#------------------------------------------------------------------------------
#$Date: 2016-03-25 09:04:38 +0100 (vie 25 de mar de 2016) $
#$Revision: 179739 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/35/7003576.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_7003576
loop_
_publ_author_name
'Robertson, Stuart D.'
'Chivers, Tristram'
_publ_section_title
;
 Synthesis, NMR characterisation and X-ray structures of mixed
 chalcogenido PNP ligands containing tellurium: crystal structures of
 SeiPr2PNP(H)iPr2 and [NaN(EPiPr2)2]∞ (E = Se, Te)
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              1765
_journal_page_last               1772
_journal_paper_doi               10.1039/b717287g
_journal_year                    2008
_chemical_formula_moiety         'C12 H28 N Na P2 Se2'
_chemical_formula_sum            'C12 H28 N Na P2 Se2'
_chemical_formula_weight         429.20
_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                106.746(3)
_cell_angle_beta                 99.958(3)
_cell_angle_gamma                104.559(3)
_cell_formula_units_Z            2
_cell_length_a                   7.9188(4)
_cell_length_b                   9.6259(4)
_cell_length_c                   13.0855(6)
_cell_measurement_temperature    173(2)
_cell_volume                     891.50(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    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.0265
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12986
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.59
_exptl_absorpt_coefficient_mu    4.337
_exptl_absorpt_correction_T_max  0.7229
_exptl_absorpt_correction_T_min  0.4775
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'HKL Scalepack (Otwinowski and Minor 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         3139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²+0.5108P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0597
_reflns_number_gt                2644
_reflns_number_total             3139
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b717287g.txt
_cod_data_source_block           4Na
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               7003576
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
Se1 Se 0.00681(4) 0.80065(3) 0.04100(2) 0.02192(10) Uani 1 1 d . . .
Se2 Se 0.53202(4) 1.16556(3) 0.16448(2) 0.02343(10) Uani 1 1 d . . .
P1 P 0.17407(10) 0.79164(8) 0.18778(6) 0.01603(17) Uani 1 1 d . . .
P2 P 0.42679(10) 1.11583(8) 0.29735(6) 0.01685(17) Uani 1 1 d . . .
N1 N 0.3114(3) 0.9459(3) 0.28095(19) 0.0184(5) Uani 1 1 d . . .
Na1 Na 0.24269(18) 1.00606(14) -0.04082(10) 0.0303(3) Uani 1 1 d . . .
C10 C 0.2951(4) 0.6549(3) 0.1405(2) 0.0188(6) Uani 1 1 d . . .
H10 H 0.2043 0.5598 0.0836 0.023 Uiso 1 1 calc R . .
C11 C 0.3828(5) 0.6102(4) 0.2342(3) 0.0292(8) Uani 1 1 d . . .
H11A H 0.4521 0.5432 0.2066 0.044 Uiso 1 1 calc R . .
H11B H 0.2886 0.5562 0.2616 0.044 Uiso 1 1 calc R . .
H11C H 0.4640 0.7026 0.2945 0.044 Uiso 1 1 calc R . .
C12 C 0.4347(4) 0.7188(4) 0.0853(3) 0.0269(7) Uani 1 1 d . . .
H12A H 0.5246 0.8133 0.1388 0.040 Uiso 1 1 calc R . .
H12B H 0.3745 0.7407 0.0226 0.040 Uiso 1 1 calc R . .
H12C H 0.4950 0.6435 0.0588 0.040 Uiso 1 1 calc R . .
C20 C 0.0246(4) 0.7024(3) 0.2593(2) 0.0213(7) Uani 1 1 d . . .
H20 H 0.1033 0.6934 0.3240 0.026 Uiso 1 1 calc R . .
C21 C -0.0852(4) 0.8029(3) 0.3046(3) 0.0260(7) Uani 1 1 d . . .
H21A H -0.1683 0.8102 0.2430 0.039 Uiso 1 1 calc R . .
H21B H -0.0033 0.9054 0.3511 0.039 Uiso 1 1 calc R . .
H21C H -0.1547 0.7579 0.3488 0.039 Uiso 1 1 calc R . .
C22 C -0.1007(5) 0.5411(3) 0.1877(3) 0.0319(8) Uani 1 1 d . . .
H22A H -0.1706 0.4968 0.2320 0.048 Uiso 1 1 calc R . .
H22B H -0.0282 0.4770 0.1603 0.048 Uiso 1 1 calc R . .
H22C H -0.1834 0.5461 0.1249 0.048 Uiso 1 1 calc R . .
C30 C 0.3028(4) 1.2504(3) 0.3416(2) 0.0210(7) Uani 1 1 d . . .
H30 H 0.3821 1.3556 0.3534 0.025 Uiso 1 1 calc R . .
C31 C 0.2578(4) 1.2508(3) 0.4511(2) 0.0258(7) Uani 1 1 d . . .
H31A H 0.1758 1.3107 0.4661 0.039 Uiso 1 1 calc R . .
H31B H 0.3695 1.2965 0.5113 0.039 Uiso 1 1 calc R . .
H31C H 0.1995 1.1454 0.4458 0.039 Uiso 1 1 calc R . .
C32 C 0.1294(4) 1.2142(4) 0.2521(3) 0.0289(8) Uani 1 1 d . . .
H32A H 0.0518 1.1095 0.2365 0.043 Uiso 1 1 calc R . .
H32B H 0.1604 1.2234 0.1845 0.043 Uiso 1 1 calc R . .
H32C H 0.0650 1.2864 0.2782 0.043 Uiso 1 1 calc R . .
C40 C 0.6178(4) 1.1730(3) 0.4194(2) 0.0221(7) Uani 1 1 d . . .
H40 H 0.5667 1.1588 0.4818 0.026 Uiso 1 1 calc R . .
C41 C 0.7315(4) 1.3424(3) 0.4554(3) 0.0338(8) Uani 1 1 d . . .
H41A H 0.8356 1.3662 0.5176 0.051 Uiso 1 1 calc R . .
H41B H 0.6572 1.4070 0.4782 0.051 Uiso 1 1 calc R . .
H41C H 0.7743 1.3619 0.3933 0.051 Uiso 1 1 calc R . .
C42 C 0.7342(4) 1.0693(4) 0.3979(3) 0.0292(8) Uani 1 1 d . . .
H42A H 0.7890 1.0830 0.3383 0.044 Uiso 1 1 calc R . .
H42B H 0.6588 0.9624 0.3762 0.044 Uiso 1 1 calc R . .
H42C H 0.8298 1.0957 0.4654 0.044 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'
Na Na 0.0362 0.0249 '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'
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 Se1 Na1 107.04(4) . . ?
P1 Se1 Na1 125.36(4) . 2_575 ?
Na1 Se1 Na1 88.01(4) . 2_575 ?
P2 Se2 Na1 107.61(4) . . ?
P2 Se2 Na1 124.67(4) . 2_675 ?
Na1 Se2 Na1 85.37(4) . 2_675 ?
N1 P1 C20 105.25(13) . . ?
N1 P1 C10 110.26(13) . . ?
C20 P1 C10 104.52(13) . . ?
N1 P1 Se1 120.23(9) . . ?
C20 P1 Se1 108.20(10) . . ?
C10 P1 Se1 107.27(10) . . ?
N1 P2 C40 105.48(13) . . ?
N1 P2 C30 110.91(14) . . ?
C40 P2 C30 103.20(13) . . ?
N1 P2 Se2 120.41(10) . . ?
C40 P2 Se2 108.52(11) . . ?
C30 P2 Se2 106.98(10) . . ?
P2 N1 P1 141.59(16) . . ?
Se2 Na1 Se1 97.23(5) . . ?
Se2 Na1 Se1 106.40(5) . 2_575 ?
Se1 Na1 Se1 91.99(4) . 2_575 ?
Se2 Na1 Se2 94.63(4) . 2_675 ?
Se1 Na1 Se2 109.10(4) . 2_675 ?
Se1 Na1 Se2 148.16(5) 2_575 2_675 ?
C12 C10 C11 110.8(3) . . ?
C12 C10 P1 110.6(2) . . ?
C11 C10 P1 112.3(2) . . ?
C12 C10 H10 107.6 . . ?
C11 C10 H10 107.6 . . ?
P1 C10 H10 107.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C21 C20 C22 110.3(3) . . ?
C21 C20 P1 111.0(2) . . ?
C22 C20 P1 113.4(2) . . ?
C21 C20 H20 107.3 . . ?
C22 C20 H20 107.3 . . ?
P1 C20 H20 107.3 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C32 C30 C31 110.1(3) . . ?
C32 C30 P2 111.1(2) . . ?
C31 C30 P2 111.7(2) . . ?
C32 C30 H30 107.9 . . ?
C31 C30 H30 107.9 . . ?
P2 C30 H30 107.9 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C42 C40 C41 111.2(3) . . ?
C42 C40 P2 110.3(2) . . ?
C41 C40 P2 112.3(2) . . ?
C42 C40 H40 107.6 . . ?
C41 C40 H40 107.6 . . ?
P2 C40 H40 107.6 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
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
Se1 P1 2.1737(10) . ?
Se1 Na1 2.9325(16) . ?
Se1 Na1 3.0356(15) 2_575 ?
Se2 P2 2.1741(10) . ?
Se2 Na1 2.924(2) . ?
Se2 Na1 3.0772(16) 2_675 ?
P1 N1 1.600(2) . ?
P1 C20 1.831(3) . ?
P1 C10 1.845(3) . ?
P2 N1 1.592(2) . ?
P2 C40 1.838(3) . ?
P2 C30 1.839(3) . ?
C10 C12 1.521(4) . ?
C10 C11 1.526(4) . ?
C10 H10 1.0000 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C20 C21 1.521(4) . ?
C20 C22 1.529(4) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C30 C32 1.532(4) . ?
C30 C31 1.534(4) . ?
C30 H30 1.0000 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C40 C42 1.522(4) . ?
C40 C41 1.537(4) . ?
C40 H40 1.0000 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
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
Na1 Se1 P1 N1 46.10(12) . . . . ?
Na1 Se1 P1 N1 -53.85(12) 2_575 . . . ?
Na1 Se1 P1 C20 166.91(10) . . . . ?
Na1 Se1 P1 C20 66.96(11) 2_575 . . . ?
Na1 Se1 P1 C10 -80.84(11) . . . . ?
Na1 Se1 P1 C10 179.21(10) 2_575 . . . ?
Na1 Se2 P2 N1 44.52(12) . . . . ?
Na1 Se2 P2 N1 -52.18(12) 2_675 . . . ?
Na1 Se2 P2 C40 166.06(10) . . . . ?
Na1 Se2 P2 C40 69.36(11) 2_675 . . . ?
Na1 Se2 P2 C30 -83.21(11) . . . . ?
Na1 Se2 P2 C30 -179.90(10) 2_675 . . . ?
C40 P2 N1 P1 -154.0(3) . . . . ?
C30 P2 N1 P1 94.9(3) . . . . ?
Se2 P2 N1 P1 -31.0(3) . . . . ?
C20 P1 N1 P2 -148.7(3) . . . . ?
C10 P1 N1 P2 99.1(3) . . . . ?
Se1 P1 N1 P2 -26.5(3) . . . . ?
P2 Se2 Na1 Se1 -15.02(4) . . . . ?
Na1 Se2 Na1 Se1 109.95(5) 2_675 . . . ?
P2 Se2 Na1 Se1 79.22(5) . . . 2_575 ?
Na1 Se2 Na1 Se1 -155.82(6) 2_675 . . 2_575 ?
P2 Se2 Na1 Se2 -124.97(4) . . . 2_675 ?
Na1 Se2 Na1 Se2 0.0 2_675 . . 2_675 ?
P1 Se1 Na1 Se2 -19.70(4) . . . . ?
Na1 Se1 Na1 Se2 106.81(5) 2_575 . . . ?
P1 Se1 Na1 Se1 -126.51(4) . . . 2_575 ?
Na1 Se1 Na1 Se1 0.0 2_575 . . 2_575 ?
P1 Se1 Na1 Se2 77.77(5) . . . 2_675 ?
Na1 Se1 Na1 Se2 -155.72(6) 2_575 . . 2_675 ?
N1 P1 C10 C12 -63.7(2) . . . . ?
C20 P1 C10 C12 -176.4(2) . . . . ?
Se1 P1 C10 C12 68.9(2) . . . . ?
N1 P1 C10 C11 60.6(2) . . . . ?
C20 P1 C10 C11 -52.0(2) . . . . ?
Se1 P1 C10 C11 -166.75(19) . . . . ?
N1 P1 C20 C21 63.4(2) . . . . ?
C10 P1 C20 C21 179.6(2) . . . . ?
Se1 P1 C20 C21 -66.3(2) . . . . ?
N1 P1 C20 C22 -171.8(2) . . . . ?
C10 P1 C20 C22 -55.6(2) . . . . ?
Se1 P1 C20 C22 58.5(2) . . . . ?
N1 P2 C30 C32 -63.9(2) . . . . ?
C40 P2 C30 C32 -176.4(2) . . . . ?
Se2 P2 C30 C32 69.2(2) . . . . ?
N1 P2 C30 C31 59.4(2) . . . . ?
C40 P2 C30 C31 -53.1(2) . . . . ?
Se2 P2 C30 C31 -167.46(18) . . . . ?
N1 P2 C40 C42 62.2(2) . . . . ?
C30 P2 C40 C42 178.6(2) . . . . ?
Se2 P2 C40 C42 -68.1(2) . . . . ?
N1 P2 C40 C41 -173.2(2) . . . . ?
C30 P2 C40 C41 -56.8(3) . . . . ?
Se2 P2 C40 C41 56.5(2) . . . . ?
