# 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).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
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# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
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data_ph509_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1507755'
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date 2016-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H20 N4 O4 Te4, C6 H6'
_chemical_formula_sum 'C34 H26 N4 O4 Te4'
_chemical_formula_weight 1064.99
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 18.646(3)
_cell_length_b 17.433(2)
_cell_length_c 10.6572(15)
_cell_angle_alpha 90
_cell_angle_beta 95.384(2)
_cell_angle_gamma 90
_cell_volume 3448.9(8)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 3040
_cell_measurement_temperature 173
_cell_measurement_theta_max 25.83
_cell_measurement_theta_min 3.02
_shelx_estimated_absorpt_T_max 0.899
_shelx_estimated_absorpt_T_min 0.509
_exptl_absorpt_coefficient_mu 3.393
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.6097
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0463 before and 0.0317 after correction.
The Ratio of minimum to maximum transmission is 0.6097.
The \l/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.051
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description rod
_exptl_crystal_F_000 1992
_exptl_crystal_size_max 0.23
_exptl_crystal_size_mid 0.067
_exptl_crystal_size_min 0.032
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0276
_diffrn_reflns_av_unetI/netI 0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 24
_diffrn_reflns_limit_h_min -24
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_number 13318
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.299
_diffrn_reflns_theta_min 3.206
_diffrn_ambient_temperature 173
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 2913
_reflns_number_total 4255
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 0.968
_refine_diff_density_min -1.514
_refine_diff_density_rms 0.107
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.036
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 208
_refine_ls_number_reflns 4255
_refine_ls_number_restraints 177
_refine_ls_R_factor_all 0.0697
_refine_ls_R_factor_gt 0.0410
_refine_ls_restrained_S_all 1.039
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+15.4489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0820
_refine_ls_wR_factor_ref 0.0917
_refine_special_details ?
_olex2_refinement_description
;
1. Others
Fixed Uiso: H11(0.068) H12(0.086) H7(0.082) H6(0.092) H14(0.081) H5(0.09)
H10(0.07) H13(0.093) H4(0.083) H3(0.067) H17(0.112) H16(0.108) H15(0.103)
Fixed X: H11(0.5576) H12(0.5915) H7(0.2985) H6(0.1771) H14(0.7167) H5(0.1391)
H10(0.7257) H13(0.6705) H4(0.2212) H3(0.4291) H17(0.0213) H16(0.0444)
H15(0.0208)
Fixed Y: H11(0.6966) H12(0.8002) H7(0.5092) H6(0.5232) H14(0.8802) H5(0.587)
H10(0.804) H13(0.8906) H4(0.6427) H3(0.5321) H17(0.4658) H16(0.5791)
H15(0.6935)
Fixed Z: H11(0.2981) H12(0.1809) H7(0.1843) H6(0.2056) H14(0.4758) H5(0.3746)
H10(0.6851) H13(0.2694) H4(0.5267) H3(0.2724) H17(0.154) H16(0.0563)
H15(0.1509)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te2 Te 0.59177(2) 0.63692(2) 0.57970(4) 0.05082(12) Uani 1 1 d . U . . .
Te1 Te 0.39432(2) 0.65267(2) 0.57138(4) 0.05815(13) Uani 1 1 d . U . . .
O1 O 0.52481(19) 0.5846(2) 0.4213(4) 0.0626(10) Uani 1 1 d . U . . .
O2 O 0.6932(2) 0.6974(3) 0.8224(4) 0.0721(11) Uani 1 1 d . U . . .
N2 N 0.6675(2) 0.7125(2) 0.7012(5) 0.0570(11) Uani 1 1 d . U . . .
N1 N 0.4520(2) 0.5918(2) 0.4249(5) 0.0541(11) Uani 1 1 d . U . . .
C11 C 0.5893(3) 0.7333(3) 0.3346(6) 0.0569(13) Uani 1 1 d . U . . .
H11 H 0.5576 0.6966 0.2981 0.068 Uiso 1 1 calc R . . . .
C12 C 0.6098(3) 0.7952(3) 0.2646(7) 0.0718(17) Uani 1 1 d . U . . .
H12 H 0.5915 0.8002 0.1809 0.086 Uiso 1 1 calc R . . . .
C8 C 0.6165(2) 0.7266(3) 0.4590(6) 0.0487(12) Uani 1 1 d . U . . .
C1 C 0.3109(3) 0.6077(3) 0.4465(6) 0.0565(13) Uani 1 1 d . U . . .
C7 C 0.2833(3) 0.5355(3) 0.2530(7) 0.0683(16) Uani 1 1 d . U . . .
H7 H 0.2985 0.5092 0.1843 0.082 Uiso 1 1 calc R . . . .
C2 C 0.3340(3) 0.5669(3) 0.3442(6) 0.0586(13) Uani 1 1 d . U . . .
C6 C 0.2109(3) 0.5439(3) 0.2659(8) 0.0766(18) Uani 1 1 d . U . . .
H6 H 0.1771 0.5232 0.2056 0.092 Uiso 1 1 calc R . . . .
C9 C 0.6646(2) 0.7815(3) 0.5159(6) 0.0533(12) Uani 1 1 d . U . . .
C14 C 0.6846(3) 0.8434(3) 0.4411(7) 0.0672(16) Uani 1 1 d . U . . .
H14 H 0.7167 0.8802 0.4758 0.081 Uiso 1 1 calc R . . . .
C5 C 0.1882(3) 0.5827(4) 0.3670(7) 0.0754(17) Uani 1 1 d . U . . .
H5 H 0.1391 0.5870 0.3746 0.090 Uiso 1 1 calc R . . . .
C10 C 0.6920(3) 0.7707(3) 0.6446(6) 0.0583(13) Uani 1 1 d . U . . .
H10 H 0.7257 0.8040 0.6851 0.070 Uiso 1 1 calc R . . . .
C13 C 0.6571(3) 0.8495(3) 0.3178(8) 0.0778(18) Uani 1 1 d . U . . .
H13 H 0.6705 0.8906 0.2694 0.093 Uiso 1 1 calc R . . . .
C4 C 0.2372(3) 0.6159(3) 0.4592(7) 0.0688(16) Uani 1 1 d . U . . .
H4 H 0.2212 0.6427 0.5267 0.083 Uiso 1 1 calc R . . . .
C3 C 0.4106(3) 0.5592(3) 0.3372(6) 0.0560(13) Uani 1 1 d . U . . .
H3 H 0.4291 0.5321 0.2724 0.067 Uiso 1 1 calc R . . . .
C17 C 0.0127(4) 0.5122(4) 0.1932(7) 0.094(2) Uani 1 1 d . U . . .
H17 H 0.0213 0.4658 0.1540 0.112 Uiso 1 1 calc R . . . .
C16 C 0.0262(3) 0.5796(5) 0.1346(8) 0.090(2) Uani 1 1 d . U . . .
H16 H 0.0444 0.5791 0.0563 0.108 Uiso 1 1 calc R . . . .
C15 C 0.0128(3) 0.6474(4) 0.1912(8) 0.086(2) Uani 1 1 d . U . . .
H15 H 0.0208 0.6935 0.1509 0.103 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Te2 0.03563(18) 0.03894(18) 0.0792(3) 0.00207(16) 0.01240(16) -0.00957(13)
Te1 0.0390(2) 0.0573(2) 0.0789(3) 0.00889(19) 0.00972(18) -0.00910(15)
O1 0.0423(19) 0.063(2) 0.085(3) -0.008(2) 0.0182(18) -0.0219(17)
O2 0.043(2) 0.087(3) 0.086(3) -0.007(2) 0.006(2) -0.013(2)
N2 0.028(2) 0.050(2) 0.094(3) -0.008(2) 0.011(2) -0.0051(18)
N1 0.040(2) 0.040(2) 0.083(3) 0.006(2) 0.011(2) -0.0158(17)
C11 0.037(3) 0.041(3) 0.094(4) 0.008(2) 0.014(3) 0.005(2)
C12 0.055(3) 0.052(3) 0.110(5) 0.025(3) 0.017(3) 0.008(2)
C8 0.024(2) 0.031(2) 0.094(3) 0.003(2) 0.020(2) -0.0005(17)
C1 0.038(2) 0.040(3) 0.090(4) 0.022(2) -0.005(2) -0.008(2)
C7 0.057(3) 0.035(3) 0.109(4) 0.008(3) -0.013(3) -0.001(2)
C2 0.048(3) 0.029(2) 0.096(4) 0.014(2) -0.003(2) -0.006(2)
C6 0.054(3) 0.042(3) 0.130(5) 0.012(3) -0.015(3) -0.001(2)
C9 0.024(2) 0.032(2) 0.107(4) 0.000(2) 0.018(2) 0.0011(17)
C14 0.033(3) 0.038(3) 0.131(5) 0.008(3) 0.014(3) -0.002(2)
C5 0.043(3) 0.056(3) 0.124(5) 0.024(3) -0.010(3) -0.001(3)
C10 0.028(2) 0.041(3) 0.107(4) -0.011(2) 0.012(2) -0.007(2)
C13 0.058(4) 0.043(3) 0.135(5) 0.025(3) 0.020(3) 0.004(2)
C4 0.043(3) 0.055(3) 0.107(5) 0.023(3) -0.002(3) 0.002(2)
C3 0.050(3) 0.030(2) 0.088(4) 0.008(2) 0.005(2) -0.012(2)
C17 0.073(5) 0.071(4) 0.132(7) -0.026(4) -0.017(5) 0.012(4)
C16 0.043(3) 0.119(5) 0.106(6) 0.003(4) -0.001(4) 0.005(4)
C15 0.029(3) 0.076(4) 0.149(7) 0.032(4) -0.010(4) -0.010(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te2 O1 2.201(4) . ?
Te2 N2 2.250(5) . ?
Te2 C8 2.104(5) . ?
Te1 O2 2.214(4) 2_656 ?
Te1 N1 2.244(5) . ?
Te1 C1 2.102(6) . ?
O1 N1 1.368(5) . ?
O2 Te1 2.214(4) 2_656 ?
O2 N2 1.361(6) . ?
N2 C10 1.286(7) . ?
N1 C3 1.287(7) . ?
C11 H11 0.9300 . ?
C11 C12 1.386(8) . ?
C11 C8 1.380(8) . ?
C12 H12 0.9300 . ?
C12 C13 1.379(9) . ?
C8 C9 1.408(7) . ?
C1 C2 1.403(8) . ?
C1 C4 1.401(8) . ?
C7 H7 0.9300 . ?
C7 C2 1.401(8) . ?
C7 C6 1.378(8) . ?
C2 C3 1.444(7) . ?
C6 H6 0.9300 . ?
C6 C5 1.371(10) . ?
C9 C14 1.412(8) . ?
C9 C10 1.431(8) . ?
C14 H14 0.9300 . ?
C14 C13 1.369(10) . ?
C5 H5 0.9300 . ?
C5 C4 1.402(9) . ?
C10 H10 0.9300 . ?
C13 H13 0.9300 . ?
C4 H4 0.9300 . ?
C3 H3 0.9300 . ?
C17 C17 1.341(15) 2 ?
C17 H17 0.9300 . ?
C17 C16 1.365(10) . ?
C16 H16 0.9300 . ?
C16 C15 1.360(10) . ?
C15 C15 1.383(16) 2 ?
C15 H15 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Te2 N2 164.59(17) . . ?
C8 Te2 O1 88.87(18) . . ?
C8 Te2 N2 75.8(2) . . ?
O2 Te1 N1 161.21(16) 2_656 . ?
C1 Te1 O2 85.3(2) . 2_656 ?
C1 Te1 N1 75.9(2) . . ?
N1 O1 Te2 115.7(3) . . ?
N2 O2 Te1 110.0(3) . 2_656 ?
O2 N2 Te2 125.4(3) . . ?
C10 N2 Te2 115.1(4) . . ?
C10 N2 O2 119.2(5) . . ?
O1 N1 Te1 127.2(3) . . ?
C3 N1 Te1 114.8(4) . . ?
C3 N1 O1 118.0(5) . . ?
C12 C11 H11 120.4 . . ?
C8 C11 H11 120.4 . . ?
C8 C11 C12 119.1(6) . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.8(7) . . ?
C13 C12 H12 119.6 . . ?
C11 C8 Te2 124.6(4) . . ?
C11 C8 C9 121.2(5) . . ?
C9 C8 Te2 114.2(4) . . ?
C2 C1 Te1 114.8(4) . . ?
C4 C1 Te1 125.1(5) . . ?
C4 C1 C2 120.1(6) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C6 C7 C2 119.4(7) . . ?
C1 C2 C3 117.7(5) . . ?
C7 C2 C1 120.1(5) . . ?
C7 C2 C3 122.2(6) . . ?
C7 C6 H6 119.7 . . ?
C5 C6 C7 120.5(6) . . ?
C5 C6 H6 119.7 . . ?
C8 C9 C14 117.9(6) . . ?
C8 C9 C10 118.7(5) . . ?
C14 C9 C10 123.5(5) . . ?
C9 C14 H14 119.8 . . ?
C13 C14 C9 120.4(6) . . ?
C13 C14 H14 119.8 . . ?
C6 C5 H5 119.1 . . ?
C6 C5 C4 121.7(6) . . ?
C4 C5 H5 119.1 . . ?
N2 C10 C9 116.2(5) . . ?
N2 C10 H10 121.9 . . ?
C9 C10 H10 121.9 . . ?
C12 C13 H13 119.7 . . ?
C14 C13 C12 120.5(6) . . ?
C14 C13 H13 119.7 . . ?
C1 C4 C5 118.0(7) . . ?
C1 C4 H4 121.0 . . ?
C5 C4 H4 121.0 . . ?
N1 C3 C2 116.8(6) . . ?
N1 C3 H3 121.6 . . ?
C2 C3 H3 121.6 . . ?
C17 C17 H17 119.7 2 . ?
C17 C17 C16 120.6(5) 2 . ?
C16 C17 H17 119.7 . . ?
C17 C16 H16 120.1 . . ?
C15 C16 C17 119.7(8) . . ?
C15 C16 H16 120.1 . . ?
C16 C15 C15 119.7(5) . 2 ?
C16 C15 H15 120.2 . . ?
C15 C15 H15 120.2 2 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Te2 O1 N1 Te1 1.4(5) . . . . ?
Te2 O1 N1 C3 -177.0(3) . . . . ?
Te2 N2 C10 C9 3.6(6) . . . . ?
Te2 C8 C9 C14 179.4(4) . . . . ?
Te2 C8 C9 C10 1.1(6) . . . . ?
Te1 O2 N2 Te2 -42.6(4) 2_656 . . . ?
Te1 O2 N2 C10 143.8(4) 2_656 . . . ?
Te1 N1 C3 C2 0.6(6) . . . . ?
Te1 C1 C2 C7 -178.7(4) . . . . ?
Te1 C1 C2 C3 1.1(6) . . . . ?
Te1 C1 C4 C5 179.6(4) . . . . ?
O1 N1 C3 C2 179.3(4) . . . . ?
O2 N2 C10 C9 177.7(4) . . . . ?
C11 C12 C13 C14 -0.2(9) . . . . ?
C11 C8 C9 C14 -0.6(7) . . . . ?
C11 C8 C9 C10 -178.8(4) . . . . ?
C12 C11 C8 Te2 -180.0(4) . . . . ?
C12 C11 C8 C9 0.0(7) . . . . ?
C8 C11 C12 C13 0.4(8) . . . . ?
C8 C9 C14 C13 0.8(8) . . . . ?
C8 C9 C10 N2 -3.2(7) . . . . ?
C1 C2 C3 N1 -1.2(7) . . . . ?
C7 C2 C3 N1 178.6(5) . . . . ?
C7 C6 C5 C4 1.0(9) . . . . ?
C2 C1 C4 C5 -0.2(8) . . . . ?
C2 C7 C6 C5 0.0(9) . . . . ?
C6 C7 C2 C1 -1.1(8) . . . . ?
C6 C7 C2 C3 179.1(5) . . . . ?
C6 C5 C4 C1 -0.9(9) . . . . ?
C9 C14 C13 C12 -0.4(9) . . . . ?
C14 C9 C10 N2 178.6(5) . . . . ?
C10 C9 C14 C13 178.9(5) . . . . ?
C4 C1 C2 C7 1.2(8) . . . . ?
C4 C1 C2 C3 -179.0(5) . . . . ?
C17 C17 C16 C15 -0.8(14) 2 . . . ?
C17 C16 C15 C15 1.4(12) . . . 2 ?
_shelx_res_file
;
ph509_0m_a.res created by SHELXL-2014/7
TITL PH509_0m_a.res in C2/c
REM Old TITL PH509_0m in C2/c
REM SHELXT solution in C2/c
REM R1 0.196, Rweak 0.004, Alpha 0.027, Orientation as input
REM Formula found by SHELXT: C18 N2 O Te2
CELL 0.71073 18.646 17.433 10.6572 90 95.384 90
ZERR 4 0.0025 0.0024 0.0015 0 0.002 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N O Te
UNIT 136 104 16 16 16
RIGU
L.S. 10
PLAN 20
SIZE 0.032 0.067 0.23
TEMP 23
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta
OMIT 2 0 0
OMIT 1 1 1
OMIT 0 2 0
OMIT -1 1 1
OMIT 1 1 0
REM
REM
REM
WGHT 0.031400 15.448900
FVAR 0.15661
TE2 5 0.591766 0.636919 0.579698 11.00000 0.03563 0.03894 =
0.07922 0.00207 0.01240 -0.00957
TE1 5 0.394322 0.652673 0.571385 11.00000 0.03904 0.05730 =
0.07891 0.00889 0.00972 -0.00910
O1 4 0.524813 0.584621 0.421286 11.00000 0.04227 0.06251 =
0.08520 -0.00834 0.01822 -0.02190
O2 4 0.693242 0.697376 0.822422 11.00000 0.04312 0.08736 =
0.08593 -0.00709 0.00588 -0.01260
N2 3 0.667509 0.712487 0.701153 11.00000 0.02840 0.04954 =
0.09391 -0.00754 0.01065 -0.00513
N1 3 0.451978 0.591751 0.424880 11.00000 0.04032 0.03987 =
0.08308 0.00566 0.01061 -0.01580
C11 1 0.589318 0.733264 0.334577 11.00000 0.03704 0.04074 =
0.09440 0.00806 0.01352 0.00503
AFIX 43
H11 2 0.557626 0.696642 0.298086 11.00000 -1.20000
AFIX 0
C12 1 0.609831 0.795203 0.264637 11.00000 0.05523 0.05175 =
0.11041 0.02484 0.01748 0.00755
AFIX 43
H12 2 0.591453 0.800200 0.180852 11.00000 -1.20000
AFIX 0
C8 1 0.616524 0.726647 0.459029 11.00000 0.02399 0.03077 =
0.09416 0.00298 0.02030 -0.00046
C1 1 0.310906 0.607672 0.446526 11.00000 0.03763 0.04029 =
0.08954 0.02180 -0.00460 -0.00815
C7 1 0.283335 0.535501 0.252990 11.00000 0.05702 0.03465 =
0.10932 0.00756 -0.01349 -0.00063
AFIX 43
H7 2 0.298479 0.509179 0.184304 11.00000 -1.20000
AFIX 0
C2 1 0.333970 0.566904 0.344197 11.00000 0.04814 0.02942 =
0.09625 0.01423 -0.00337 -0.00572
C6 1 0.210897 0.543947 0.265925 11.00000 0.05362 0.04177 =
0.13001 0.01208 -0.01486 -0.00149
AFIX 43
H6 2 0.177113 0.523217 0.205586 11.00000 -1.20000
AFIX 0
C9 1 0.664567 0.781496 0.515866 11.00000 0.02362 0.03170 =
0.10670 -0.00030 0.01751 0.00113
C14 1 0.684645 0.843360 0.441053 11.00000 0.03332 0.03812 =
0.13138 0.00772 0.01401 -0.00159
AFIX 43
H14 2 0.716743 0.880154 0.475758 11.00000 -1.20000
AFIX 0
C5 1 0.188236 0.582661 0.367017 11.00000 0.04289 0.05616 =
0.12378 0.02364 -0.00967 -0.00079
AFIX 43
H5 2 0.139121 0.586965 0.374642 11.00000 -1.20000
AFIX 0
C10 1 0.692041 0.770734 0.644630 11.00000 0.02782 0.04144 =
0.10667 -0.01099 0.01236 -0.00658
AFIX 43
H10 2 0.725708 0.803957 0.685122 11.00000 -1.20000
AFIX 0
C13 1 0.657143 0.849492 0.317752 11.00000 0.05773 0.04302 =
0.13482 0.02533 0.02043 0.00426
AFIX 43
H13 2 0.670487 0.890612 0.269440 11.00000 -1.20000
AFIX 0
C4 1 0.237165 0.615918 0.459167 11.00000 0.04282 0.05490 =
0.10705 0.02295 -0.00205 0.00166
AFIX 43
H4 2 0.221166 0.642669 0.526708 11.00000 -1.20000
AFIX 0
C3 1 0.410574 0.559221 0.337198 11.00000 0.04989 0.02998 =
0.08792 0.00765 0.00538 -0.01178
AFIX 43
H3 2 0.429109 0.532063 0.272424 11.00000 -1.20000
AFIX 0
C17 1 0.012726 0.512154 0.193191 11.00000 0.07285 0.07114 =
0.13162 -0.02567 -0.01682 0.01196
AFIX 43
H17 2 0.021298 0.465818 0.154012 11.00000 -1.20000
AFIX 0
C16 1 0.026160 0.579565 0.134562 11.00000 0.04289 0.11873 =
0.10605 0.00278 -0.00101 0.00511
AFIX 43
H16 2 0.044367 0.579147 0.056256 11.00000 -1.20000
AFIX 0
C15 1 0.012802 0.647357 0.191157 11.00000 0.02941 0.07577 =
0.14886 0.03203 -0.01005 -0.00956
AFIX 43
H15 2 0.020847 0.693477 0.150918 11.00000 -1.20000
AFIX 0
HKLF 4
REM PH509_0m_a.res in C2/c
REM R1 = 0.0410 for 2913 Fo > 4sig(Fo) and 0.0697 for all 4255 data
REM 208 parameters refined using 177 restraints
END
WGHT 0.0315 15.4268
REM Highest difference peak 0.968, deepest hole -1.514, 1-sigma level 0.107
Q1 1 0.3936 0.6826 0.6181 11.00000 0.05 0.97
Q2 1 0.5615 0.6404 0.5032 11.00000 0.05 0.84
Q3 1 0.3589 0.6510 0.5037 11.00000 0.05 0.78
Q4 1 0.4166 0.6604 0.5242 11.00000 0.05 0.77
Q5 1 0.4009 0.6171 0.5823 11.00000 0.05 0.73
Q6 1 0.6310 0.6093 0.5741 11.00000 0.05 0.66
Q7 1 0.5886 0.6828 0.5613 11.00000 0.05 0.60
Q8 1 0.6312 0.6334 0.6381 11.00000 0.05 0.59
Q9 1 0.5694 0.5954 0.5569 11.00000 0.05 0.56
Q10 1 0.6205 0.6471 0.6572 11.00000 0.05 0.53
Q11 1 0.3830 0.6282 0.6738 11.00000 0.05 0.47
Q12 1 0.0173 0.6216 0.1251 11.00000 0.05 0.44
Q13 1 0.6579 0.8669 0.3795 11.00000 0.05 0.42
Q14 1 0.5761 0.6439 0.2243 11.00000 0.05 0.41
Q15 1 0.7068 0.8536 0.4054 11.00000 0.05 0.39
Q16 1 0.1964 0.6712 0.5739 11.00000 0.05 0.39
Q17 1 0.5408 0.6709 0.5722 11.00000 0.05 0.39
Q18 1 0.1805 0.6034 0.4560 11.00000 0.05 0.38
Q19 1 0.5721 0.6392 0.6570 11.00000 0.05 0.38
Q20 1 0.0120 0.5479 0.1551 11.00000 0.05 0.36
;
_shelx_res_checksum 90705
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_twin4
_database_code_depnum_ccdc_archive 'CCDC 1530647'
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date 2017-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C7 H5 N O Se'
_chemical_formula_sum 'C7 H5 N O Se'
_chemical_formula_weight 198.08
_chemical_absolute_configuration ?
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a 7.3324(9)
_cell_length_b 8.0016(10)
_cell_length_c 11.8324(15)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 694.22(15)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 4214
_cell_measurement_temperature 100.0
_cell_measurement_theta_max 26.60
_cell_measurement_theta_min 3.074
_shelx_estimated_absorpt_T_max 0.618
_shelx_estimated_absorpt_T_min 0.415
_exptl_absorpt_coefficient_mu 5.327
_exptl_absorpt_correction_T_max 0.75
_exptl_absorpt_correction_T_min 0.43
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
For component 1:
wR2(int) was 0.1010 before and 0.0567 after correction.
The Ratio of minimum to maximum transmission not present.
The \l/2 correction factor is Not present
For component 2:
wR2(int) was 0.1186 before and 0.0645 after correction.
The Ratio of minimum to maximum transmission not present.
The \l/2 correction factor is Not present
For component 3:
wR2(int) was 0.1040 before and 0.0575 after correction.
The Ratio of minimum to maximum transmission is 0.58.
The \l/2 correction factor is Not present
Final HKLF 4 output contains 25696 reflections, Rint = 0.0614
(14788 with I > 3sig(I), Rint = 0.0507)
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.895
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 384
_exptl_crystal_size_max 0.2
_exptl_crystal_size_mid 0.1
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents ?
_diffrn_reflns_av_unetI/netI 0.0564
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -10
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_number 7086
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.391
_diffrn_reflns_theta_min 3.073
_diffrn_ambient_temperature 100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.691
_reflns_Friedel_fraction_full 1.000
_reflns_Friedel_fraction_max 0.992
_reflns_number_gt 6534
_reflns_number_total 7086
_reflns_special_details
;
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection 'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction 'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.622
_refine_diff_density_min -0.492
_refine_diff_density_rms 0.108
_refine_ls_abs_structure_details
;
Flack x determined using 665 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack 0.017(7)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.059
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 93
_refine_ls_number_reflns 7086
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0400
_refine_ls_R_factor_gt 0.0351
_refine_ls_restrained_S_all 1.059
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.1724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0859
_refine_ls_wR_factor_ref 0.0876
_refine_special_details
;
Refined as a 3-component twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.399(2) 0.1669(10) 0.4343(17)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
C4(H4), C5(H5), C6(H6), C7(H7), C3(H3)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2854(7) 0.6462(7) 0.6773(5) 0.0113(12) Uani 1 1 d . . . . .
C4 C 0.4033(8) 0.7758(8) 0.7075(5) 0.0153(13) Uani 1 1 d . . . . .
H4 H 0.3699 0.8550 0.7636 0.018 Uiso 1 1 calc R . . . .
C5 C 0.5706(9) 0.7853(8) 0.6532(5) 0.0161(12) Uani 1 1 d . . . . .
H5 H 0.6522 0.8732 0.6721 0.019 Uiso 1 1 calc R . . . .
C6 C 0.6220(8) 0.6676(8) 0.5709(5) 0.0141(12) Uani 1 1 d . . . . .
H6 H 0.7383 0.6756 0.5360 0.017 Uiso 1 1 calc R . . . .
C7 C 0.5047(8) 0.5406(7) 0.5405(5) 0.0132(13) Uani 1 1 d . . . . .
H7 H 0.5391 0.4617 0.4845 0.016 Uiso 1 1 calc R . . . .
C2 C 0.3331(8) 0.5293(7) 0.5937(5) 0.0128(12) Uani 1 1 d . . . . .
C3 C 0.1980(7) 0.4026(9) 0.5696(5) 0.0155(12) Uani 1 1 d . . . . .
H3 H 0.2159 0.3155 0.5162 0.019 Uiso 1 1 calc R . . . .
N1 N 0.0485(7) 0.4203(6) 0.6287(4) 0.0116(9) Uani 1 1 d . . . . .
O1 O -0.0938(5) 0.3204(6) 0.6252(4) 0.0150(9) Uani 1 1 d . . . . .
Se1 Se 0.04975(7) 0.60273(7) 0.73639(5) 0.01196(17) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.009(2) 0.012(3) 0.013(3) 0.004(2) -0.002(2) 0.001(2)
C4 0.016(3) 0.015(3) 0.014(3) -0.001(2) -0.002(2) -0.002(2)
C5 0.015(3) 0.014(3) 0.019(3) -0.001(2) -0.001(3) -0.005(2)
C6 0.013(3) 0.017(3) 0.013(3) 0.003(2) 0.000(2) 0.000(2)
C7 0.015(3) 0.014(3) 0.011(3) 0.001(2) 0.001(2) 0.003(2)
C2 0.015(3) 0.012(3) 0.012(3) 0.003(2) -0.002(2) -0.001(2)
C3 0.014(3) 0.018(3) 0.014(3) 0.004(3) -0.002(2) -0.002(3)
N1 0.014(2) 0.009(2) 0.012(2) -0.0002(17) 0.001(2) -0.003(2)
O1 0.014(2) 0.015(2) 0.017(2) 0.0023(18) -0.0032(16) -0.0048(17)
Se1 0.0114(2) 0.0120(2) 0.0125(3) -0.0001(2) 0.0004(2) 0.0005(2)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C4 1.397(8) . ?
C1 C2 1.405(8) . ?
C1 Se1 1.896(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.387(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.407(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.379(9) . ?
C7 H7 0.9500 . ?
C7 C2 1.410(8) . ?
C2 C3 1.446(8) . ?
C3 H3 0.9500 . ?
C3 N1 1.308(7) . ?
N1 O1 1.315(6) . ?
N1 Se1 1.938(5) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C4 C1 C2 121.4(5) . . ?
C4 C1 Se1 127.3(5) . . ?
C2 C1 Se1 111.3(4) . . ?
C1 C4 H4 121.0 . . ?
C5 C4 C1 118.0(6) . . ?
C5 C4 H4 121.0 . . ?
C4 C5 H5 119.3 . . ?
C4 C5 C6 121.4(6) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 119.8 . . ?
C7 C6 C5 120.5(6) . . ?
C7 C6 H6 119.8 . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C2 119.2(6) . . ?
C2 C7 H7 120.4 . . ?
C1 C2 C7 119.6(6) . . ?
C1 C2 C3 115.8(5) . . ?
C7 C2 C3 124.6(6) . . ?
C2 C3 H3 123.4 . . ?
N1 C3 C2 113.1(6) . . ?
N1 C3 H3 123.4 . . ?
C3 N1 O1 125.6(5) . . ?
C3 N1 Se1 115.4(4) . . ?
O1 N1 Se1 118.8(4) . . ?
C1 Se1 N1 84.3(2) . . ?
_shelx_res_file
;
twin4.res created by SHELXL-2014/7
TITL twin4_a.res in P2(1)2(1)2(1)
REM Old TITL twin4 in P2(1)2(1)2(1)
REM SHELXT solution in P2(1)2(1)2(1)
REM R1 0.038, Rweak 0.034, Alpha 0.003, Orientation as input
REM Flack x = 0.010 ( 0.007 ) from Parsons' quotients
REM Formula found by SHELXT: C3 N O Se
CELL 0.71073 7.3324 8.0016 11.8324 90 90 90
ZERR 4 0.0009 0.001 0.0015 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM -X,0.5+Y,0.5-Z
SYMM 0.5+X,0.5-Y,-Z
SFAC C H N O Se
UNIT 28 20 4 4 4
L.S. 10
PLAN 10
SIZE 0.1 0.1 0.2
TEMP -173.15
BOND $H
list 4
fmap 2
acta
REM
REM
REM
WGHT 0.044700 0.172400
BASF 0.16689 0.43425
FVAR 0.76051
C1 1 0.285399 0.646194 0.677280 11.00000 0.00935 0.01178 =
0.01274 0.00357 -0.00167 0.00062
C4 1 0.403296 0.775795 0.707532 11.00000 0.01643 0.01535 =
0.01422 -0.00149 -0.00156 -0.00151
AFIX 43
H4 2 0.369887 0.855039 0.763620 11.00000 -1.20000
AFIX 0
C5 1 0.570556 0.785326 0.653248 11.00000 0.01466 0.01433 =
0.01921 -0.00113 -0.00083 -0.00532
AFIX 43
H5 2 0.652173 0.873237 0.672057 11.00000 -1.20000
AFIX 0
C6 1 0.621953 0.667584 0.570916 11.00000 0.01262 0.01693 =
0.01265 0.00278 0.00003 -0.00011
AFIX 43
H6 2 0.738288 0.675625 0.535997 11.00000 -1.20000
AFIX 0
C7 1 0.504718 0.540609 0.540536 11.00000 0.01486 0.01359 =
0.01116 0.00145 0.00070 0.00287
AFIX 43
H7 2 0.539136 0.461709 0.484461 11.00000 -1.20000
AFIX 0
C2 1 0.333051 0.529305 0.593743 11.00000 0.01467 0.01169 =
0.01196 0.00288 -0.00243 -0.00068
C3 1 0.197953 0.402610 0.569553 11.00000 0.01395 0.01813 =
0.01430 0.00426 -0.00167 -0.00176
AFIX 43
H3 2 0.215921 0.315464 0.516175 11.00000 -1.20000
AFIX 0
N1 3 0.048466 0.420279 0.628693 11.00000 0.01382 0.00947 =
0.01162 -0.00015 0.00054 -0.00252
O1 4 -0.093811 0.320449 0.625238 11.00000 0.01362 0.01451 =
0.01699 0.00230 -0.00316 -0.00478
SE1 5 0.049752 0.602732 0.736394 11.00000 0.01142 0.01195 =
0.01250 -0.00011 0.00041 0.00053
HKLF 5
REM twin4_a.res in P2(1)2(1)2(1)
REM R1 = 0.0351 for 6534 Fo > 4sig(Fo) and 0.0400 for all 7086 data
REM 93 parameters refined using 0 restraints
END
WGHT 0.0446 0.1791
REM Highest difference peak 1.622, deepest hole -0.492, 1-sigma level 0.108
Q1 1 0.2151 0.4596 0.5400 11.00000 0.05 0.58
Q2 1 -0.1129 0.3206 0.5287 11.00000 0.05 0.55
Q3 1 0.1907 0.6131 0.7559 11.00000 0.05 0.48
Q4 1 0.1914 0.1912 0.4781 11.00000 0.05 0.48
Q5 1 0.0132 0.6148 0.6627 11.00000 0.05 0.45
Q6 1 0.7716 0.8212 0.5012 11.00000 0.05 0.45
Q7 1 0.0597 0.5290 0.6829 11.00000 0.05 0.42
Q8 1 0.7097 0.6177 0.4773 11.00000 0.05 0.41
Q9 1 0.1326 0.4051 0.5827 11.00000 0.05 0.40
Q10 1 0.0610 0.5096 0.7790 11.00000 0.05 0.38
;
_shelx_res_checksum 55405
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.399(2)
2 0.1669(10)
3 0.4343(17)
# start Validation Reply Form
_vrf_PLAT430_twin4
;
PROBLEM: Short Inter D...A Contact Se1 .. O1 .. 2.41 Ang.
RESPONSE: The short contact is expected due to chalcogen bonding interaction
;
# end Validation Reply Form
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_ph462yellow_b
_database_code_depnum_ccdc_archive 'CCDC 1507754'
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date 2016-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C28 H20 N4 O4 Te4'
_chemical_formula_sum 'C28 H20 N4 O4 Te4'
_chemical_formula_weight 986.88
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 7.2250(2)
_cell_length_b 8.7915(3)
_cell_length_c 12.1257(4)
_cell_angle_alpha 106.411(2)
_cell_angle_beta 102.489(2)
_cell_angle_gamma 90.001(2)
_cell_volume 719.81(4)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 9892
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 33.13
_cell_measurement_theta_min 2.56
_shelx_estimated_absorpt_T_max 0.848
_shelx_estimated_absorpt_T_min 0.418
_exptl_absorpt_coefficient_mu 4.054
_exptl_absorpt_correction_T_max 0.8668
_exptl_absorpt_correction_T_min 0.5443
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0387 before and 0.0347 after correction.
The Ratio of minimum to maximum transmission is 0.6279.
The \l/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 2.277
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description plate
_exptl_crystal_F_000 456
_exptl_crystal_size_max 0.261
_exptl_crystal_size_mid 0.129
_exptl_crystal_size_min 0.042
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0239
_diffrn_reflns_av_unetI/netI 0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -18
_diffrn_reflns_number 23510
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 33.131
_diffrn_reflns_theta_min 2.894
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4690
_reflns_number_total 5456
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.419
_refine_diff_density_min -0.551
_refine_diff_density_rms 0.133
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.009
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 181
_refine_ls_number_reflns 5456
_refine_ls_number_restraints 168
_refine_ls_R_factor_all 0.0299
_refine_ls_R_factor_gt 0.0238
_refine_ls_restrained_S_all 0.996
_refine_ls_shift/su_max 0.002
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0637
_refine_ls_wR_factor_ref 0.0677
_refine_special_details ?
_olex2_refinement_description
;
1. Others
Fixed Uiso: H10(0.027) H5(0.05) H11(0.03) H7(0.042) H12(0.034) H6(0.052)
H4(0.038) H14(0.031) H13(0.033) H3(0.034)
Fixed X: H10(0.0906) H5(1.3298) H11(0.4353) H7(0.949) H12(0.4628) H6(1.2286)
H4(1.1502) H14(0.2088) H13(0.3576) H3(0.6587)
Fixed Y: H10(0.0652) H5(0.9083) H11(0.1466) H7(0.7442) H12(-0.1266)
H6(0.8904) H4(0.7813) H14(-0.1816) H13(-0.291) H3(0.5686)
Fixed Z: H10(0.3377) H5(1.0058) H11(0.7877) H7(1.1519) H12(0.7426) H6(1.1719)
H4(0.8154) H14(0.4003) H13(0.5486) H3(1.0165)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 0.75629(2) 0.56416(2) 0.70944(2) 0.01879(4) Uani 1 1 d . U . . .
Te2 Te 0.26463(2) 0.38930(2) 0.64186(2) 0.01942(4) Uani 1 1 d . U . . .
O2 O 0.0395(2) 0.3585(2) 0.38298(14) 0.0249(3) Uani 1 1 d . U . . .
O1 O 0.4476(2) 0.4340(2) 0.82325(14) 0.0290(4) Uani 1 1 d . U . . .
N2 N 0.1250(3) 0.2752(2) 0.45640(16) 0.0205(3) Uani 1 1 d . U . . .
N1 N 0.6125(3) 0.5218(2) 0.84477(16) 0.0216(3) Uani 1 1 d . U . . .
C9 C 0.2348(3) 0.0488(3) 0.5046(2) 0.0203(4) Uani 1 1 d . U . . .
C1 C 0.9406(3) 0.6861(3) 0.87010(19) 0.0225(4) Uani 1 1 d . U . . .
C2 C 0.8800(3) 0.6739(3) 0.9704(2) 0.0260(4) Uani 1 1 d . U . . .
C10 C 0.1395(3) 0.1236(3) 0.41785(19) 0.0223(4) Uani 1 1 d . U . . .
H10 H 0.0906 0.0652 0.3377 0.027 Uiso 1 1 calc R . . . .
C5 C 1.2148(4) 0.8487(4) 0.9962(3) 0.0416(7) Uani 1 1 d . U . . .
H5 H 1.3298 0.9083 1.0058 0.050 Uiso 1 1 calc R . . . .
C11 C 0.3903(3) 0.0810(3) 0.7091(2) 0.0252(4) Uani 1 1 d . U . . .
H11 H 0.4353 0.1466 0.7877 0.030 Uiso 1 1 calc R . . . .
C8 C 0.3071(3) 0.1478(3) 0.62006(19) 0.0198(4) Uani 1 1 d . U . . .
C7 C 0.9892(4) 0.7514(3) 1.0839(2) 0.0354(6) Uani 1 1 d . U . . .
H7 H 0.9490 0.7442 1.1519 0.042 Uiso 1 1 calc R . . . .
C12 C 0.4067(3) -0.0812(3) 0.6819(2) 0.0284(5) Uani 1 1 d . U . . .
H12 H 0.4628 -0.1266 0.7426 0.034 Uiso 1 1 calc R . . . .
C6 C 1.1547(4) 0.8377(4) 1.0954(3) 0.0433(7) Uani 1 1 d . U . . .
H6 H 1.2286 0.8904 1.1719 0.052 Uiso 1 1 calc R . . . .
C4 C 1.1085(3) 0.7732(3) 0.8828(2) 0.0317(5) Uani 1 1 d . U . . .
H4 H 1.1502 0.7813 0.8154 0.038 Uiso 1 1 calc R . . . .
C14 C 0.2550(3) -0.1150(3) 0.4785(2) 0.0258(4) Uani 1 1 d . U . . .
H14 H 0.2088 -0.1816 0.4003 0.031 Uiso 1 1 calc R . . . .
C13 C 0.3419(3) -0.1801(3) 0.5664(2) 0.0278(5) Uani 1 1 d . U . . .
H13 H 0.3576 -0.2910 0.5486 0.033 Uiso 1 1 calc R . . . .
C3 C 0.7045(3) 0.5828(3) 0.9521(2) 0.0281(5) Uani 1 1 d . U . . .
H3 H 0.6587 0.5686 1.0165 0.034 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Te1 0.01967(7) 0.02201(7) 0.01485(7) 0.00609(5) 0.00318(5) -0.00070(5)
Te2 0.01921(7) 0.02133(7) 0.01847(7) 0.00680(5) 0.00443(5) -0.00118(5)
O2 0.0210(7) 0.0372(9) 0.0232(8) 0.0187(7) 0.0060(6) 0.0044(6)
O1 0.0299(8) 0.0389(9) 0.0173(7) 0.0079(7) 0.0036(6) -0.0136(7)
N2 0.0181(8) 0.0281(9) 0.0169(8) 0.0095(7) 0.0031(6) -0.0003(6)
N1 0.0221(8) 0.0252(9) 0.0183(8) 0.0076(7) 0.0041(6) -0.0027(7)
C9 0.0170(8) 0.0233(9) 0.0212(9) 0.0065(7) 0.0052(7) -0.0007(7)
C1 0.0227(9) 0.0241(10) 0.0184(9) 0.0043(7) 0.0025(7) -0.0009(8)
C2 0.0244(10) 0.0347(12) 0.0164(9) 0.0044(8) 0.0033(8) -0.0016(8)
C10 0.0214(9) 0.0271(10) 0.0182(9) 0.0065(8) 0.0046(7) -0.0017(8)
C5 0.0262(12) 0.0563(17) 0.0330(13) 0.0017(12) 0.0022(10) -0.0131(11)
C11 0.0242(10) 0.0320(11) 0.0215(10) 0.0119(9) 0.0038(8) 0.0026(8)
C8 0.0171(8) 0.0236(9) 0.0202(9) 0.0085(7) 0.0046(7) 0.0001(7)
C7 0.0274(11) 0.0538(16) 0.0185(10) 0.0015(10) 0.0039(9) -0.0040(11)
C12 0.0265(11) 0.0319(11) 0.0326(12) 0.0187(10) 0.0062(9) 0.0037(9)
C6 0.0298(12) 0.0587(18) 0.0261(12) -0.0070(12) -0.0003(10) -0.0127(12)
C4 0.0259(11) 0.0400(13) 0.0257(11) 0.0046(10) 0.0050(9) -0.0086(9)
C14 0.0239(10) 0.0229(10) 0.0277(11) 0.0018(8) 0.0071(8) -0.0030(8)
C13 0.0249(10) 0.0227(10) 0.0396(13) 0.0119(9) 0.0110(9) 0.0015(8)
C3 0.0277(10) 0.0401(13) 0.0163(9) 0.0067(9) 0.0066(8) -0.0058(9)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te1 O2 2.2448(15) 2_666 ?
Te1 N1 2.2345(18) . ?
Te1 C1 2.101(2) . ?
Te2 O1 2.2347(16) . ?
Te2 N2 2.1966(18) . ?
Te2 C8 2.096(2) . ?
O2 Te1 2.2448(15) 2_666 ?
O2 N2 1.357(2) . ?
O1 N1 1.354(2) . ?
N2 C10 1.294(3) . ?
N1 C3 1.286(3) . ?
C9 C10 1.445(3) . ?
C9 C8 1.409(3) . ?
C9 C14 1.399(3) . ?
C1 C2 1.409(3) . ?
C1 C4 1.391(3) . ?
C2 C7 1.408(3) . ?
C2 C3 1.441(3) . ?
C10 H10 0.9500 . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C5 C4 1.396(4) . ?
C11 H11 0.9500 . ?
C11 C8 1.396(3) . ?
C11 C12 1.381(3) . ?
C7 H7 0.9500 . ?
C7 C6 1.376(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.402(4) . ?
C6 H6 0.9500 . ?
C4 H4 0.9500 . ?
C14 H14 0.9500 . ?
C14 C13 1.383(3) . ?
C13 H13 0.9500 . ?
C3 H3 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Te1 O2 164.46(7) . 2_666 ?
C1 Te1 O2 87.86(8) . 2_666 ?
C1 Te1 N1 76.61(8) . . ?
N2 Te2 O1 162.38(7) . . ?
C8 Te2 O1 86.72(8) . . ?
C8 Te2 N2 76.40(8) . . ?
N2 O2 Te1 111.60(12) . 2_666 ?
N1 O1 Te2 115.49(12) . . ?
O2 N2 Te2 122.67(14) . . ?
C10 N2 Te2 116.13(14) . . ?
C10 N2 O2 121.04(18) . . ?
O1 N1 Te1 126.29(13) . . ?
C3 N1 Te1 114.46(15) . . ?
C3 N1 O1 119.18(19) . . ?
C8 C9 C10 117.3(2) . . ?
C14 C9 C10 122.9(2) . . ?
C14 C9 C8 119.8(2) . . ?
C2 C1 Te1 113.83(16) . . ?
C4 C1 Te1 125.89(17) . . ?
C4 C1 C2 120.3(2) . . ?
C1 C2 C3 118.0(2) . . ?
C7 C2 C1 119.8(2) . . ?
C7 C2 C3 122.2(2) . . ?
N2 C10 C9 115.7(2) . . ?
N2 C10 H10 122.1 . . ?
C9 C10 H10 122.1 . . ?
C6 C5 H5 119.5 . . ?
C6 C5 C4 120.9(3) . . ?
C4 C5 H5 119.5 . . ?
C8 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C12 C11 C8 119.5(2) . . ?
C9 C8 Te2 114.28(15) . . ?
C11 C8 Te2 125.81(17) . . ?
C11 C8 C9 119.8(2) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 C2 119.4(2) . . ?
C6 C7 H7 120.3 . . ?
C11 C12 H12 119.4 . . ?
C11 C12 C13 121.2(2) . . ?
C13 C12 H12 119.4 . . ?
C5 C6 H6 119.7 . . ?
C7 C6 C5 120.7(2) . . ?
C7 C6 H6 119.7 . . ?
C1 C4 C5 118.9(2) . . ?
C1 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C9 C14 H14 119.9 . . ?
C13 C14 C9 120.1(2) . . ?
C13 C14 H14 119.9 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
N1 C3 C2 117.1(2) . . ?
N1 C3 H3 121.5 . . ?
C2 C3 H3 121.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Te1 O2 N2 Te2 89.38(14) 2_666 . . . ?
Te1 O2 N2 C10 -85.9(2) 2_666 . . . ?
Te1 N1 C3 C2 2.4(3) . . . . ?
Te1 C1 C2 C7 -179.3(2) . . . . ?
Te1 C1 C2 C3 -0.2(3) . . . . ?
Te1 C1 C4 C5 179.5(2) . . . . ?
Te2 O1 N1 Te1 -19.0(2) . . . . ?
Te2 O1 N1 C3 164.45(18) . . . . ?
Te2 N2 C10 C9 4.0(2) . . . . ?
O2 N2 C10 C9 179.54(17) . . . . ?
O1 N1 C3 C2 179.4(2) . . . . ?
C9 C14 C13 C12 1.1(3) . . . . ?
C1 C2 C7 C6 -0.3(4) . . . . ?
C1 C2 C3 N1 -1.6(4) . . . . ?
C2 C1 C4 C5 -0.3(4) . . . . ?
C2 C7 C6 C5 -0.1(5) . . . . ?
C10 C9 C8 Te2 -1.1(2) . . . . ?
C10 C9 C8 C11 176.13(19) . . . . ?
C10 C9 C14 C13 -177.8(2) . . . . ?
C11 C12 C13 C14 -1.9(4) . . . . ?
C8 C9 C10 N2 -2.0(3) . . . . ?
C8 C9 C14 C13 1.4(3) . . . . ?
C8 C11 C12 C13 0.3(3) . . . . ?
C7 C2 C3 N1 177.5(2) . . . . ?
C12 C11 C8 Te2 179.08(16) . . . . ?
C12 C11 C8 C9 2.2(3) . . . . ?
C6 C5 C4 C1 -0.1(5) . . . . ?
C4 C1 C2 C7 0.6(4) . . . . ?
C4 C1 C2 C3 179.7(2) . . . . ?
C4 C5 C6 C7 0.4(5) . . . . ?
C14 C9 C10 N2 177.2(2) . . . . ?
C14 C9 C8 Te2 179.73(15) . . . . ?
C14 C9 C8 C11 -3.1(3) . . . . ?
C3 C2 C7 C6 -179.4(3) . . . . ?
_shelx_res_file
;
ph462yellow_b.res created by SHELXL-2014/7
TITL ph462yellow_b_a.res in P-1
REM Old TITL ph462yellow_b in P-1 #2
REM SHELXT solution in P-1
REM R1 0.050, Rweak 0.003, Alpha 0.032, Orientation as input
REM Formula found by SHELXT: C15 N2 O Te2
CELL 0.71073 7.225 8.7915 12.1257 106.411 102.489 90.001
ZERR 1 0.0002 0.0003 0.0004 0.002 0.002 0.002
LATT 1
SFAC C H N O Te
UNIT 28 20 4 4 4
RIGU
L.S. 10
PLAN 20
SIZE 0.042 0.129 0.261
TEMP -173
BOND $H
LIST 4
MORE -1
CONF
fmap 2
acta 52
OMIT 0 0 1
OMIT 0 1 0
OMIT 2 2 2
REM
REM
REM
WGHT 0.045500
FVAR 0.39488
TE1 5 0.756288 0.564156 0.709439 11.00000 0.01967 0.02201 =
0.01485 0.00609 0.00318 -0.00070
TE2 5 0.264630 0.389304 0.641859 11.00000 0.01921 0.02133 =
0.01847 0.00680 0.00443 -0.00118
O2 4 0.039543 0.358540 0.382981 11.00000 0.02105 0.03719 =
0.02324 0.01872 0.00604 0.00445
O1 4 0.447611 0.434031 0.823253 11.00000 0.02985 0.03893 =
0.01729 0.00788 0.00356 -0.01359
N2 3 0.125033 0.275229 0.456399 11.00000 0.01812 0.02805 =
0.01686 0.00952 0.00308 -0.00030
N1 3 0.612534 0.521758 0.844768 11.00000 0.02207 0.02518 =
0.01826 0.00757 0.00407 -0.00271
C9 1 0.234803 0.048833 0.504565 11.00000 0.01702 0.02333 =
0.02115 0.00655 0.00520 -0.00068
C1 1 0.940591 0.686078 0.870100 11.00000 0.02268 0.02407 =
0.01844 0.00432 0.00252 -0.00088
C2 1 0.880045 0.673871 0.970369 11.00000 0.02441 0.03468 =
0.01636 0.00436 0.00328 -0.00162
C10 1 0.139474 0.123598 0.417846 11.00000 0.02142 0.02713 =
0.01819 0.00645 0.00457 -0.00165
AFIX 43
H10 2 0.090558 0.065194 0.337699 11.00000 -1.20000
AFIX 0
C5 1 1.214797 0.848664 0.996245 11.00000 0.02618 0.05633 =
0.03304 0.00169 0.00221 -0.01314
AFIX 43
H5 2 1.329800 0.908295 1.005833 11.00000 -1.20000
AFIX 0
C11 1 0.390299 0.081013 0.709094 11.00000 0.02421 0.03203 =
0.02145 0.01193 0.00382 0.00259
AFIX 43
H11 2 0.435274 0.146623 0.787719 11.00000 -1.20000
AFIX 0
C8 1 0.307125 0.147754 0.620056 11.00000 0.01712 0.02358 =
0.02018 0.00852 0.00461 0.00007
C7 1 0.989218 0.751428 1.083897 11.00000 0.02744 0.05385 =
0.01854 0.00147 0.00386 -0.00403
AFIX 43
H7 2 0.948983 0.744214 1.151937 11.00000 -1.20000
AFIX 0
C12 1 0.406676 -0.081221 0.681946 11.00000 0.02652 0.03187 =
0.03263 0.01869 0.00619 0.00366
AFIX 43
H12 2 0.462812 -0.126632 0.742643 11.00000 -1.20000
AFIX 0
C6 1 1.154675 0.837748 1.095416 11.00000 0.02977 0.05871 =
0.02607 -0.00701 -0.00035 -0.01270
AFIX 43
H6 2 1.228623 0.890435 1.171865 11.00000 -1.20000
AFIX 0
C4 1 1.108490 0.773212 0.882825 11.00000 0.02586 0.04000 =
0.02571 0.00464 0.00501 -0.00862
AFIX 43
H4 2 1.150157 0.781254 0.815430 11.00000 -1.20000
AFIX 0
C14 1 0.254960 -0.114987 0.478518 11.00000 0.02387 0.02293 =
0.02774 0.00185 0.00710 -0.00300
AFIX 43
H14 2 0.208829 -0.181612 0.400334 11.00000 -1.20000
AFIX 0
C13 1 0.341899 -0.180051 0.566374 11.00000 0.02486 0.02269 =
0.03961 0.01192 0.01105 0.00152
AFIX 43
H13 2 0.357647 -0.290994 0.548556 11.00000 -1.20000
AFIX 0
C3 1 0.704499 0.582837 0.952102 11.00000 0.02775 0.04010 =
0.01633 0.00673 0.00662 -0.00579
AFIX 43
H3 2 0.658688 0.568553 1.016510 11.00000 -1.20000
AFIX 0
HKLF 4
REM ph462yellow_b_a.res in P-1
REM R1 = 0.0238 for 4690 Fo > 4sig(Fo) and 0.0299 for all 5456 data
REM 181 parameters refined using 168 restraints
END
WGHT 0.0353 0.1968
REM Highest difference peak 1.419, deepest hole -0.551, 1-sigma level 0.133
Q1 1 0.7928 0.4870 0.7093 11.00000 0.05 1.42
Q2 1 0.7198 0.6432 0.7160 11.00000 0.05 1.36
Q3 1 0.3206 0.3141 0.6432 11.00000 0.05 1.36
Q4 1 0.2313 0.4644 0.6384 11.00000 0.05 1.25
Q5 1 0.7134 0.4735 0.6669 11.00000 0.05 0.97
Q6 1 0.3131 0.4296 0.6993 11.00000 0.05 0.96
Q7 1 0.7391 0.5402 0.6477 11.00000 0.05 0.92
Q8 1 0.2256 0.3253 0.5969 11.00000 0.05 0.85
Q9 1 0.6725 0.5541 0.7288 11.00000 0.05 0.84
Q10 1 0.2248 0.3613 0.5805 11.00000 0.05 0.81
Q11 1 0.3575 0.4383 0.6587 11.00000 0.05 0.71
Q12 1 0.8126 0.5589 0.6705 11.00000 0.05 0.65
Q13 1 0.2637 -0.0311 0.4779 11.00000 0.05 0.63
Q14 1 0.3729 -0.0064 0.6859 11.00000 0.05 0.61
Q15 1 0.1598 0.0960 0.4723 11.00000 0.05 0.58
Q16 1 0.2647 0.1161 0.5623 11.00000 0.05 0.54
Q17 1 0.1482 0.2061 0.4204 11.00000 0.05 0.52
Q18 1 0.8732 0.6644 0.8315 11.00000 0.05 0.51
Q19 1 0.9379 0.7053 1.0249 11.00000 0.05 0.50
Q20 1 0.8960 0.6762 0.9137 11.00000 0.05 0.50
;
_shelx_res_checksum 54324
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_ph462_2_0m_a
_database_code_depnum_ccdc_archive 'CCDC 1507753'
_audit_update_record
;
2017-03-16 deposited with the CCDC.
2017-04-03 downloaded from the CCDC.
;
_audit_creation_date 2016-10-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety
'C42 H30 N6 O6 Te6, 1.78(C H2 Cl2), 0.22(H2 O1)'
_chemical_formula_sum 'C43.78 H34 Cl3.56 N6 O6.22 Te6'
_chemical_formula_weight 1635.57
_chemical_absolute_configuration ?
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system trigonal
_space_group_IT_number 144
_space_group_name_H-M_alt 'P 31'
_space_group_name_Hall 'P 31'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
_cell_length_a 14.4246(7)
_cell_length_b 14.4246(7)
_cell_length_c 21.3472(12)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 120
_cell_volume 3846.6(4)
_cell_formula_units_Z 3
_cell_measurement_reflns_used 9854
_cell_measurement_temperature 100(2)
_cell_measurement_theta_max 32.255
_cell_measurement_theta_min 2.510
_shelx_estimated_absorpt_T_max 0.714
_shelx_estimated_absorpt_T_min 0.581
_exptl_absorpt_coefficient_mu 3.605
_exptl_absorpt_correction_T_max 0.7000
_exptl_absorpt_correction_T_min 0.5727
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0631 before and 0.0552 after correction.
The Ratio of minimum to maximum transmission is 0.8181.
The \l/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 2.118
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 2283
_exptl_crystal_size_max 0.169
_exptl_crystal_size_mid 0.125
_exptl_crystal_size_min 0.1
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0477
_diffrn_reflns_av_unetI/netI 0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_l_max 33
_diffrn_reflns_limit_l_min -33
_diffrn_reflns_number 131669
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full 26.000
_diffrn_reflns_theta_max 33.536
_diffrn_reflns_theta_min 2.510
_diffrn_ambient_temperature 100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type 'Bruker APEX-II CCD'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 1.000
_reflns_Friedel_fraction_full 0.999
_reflns_Friedel_fraction_max 0.998
_reflns_number_gt 17518
_reflns_number_total 20091
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection 'APEX2 v2014.9-0 (Bruker, 2014)'
_computing_data_reduction 'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max 1.669
_refine_diff_density_min -0.673
_refine_diff_density_rms 0.149
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.51(2)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.031
_refine_ls_hydrogen_treatment mixed
_refine_ls_matrix_type full
_refine_ls_number_parameters 602
_refine_ls_number_reflns 20091
_refine_ls_number_restraints 1
_refine_ls_R_factor_all 0.0434
_refine_ls_R_factor_gt 0.0330
_refine_ls_restrained_S_all 1.031
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+4.2435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0644
_refine_ls_wR_factor_ref 0.0686
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.49(2) 0.51(2)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All O(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uiso(C44) = Uiso(O44A)
4. Rigid body (RIGU) restrains
C44, Cl4, Cl3
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Sof(O44A)=Sof(H44C)=Sof(H44D)=1-FVAR(1)
Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(Cl3)=Sof(Cl4)=FVAR(1)
6.a Free rotating group:
O44A(H44C,H44D)
6.b Secondary CH2 refined with riding coordinates:
C43(H43A,H43B), C44(H44A,H44B)
6.c Aromatic/amide H refined with riding coordinates:
C42(H42), C4(H4), C41(H41), C12(H12), C28(H28), C32(H32), C13(H13), C5(H5),
C6(H6), C19(H19), C14(H14), C21(H21), C40(H40), C31(H31), C20(H20), C7(H7),
C34(H34), C3(H3), C35(H35), C17(H17), C25(H25), C11(H11), C38(H38), C33(H33),
C26(H26), C10(H10), C27(H27), C24(H24), C39(H39)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te3 Te 0.44432(3) 0.39457(3) 0.48611(2) 0.01624(7) Uani 1 1 d . . . . .
Te5 Te 0.94027(3) 0.68766(3) 0.49258(2) 0.01785(8) Uani 1 1 d . . . . .
Te1 Te 0.66629(3) 0.90635(3) 0.48191(2) 0.01845(8) Uani 1 1 d . . . . .
Te6 Te 0.92058(3) 0.92762(3) 0.52407(2) 0.01696(7) Uani 1 1 d . . . . .
Te2 Te 0.42482(3) 0.64024(3) 0.51173(2) 0.01823(8) Uani 1 1 d . . . . .
Te4 Te 0.70577(3) 0.42082(3) 0.51580(2) 0.01794(8) Uani 1 1 d . . . . .
O6 O 0.7994(4) 0.9887(4) 0.4161(2) 0.0266(10) Uani 1 1 d . . . . .
O4 O 0.9017(4) 0.5673(4) 0.4197(2) 0.0253(9) Uani 1 1 d . . . . .
O2 O 0.3644(4) 0.4410(3) 0.41517(19) 0.0224(9) Uani 1 1 d . . . . .
O5 O 0.9902(4) 0.8740(4) 0.59676(18) 0.0228(9) Uani 1 1 d . . . . .
O1 O 0.4702(4) 0.7676(4) 0.5803(2) 0.0254(9) Uani 1 1 d . . . . .
O3 O 0.5785(3) 0.3327(4) 0.5844(2) 0.0230(9) Uani 1 1 d . . . . .
N5 N 1.0078(4) 0.7932(4) 0.5784(2) 0.0205(10) Uani 1 1 d . . . . .
N3 N 0.4820(4) 0.3237(4) 0.5702(2) 0.0197(10) Uani 1 1 d . . . . .
N1 N 0.5535(4) 0.8668(4) 0.5640(2) 0.0195(10) Uani 1 1 d . . . . .
N2 N 0.3496(4) 0.5247(4) 0.4306(2) 0.0190(9) Uani 1 1 d . . . . .
N6 N 0.8936(4) 0.9985(4) 0.4361(2) 0.0194(9) Uani 1 1 d . . . . .
N4 N 0.8176(4) 0.4682(4) 0.4327(2) 0.0192(9) Uani 1 1 d . . . . .
C29 C 1.0318(5) 0.6309(5) 0.5381(3) 0.0210(12) Uani 1 1 d . . . . .
C18 C 0.2019(5) 0.3028(5) 0.5150(3) 0.0242(12) Uani 1 1 d . . . . .
C1 C 0.7228(5) 1.0528(5) 0.5291(3) 0.0208(11) Uani 1 1 d . . . . .
C42 C 1.1710(5) 1.1086(5) 0.3894(3) 0.0260(13) Uani 1 1 d . . . . .
H42 H 1.1730 1.1400 0.3499 0.031 Uiso 1 1 calc R . . . .
C4 C 0.8080(5) 1.1511(5) 0.5093(3) 0.0247(12) Uani 1 1 d . . . . .
H4 H 0.8445 1.1564 0.4712 0.030 Uiso 1 1 calc R . . . .
C9 C 0.2745(5) 0.6333(5) 0.4128(3) 0.0210(12) Uani 1 1 d . . . . .
C41 C 1.2634(5) 1.1170(5) 0.4141(3) 0.0266(13) Uani 1 1 d . . . . .
H41 H 1.3284 1.1522 0.3911 0.032 Uiso 1 1 calc R . . . .
C15 C 0.2990(5) 0.3143(5) 0.5353(3) 0.0193(11) Uani 1 1 d . . . . .
C12 C 0.2502(6) 0.8034(6) 0.4509(4) 0.0347(17) Uani 1 1 d . . . . .
H12 H 0.2413 0.8615 0.4639 0.042 Uiso 1 1 calc R . . . .
C28 C 0.6733(6) 0.1976(5) 0.3696(3) 0.0278(13) Uani 1 1 d . . . . .
H28 H 0.7110 0.2040 0.3319 0.033 Uiso 1 1 calc R . . . .
C32 C 1.0446(5) 0.5470(5) 0.5157(3) 0.0282(14) Uani 1 1 d . . . . .
H32 H 1.0109 0.5106 0.4780 0.034 Uiso 1 1 calc R . . . .
C13 C 0.1964(6) 0.7451(6) 0.3987(3) 0.0312(15) Uani 1 1 d . . . . .
H13 H 0.1522 0.7643 0.3757 0.037 Uiso 1 1 calc R . . . .
C2 C 0.6673(5) 1.0472(5) 0.5842(3) 0.0205(11) Uani 1 1 d . . . . .
C5 C 0.8382(6) 1.2407(6) 0.5465(4) 0.0327(15) Uani 1 1 d . . . . .
H5 H 0.8974 1.3071 0.5338 0.039 Uiso 1 1 calc R . . . .
C6 C 0.7852(6) 1.2368(5) 0.6015(3) 0.0306(15) Uani 1 1 d . . . . .
H6 H 0.8071 1.2997 0.6257 0.037 Uiso 1 1 calc R . . . .
C16 C 0.3040(5) 0.2670(5) 0.5921(3) 0.0212(12) Uani 1 1 d . . . . .
C19 C 0.1125(5) 0.2473(5) 0.5529(3) 0.0276(14) Uani 1 1 d . . . . .
H19 H 0.0460 0.2387 0.5392 0.033 Uiso 1 1 calc R . . . .
C14 C 0.2062(5) 0.6588(6) 0.3795(3) 0.0289(14) Uani 1 1 d . . . . .
H14 H 0.1673 0.6173 0.3443 0.035 Uiso 1 1 calc R . . . .
C30 C 1.0822(5) 0.6853(5) 0.5934(3) 0.0234(12) Uani 1 1 d . . . . .
C21 C 0.2112(6) 0.2120(5) 0.6295(3) 0.0281(14) Uani 1 1 d . . . . .
H21 H 0.2139 0.1806 0.6681 0.034 Uiso 1 1 calc R . . . .
C40 C 1.2612(5) 1.0738(5) 0.4728(3) 0.0247(12) Uani 1 1 d . . . . .
H40 H 1.3253 1.0811 0.4900 0.030 Uiso 1 1 calc R . . . .
C8 C 0.3298(5) 0.6932(5) 0.4658(3) 0.0197(11) Uani 1 1 d . . . . .
C31 C 1.0667(5) 0.7717(5) 0.6140(3) 0.0235(12) Uani 1 1 d . . . . .
H31 H 1.0979 0.8103 0.6515 0.028 Uiso 1 1 calc R . . . .
C20 C 0.1165(5) 0.2044(5) 0.6095(3) 0.0309(15) Uani 1 1 d . . . . .
H20 H 0.0542 0.1695 0.6349 0.037 Uiso 1 1 calc R . . . .
C7 C 0.7007(6) 1.1408(5) 0.6205(3) 0.0294(14) Uani 1 1 d . . . . .
H7 H 0.6643 1.1370 0.6583 0.035 Uiso 1 1 calc R . . . .
C34 C 1.1575(6) 0.5704(6) 0.6048(3) 0.0357(17) Uani 1 1 d . . . . .
H34 H 1.2000 0.5486 0.6275 0.043 Uiso 1 1 calc R . . . .
C3 C 0.5780(5) 0.9451(5) 0.6018(3) 0.0223(12) Uani 1 1 d . . . . .
H3 H 0.5392 0.9361 0.6394 0.027 Uiso 1 1 calc R . . . .
C35 C 1.1465(6) 0.6529(6) 0.6270(3) 0.0318(15) Uani 1 1 d . . . . .
H35 H 1.1815 0.6885 0.6646 0.038 Uiso 1 1 calc R . . . .
C17 C 0.4040(5) 0.2744(5) 0.6094(3) 0.0210(11) Uani 1 1 d . . . . .
H17 H 0.4121 0.2449 0.6473 0.025 Uiso 1 1 calc R . . . .
C36 C 1.0726(5) 1.0093(5) 0.4811(3) 0.0195(11) Uani 1 1 d . . . . .
C25 C 0.5639(5) 0.1795(5) 0.4817(3) 0.0239(12) Uani 1 1 d . . . . .
H25 H 0.5265 0.1727 0.5196 0.029 Uiso 1 1 calc R . . . .
C11 C 0.3180(5) 0.7786(5) 0.4852(3) 0.0248(13) Uani 1 1 d . . . . .
H11 H 0.3550 0.8194 0.5210 0.030 Uiso 1 1 calc R . . . .
C43 C 0.7200(8) 0.7193(8) 0.6470(5) 0.076(3) Uani 1 1 d . . . A 1
H43A H 0.7212 0.7851 0.6327 0.091 Uiso 1 1 calc R . . A 1
H43B H 0.7941 0.7322 0.6446 0.091 Uiso 1 1 calc R . . A 1
C44 C 0.6308(7) 0.6019(8) 0.3582(4) 0.0339(17) Uiso 0.780(5) 1 d . U P B 1
H44A H 0.5594 0.5782 0.3767 0.041 Uiso 0.780(5) 1 calc R . P B 1
H44B H 0.6435 0.5404 0.3590 0.041 Uiso 0.780(5) 1 calc R . P B 1
C37 C 1.0740(5) 1.0538(5) 0.4225(3) 0.0200(11) Uani 1 1 d . . . . .
C38 C 0.9760(5) 1.0449(5) 0.3999(3) 0.0207(11) Uani 1 1 d . . . . .
H38 H 0.9722 1.0721 0.3601 0.025 Uiso 1 1 calc R . . . .
C33 C 1.1090(6) 0.5182(6) 0.5506(4) 0.0334(16) Uani 1 1 d . . . . .
H33 H 1.1189 0.4615 0.5363 0.040 Uiso 1 1 calc R . . . .
C23 C 0.7048(5) 0.2876(5) 0.4084(3) 0.0211(12) Uani 1 1 d . . . . .
C26 C 0.5329(6) 0.0900(5) 0.4432(4) 0.0314(15) Uani 1 1 d . . . . .
H26 H 0.4749 0.0223 0.4553 0.038 Uiso 1 1 calc R . . . .
C10 C 0.2869(5) 0.5430(5) 0.3955(3) 0.0206(11) Uani 1 1 d . . . . .
H10 H 0.2509 0.4993 0.3603 0.025 Uiso 1 1 calc R . . . .
C27 C 0.5872(6) 0.0999(5) 0.3869(3) 0.0295(14) Uani 1 1 d . . . . .
H27 H 0.5647 0.0394 0.3605 0.035 Uiso 1 1 calc R . . . .
C24 C 0.7955(5) 0.3916(5) 0.3931(3) 0.0225(12) Uani 1 1 d . . . . .
H24 H 0.8364 0.4030 0.3561 0.027 Uiso 1 1 calc R . . . .
C22 C 0.6497(5) 0.2781(5) 0.4643(3) 0.0202(11) Uani 1 1 d . . . . .
C39 C 1.1658(5) 1.0199(5) 0.5069(3) 0.0212(11) Uani 1 1 d . . . . .
H39 H 1.1648 0.9909 0.5470 0.025 Uiso 1 1 calc R . . . .
Cl3 Cl 0.7290(2) 0.7069(2) 0.40286(12) 0.0468(8) Uani 0.780(5) 1 d . U P B 1
Cl4 Cl 0.63286(19) 0.6426(2) 0.27975(11) 0.0377(7) Uani 0.780(5) 1 d . U P B 1
Cl2 Cl 0.63948(18) 0.61520(17) 0.59736(9) 0.0452(4) Uani 1 1 d . . . A 1
Cl1 Cl 0.67636(16) 0.69386(19) 0.72578(10) 0.0438(5) Uani 1 1 d . . . A 1
H18 H 0.197(5) 0.328(5) 0.478(3) 0.017(16) Uiso 1 1 d . . . C 1
O44A O 0.6823(19) 0.6154(19) 0.4084(10) 0.0339(17) Uiso 0.220(5) 1 d . . P B 2
H44C H 0.6283 0.5508 0.4124 0.051 Uiso 0.220(5) 1 d G . P B 2
H44D H 0.7365 0.6126 0.3925 0.051 Uiso 0.220(5) 1 d G . P B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Te3 0.01547(17) 0.01449(16) 0.01857(15) 0.00039(12) 0.00240(12) 0.00736(14)
Te5 0.01589(17) 0.01607(17) 0.02154(17) 0.00208(13) -0.00023(13) 0.00796(14)
Te1 0.01827(18) 0.01935(18) 0.01917(16) -0.00354(13) -0.00321(13) 0.01049(14)
Te6 0.01704(17) 0.01707(17) 0.01668(15) 0.00093(12) 0.00244(12) 0.00845(14)
Te2 0.01693(17) 0.01662(17) 0.02031(17) 0.00044(12) 0.00031(12) 0.00778(14)
Te4 0.01637(18) 0.01806(17) 0.02039(16) -0.00347(13) -0.00192(13) 0.00935(14)
O6 0.025(2) 0.035(3) 0.022(2) 0.0044(18) -0.0005(17) 0.017(2)
O4 0.025(2) 0.020(2) 0.027(2) -0.0014(16) 0.0041(17) 0.0090(19)
O2 0.025(2) 0.022(2) 0.0219(19) -0.0030(16) -0.0031(16) 0.0135(19)
O5 0.028(2) 0.028(2) 0.0168(18) -0.0013(16) -0.0020(15) 0.018(2)
O1 0.027(2) 0.018(2) 0.021(2) -0.0019(16) 0.0046(17) 0.0035(18)
O3 0.018(2) 0.031(2) 0.024(2) 0.0027(17) 0.0017(15) 0.0149(18)
N5 0.019(2) 0.023(3) 0.018(2) 0.0026(18) 0.0005(18) 0.010(2)
N3 0.020(2) 0.018(2) 0.021(2) 0.0009(18) 0.0013(18) 0.009(2)
N1 0.020(2) 0.020(2) 0.019(2) -0.0021(17) -0.0024(17) 0.010(2)
N2 0.016(2) 0.018(2) 0.023(2) 0.0029(18) 0.0029(18) 0.009(2)
N6 0.019(2) 0.022(2) 0.019(2) -0.0013(18) 0.0005(17) 0.011(2)
N4 0.019(2) 0.018(2) 0.023(2) 0.0007(18) 0.0001(18) 0.011(2)
C29 0.014(3) 0.019(3) 0.030(3) 0.013(2) 0.009(2) 0.008(2)
C18 0.023(3) 0.014(3) 0.033(3) -0.001(2) 0.004(2) 0.008(2)
C1 0.020(3) 0.021(3) 0.024(3) -0.003(2) -0.009(2) 0.012(2)
C42 0.029(3) 0.021(3) 0.020(3) -0.001(2) 0.007(2) 0.007(3)
C4 0.018(3) 0.021(3) 0.036(3) -0.002(2) -0.004(2) 0.010(2)
C9 0.022(3) 0.027(3) 0.019(2) 0.009(2) 0.006(2) 0.016(3)
C41 0.022(3) 0.021(3) 0.027(3) -0.004(2) 0.008(2) 0.004(2)
C15 0.021(3) 0.017(3) 0.021(3) -0.0039(19) 0.003(2) 0.010(2)
C12 0.029(4) 0.025(3) 0.056(5) 0.020(3) 0.020(3) 0.019(3)
C28 0.042(4) 0.023(3) 0.023(3) -0.007(2) -0.008(3) 0.020(3)
C32 0.020(3) 0.016(3) 0.046(4) 0.010(3) 0.006(3) 0.007(2)
C13 0.029(3) 0.040(4) 0.034(3) 0.014(3) 0.006(3) 0.025(3)
C2 0.026(3) 0.019(3) 0.021(3) -0.006(2) -0.010(2) 0.015(2)
C5 0.025(3) 0.022(3) 0.050(4) 0.002(3) -0.012(3) 0.011(3)
C6 0.039(4) 0.022(3) 0.034(3) -0.007(3) -0.017(3) 0.017(3)
C16 0.018(3) 0.013(2) 0.025(3) -0.004(2) 0.005(2) 0.003(2)
C19 0.017(3) 0.018(3) 0.045(4) -0.006(3) 0.003(3) 0.007(2)
C14 0.027(3) 0.038(4) 0.027(3) 0.013(3) 0.009(2) 0.021(3)
C30 0.018(3) 0.031(3) 0.024(3) 0.012(2) 0.006(2) 0.014(3)
C21 0.029(3) 0.024(3) 0.022(3) -0.003(2) 0.006(2) 0.006(3)
C40 0.020(3) 0.022(3) 0.032(3) -0.007(2) 0.001(2) 0.010(2)
C8 0.013(2) 0.015(3) 0.029(3) 0.007(2) 0.004(2) 0.006(2)
C31 0.025(3) 0.033(3) 0.016(2) 0.003(2) 0.002(2) 0.017(3)
C20 0.019(3) 0.024(3) 0.038(4) -0.007(3) 0.009(3) 0.002(3)
C7 0.044(4) 0.023(3) 0.025(3) -0.010(2) -0.014(3) 0.020(3)
C34 0.032(4) 0.046(4) 0.038(4) 0.022(3) 0.011(3) 0.026(3)
C3 0.026(3) 0.022(3) 0.019(3) -0.003(2) -0.004(2) 0.013(3)
C35 0.026(3) 0.051(5) 0.027(3) 0.015(3) 0.005(2) 0.025(3)
C17 0.023(3) 0.017(3) 0.017(2) 0.0019(19) 0.003(2) 0.006(2)
C36 0.017(3) 0.014(3) 0.023(3) -0.002(2) 0.004(2) 0.004(2)
C25 0.019(3) 0.022(3) 0.033(3) -0.002(2) -0.003(2) 0.012(3)
C11 0.020(3) 0.019(3) 0.037(3) 0.006(2) 0.009(2) 0.011(3)
C43 0.056(6) 0.047(5) 0.078(7) -0.012(5) 0.030(5) -0.009(5)
C37 0.020(3) 0.019(3) 0.019(2) -0.006(2) 0.001(2) 0.009(2)
C38 0.026(3) 0.016(3) 0.016(2) -0.0013(19) 0.000(2) 0.007(2)
C33 0.025(3) 0.027(3) 0.057(4) 0.015(3) 0.012(3) 0.019(3)
C23 0.027(3) 0.023(3) 0.018(2) -0.004(2) -0.005(2) 0.016(3)
C26 0.026(3) 0.014(3) 0.053(4) -0.005(3) -0.017(3) 0.010(3)
C10 0.018(3) 0.025(3) 0.019(2) 0.003(2) 0.001(2) 0.011(2)
C27 0.035(4) 0.025(3) 0.031(3) -0.013(2) -0.012(3) 0.016(3)
C24 0.030(3) 0.026(3) 0.017(2) 0.001(2) -0.001(2) 0.018(3)
C22 0.019(3) 0.018(3) 0.028(3) -0.006(2) -0.006(2) 0.012(2)
C39 0.016(3) 0.018(3) 0.027(3) -0.003(2) 0.002(2) 0.007(2)
Cl3 0.0440(14) 0.069(2) 0.0400(13) -0.0186(12) -0.0157(10) 0.0374(14)
Cl4 0.0292(11) 0.0491(15) 0.0211(10) 0.0034(8) 0.0000(8) 0.0095(10)
Cl2 0.0637(13) 0.0420(10) 0.0357(9) -0.0084(8) -0.0101(8) 0.0308(10)
Cl1 0.0474(12) 0.0611(13) 0.0318(10) -0.0118(8) -0.0063(7) 0.0338(11)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te3 O2 2.201(4) . ?
Te3 N3 2.262(5) . ?
Te3 C15 2.099(6) . ?
Te5 O4 2.185(4) . ?
Te5 N5 2.268(5) . ?
Te5 C29 2.107(6) . ?
Te1 O6 2.189(5) . ?
Te1 N1 2.261(5) . ?
Te1 C1 2.102(6) . ?
Te6 O5 2.189(4) . ?
Te6 N6 2.264(5) . ?
Te6 C36 2.110(6) . ?
Te2 O1 2.178(4) . ?
Te2 N2 2.268(5) . ?
Te2 C8 2.114(6) . ?
Te4 O3 2.190(4) . ?
Te4 N4 2.261(5) . ?
Te4 C22 2.105(6) . ?
O6 N6 1.361(6) . ?
O4 N4 1.363(7) . ?
O2 N2 1.368(7) . ?
O5 N5 1.368(7) . ?
O1 N1 1.375(7) . ?
O3 N3 1.366(7) . ?
N5 C31 1.288(8) . ?
N3 C17 1.293(7) . ?
N1 C3 1.286(7) . ?
N2 C10 1.300(7) . ?
N6 C38 1.289(8) . ?
N4 C24 1.298(8) . ?
C29 C32 1.397(9) . ?
C29 C30 1.403(9) . ?
C18 C15 1.395(9) . ?
C18 C19 1.388(9) . ?
C18 H18 0.88(6) . ?
C1 C4 1.399(9) . ?
C1 C2 1.401(9) . ?
C42 H42 0.9500 . ?
C42 C41 1.382(10) . ?
C42 C37 1.405(8) . ?
C4 H4 0.9500 . ?
C4 C5 1.388(10) . ?
C9 C14 1.404(9) . ?
C9 C8 1.405(9) . ?
C9 C10 1.447(9) . ?
C41 H41 0.9500 . ?
C41 C40 1.393(9) . ?
C15 C16 1.411(9) . ?
C12 H12 0.9500 . ?
C12 C13 1.378(11) . ?
C12 C11 1.403(10) . ?
C28 H28 0.9500 . ?
C28 C23 1.409(8) . ?
C28 C27 1.384(10) . ?
C32 H32 0.9500 . ?
C32 C33 1.405(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.383(10) . ?
C2 C7 1.416(8) . ?
C2 C3 1.440(9) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(10) . ?
C6 H6 0.9500 . ?
C6 C7 1.371(10) . ?
C16 C21 1.413(9) . ?
C16 C17 1.440(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.370(10) . ?
C14 H14 0.9500 . ?
C30 C31 1.440(9) . ?
C30 C35 1.425(8) . ?
C21 H21 0.9500 . ?
C21 C20 1.383(10) . ?
C40 H40 0.9500 . ?
C40 C39 1.398(8) . ?
C8 C11 1.388(9) . ?
C31 H31 0.9500 . ?
C20 H20 0.9500 . ?
C7 H7 0.9500 . ?
C34 H34 0.9500 . ?
C34 C35 1.362(11) . ?
C34 C33 1.367(11) . ?
C3 H3 0.9500 . ?
C35 H35 0.9500 . ?
C17 H17 0.9500 . ?
C36 C37 1.402(8) . ?
C36 C39 1.389(8) . ?
C25 H25 0.9500 . ?
C25 C26 1.402(9) . ?
C25 C22 1.391(9) . ?
C11 H11 0.9500 . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C43 Cl2 1.727(10) . ?
C43 Cl1 1.769(10) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 Cl3 1.751(10) . ?
C44 Cl4 1.770(9) . ?
C37 C38 1.438(9) . ?
C38 H38 0.9500 . ?
C33 H33 0.9500 . ?
C23 C24 1.451(9) . ?
C23 C22 1.403(9) . ?
C26 H26 0.9500 . ?
C26 C27 1.402(10) . ?
C10 H10 0.9500 . ?
C27 H27 0.9500 . ?
C24 H24 0.9500 . ?
C39 H39 0.9500 . ?
O44A H44C 0.8699 . ?
O44A H44D 0.8701 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Te3 N3 164.65(18) . . ?
C15 Te3 O2 88.9(2) . . ?
C15 Te3 N3 75.7(2) . . ?
O4 Te5 N5 164.10(19) . . ?
C29 Te5 O4 88.8(2) . . ?
C29 Te5 N5 75.3(2) . . ?
O6 Te1 N1 163.62(18) . . ?
C1 Te1 O6 88.2(2) . . ?
C1 Te1 N1 75.6(2) . . ?
O5 Te6 N6 163.93(17) . . ?
C36 Te6 O5 88.5(2) . . ?
C36 Te6 N6 75.7(2) . . ?
O1 Te2 N2 164.70(19) . . ?
C8 Te2 O1 89.0(2) . . ?
C8 Te2 N2 75.7(2) . . ?
O3 Te4 N4 164.60(18) . . ?
C22 Te4 O3 88.9(2) . . ?
C22 Te4 N4 75.7(2) . . ?
N6 O6 Te1 114.5(3) . . ?
N4 O4 Te5 115.4(3) . . ?
N2 O2 Te3 116.0(3) . . ?
N5 O5 Te6 114.3(3) . . ?
N1 O1 Te2 116.4(3) . . ?
N3 O3 Te4 115.2(3) . . ?
O5 N5 Te5 127.0(4) . . ?
C31 N5 Te5 115.4(4) . . ?
C31 N5 O5 117.6(5) . . ?
O3 N3 Te3 126.7(4) . . ?
C17 N3 Te3 114.9(4) . . ?
C17 N3 O3 118.3(5) . . ?
O1 N1 Te1 127.1(3) . . ?
C3 N1 Te1 114.7(4) . . ?
C3 N1 O1 117.9(5) . . ?
O2 N2 Te2 127.2(3) . . ?
C10 N2 Te2 114.6(4) . . ?
C10 N2 O2 118.1(5) . . ?
O6 N6 Te6 126.9(4) . . ?
C38 N6 Te6 114.1(4) . . ?
C38 N6 O6 118.7(5) . . ?
O4 N4 Te4 127.1(3) . . ?
C24 N4 Te4 114.8(4) . . ?
C24 N4 O4 118.1(5) . . ?
C32 C29 Te5 123.9(5) . . ?
C32 C29 C30 121.2(6) . . ?
C30 C29 Te5 114.9(4) . . ?
C15 C18 H18 120(4) . . ?
C19 C18 C15 118.4(6) . . ?
C19 C18 H18 121(4) . . ?
C4 C1 Te1 125.2(5) . . ?
C4 C1 C2 119.9(6) . . ?
C2 C1 Te1 114.9(5) . . ?
C41 C42 H42 119.9 . . ?
C41 C42 C37 120.1(6) . . ?
C37 C42 H42 119.9 . . ?
C1 C4 H4 120.7 . . ?
C5 C4 C1 118.6(6) . . ?
C5 C4 H4 120.7 . . ?
C14 C9 C8 120.2(6) . . ?
C14 C9 C10 121.7(6) . . ?
C8 C9 C10 118.1(5) . . ?
C42 C41 H41 120.0 . . ?
C42 C41 C40 120.0(6) . . ?
C40 C41 H41 120.0 . . ?
C18 C15 Te3 125.3(5) . . ?
C18 C15 C16 120.0(6) . . ?
C16 C15 Te3 114.7(4) . . ?
C13 C12 H12 119.4 . . ?
C13 C12 C11 121.2(7) . . ?
C11 C12 H12 119.4 . . ?
C23 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C27 C28 C23 119.6(6) . . ?
C29 C32 H32 121.1 . . ?
C29 C32 C33 117.8(7) . . ?
C33 C32 H32 121.1 . . ?
C12 C13 H13 119.7 . . ?
C12 C13 C14 120.6(6) . . ?
C14 C13 H13 119.7 . . ?
C1 C2 C7 119.5(6) . . ?
C1 C2 C3 118.1(5) . . ?
C7 C2 C3 122.4(6) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 C4 122.5(7) . . ?
C6 C5 H5 118.8 . . ?
C5 C6 H6 120.5 . . ?
C7 C6 C5 119.0(6) . . ?
C7 C6 H6 120.5 . . ?
C15 C16 C21 119.6(6) . . ?
C15 C16 C17 118.4(5) . . ?
C21 C16 C17 122.0(6) . . ?
C18 C19 H19 118.7 . . ?
C20 C19 C18 122.5(6) . . ?
C20 C19 H19 118.7 . . ?
C9 C14 H14 120.4 . . ?
C13 C14 C9 119.1(7) . . ?
C13 C14 H14 120.4 . . ?
C29 C30 C31 118.7(5) . . ?
C29 C30 C35 118.7(6) . . ?
C35 C30 C31 122.6(6) . . ?
C16 C21 H21 120.3 . . ?
C20 C21 C16 119.4(6) . . ?
C20 C21 H21 120.3 . . ?
C41 C40 H40 119.6 . . ?
C41 C40 C39 120.8(6) . . ?
C39 C40 H40 119.6 . . ?
C9 C8 Te2 115.0(4) . . ?
C11 C8 Te2 124.8(5) . . ?
C11 C8 C9 120.2(6) . . ?
N5 C31 C30 115.8(6) . . ?
N5 C31 H31 122.1 . . ?
C30 C31 H31 122.1 . . ?
C19 C20 C21 120.0(6) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C2 C7 H7 119.7 . . ?
C6 C7 C2 120.5(6) . . ?
C6 C7 H7 119.7 . . ?
C35 C34 H34 119.2 . . ?
C35 C34 C33 121.6(6) . . ?
C33 C34 H34 119.2 . . ?
N1 C3 C2 116.5(6) . . ?
N1 C3 H3 121.7 . . ?
C2 C3 H3 121.7 . . ?
C30 C35 H35 120.3 . . ?
C34 C35 C30 119.4(7) . . ?
C34 C35 H35 120.3 . . ?
N3 C17 C16 116.1(6) . . ?
N3 C17 H17 121.9 . . ?
C16 C17 H17 121.9 . . ?
C37 C36 Te6 114.7(4) . . ?
C39 C36 Te6 124.6(4) . . ?
C39 C36 C37 120.7(5) . . ?
C26 C25 H25 120.1 . . ?
C22 C25 H25 120.1 . . ?
C22 C25 C26 119.8(6) . . ?
C12 C11 H11 120.6 . . ?
C8 C11 C12 118.7(7) . . ?
C8 C11 H11 120.6 . . ?
H43A C43 H43B 107.8 . . ?
Cl2 C43 H43A 109.0 . . ?
Cl2 C43 H43B 109.0 . . ?
Cl2 C43 Cl1 112.8(5) . . ?
Cl1 C43 H43A 109.0 . . ?
Cl1 C43 H43B 109.0 . . ?
H44A C44 H44B 108.1 . . ?
Cl3 C44 H44A 109.5 . . ?
Cl3 C44 H44B 109.5 . . ?
Cl3 C44 Cl4 110.8(5) . . ?
Cl4 C44 H44A 109.5 . . ?
Cl4 C44 H44B 109.5 . . ?
C42 C37 C38 122.6(6) . . ?
C36 C37 C42 119.3(6) . . ?
C36 C37 C38 118.0(5) . . ?
N6 C38 C37 117.2(5) . . ?
N6 C38 H38 121.4 . . ?
C37 C38 H38 121.4 . . ?
C32 C33 H33 119.4 . . ?
C34 C33 C32 121.3(7) . . ?
C34 C33 H33 119.4 . . ?
C28 C23 C24 121.9(6) . . ?
C22 C23 C28 120.3(6) . . ?
C22 C23 C24 117.8(5) . . ?
C25 C26 H26 119.9 . . ?
C25 C26 C27 120.3(6) . . ?
C27 C26 H26 119.9 . . ?
N2 C10 C9 116.6(6) . . ?
N2 C10 H10 121.7 . . ?
C9 C10 H10 121.7 . . ?
C28 C27 C26 120.2(6) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
N4 C24 C23 116.4(5) . . ?
N4 C24 H24 121.8 . . ?
C23 C24 H24 121.8 . . ?
C25 C22 Te4 124.9(5) . . ?
C25 C22 C23 119.8(6) . . ?
C23 C22 Te4 115.3(4) . . ?
C40 C39 H39 120.5 . . ?
C36 C39 C40 119.0(6) . . ?
C36 C39 H39 120.5 . . ?
H44C O44A H44D 109.4 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Te3 O2 N2 Te2 12.6(5) . . . . ?
Te3 O2 N2 C10 -168.2(4) . . . . ?
Te3 N3 C17 C16 3.3(7) . . . . ?
Te3 C15 C16 C21 179.2(4) . . . . ?
Te3 C15 C16 C17 -2.2(7) . . . . ?
Te5 O4 N4 Te4 6.7(6) . . . . ?
Te5 O4 N4 C24 -175.5(4) . . . . ?
Te5 N5 C31 C30 1.0(7) . . . . ?
Te5 C29 C32 C33 179.3(5) . . . . ?
Te5 C29 C30 C31 0.7(7) . . . . ?
Te5 C29 C30 C35 -179.5(5) . . . . ?
Te1 O6 N6 Te6 5.5(6) . . . . ?
Te1 O6 N6 C38 179.2(4) . . . . ?
Te1 N1 C3 C2 4.7(7) . . . . ?
Te1 C1 C4 C5 -178.2(5) . . . . ?
Te1 C1 C2 C7 178.3(4) . . . . ?
Te1 C1 C2 C3 -1.3(7) . . . . ?
Te6 O5 N5 Te5 -15.0(5) . . . . ?
Te6 O5 N5 C31 167.0(4) . . . . ?
Te6 N6 C38 C37 -5.4(7) . . . . ?
Te6 C36 C37 C42 -179.1(4) . . . . ?
Te6 C36 C37 C38 3.5(7) . . . . ?
Te6 C36 C39 C40 178.4(4) . . . . ?
Te2 O1 N1 Te1 -11.3(6) . . . . ?
Te2 O1 N1 C3 175.9(4) . . . . ?
Te2 N2 C10 C9 0.2(7) . . . . ?
Te2 C8 C11 C12 -178.6(5) . . . . ?
Te4 O3 N3 Te3 -2.2(6) . . . . ?
Te4 O3 N3 C17 -178.6(4) . . . . ?
Te4 N4 C24 C23 -1.3(7) . . . . ?
O6 N6 C38 C37 -179.9(5) . . . . ?
O4 N4 C24 C23 -179.4(5) . . . . ?
O2 N2 C10 C9 -179.1(5) . . . . ?
O5 N5 C31 C30 179.3(5) . . . . ?
O1 N1 C3 C2 178.4(5) . . . . ?
O3 N3 C17 C16 -179.9(5) . . . . ?
C29 C32 C33 C34 0.0(10) . . . . ?
C29 C30 C31 N5 -1.1(9) . . . . ?
C29 C30 C35 C34 0.1(9) . . . . ?
C18 C15 C16 C21 -2.8(9) . . . . ?
C18 C15 C16 C17 175.8(6) . . . . ?
C18 C19 C20 C21 -2.5(10) . . . . ?
C1 C4 C5 C6 -1.8(10) . . . . ?
C1 C2 C7 C6 1.4(9) . . . . ?
C1 C2 C3 N1 -2.5(9) . . . . ?
C42 C41 C40 C39 1.2(9) . . . . ?
C42 C37 C38 N6 -175.7(6) . . . . ?
C4 C1 C2 C7 -2.4(9) . . . . ?
C4 C1 C2 C3 178.1(5) . . . . ?
C4 C5 C6 C7 0.9(10) . . . . ?
C9 C8 C11 C12 0.0(9) . . . . ?
C41 C42 C37 C36 1.0(9) . . . . ?
C41 C42 C37 C38 178.2(6) . . . . ?
C41 C40 C39 C36 0.4(9) . . . . ?
C15 C18 C19 C20 0.5(10) . . . . ?
C15 C16 C21 C20 0.8(9) . . . . ?
C15 C16 C17 N3 -0.9(8) . . . . ?
C12 C13 C14 C9 -2.0(10) . . . . ?
C28 C23 C24 N4 -179.2(6) . . . . ?
C28 C23 C22 Te4 -179.1(5) . . . . ?
C28 C23 C22 C25 0.3(9) . . . . ?
C32 C29 C30 C31 179.5(6) . . . . ?
C32 C29 C30 C35 -0.6(9) . . . . ?
C13 C12 C11 C8 -0.3(9) . . . . ?
C2 C1 C4 C5 2.5(9) . . . . ?
C5 C6 C7 C2 -0.7(10) . . . . ?
C16 C21 C20 C19 1.9(10) . . . . ?
C19 C18 C15 Te3 180.0(4) . . . . ?
C19 C18 C15 C16 2.1(9) . . . . ?
C14 C9 C8 Te2 178.0(4) . . . . ?
C14 C9 C8 C11 -0.6(9) . . . . ?
C14 C9 C10 N2 -178.0(6) . . . . ?
C30 C29 C32 C33 0.6(9) . . . . ?
C21 C16 C17 N3 177.7(5) . . . . ?
C8 C9 C14 C13 1.7(9) . . . . ?
C8 C9 C10 N2 -0.5(8) . . . . ?
C31 C30 C35 C34 179.9(6) . . . . ?
C7 C2 C3 N1 178.0(6) . . . . ?
C3 C2 C7 C6 -179.0(6) . . . . ?
C35 C30 C31 N5 179.0(6) . . . . ?
C35 C34 C33 C32 -0.6(11) . . . . ?
C17 C16 C21 C20 -177.8(6) . . . . ?
C36 C37 C38 N6 1.5(8) . . . . ?
C25 C26 C27 C28 1.5(10) . . . . ?
C11 C12 C13 C14 1.3(10) . . . . ?
C37 C42 C41 C40 -1.9(9) . . . . ?
C37 C36 C39 C40 -1.3(9) . . . . ?
C33 C34 C35 C30 0.5(11) . . . . ?
C23 C28 C27 C26 -1.3(10) . . . . ?
C26 C25 C22 Te4 179.2(5) . . . . ?
C26 C25 C22 C23 -0.1(9) . . . . ?
C10 C9 C14 C13 179.1(6) . . . . ?
C10 C9 C8 Te2 0.5(7) . . . . ?
C10 C9 C8 C11 -178.1(5) . . . . ?
C27 C28 C23 C24 179.1(6) . . . . ?
C27 C28 C23 C22 0.4(9) . . . . ?
C24 C23 C22 Te4 2.2(7) . . . . ?
C24 C23 C22 C25 -178.4(6) . . . . ?
C22 C25 C26 C27 -0.8(9) . . . . ?
C22 C23 C24 N4 -0.6(8) . . . . ?
C39 C36 C37 C42 0.6(9) . . . . ?
C39 C36 C37 C38 -176.8(5) . . . . ?
_shelx_res_file
;
ph462_2_0m_a.res created by SHELXL-2014/7
TITL ph4622_p32_a.res in P3(1)
REM Old TITL ph4622_p32 in P3(2)
REM SHELXT solution in P3(1)
REM R1 0.050, Rweak 0.013, Alpha 0.010, Orientation as input
REM Flack x = 0.496 ( 0.010 ) from Parsons' quotients
REM Formula found by SHELXT: C41 N12 O3 Cl4 Te6
CELL 0.71073 14.4246 14.4246 21.3472 90 90 120
ZERR 3 0.0007 0.0007 0.0012 0 0 0
LATT -1
SYMM -Y,+X-Y,0.333+Z
SYMM +Y-X,-X,0.667+Z
SFAC C H Cl N O Te
UNIT 131.34 102 10.69 18 18.66 18
RIGU C44 Cl4 Cl3
EADP C44 O44A
L.S. 10
PLAN 30
SIZE 0.1 0.125 0.169
TEMP -173
BOND $H
LIST 6
MORE -1
CONF
fmap 2
acta 52
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT 0 1 -1
OMIT -1 1 1
OMIT -1 1 0
OMIT 0 1 0
OMIT -1 1 -1
OMIT 0 1 1
REM
REM
REM
WGHT 0.026400 4.243500
BASF 0.50717
FVAR 0.11588 0.78011
TE3 6 0.444323 0.394569 0.486111 11.00000 0.01547 0.01449 =
0.01857 0.00039 0.00240 0.00736
TE5 6 0.940271 0.687660 0.492580 11.00000 0.01589 0.01607 =
0.02154 0.00208 -0.00023 0.00796
TE1 6 0.666287 0.906345 0.481915 11.00000 0.01827 0.01935 =
0.01917 -0.00354 -0.00321 0.01049
TE6 6 0.920578 0.927620 0.524072 11.00000 0.01704 0.01707 =
0.01668 0.00093 0.00244 0.00845
TE2 6 0.424817 0.640244 0.511728 11.00000 0.01693 0.01662 =
0.02031 0.00044 0.00031 0.00778
TE4 6 0.705774 0.420825 0.515804 11.00000 0.01637 0.01806 =
0.02039 -0.00347 -0.00192 0.00935
O6 5 0.799408 0.988739 0.416130 11.00000 0.02502 0.03492 =
0.02234 0.00439 -0.00049 0.01686
O4 5 0.901661 0.567294 0.419728 11.00000 0.02512 0.02026 =
0.02735 -0.00139 0.00412 0.00901
O2 5 0.364400 0.440988 0.415171 11.00000 0.02500 0.02240 =
0.02191 -0.00297 -0.00312 0.01349
O5 5 0.990169 0.873993 0.596758 11.00000 0.02815 0.02843 =
0.01680 -0.00125 -0.00199 0.01782
O1 5 0.470233 0.767603 0.580297 11.00000 0.02701 0.01787 =
0.02109 -0.00192 0.00456 0.00350
O3 5 0.578518 0.332680 0.584385 11.00000 0.01801 0.03051 =
0.02434 0.00267 0.00169 0.01492
N5 4 1.007819 0.793226 0.578445 11.00000 0.01942 0.02280 =
0.01826 0.00263 0.00046 0.00980
N3 4 0.482033 0.323667 0.570173 11.00000 0.01988 0.01785 =
0.02145 0.00086 0.00126 0.00946
N1 4 0.553464 0.866768 0.563975 11.00000 0.01958 0.01972 =
0.01880 -0.00209 -0.00240 0.00956
N2 4 0.349638 0.524715 0.430640 11.00000 0.01640 0.01845 =
0.02271 0.00293 0.00287 0.00913
N6 4 0.893561 0.998546 0.436075 11.00000 0.01927 0.02190 =
0.01871 -0.00135 0.00047 0.01147
N4 4 0.817640 0.468176 0.432735 11.00000 0.01910 0.01794 =
0.02280 0.00073 0.00015 0.01092
C29 1 1.031780 0.630857 0.538127 11.00000 0.01442 0.01881 =
0.02956 0.01348 0.00881 0.00805
C18 1 0.201853 0.302770 0.515000 11.00000 0.02265 0.01439 =
0.03347 -0.00104 0.00413 0.00765
C1 1 0.722833 1.052775 0.529149 11.00000 0.01957 0.02138 =
0.02415 -0.00272 -0.00904 0.01230
C42 1 1.170959 1.108592 0.389381 11.00000 0.02851 0.02150 =
0.02017 -0.00143 0.00720 0.00672
AFIX 43
H42 2 1.172983 1.139969 0.349909 11.00000 -1.20000
AFIX 0
C4 1 0.808040 1.151063 0.509324 11.00000 0.01807 0.02099 =
0.03560 -0.00159 -0.00424 0.01016
AFIX 43
H4 2 0.844468 1.156372 0.471246 11.00000 -1.20000
AFIX 0
C9 1 0.274510 0.633257 0.412777 11.00000 0.02163 0.02720 =
0.01872 0.00917 0.00580 0.01565
C41 1 1.263394 1.116992 0.414148 11.00000 0.02169 0.02144 =
0.02738 -0.00384 0.00777 0.00380
AFIX 43
H41 2 1.328409 1.152220 0.391135 11.00000 -1.20000
AFIX 0
C15 1 0.299018 0.314304 0.535265 11.00000 0.02105 0.01674 =
0.02061 -0.00391 0.00253 0.00985
C12 1 0.250242 0.803383 0.450915 11.00000 0.02893 0.02548 =
0.05629 0.01958 0.02003 0.01865
AFIX 43
H12 2 0.241340 0.861451 0.463902 11.00000 -1.20000
AFIX 0
C28 1 0.673344 0.197635 0.369640 11.00000 0.04212 0.02347 =
0.02295 -0.00679 -0.00766 0.02017
AFIX 43
H28 2 0.711027 0.204031 0.331912 11.00000 -1.20000
AFIX 0
C32 1 1.044608 0.547007 0.515666 11.00000 0.01970 0.01629 =
0.04568 0.01029 0.00601 0.00675
AFIX 43
H32 2 1.010939 0.510616 0.478014 11.00000 -1.20000
AFIX 0
C13 1 0.196423 0.745059 0.398739 11.00000 0.02945 0.03986 =
0.03385 0.01406 0.00635 0.02454
AFIX 43
H13 2 0.152165 0.764278 0.375737 11.00000 -1.20000
AFIX 0
C2 1 0.667275 1.047211 0.584157 11.00000 0.02582 0.01928 =
0.02096 -0.00633 -0.00994 0.01463
C5 1 0.838213 1.240675 0.546498 11.00000 0.02538 0.02173 =
0.04985 0.00203 -0.01214 0.01099
AFIX 43
H5 2 0.897367 1.307118 0.533784 11.00000 -1.20000
AFIX 0
C6 1 0.785195 1.236814 0.601528 11.00000 0.03862 0.02229 =
0.03370 -0.00698 -0.01719 0.01737
AFIX 43
H6 2 0.807110 1.299728 0.625683 11.00000 -1.20000
AFIX 0
C16 1 0.303979 0.266990 0.592079 11.00000 0.01843 0.01305 =
0.02517 -0.00416 0.00521 0.00258
C19 1 0.112473 0.247285 0.552943 11.00000 0.01730 0.01784 =
0.04516 -0.00610 0.00257 0.00683
AFIX 43
H19 2 0.045984 0.238696 0.539194 11.00000 -1.20000
AFIX 0
C14 1 0.206231 0.658792 0.379539 11.00000 0.02739 0.03809 =
0.02683 0.01260 0.00898 0.02062
AFIX 43
H14 2 0.167280 0.617342 0.344319 11.00000 -1.20000
AFIX 0
C30 1 1.082187 0.685319 0.593407 11.00000 0.01813 0.03054 =
0.02383 0.01205 0.00645 0.01380
C21 1 0.211185 0.212037 0.629521 11.00000 0.02906 0.02359 =
0.02244 -0.00343 0.00646 0.00615
AFIX 43
H21 2 0.213852 0.180624 0.668101 11.00000 -1.20000
AFIX 0
C40 1 1.261202 1.073804 0.472844 11.00000 0.01980 0.02231 =
0.03174 -0.00750 0.00068 0.01035
AFIX 43
H40 2 1.325290 1.081065 0.489977 11.00000 -1.20000
AFIX 0
C8 1 0.329766 0.693160 0.465800 11.00000 0.01335 0.01491 =
0.02927 0.00744 0.00351 0.00599
C31 1 1.066704 0.771696 0.614026 11.00000 0.02532 0.03313 =
0.01591 0.00287 0.00157 0.01743
AFIX 43
H31 2 1.097949 0.810342 0.651497 11.00000 -1.20000
AFIX 0
C20 1 0.116493 0.204448 0.609452 11.00000 0.01909 0.02366 =
0.03846 -0.00744 0.00930 0.00200
AFIX 43
H20 2 0.054210 0.169517 0.634858 11.00000 -1.20000
AFIX 0
C7 1 0.700693 1.140801 0.620504 11.00000 0.04404 0.02342 =
0.02526 -0.00992 -0.01357 0.02030
AFIX 43
H7 2 0.664266 1.137017 0.658332 11.00000 -1.20000
AFIX 0
C34 1 1.157519 0.570408 0.604817 11.00000 0.03151 0.04639 =
0.03761 0.02237 0.01104 0.02573
AFIX 43
H34 2 1.199973 0.548567 0.627542 11.00000 -1.20000
AFIX 0
C3 1 0.577966 0.945102 0.601799 11.00000 0.02591 0.02239 =
0.01927 -0.00333 -0.00394 0.01258
AFIX 43
H3 2 0.539156 0.936063 0.639424 11.00000 -1.20000
AFIX 0
C35 1 1.146538 0.652874 0.627046 11.00000 0.02553 0.05128 =
0.02683 0.01485 0.00546 0.02534
AFIX 43
H35 2 1.181454 0.688458 0.664636 11.00000 -1.20000
AFIX 0
C17 1 0.403972 0.274426 0.609354 11.00000 0.02309 0.01728 =
0.01740 0.00187 0.00302 0.00610
AFIX 43
H17 2 0.412123 0.244881 0.647322 11.00000 -1.20000
AFIX 0
C36 1 1.072564 1.009310 0.481107 11.00000 0.01688 0.01359 =
0.02328 -0.00194 0.00401 0.00402
C25 1 0.563946 0.179453 0.481748 11.00000 0.01869 0.02220 =
0.03261 -0.00176 -0.00341 0.01151
AFIX 43
H25 2 0.526480 0.172702 0.519619 11.00000 -1.20000
AFIX 0
C11 1 0.317977 0.778551 0.485223 11.00000 0.01998 0.01948 =
0.03669 0.00610 0.00915 0.01114
AFIX 43
H11 2 0.355044 0.819378 0.521043 11.00000 -1.20000
AFIX 0
PART 1
C43 1 0.720035 0.719306 0.646978 11.00000 0.05564 0.04694 =
0.07751 -0.01153 0.03033 -0.00948
AFIX 23
H43A 2 0.721170 0.785145 0.632658 11.00000 -1.20000
H43B 2 0.794107 0.732188 0.644631 11.00000 -1.20000
AFIX 0
C44 1 0.630791 0.601855 0.358201 21.00000 0.03388
AFIX 23
H44A 2 0.559443 0.578206 0.376681 21.00000 -1.20000
H44B 2 0.643454 0.540446 0.358994 21.00000 -1.20000
AFIX 0
PART 0
C37 1 1.074045 1.053761 0.422455 11.00000 0.01976 0.01924 =
0.01930 -0.00613 0.00102 0.00850
C38 1 0.976016 1.044935 0.399911 11.00000 0.02587 0.01595 =
0.01574 -0.00129 0.00023 0.00700
AFIX 43
H38 2 0.972160 1.072129 0.360059 11.00000 -1.20000
AFIX 0
C33 1 1.108955 0.518246 0.550593 11.00000 0.02515 0.02665 =
0.05671 0.01502 0.01172 0.01911
AFIX 43
H33 2 1.118907 0.461472 0.536258 11.00000 -1.20000
AFIX 0
C23 1 0.704800 0.287571 0.408411 11.00000 0.02705 0.02272 =
0.01812 -0.00407 -0.00537 0.01578
C26 1 0.532935 0.089970 0.443214 11.00000 0.02626 0.01445 =
0.05270 -0.00478 -0.01708 0.00961
AFIX 43
H26 2 0.474934 0.022319 0.455313 11.00000 -1.20000
AFIX 0
C10 1 0.286863 0.542988 0.395523 11.00000 0.01803 0.02500 =
0.01910 0.00296 0.00150 0.01100
AFIX 43
H10 2 0.250947 0.499339 0.360347 11.00000 -1.20000
AFIX 0
C27 1 0.587170 0.099905 0.386893 11.00000 0.03507 0.02468 =
0.03074 -0.01296 -0.01236 0.01646
AFIX 43
H27 2 0.564694 0.039357 0.360487 11.00000 -1.20000
AFIX 0
C24 1 0.795490 0.391596 0.393115 11.00000 0.02950 0.02608 =
0.01702 0.00067 -0.00057 0.01783
AFIX 43
H24 2 0.836421 0.403016 0.356110 11.00000 -1.20000
AFIX 0
C22 1 0.649736 0.278134 0.464348 11.00000 0.01928 0.01765 =
0.02775 -0.00552 -0.00590 0.01222
C39 1 1.165816 1.019876 0.506875 11.00000 0.01573 0.01806 =
0.02740 -0.00332 0.00218 0.00660
AFIX 43
H39 2 1.164799 0.990908 0.547003 11.00000 -1.20000
AFIX 0
PART 1
CL3 3 0.729044 0.706907 0.402856 21.00000 0.04402 0.06864 =
0.04004 -0.01863 -0.01569 0.03739
CL4 3 0.632864 0.642629 0.279749 21.00000 0.02921 0.04914 =
0.02115 0.00343 0.00003 0.00948
CL2 3 0.639477 0.615198 0.597356 11.00000 0.06373 0.04195 =
0.03573 -0.00841 -0.01008 0.03081
CL1 3 0.676365 0.693864 0.725777 11.00000 0.04743 0.06110 =
0.03177 -0.01184 -0.00625 0.03382
H18 2 0.196981 0.327538 0.478074 11.00000 0.01653
PART 0
PART 2
AFIX 6
O44A 5 0.682341 0.615410 0.408394 -21.00000 0.03388
H44C 2 0.628282 0.550824 0.412359 -21.00000 -1.50000
H44D 2 0.736464 0.612624 0.392531 -21.00000 -1.50000
AFIX 0
HKLF 4
REM ph4622_p32_a.res in P3(1)
REM R1 = 0.0330 for 17518 Fo > 4sig(Fo) and 0.0434 for all 20091 data
REM 602 parameters refined using 1 restraints
END
WGHT 0.0263 4.2720
REM Highest difference peak 1.669, deepest hole -0.673, 1-sigma level 0.149
Q1 1 0.3978 0.3898 0.4739 11.00000 0.05 1.67
Q2 1 0.6588 0.4082 0.5354 11.00000 0.05 1.64
Q3 1 0.6952 0.4615 0.5309 11.00000 0.05 1.61
Q4 1 0.9033 0.6803 0.4679 11.00000 0.05 1.48
Q5 1 0.8799 0.6577 0.4981 11.00000 0.05 1.42
Q6 1 0.6374 0.9352 0.4955 11.00000 0.05 1.40
Q7 1 0.4395 0.4277 0.5094 11.00000 0.05 1.34
Q8 1 0.8608 0.8915 0.5277 11.00000 0.05 1.32
Q9 1 0.6302 0.8803 0.5057 11.00000 0.05 1.31
Q10 1 0.8964 0.9319 0.4979 11.00000 0.05 1.28
Q11 1 0.9201 0.6370 0.4718 11.00000 0.05 1.21
Q12 1 0.9698 0.9822 0.5119 11.00000 0.05 1.16
Q13 1 0.6632 0.4170 0.4955 11.00000 0.05 1.16
Q14 1 0.3838 0.6245 0.5394 11.00000 0.05 1.15
Q15 1 0.7208 0.6694 0.5971 11.00000 0.05 1.14
Q16 1 0.9041 0.9652 0.5310 11.00000 0.05 1.13
Q17 1 0.4285 0.6767 0.5294 11.00000 0.05 1.09
Q18 1 0.3702 0.6268 0.5041 11.00000 0.05 1.07
Q19 1 0.6339 0.9093 0.4630 11.00000 0.05 1.04
Q20 1 0.9296 0.7298 0.4999 11.00000 0.05 1.04
Q21 1 0.6621 0.8466 0.4809 11.00000 0.05 1.02
Q22 1 0.4032 0.3858 0.5116 11.00000 0.05 0.97
Q23 1 0.5098 0.4514 0.4826 11.00000 0.05 0.96
Q24 1 0.6516 0.6993 0.3665 11.00000 0.05 0.93
Q25 1 0.9952 0.7413 0.4833 11.00000 0.05 0.91
Q26 1 0.6074 0.6740 0.2904 11.00000 0.05 0.89
Q27 1 0.9208 0.8805 0.5172 11.00000 0.05 0.88
Q28 1 0.3969 0.3355 0.4954 11.00000 0.05 0.87
Q29 1 0.6203 0.5995 0.2866 11.00000 0.05 0.83
Q30 1 0.6799 0.7084 0.5966 11.00000 0.05 0.83
;
_shelx_res_checksum 87338
_shelx_SHELXL_version_number 2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.49(2)
2 0.51(2)