#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/24/4342437.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4342437
loop_
_publ_author_name
'Nordheider, Andreas'
'Hupf, Emanuel'
'Chalmers, Brian A.'
'Knight, Fergus R.'
'Bühl, Michael'
'Mebs, Stefan'
'Chęcińska, Lilianna'
'Lork, Enno'
'Camacho, Paula Sanz'
'Ashbrook, Sharon E.'
'Athukorala Arachchige, Kasun S.'
'Cordes, David B.'
'Slawin, Alexandra M. Z.'
'Beckmann, Jens'
'Woollins, J. Derek'
_publ_section_title
;
 Peri-Substituted Phosphorus-Tellurium Systems-An Experimental and
 Theoretical Investigation of the P···Te
 through-Space Interaction.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2435
_journal_paper_doi               10.1021/ic503056z
_journal_volume                  54
_journal_year                    2015
_chemical_formula_sum            'C33.5 H30 Cl P S Te'
_chemical_formula_weight         658.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.64(2)
_cell_angle_beta                 85.15(2)
_cell_angle_gamma                71.93(2)
_cell_formula_units_Z            2
_cell_length_a                   8.514(2)
_cell_length_b                   12.441(4)
_cell_length_c                   15.166(5)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.956
_cell_measurement_theta_min      6.976
_cell_volume                     1472.6(8)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGX
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0440
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6688
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.52
_diffrn_standards_interval_count 3
_diffrn_standards_interval_time  197
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7490
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             662
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0561P)²+1.7264P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1048
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                5930
_reflns_number_total             6688
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic503056z_si_001.cif
_cod_data_source_block           6b
_cod_depositor_comments
'Adding full bibliography for 4342430--4342441.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C33.50 H30 Cl P S Te'
_cod_database_code               4342437
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.8140(4) 0.3641(3) 1.0973(2) 0.0335(7) Uani 1 1 d . . .
H1A H 0.9047 0.3440 1.1391 0.040 Uiso 1 1 calc R . .
H1B H 0.7805 0.2950 1.1019 0.040 Uiso 1 1 calc R . .
C2 C 0.6672(4) 0.4641(3) 1.1188(2) 0.0335(7) Uani 1 1 d . . .
H2A H 0.5694 0.4387 1.1351 0.040 Uiso 1 1 calc R . .
H2B H 0.6941 0.4905 1.1687 0.040 Uiso 1 1 calc R . .
C3 C 1.043(4) 0.904(2) 1.0842(14) 0.237(18) Uani 0.50 1 d P . .
H3A H 1.1317 0.8936 1.1247 0.284 Uiso 0.50 1 calc PR A 1
H3B H 0.9803 0.8491 1.1063 0.284 Uiso 0.50 1 calc PR A 1
C10 C 0.8908(4) 0.5389(3) 0.8168(2) 0.0277(6) Uani 1 1 d . . .
C11 C 0.9965(4) 0.4293(3) 0.8543(2) 0.0333(7) Uani 1 1 d . . .
H11 H 1.0796 0.3960 0.8171 0.040 Uiso 1 1 calc R . .
C12 C 0.9875(4) 0.3643(3) 0.9453(2) 0.0346(7) Uani 1 1 d . . .
H12 H 1.0630 0.2911 0.9673 0.042 Uiso 1 1 calc R . .
C13 C 0.8638(4) 0.4122(3) 1.0003(2) 0.0294(6) Uani 1 1 d . . .
C14 C 0.7587(4) 0.5261(3) 0.9647(2) 0.0249(6) Uani 1 1 d . . .
C15 C 0.6403(4) 0.5600(3) 1.0312(2) 0.0287(6) Uani 1 1 d . . .
C16 C 0.5241(4) 0.6665(3) 1.0099(2) 0.0329(7) Uani 1 1 d . . .
H16 H 0.4406 0.6891 1.0509 0.040 Uiso 1 1 calc R . .
C17 C 0.5355(4) 0.7413(3) 0.9231(2) 0.0327(7) Uani 1 1 d . . .
H17 H 0.4597 0.8156 0.9095 0.039 Uiso 1 1 calc R . .
C18 C 0.6510(4) 0.7123(3) 0.8567(2) 0.0269(6) Uani 1 1 d . . .
C19 C 0.7671(4) 0.5961(3) 0.8749(2) 0.0248(6) Uani 1 1 d . . .
C20 C 0.5445(5) 0.9637(3) 0.7914(3) 0.0416(8) Uani 1 1 d . . .
C21 C 0.6267(7) 0.9970(5) 0.8497(5) 0.088(2) Uani 1 1 d . . .
H21 H 0.7345 0.9533 0.8676 0.105 Uiso 1 1 calc R . .
C22 C 0.5482(8) 1.0961(5) 0.8817(6) 0.104(3) Uani 1 1 d . . .
H22 H 0.5997 1.1136 0.9255 0.125 Uiso 1 1 calc R . .
C23 C 0.3984(7) 1.1665(4) 0.8497(4) 0.0682(14) Uani 1 1 d . . .
H23 H 0.3504 1.2353 0.8680 0.082 Uiso 1 1 calc R . .
C24 C 0.3184(7) 1.1374(4) 0.7913(3) 0.0697(16) Uani 1 1 d . . .
H24 H 0.2143 1.1854 0.7701 0.084 Uiso 1 1 calc R . .
C25 C 0.3916(6) 1.0342(4) 0.7621(3) 0.0582(12) Uani 1 1 d . . .
H25 H 0.3344 1.0142 0.7224 0.070 Uiso 1 1 calc R . .
C30 C 0.5215(4) 0.8206(3) 0.6717(2) 0.0315(6) Uani 1 1 d . . .
C31 C 0.5491(5) 0.8606(3) 0.5790(2) 0.0399(8) Uani 1 1 d . . .
H31 H 0.6304 0.8974 0.5598 0.048 Uiso 1 1 calc R . .
C32 C 0.4556(5) 0.8460(4) 0.5150(3) 0.0499(10) Uani 1 1 d . . .
H32 H 0.4735 0.8736 0.4529 0.060 Uiso 1 1 calc R . .
C33 C 0.3357(5) 0.7902(4) 0.5435(3) 0.0534(11) Uani 1 1 d . . .
H33 H 0.2763 0.7773 0.5006 0.064 Uiso 1 1 calc R . .
C34 C 0.3046(6) 0.7540(4) 0.6354(3) 0.0551(11) Uani 1 1 d . . .
H34 H 0.2215 0.7189 0.6545 0.066 Uiso 1 1 calc R . .
C35 C 0.3966(5) 0.7696(4) 0.6995(3) 0.0430(8) Uani 1 1 d . . .
H35 H 0.3743 0.7458 0.7615 0.052 Uiso 1 1 calc R . .
C40 C 0.9570(4) 0.4256(3) 0.6490(2) 0.0306(6) Uani 1 1 d . . .
C41 C 0.8408(4) 0.3645(3) 0.6734(2) 0.0360(7) Uani 1 1 d . . .
C42 C 0.8728(5) 0.2572(3) 0.6524(3) 0.0411(8) Uani 1 1 d . . .
H42 H 0.7978 0.2148 0.6710 0.049 Uiso 1 1 calc R . .
C43 C 1.0131(5) 0.2116(3) 0.6046(3) 0.0406(8) Uani 1 1 d . . .
C44 C 1.1252(4) 0.2756(3) 0.5788(2) 0.0395(8) Uani 1 1 d . . .
H44 H 1.2187 0.2470 0.5457 0.047 Uiso 1 1 calc R . .
C45 C 1.1016(4) 0.3811(3) 0.6012(2) 0.0351(7) Uani 1 1 d . . .
C46 C 0.6804(5) 0.4112(4) 0.7220(3) 0.0507(10) Uani 1 1 d . . .
H46A H 0.7034 0.4054 0.7842 0.076 Uiso 1 1 calc R . .
H46B H 0.6075 0.3661 0.7209 0.076 Uiso 1 1 calc R . .
H46C H 0.6289 0.4915 0.6915 0.076 Uiso 1 1 calc R . .
C47 C 1.0471(6) 0.0962(4) 0.5804(3) 0.0546(11) Uani 1 1 d . . .
H47A H 1.0324 0.1099 0.5159 0.082 Uiso 1 1 calc R . .
H47B H 0.9720 0.0558 0.6133 0.082 Uiso 1 1 calc R . .
H47C H 1.1586 0.0494 0.5967 0.082 Uiso 1 1 calc R . .
C48 C 1.2344(5) 0.4410(4) 0.5743(3) 0.0473(9) Uani 1 1 d . . .
H48A H 1.3210 0.3960 0.5422 0.071 Uiso 1 1 calc R . .
H48B H 1.2786 0.4473 0.6282 0.071 Uiso 1 1 calc R . .
H48C H 1.1878 0.5176 0.5354 0.071 Uiso 1 1 calc R . .
P1 P 0.65136(11) 0.83120(7) 0.75602(6) 0.03043(18) Uani 1 1 d . . .
S1 S 0.86982(13) 0.84183(9) 0.71273(7) 0.0457(2) Uani 1 1 d . . .
Te1 Te 0.91403(3) 0.596057(18) 0.671724(14) 0.03139(8) Uani 1 1 d . . .
Cl1 Cl 0.9155(7) 1.0657(6) 1.0280(4) 0.1327(19) Uani 0.50 1 d P . 1
Cl1' Cl 0.9332(7) 1.0521(6) 1.1092(8) 0.195(4) Uani 0.50 1 d P . -1
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C13 C1 C2 104.8(3) . .
C15 C2 C1 104.5(3) . .
Cl1 C3 Cl1' 105.3(14) 2_777 .
Cl1 C3 Cl1 71.3(11) 2_777 .
Cl1' C3 Cl1 36.6(6) . .
C11 C10 C19 118.9(3) . .
C11 C10 Te1 113.7(2) . .
C19 C10 Te1 127.1(2) . .
C10 C11 C12 124.6(3) . .
C13 C12 C11 118.0(3) . .
C12 C13 C14 118.4(3) . .
C12 C13 C1 131.3(3) . .
C14 C13 C1 110.2(3) . .
C13 C14 C15 110.0(3) . .
C13 C14 C19 125.4(3) . .
C15 C14 C19 124.6(3) . .
C16 C15 C14 119.5(3) . .
C16 C15 C2 130.1(3) . .
C14 C15 C2 110.4(3) . .
C15 C16 C17 117.4(3) . .
C18 C17 C16 124.8(3) . .
C17 C18 C19 118.8(3) . .
C17 C18 P1 115.4(2) . .
C19 C18 P1 125.7(2) . .
C14 C19 C18 114.7(3) . .
C14 C19 C10 114.4(3) . .
C18 C19 C10 130.9(3) . .
C25 C20 C21 118.0(4) . .
C25 C20 P1 124.2(3) . .
C21 C20 P1 117.7(3) . .
C20 C21 C22 120.2(5) . .
C23 C22 C21 120.5(5) . .
C24 C23 C22 120.0(4) . .
C23 C24 C25 120.3(4) . .
C20 C25 C24 120.7(4) . .
C35 C30 C31 119.5(3) . .
C35 C30 P1 120.0(3) . .
C31 C30 P1 120.5(3) . .
C30 C31 C32 120.1(4) . .
C33 C32 C31 120.0(4) . .
C34 C33 C32 119.8(4) . .
C33 C34 C35 120.3(4) . .
C30 C35 C34 120.2(4) . .
C41 C40 C45 120.4(3) . .
C41 C40 Te1 121.9(2) . .
C45 C40 Te1 117.5(2) . .
C42 C41 C40 118.9(3) . .
C42 C41 C46 118.9(3) . .
C40 C41 C46 122.2(3) . .
C43 C42 C41 122.0(4) . .
C42 C43 C44 118.0(3) . .
C42 C43 C47 122.2(4) . .
C44 C43 C47 119.8(4) . .
C45 C44 C43 122.1(3) . .
C44 C45 C40 118.6(3) . .
C44 C45 C48 118.1(3) . .
C40 C45 C48 123.4(3) . .
C20 P1 C30 106.86(16) . .
C20 P1 C18 105.13(16) . .
C30 P1 C18 106.54(15) . .
C20 P1 S1 107.17(15) . .
C30 P1 S1 115.36(12) . .
C18 P1 S1 115.04(11) . .
C10 Te1 C40 94.59(12) . .
Cl1' Cl1 C3 158.7(12) . 2_777
Cl1' Cl1 C3 69.5(7) . .
C3 Cl1 C3 108.7(11) 2_777 .
Cl1' Cl1 Cl1 114.2(7) . 2_777
C3 Cl1 Cl1 60.6(11) 2_777 2_777
C3 Cl1 Cl1 48.1(6) . 2_777
Cl1 Cl1' C3 73.9(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C13 1.513(5) .
C1 C2 1.548(5) .
C2 C15 1.511(4) .
C3 Cl1 1.674(19) 2_777
C3 Cl1' 1.91(2) .
C3 Cl1 1.96(3) .
C10 C11 1.381(5) .
C10 C19 1.450(4) .
C10 Te1 2.137(3) .
C11 C12 1.412(5) .
C12 C13 1.373(5) .
C13 C14 1.410(4) .
C14 C15 1.414(4) .
C14 C19 1.419(4) .
C15 C16 1.362(5) .
C16 C17 1.412(5) .
C17 C18 1.385(5) .
C18 C19 1.446(4) .
C18 P1 1.824(3) .
C20 C25 1.358(6) .
C20 C21 1.386(6) .
C20 P1 1.814(4) .
C21 C22 1.398(7) .
C22 C23 1.348(7) .
C23 C24 1.343(7) .
C24 C25 1.411(6) .
C30 C35 1.382(5) .
C30 C31 1.387(5) .
C30 P1 1.815(3) .
C31 C32 1.387(5) .
C32 C33 1.385(7) .
C33 C34 1.376(7) .
C34 C35 1.387(5) .
C40 C41 1.396(5) .
C40 C45 1.410(5) .
C40 Te1 2.153(3) .
C41 C42 1.394(5) .
C41 C46 1.520(5) .
C42 C43 1.388(6) .
C43 C44 1.393(6) .
C43 C47 1.511(5) .
C44 C45 1.392(5) .
C45 C48 1.511(5) .
P1 S1 1.9514(15) .
Cl1 Cl1' 1.215(11) .
Cl1 C3 1.674(19) 2_777
Cl1 Cl1 2.129(13) 2_777
