#------------------------------------------------------------------------------
#$Date: 2017-06-16 05:10:18 +0300 (Fri, 16 Jun 2017) $
#$Revision: 197876 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/33/7043344.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7043344
loop_
_publ_author_name
'Noschang Cabral, Bruno'
'Kirsten, Lars'
'Hagenbach, Adelheid'
'Piquini, Paulo Cesar'
'Patzschke, Michael'
'Lang, Ernesto'
'Abram, Ulrich'
_publ_section_title
;
 Technetium Complexes with Arylselenolato and Aryltellurolato Ligands
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02041D
_journal_year                    2017
_chemical_formula_moiety
'C24 H20 O Tc Te4 1-, C16 H36 N1 1+, C H2 Cl2'
_chemical_formula_sum            'C41 H58 Cl2 N O Tc Te4'
_chemical_formula_weight         1260.18
_chemical_name_systematic
;
 Tetrabutylammoniumtetra(phenyltelurolato)oxidotechnetate(V)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-07 deposited with the CCDC.
2017-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.907(2)
_cell_length_b                   18.392(2)
_cell_length_c                   16.246(2)
_cell_measurement_reflns_used    15908
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      3.34
_cell_volume                     4752.9(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0611
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22751
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         3.346
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.8045
_exptl_absorpt_correction_T_min  0.6478
_exptl_absorpt_correction_type   integration
_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_crystal_colour            brown
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.841
_refine_diff_density_min         -1.233
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         5191
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.930
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0464
_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)+(0.0733P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1320
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3175
_reflns_number_total             5191
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02041d1.cif
_cod_data_source_block           TcOTePh
_cod_original_formula_sum        'C41 H58 Cl2 N1 O1 Tc1 Te4'
_cod_database_code               7043344
_shelx_shelxl_version_number     2014/7
_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'
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
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 .
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'
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
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 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
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 .
