 121.1(5) . . ?
C105 C102 C101 121.2(8) . . ?
C74 C75 C76 122.6(7) . . ?
C75 C74 C73 119.7(7) . . ?
C75 C74 C78 119.2(7) . . ?
C73 C74 C78 121.1(7) . . ?
C32 C31 C36 118.9(7) . . ?
C32 C31 C38 122.4(7) . . ?
C36 C31 C38 118.7(7) . . ?
C77 C76 C75 117.2(7) . . ?
C77 C76 C79 120.8(7) . . ?
C75 C76 C79 122.0(7) . . ?
C35 C34 C33 121.4(7) . . ?
C73 C72 C77 118.6(7) . . ?
C73 C72 C71 123.7(7) . . ?
C77 C72 C71 117.7(7) . . ?
C98 C96 C95 121.7(7) . . ?
C12 C13 C17 122.7(8) . . ?
C34 C33 C32 118.7(7) . . ?
C34 C33 C37 118.7(7) . . ?
C32 C33 C37 122.6(7) . . ?
C31 C32 C33 120.6(7) . . ?
C31 C32 Te3 120.1(5) . . ?
C33 C32 Te3 119.3(6) . . ?
C15 C11 C12 119.7(7) . . ?
C15 C11 Te1 121.6(6) . . ?
C12 C11 Te1 118.7(6) . . ?
C74 C73 C72 119.6(7) . . ?
C74 C73 Te4 122.0(5) . . ?
C72 C73 Te4 118.4(5) . . ?
N1 C1 C2 179.2(9) . . ?
C41 C42 C45 120.3(8) . . ?
C96 C95 C91 119.0(7) . . ?
C96 C95 C94 118.4(7) . . ?
C91 C95 C94 122.6(6) . . ?
C36 C35 C34 118.9(7) . . ?
C36 C35 C39 119.7(7) . . ?
C34 C35 C39 121.4(7) . . ?
C13 C12 C11 119.2(7) . . ?
C13 C12 C14 119.3(7) . . ?
C11 C12 C14 121.4(7) . . ?
C24 C23 C22 122.6(7) . . ?
C84 C81 C82 119.6(7) . . ?
C84 C81 Te5 121.4(5) . . ?
C82 C81 Te5 119.0(6) . . ?
C103 C104 C106 119.1(8) . . ?
C88 C84 C81 119.3(7) . . ?
C88 C84 C85 118.9(7) . . ?
C81 C84 C85 121.7(7) . . ?
C104 C103 C101 121.0(8) . . ?
C86 C82 C81 118.9(8) . . ?
C86 C82 C83 119.9(7) . . ?
C81 C82 C83 121.3(7) . . ?
C44 C43 C41 122.2(8) . . ?
C23 C24 C25 117.9(7) . . ?
C23 C24 C28 122.2(8) . . ?
C25 C24 C28 119.8(8) . . ?
C24 C25 C26 121.7(7) . . ?
C43 C44 C46 119.0(8) . . ?
C23 C22 C21 119.2(7) . . ?
C23 C22 C27 119.0(7) . . ?
C21 C22 C27 121.7(7) . . ?
C35 C36 C31 121.6(7) . . ?
C121 C124 C126 120.7(7) . . ?
C17 C16 C15 122.6(8) . . ?
C76 C77 C72 122.2(7) . . ?
C25 C26 C21 119.1(7) . . ?
C25 C26 C29 119.4(7) . . ?
C21 C26 C29 121.5(7) . . ?
C93 C98 C96 118.2(7) . . ?
C93 C98 C99 120.8(7) . . ?
C96 C98 C99 121.0(7) . . ?
C54 C56 C55 120.1(8) . . ?
C56 C55 C51 121.1(8) . . ?
C16 C15 C11 118.5(8) . . ?
C16 C15 C18 119.3(8) . . ?
C11 C15 C18 122.2(7) . . ?
C16 C17 C13 117.3(7) . . ?
C16 C17 C19 122.4(8) . . ?
C13 C17 C19 120.4(8) . . ?
C63 C64 C65 119.3(7) . . ?
C66 C65 C64 120.1(7) . . ?
C86 C87 C88 116.0(7) . . ?
C86 C87 C89 121.5(8) . . ?
C88 C87 C89 122.5(8) . . ?
C64 C63 C62 120.9(7) . . ?
C114 C116 C115 120.3(7) . . ?
C84 C88 C87 122.7(8) . . ?
C82 C86 C87 123.6(8) . . ?
C65 C66 C61 121.3(7) . . ?
C125 C126 C124 119.1(8) . . ?
C106 C105 C102 119.9(8) . . ?
C46 C45 C42 120.8(8) . . ?
C126 C125 C123 120.2(8) . . ?
C45 C46 C44 119.7(8) . . ?
C105 C106 C104 121.4(8) . . ?
C73 Te4 Tc2 102.4(2) . . ?
C81 Te5 Tc2 104.81(18) . . ?
C91 Te6 Tc2 105.65(18) . . ?
N2 Tc2 P2 177.49(17) . . ?
N2 Tc2 Te4 92.62(16) . . ?
P2 Tc2 Te4 89.69(5) . . ?
N2 Tc2 Te5 88.66(16) . . ?
P2 Tc2 Te5 89.42(5) . . ?
Te4 Tc2 Te5 117.63(3) . . ?
N2 Tc2 Te6 88.52(17) . . ?
P2 Tc2 Te6 91.19(5) . . ?
Te4 Tc2 Te6 119.15(3) . . ?
Te5 Tc2 Te6 123.22(3) . . ?
C101 P2 C121 102.8(3) . . ?
C101 P2 C111 101.1(3) . . ?
C121 P2 C111 102.8(3) . . ?
C101 P2 Tc2 116.6(2) . . ?
C121 P2 Tc2 115.9(2) . . ?
C111 P2 Tc2 115.6(2) . . ?
C3 N2 Tc2 174.9(6) . . ?
C21 Te2 Tc1 105.25(19) . . ?
C11 Te1 Tc1 103.2(2) . . ?
C32 Te3 Tc1 104.70(19) . . ?
N1 Tc1 P1 177.10(19) . . ?
N1 Tc1 Te3 91.04(18) . . ?
P1 Tc1 Te3 91.32(5) . . ?
N1 Tc1 Te1 90.04(17) . . ?
P1 Tc1 Te1 90.44(5) . . ?
Te3 Tc1 Te1 115.57(3) . . ?
N1 Tc1 Te2 89.25(18) . . ?
P1 Tc1 Te2 88.08(5) . . ?
Te3 Tc1 Te2 122.23(3) . . ?
Te1 Tc1 Te2 122.20(3) . . ?
C51 P1 C41 101.6(3) . . ?
C51 P1 C61 102.7(3) . . ?
C41 P1 C61 101.3(3) . . ?
C51 P1 Tc1 117.2(2) . . ?
C41 P1 Tc1 115.3(2) . . ?
C61 P1 Tc1 116.4(2) . . ?
C1 N1 Tc1 177.4(7) . . ?

_refine_diff_density_max         1.620
_refine_diff_density_min         -2.097
_refine_diff_density_rms         0.190







