#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:32:08 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179065 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/27/4302730.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_4302730
loop_
_publ_author_name
'Stuart D. Robertson'
'Tristram Chivers'
'Heikki M. Tuononen'
_publ_contact_author_address
;
Department of Chemistry
University of Calgary, Calgary, Alberta 
T2N 1N4, Canada
;
_publ_contact_author_name        'Prof. T. Chivers'
_publ_section_title
;
Experimental and Theoretical Investigations of the Contact Ion Pairs Formed
by Reactions of the Anions [(EPR2)2N]- (R =iPr,tBu; E = S, Se) with the
Cations [(TePR2)2N]+ (R =iPr,tBu)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6755
_journal_page_last               6762
_journal_paper_doi               10.1021/ic900703e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C24 H56 N2 P4 Se2 Te2'
_chemical_formula_sum            'C24 H56 N2 P4 Se2 Te2'
_chemical_formula_weight         909.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.08(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.642(2)
_cell_length_b                   22.718(5)
_cell_length_c                   15.812(3)
_cell_measurement_reflns_used    51163
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3634.0(14)
_computing_cell_refinement       'Nonius DENZO'
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'Nonius DENZO'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phiω 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  0.1125
_diffrn_reflns_av_sigmaI/netI    0.0731
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            45208
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    3.801
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.635
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6400
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0902
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0398P)²+5.0459P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                4317
_reflns_number_total             6400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900703e_si_001_3.cif
_cod_data_source_block           sdr7b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4302730
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 0.50433(4) 0.097712(18) 0.22067(3) 0.02802(13) Uani 1 1 d . . .
Te2 Te 0.69236(4) 0.08809(2) 0.11731(3) 0.03749(15) Uani 1 1 d . . .
P1 P 0.55854(15) -0.00925(7) 0.25206(11) 0.0242(4) Uani 1 1 d . . .
P2 P 0.80514(15) 0.00895(7) 0.21634(11) 0.0253(4) Uani 1 1 d . . .
N1 N 0.7085(4) -0.0238(2) 0.2615(3) 0.0250(12) Uani 1 1 d . . .
C10 C 0.5316(6) -0.0276(3) 0.3580(4) 0.0251(14) Uani 1 1 d . . .
H10A H 0.4389 -0.0166 0.3538 0.030 Uiso 1 1 calc R . .
C11 C 0.5505(7) -0.0934(3) 0.3801(5) 0.0450(19) Uani 1 1 d . . .
H11A H 0.5472 -0.1001 0.4407 0.068 Uiso 1 1 calc R . .
H11B H 0.6363 -0.1062 0.3761 0.068 Uiso 1 1 calc R . .
H11C H 0.4799 -0.1158 0.3378 0.068 Uiso 1 1 calc R . .
C12 C 0.6258(6) 0.0084(3) 0.4329(4) 0.0394(17) Uani 1 1 d . . .
H12A H 0.6107 -0.0012 0.4894 0.059 Uiso 1 1 calc R . .
H12B H 0.6098 0.0504 0.4203 0.059 Uiso 1 1 calc R . .
H12C H 0.7174 -0.0011 0.4369 0.059 Uiso 1 1 calc R . .
C20 C 0.4462(6) -0.0497(3) 0.1580(4) 0.0303(15) Uani 1 1 d . . .
H20A H 0.4644 -0.0350 0.1033 0.036 Uiso 1 1 calc R . .
C21 C 0.4715(7) -0.1167(3) 0.1613(5) 0.0410(18) Uani 1 1 d . . .
H21A H 0.4397 -0.1329 0.1010 0.062 Uiso 1 1 calc R . .
H21B H 0.4244 -0.1354 0.1985 0.062 Uiso 1 1 calc R . .
H21C H 0.5665 -0.1242 0.1867 0.062 Uiso 1 1 calc R . .
C22 C 0.3008(6) -0.0365(3) 0.1453(5) 0.0391(18) Uani 1 1 d . . .
H22A H 0.2455 -0.0578 0.0931 0.059 Uiso 1 1 calc R . .
H22B H 0.2850 0.0059 0.1364 0.059 Uiso 1 1 calc R . .
H22C H 0.2787 -0.0491 0.1982 0.059 Uiso 1 1 calc R . .
C30 C 0.8661(6) -0.0422(3) 0.1504(4) 0.0284(15) Uani 1 1 d . . .
H30A H 0.9130 -0.0743 0.1914 0.034 Uiso 1 1 calc R . .
C31 C 0.7552(6) -0.0714(3) 0.0767(5) 0.0441(19) Uani 1 1 d . . .
H31A H 0.7929 -0.1007 0.0461 0.066 Uiso 1 1 calc R . .
H31B H 0.7079 -0.0414 0.0341 0.066 Uiso 1 1 calc R . .
H31C H 0.6936 -0.0907 0.1028 0.066 Uiso 1 1 calc R . .
C32 C 0.9664(6) -0.0147(3) 0.1115(5) 0.0411(18) Uani 1 1 d . . .
H32A H 0.9973 -0.0445 0.0777 0.062 Uiso 1 1 calc R . .
H32B H 1.0416 0.0003 0.1598 0.062 Uiso 1 1 calc R . .
H32C H 0.9249 0.0178 0.0719 0.062 Uiso 1 1 calc R . .
C40 C 0.9494(6) 0.0372(3) 0.3042(5) 0.0345(17) Uani 1 1 d . . .
H40A H 1.0119 0.0545 0.2749 0.041 Uiso 1 1 calc R . .
C41 C 0.9071(7) 0.0864(3) 0.3557(5) 0.0446(19) Uani 1 1 d . . .
H41A H 0.9850 0.1022 0.4009 0.067 Uiso 1 1 calc R . .
H41B H 0.8452 0.0705 0.3847 0.067 Uiso 1 1 calc R . .
H41C H 0.8638 0.1178 0.3145 0.067 Uiso 1 1 calc R . .
C42 C 1.0206(7) -0.0118(3) 0.3648(5) 0.049(2) Uani 1 1 d . . .
H42A H 1.0994 0.0040 0.4092 0.074 Uiso 1 1 calc R . .
H42B H 1.0470 -0.0421 0.3295 0.074 Uiso 1 1 calc R . .
H42C H 0.9616 -0.0292 0.3948 0.074 Uiso 1 1 calc R . .
Se1 Se 0.32358(6) 0.09669(3) 0.32244(5) 0.0379(2) Uani 1 1 d . . .
Se2 Se 0.35084(7) 0.35199(3) 0.24684(5) 0.0408(2) Uani 1 1 d . . .
P3 P 0.26314(15) 0.18704(7) 0.27587(12) 0.0262(4) Uani 1 1 d . . .
P4 P 0.38620(15) 0.27398(7) 0.18315(11) 0.0259(4) Uani 1 1 d . . .
C50 C 0.2694(6) 0.2315(3) 0.3740(4) 0.0329(16) Uani 1 1 d . . .
H50A H 0.2385 0.2720 0.3527 0.039 Uiso 1 1 calc R . .
C51 C 0.4132(7) 0.2367(4) 0.4348(5) 0.053(2) Uani 1 1 d . . .
H51A H 0.4161 0.2608 0.4868 0.079 Uiso 1 1 calc R . .
H51B H 0.4671 0.2551 0.4020 0.079 Uiso 1 1 calc R . .
H51C H 0.4479 0.1973 0.4545 0.079 Uiso 1 1 calc R . .
C52 C 0.1782(7) 0.2080(3) 0.4247(5) 0.047(2) Uani 1 1 d . . .
H52A H 0.1767 0.2358 0.4717 0.070 Uiso 1 1 calc R . .
H52B H 0.2111 0.1698 0.4512 0.070 Uiso 1 1 calc R . .
H52C H 0.0886 0.2033 0.3834 0.070 Uiso 1 1 calc R . .
C60 C 0.0892(6) 0.1805(3) 0.2090(4) 0.0288(15) Uani 1 1 d . . .
H60A H 0.0446 0.1558 0.2436 0.035 Uiso 1 1 calc R . .
C61 C 0.0770(6) 0.1481(3) 0.1227(5) 0.0383(17) Uani 1 1 d . . .
H61A H -0.0165 0.1404 0.0911 0.057 Uiso 1 1 calc R . .
H61B H 0.1248 0.1106 0.1360 0.057 Uiso 1 1 calc R . .
H61C H 0.1148 0.1722 0.0853 0.057 Uiso 1 1 calc R . .
C62 C 0.0171(6) 0.2403(3) 0.1919(5) 0.0402(18) Uani 1 1 d . . .
H62A H -0.0750 0.2343 0.1554 0.060 Uiso 1 1 calc R . .
H62B H 0.0610 0.2665 0.1607 0.060 Uiso 1 1 calc R . .
H62C H 0.0193 0.2581 0.2489 0.060 Uiso 1 1 calc R . .
C70 C 0.5605(6) 0.2674(3) 0.1882(5) 0.0330(16) Uani 1 1 d . . .
H70A H 0.5693 0.2309 0.1551 0.040 Uiso 1 1 calc R . .
C71 C 0.6466(6) 0.2599(3) 0.2832(5) 0.0453(19) Uani 1 1 d . . .
H71A H 0.7380 0.2526 0.2846 0.068 Uiso 1 1 calc R . .
H71B H 0.6146 0.2266 0.3101 0.068 Uiso 1 1 calc R . .
H71C H 0.6432 0.2959 0.3168 0.068 Uiso 1 1 calc R . .
C72 C 0.6097(7) 0.3189(3) 0.1449(5) 0.046(2) Uani 1 1 d . . .
H72A H 0.7046 0.3144 0.1541 0.069 Uiso 1 1 calc R . .
H72B H 0.5939 0.3559 0.1719 0.069 Uiso 1 1 calc R . .
H72C H 0.5621 0.3195 0.0810 0.069 Uiso 1 1 calc R . .
C80 C 0.2886(7) 0.2740(3) 0.0647(5) 0.0413(18) Uani 1 1 d . . .
H80A H 0.1968 0.2629 0.0627 0.050 Uiso 1 1 calc R . .
C81 C 0.2756(8) 0.3335(3) 0.0169(5) 0.058(2) Uani 1 1 d . . .
H81A H 0.2090 0.3305 -0.0418 0.087 Uiso 1 1 calc R . .
H81B H 0.3609 0.3444 0.0098 0.087 Uiso 1 1 calc R . .
H81C H 0.2487 0.3637 0.0521 0.087 Uiso 1 1 calc R . .
C82 C 0.3356(8) 0.2246(4) 0.0152(5) 0.059(2) Uani 1 1 d . . .
H82A H 0.2716 0.2195 -0.0441 0.089 Uiso 1 1 calc R . .
H82B H 0.3434 0.1878 0.0488 0.089 Uiso 1 1 calc R . .
H82C H 0.4219 0.2351 0.0094 0.089 Uiso 1 1 calc R . .
N2 N 0.3538(5) 0.2120(2) 0.2211(3) 0.0276(12) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
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
P1 Te1 Se1 91.97(4) . . ?
P1 Te1 Te2 83.36(4) . . ?
Se1 Te1 Te2 175.28(2) . . ?
P2 Te2 Te1 88.98(4) . . ?
N1 P1 C10 107.7(3) . . ?
N1 P1 C20 110.7(3) . . ?
C10 P1 C20 112.3(3) . . ?
N1 P1 Te1 112.48(19) . . ?
C10 P1 Te1 108.0(2) . . ?
C20 P1 Te1 105.7(2) . . ?
N1 P2 C30 110.6(3) . . ?
N1 P2 C40 109.1(3) . . ?
C30 P2 C40 107.2(3) . . ?
N1 P2 Te2 111.81(18) . . ?
C30 P2 Te2 107.2(2) . . ?
C40 P2 Te2 110.9(2) . . ?
P1 N1 P2 128.6(3) . . ?
C12 C10 C11 109.6(5) . . ?
C12 C10 P1 109.6(4) . . ?
C11 C10 P1 112.5(4) . . ?
C22 C20 C21 110.9(5) . . ?
C22 C20 P1 112.7(5) . . ?
C21 C20 P1 113.7(4) . . ?
C32 C30 C31 110.1(6) . . ?
C32 C30 P2 113.0(4) . . ?
C31 C30 P2 112.8(4) . . ?
C42 C40 C41 111.9(6) . . ?
C42 C40 P2 111.0(5) . . ?
C41 C40 P2 110.0(4) . . ?
P3 Se1 Te1 88.97(5) . . ?
N2 P3 C60 113.0(3) . . ?
N2 P3 C50 113.3(3) . . ?
C60 P3 C50 107.3(3) . . ?
N2 P3 Se1 110.55(19) . . ?
C60 P3 Se1 104.8(2) . . ?
C50 P3 Se1 107.4(2) . . ?
N2 P4 C70 104.1(3) . . ?
N2 P4 C80 105.2(3) . . ?
C70 P4 C80 106.7(3) . . ?
N2 P4 Se2 117.5(2) . . ?
C70 P4 Se2 111.8(2) . . ?
C80 P4 Se2 110.8(2) . . ?
C52 C50 C51 111.6(6) . . ?
C52 C50 P3 112.7(5) . . ?
C51 C50 P3 109.8(5) . . ?
C61 C60 C62 111.7(6) . . ?
C61 C60 P3 110.3(4) . . ?
C62 C60 P3 112.9(4) . . ?
C71 C70 C72 110.2(6) . . ?
C71 C70 P4 110.2(5) . . ?
C72 C70 P4 113.6(5) . . ?
C81 C80 C82 112.7(6) . . ?
C81 C80 P4 116.0(5) . . ?
C82 C80 P4 110.4(5) . . ?
P3 N2 P4 138.9(3) . . ?
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 P1 2.5112(17) . ?
Te1 Se1 2.8654(10) . ?
Te1 Te2 2.9584(9) . ?
Te2 P2 2.4410(18) . ?
P1 N1 1.591(5) . ?
P1 C10 1.833(6) . ?
P1 C20 1.839(6) . ?
P2 N1 1.606(5) . ?
P2 C30 1.811(6) . ?
P2 C40 1.837(6) . ?
C10 C12 1.529(8) . ?
C10 C11 1.534(8) . ?
C20 C22 1.527(8) . ?
C20 C21 1.544(9) . ?
C30 C32 1.521(8) . ?
C30 C31 1.529(9) . ?
C40 C42 1.511(9) . ?
C40 C41 1.530(9) . ?
Se1 P3 2.2078(18) . ?
Se2 P4 2.1288(18) . ?
P3 N2 1.587(5) . ?
P3 C60 1.831(6) . ?
P3 C50 1.836(6) . ?
P4 N2 1.609(5) . ?
P4 C70 1.838(6) . ?
P4 C80 1.839(7) . ?
C50 C52 1.534(9) . ?
C50 C51 1.538(9) . ?
C60 C61 1.522(9) . ?
C60 C62 1.542(8) . ?
C70 C71 1.508(9) . ?
C70 C72 1.528(9) . ?
C80 C81 1.534(9) . ?
C80 C82 1.537(10) . ?
