#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:17:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179103 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/65/4306557.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_4306557
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 Redox Behavior of the
Heterodichalcogenido Ligands [(EPiPr2)(TePiPr2)N]-(E = S, Se): Cyclic
Cations and Acyclic Dichalcogenide Dimers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10634
_journal_page_last               10643
_journal_paper_doi               10.1021/ic801384c
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C12 H28 I N P2 S Te'
_chemical_formula_sum            'C12 H28 I N P2 S Te'
_chemical_formula_weight         534.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.7937(1)
_cell_length_b                   19.0505(2)
_cell_length_c                   22.7051(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3803.66(8)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56248
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.79
_exptl_absorpt_coefficient_mu    3.453
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.279
_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    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.492
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3267
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.255
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0273
_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)+(0.0193P)²+5.0763P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                3033
_reflns_number_total             3267
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801384c_si_001_1.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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               4306557
loop_
_symmetry_equiv_pos_as_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'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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
I1 I 0.20925(2) 0.029395(11) 0.372415(9) 0.02911(9) Uani 1 1 d . . .
Te1 Te 0.21222(2) 0.182400(11) 0.371977(8) 0.01990(9) Uani 1 1 d . . .
S1 S 0.19810(9) 0.32438(4) 0.37715(3) 0.02376(19) Uani 1 1 d . . .
P1 P -0.06373(8) 0.19152(4) 0.39729(3) 0.01620(16) Uani 1 1 d . . .
C10 C -0.0885(3) 0.17612(15) 0.47647(12) 0.0202(6) Uani 1 1 d . . .
H10A H -0.1940 0.1914 0.4866 0.024 Uiso 1 1 calc R . .
C11 C 0.0205(4) 0.22182(16) 0.51286(13) 0.0255(7) Uani 1 1 d . . .
H11A H -0.0106 0.2210 0.5543 0.038 Uiso 1 1 calc R . .
H11B H 0.0175 0.2702 0.4982 0.038 Uiso 1 1 calc R . .
H11C H 0.1242 0.2034 0.5093 0.038 Uiso 1 1 calc R . .
C12 C -0.0748(4) 0.09939(16) 0.49474(14) 0.0300(7) Uani 1 1 d . . .
H12A H -0.0937 0.0951 0.5371 0.045 Uiso 1 1 calc R . .
H12B H 0.0277 0.0823 0.4857 0.045 Uiso 1 1 calc R . .
H12C H -0.1498 0.0714 0.4731 0.045 Uiso 1 1 calc R . .
C20 C -0.1722(4) 0.12292(16) 0.35950(14) 0.0227(6) Uani 1 1 d . . .
H20A H -0.1349 0.0765 0.3742 0.027 Uiso 1 1 calc R . .
C21 C -0.1527(4) 0.12390(18) 0.29326(14) 0.0345(8) Uani 1 1 d . . .
H21A H -0.2066 0.0838 0.2760 0.052 Uiso 1 1 calc R . .
H21B H -0.0444 0.1209 0.2835 0.052 Uiso 1 1 calc R . .
H21C H -0.1947 0.1676 0.2774 0.052 Uiso 1 1 calc R . .
C22 C -0.3405(4) 0.1295(2) 0.37647(16) 0.0370(8) Uani 1 1 d . . .
H22A H -0.3995 0.0935 0.3558 0.056 Uiso 1 1 calc R . .
H22B H -0.3779 0.1761 0.3654 0.056 Uiso 1 1 calc R . .
H22C H -0.3516 0.1231 0.4191 0.056 Uiso 1 1 calc R . .
N1 N -0.1242(3) 0.26699(13) 0.37851(10) 0.0192(5) Uani 1 1 d . . .
P2 P -0.02757(8) 0.33492(4) 0.35978(3) 0.01707(16) Uani 1 1 d . . .
C30 C -0.0563(3) 0.35416(16) 0.28188(12) 0.0239(6) Uani 1 1 d . . .
H30A H -0.1685 0.3548 0.2747 0.029 Uiso 1 1 calc R . .
C31 C 0.0115(4) 0.29637(17) 0.24285(13) 0.0308(7) Uani 1 1 d . . .
H31A H -0.0060 0.3079 0.2013 0.046 Uiso 1 1 calc R . .
H31B H -0.0371 0.2514 0.2521 0.046 Uiso 1 1 calc R . .
H31C H 0.1211 0.2929 0.2502 0.046 Uiso 1 1 calc R . .
C32 C 0.0055(4) 0.42593(17) 0.26428(14) 0.0342(8) Uani 1 1 d . . .
H32A H -0.0101 0.4332 0.2220 0.051 Uiso 1 1 calc R . .
H32B H 0.1144 0.4282 0.2732 0.051 Uiso 1 1 calc R . .
H32C H -0.0481 0.4626 0.2864 0.051 Uiso 1 1 calc R . .
C40 C -0.0988(4) 0.41181(15) 0.39962(13) 0.0237(6) Uani 1 1 d . . .
H40A H -0.0406 0.4536 0.3855 0.028 Uiso 1 1 calc R . .
C41 C -0.2669(4) 0.42368(18) 0.38435(16) 0.0319(8) Uani 1 1 d . . .
H41A H -0.3077 0.4617 0.4088 0.048 Uiso 1 1 calc R . .
H41B H -0.3243 0.3805 0.3918 0.048 Uiso 1 1 calc R . .
H41C H -0.2760 0.4365 0.3427 0.048 Uiso 1 1 calc R . .
C42 C -0.0757(4) 0.40628(17) 0.46563(14) 0.0325(7) Uani 1 1 d . . .
H42A H -0.1104 0.4496 0.4846 0.049 Uiso 1 1 calc R . .
H42B H 0.0324 0.3991 0.4741 0.049 Uiso 1 1 calc R . .
H42C H -0.1343 0.3665 0.4809 0.049 Uiso 1 1 calc R . .
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'
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'
I I -0.4742 1.8119 '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 S1 82.89(2) . . ?
P1 Te1 I1 93.439(17) . . ?
S1 Te1 I1 175.871(19) . . ?
P2 S1 Te1 97.75(3) . . ?
N1 P1 C20 110.20(13) . . ?
N1 P1 C10 111.57(13) . . ?
C20 P1 C10 106.46(14) . . ?
N1 P1 Te1 109.00(9) . . ?
C20 P1 Te1 110.38(11) . . ?
C10 P1 Te1 109.23(10) . . ?
C12 C10 C11 110.4(3) . . ?
C12 C10 P1 114.3(2) . . ?
C11 C10 P1 111.3(2) . . ?
C21 C20 C22 110.9(3) . . ?
C21 C20 P1 113.4(2) . . ?
C22 C20 P1 109.0(2) . . ?
P1 N1 P2 128.50(16) . . ?
N1 P2 C30 110.21(13) . . ?
N1 P2 C40 109.44(14) . . ?
C30 P2 C40 105.71(14) . . ?
N1 P2 S1 112.68(10) . . ?
C30 P2 S1 110.06(11) . . ?
C40 P2 S1 108.49(11) . . ?
C32 C30 C31 110.7(3) . . ?
C32 C30 P2 112.7(2) . . ?
C31 C30 P2 111.2(2) . . ?
C42 C40 C41 111.3(3) . . ?
C42 C40 P2 112.8(2) . . ?
C41 C40 P2 109.6(2) . . ?
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
I1 Te1 2.9150(6) . ?
Te1 P1 2.4998(9) . ?
Te1 S1 2.7101(9) . ?
S1 P2 2.0332(12) . ?
P1 N1 1.591(2) . ?
P1 C20 1.831(3) . ?
P1 C10 1.835(3) . ?
C10 C12 1.524(4) . ?
C10 C11 1.536(4) . ?
C20 C21 1.514(4) . ?
C20 C22 1.535(5) . ?
N1 P2 1.606(2) . ?
P2 C30 1.824(3) . ?
P2 C40 1.832(3) . ?
C30 C32 1.524(4) . ?
C30 C31 1.534(4) . ?
C40 C42 1.516(4) . ?
C40 C41 1.535(4) . ?
