#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:31:10 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179752 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/48/7004804.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_7004804
loop_
_publ_author_name
'Robertson, Stuart D.'
'Chivers, Tristram'
'Akhtar, Javeed'
'Afzaal, Mohammad'
'O'Brien, Paul'
_publ_section_title
;
 Nickel(ii) complexes of heterodichalcogenido and monochalcogenido
 imidodiphosphinate ligands: AACVD synthesis of nickel ditelluride
;
_journal_issue                   48
_journal_name_full               'Dalton Transactions'
_journal_page_first              7004
_journal_page_last               7011
_journal_paper_doi               10.1039/b814065k
_journal_year                    2008
_chemical_formula_moiety         'C24 H56 N2 Ni P4 S2 Te2'
_chemical_formula_sum            'C24 H56 N2 Ni P4 S2 Te2'
_chemical_formula_weight         874.62
_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                106.053(3)
_cell_angle_beta                 98.788(3)
_cell_angle_gamma                110.508(3)
_cell_formula_units_Z            1
_cell_length_a                   8.3894(5)
_cell_length_b                   9.5766(4)
_cell_length_c                   12.7480(8)
_cell_measurement_reflns_used    30318
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     885.71(9)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0401
_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            15755
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.22
_exptl_absorpt_coefficient_mu    2.478
_exptl_absorpt_correction_T_max  0.787
_exptl_absorpt_correction_T_min  0.583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             438
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.167
_refine_diff_density_min         -1.107
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0352
_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)+(0.0594P)²+0.6786P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                2796
_reflns_number_total             3124
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b814065k.txt
_cod_data_source_block           2
_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_original_cell_volume        885.72(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7004804
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
Ni1 Ni 0.0000 0.0000 1.0000 0.01999(18) Uani 1 2 d S . .
Te1 Te 0.12940(3) 0.27678(3) 0.99436(2) 0.02494(13) Uani 1 1 d . . .
P1 P 0.18623(13) 0.26121(11) 0.81002(9) 0.0198(2) Uani 1 1 d . . .
C10 C 0.1532(5) 0.4261(5) 0.7775(4) 0.0242(9) Uani 1 1 d . . .
H10A H 0.1835 0.4259 0.7046 0.029 Uiso 1 1 calc R . .
C11 C 0.2748(6) 0.5886(5) 0.8686(4) 0.0330(10) Uani 1 1 d . . .
H11A H 0.2531 0.6728 0.8477 0.050 Uiso 1 1 calc R . .
H11B H 0.3986 0.6059 0.8748 0.050 Uiso 1 1 calc R . .
H11C H 0.2505 0.5914 0.9418 0.050 Uiso 1 1 calc R . .
C12 C -0.0398(6) 0.3998(5) 0.7592(4) 0.0320(10) Uani 1 1 d . . .
H12A H -0.0560 0.4862 0.7385 0.048 Uiso 1 1 calc R . .
H12B H -0.0737 0.3988 0.8293 0.048 Uiso 1 1 calc R . .
H12C H -0.1142 0.2975 0.6978 0.048 Uiso 1 1 calc R . .
C20 C 0.4210(5) 0.3037(5) 0.8250(4) 0.0252(9) Uani 1 1 d . . .
H20A H 0.4928 0.4043 0.8918 0.030 Uiso 1 1 calc R . .
C21 C 0.4728(6) 0.3294(6) 0.7196(4) 0.0388(11) Uani 1 1 d . . .
H21A H 0.5974 0.3479 0.7282 0.058 Uiso 1 1 calc R . .
H21B H 0.4560 0.4222 0.7109 0.058 Uiso 1 1 calc R . .
H21C H 0.3983 0.2345 0.6523 0.058 Uiso 1 1 calc R . .
C22 C 0.4611(6) 0.1689(5) 0.8480(4) 0.0331(10) Uani 1 1 d . . .
H22A H 0.5879 0.1953 0.8593 0.050 Uiso 1 1 calc R . .
H22B H 0.3929 0.0692 0.7830 0.050 Uiso 1 1 calc R . .
H22C H 0.4282 0.1560 0.9163 0.050 Uiso 1 1 calc R . .
S1 S 0.02470(13) -0.13593(11) 0.83459(8) 0.0225(2) Uani 1 1 d . . .
N1 N 0.0653(4) 0.0994(4) 0.7030(3) 0.0228(7) Uani 1 1 d . . .
P2 P -0.06369(13) -0.06641(12) 0.70811(8) 0.0199(2) Uani 1 1 d . . .
C30 C -0.2789(5) -0.0589(5) 0.7120(4) 0.0244(9) Uani 1 1 d . . .
H30A H -0.2509 0.0453 0.7724 0.029 Uiso 1 1 calc R . .
C31 C -0.3679(6) -0.0498(6) 0.6013(4) 0.0325(10) Uani 1 1 d . . .
H31A H -0.4569 -0.0075 0.6143 0.049 Uiso 1 1 calc R . .
H31B H -0.4254 -0.1567 0.5427 0.049 Uiso 1 1 calc R . .
H31C H -0.2785 0.0208 0.5762 0.049 Uiso 1 1 calc R . .
C32 C -0.4068(6) -0.1857(6) 0.7453(4) 0.0344(10) Uani 1 1 d . . .
H32A H -0.5068 -0.1590 0.7575 0.052 Uiso 1 1 calc R . .
H32B H -0.3453 -0.1899 0.8154 0.052 Uiso 1 1 calc R . .
H32C H -0.4507 -0.2898 0.6843 0.052 Uiso 1 1 calc R . .
C40 C -0.0868(5) -0.2168(5) 0.5748(3) 0.0249(9) Uani 1 1 d . . .
H40A H -0.1187 -0.1793 0.5121 0.030 Uiso 1 1 calc R . .
C41 C 0.0919(6) -0.2267(6) 0.5733(4) 0.0381(11) Uani 1 1 d . . .
H41A H 0.0802 -0.3024 0.4998 0.057 Uiso 1 1 calc R . .
H41B H 0.1277 -0.2630 0.6341 0.057 Uiso 1 1 calc R . .
H41C H 0.1818 -0.1211 0.5853 0.057 Uiso 1 1 calc R . .
C42 C -0.2337(6) -0.3814(5) 0.5496(4) 0.0356(10) Uani 1 1 d . . .
H42A H -0.2308 -0.4583 0.4815 0.053 Uiso 1 1 calc R . .
H42B H -0.3489 -0.3754 0.5367 0.053 Uiso 1 1 calc R . .
H42C H -0.2153 -0.4158 0.6143 0.053 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'
Ni Ni 0.3393 1.1124 '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
S1 Ni1 S1 180.0 2_557 . ?
S1 Ni1 Te1 80.78(4) 2_557 . ?
S1 Ni1 Te1 99.22(4) . . ?
S1 Ni1 Te1 99.22(4) 2_557 2_557 ?
S1 Ni1 Te1 80.78(4) . 2_557 ?
Te1 Ni1 Te1 180.0 . 2_557 ?
P1 Te1 Ni1 109.19(4) . . ?
N1 P1 C20 109.77(19) . . ?
N1 P1 C10 107.56(18) . . ?
C20 P1 C10 106.14(19) . . ?
N1 P1 Te1 117.69(13) . . ?
C20 P1 Te1 108.63(14) . . ?
C10 P1 Te1 106.41(14) . . ?
C12 C10 C11 111.1(4) . . ?
C12 C10 P1 110.6(3) . . ?
C11 C10 P1 112.3(3) . . ?
C21 C20 C22 111.2(4) . . ?
C21 C20 P1 110.9(3) . . ?
C22 C20 P1 110.3(3) . . ?
P2 S1 Ni1 110.72(5) . . ?
P2 N1 P1 126.3(2) . . ?
N1 P2 C40 104.47(18) . . ?
N1 P2 C30 108.00(18) . . ?
C40 P2 C30 110.10(19) . . ?
N1 P2 S1 117.25(14) . . ?
C40 P2 S1 105.93(14) . . ?
C30 P2 S1 110.77(14) . . ?
C32 C30 C31 111.5(3) . . ?
C32 C30 P2 116.8(3) . . ?
C31 C30 P2 110.9(3) . . ?
C42 C40 C41 111.2(4) . . ?
C42 C40 P2 113.8(3) . . ?
C41 C40 P2 110.0(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
Ni1 S1 2.2335(12) 2_557 ?
Ni1 S1 2.2335(12) . ?
Ni1 Te1 2.5145(8) . ?
Ni1 Te1 2.5145(8) 2_557 ?
Te1 P1 2.4434(11) . ?
P1 N1 1.612(4) . ?
P1 C20 1.833(4) . ?
P1 C10 1.837(4) . ?
C10 C12 1.518(6) . ?
C10 C11 1.529(6) . ?
C20 C21 1.529(6) . ?
C20 C22 1.533(6) . ?
S1 P2 2.0413(15) . ?
N1 P2 1.603(3) . ?
P2 C40 1.830(4) . ?
P2 C30 1.839(4) . ?
C30 C32 1.523(6) . ?
C30 C31 1.532(6) . ?
C40 C42 1.531(6) . ?
C40 C41 1.538(6) . ?
