#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2200614.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2200614
loop_
_publ_author_name
'Smith, Matt C.'
'Davies, Sian C.'
'Hughes, David L.'
'Evans, David J.'
_publ_section_title
;
 Tetraethylammonium trichloro(triphenylphosphine)nickelate(II)
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m509
_journal_page_last               m510
_journal_volume                  57
_journal_year                    2001
_chemical_formula_iupac          'C8 H20 N 1+, C18 H15 Cl3 Ni P 1-'
_chemical_formula_moiety         'C8 H20 N 1+, C18 H15 Cl3 Ni P 1-'
_chemical_formula_structural     (NEt~4~)[NiCl~3~(PPh~3~)]
_chemical_formula_sum            'C26 H35 Cl3 N Ni P'
_chemical_formula_weight         557.58
_chemical_melting_point          521
_chemical_name_systematic
;
 Tetraethylammonium trichloro(triphenylphosphine)nickelate(II)
;
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-p 2bc 2ac 3'
_symmetry_space_group_name_H-M   'P b -3'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.6676(7)
_cell_length_b                   17.6676(7)
_cell_length_c                   17.6676(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     5514.8(4)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD-4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1971)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .0215
_diffrn_reflns_av_sigmaI/netI    .1105
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1750
_diffrn_reflns_theta_max         24.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  167
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  .774
_exptl_absorpt_correction_T_min  .728
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(EMPABS; Sheldrick et al., 1977)'
_exptl_crystal_colour            'translucent intense blue'
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    none
_exptl_crystal_description       octahedra
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          .36
_exptl_crystal_size_mid          .29
_exptl_crystal_size_min          .24
_refine_diff_density_max         .274
_refine_diff_density_min         -.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   .958
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      .958
_refine_ls_restrained_S_obs      1.203
_refine_ls_R_factor_all          .1550
_refine_ls_R_factor_gt           .0546
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0626P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .1767
_refine_ls_wR_factor_ref         .1767
_reflns_number_gt                497
_reflns_number_total             1445
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    cf6111.cif
_[local]_cod_data_source_block   I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (3
times).

'_geom_bond_publ_flag' value 'No' changed to 'no' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (39
times).

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (4
times).

'_geom_angle_publ_flag' value 'No' changed to 'no' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (72
times).

'_geom_torsion_publ_flag' value 'Yes' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (3
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2200614
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'
'z, x, y'
'z+1/2, -x, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y'
'y, z, x'
'y+1/2, -z, -x+1/2'
'-y, -z+1/2, x+1/2'
'-y+1/2, z+1/2, -x'
'-x, -y, -z'
'-x-1/2, y, z-1/2'
'x, y-1/2, -z-1/2'
'x-1/2, -y-1/2, z'
'-z, -x, -y'
'-z-1/2, x, y-1/2'
'z, x-1/2, -y-1/2'
'z-1/2, -x-1/2, y'
'-y, -z, -x'
'-y-1/2, z, x-1/2'
'y, z-1/2, -x-1/2'
'y-1/2, -z-1/2, x'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ni .0722(6) .0722(6) .0722(6) .0077(6) .0077(6) -.0077(6)
Cl1 .127(2) .078(2) .129(2) .0215(15) -.025(2) -.0001(15)
P1 .0560(9) .0560(9) .0560(9) .0012(10) .0012(10) -.0012(10)
C11 .060(5) .053(5) .061(5) .006(4) .003(4) .003(4)
C12 .080(6) .066(5) .058(5) -.004(5) -.004(5) .004(5)
C13 .088(7) .096(8) .070(6) -.017(6) -.012(6) -.014(6)
C14 .106(8) .118(9) .072(7) -.024(7) -.024(6) -.017(7)
C15 .115(8) .123(9) .082(7) .021(8) -.045(6) .004(7)
C16 .111(8) .066(6) .076(6) .010(5) -.009(6) -.006(5)
N1 .071(3) .071(3) .071(3) -.002(4) .002(4) -.002(4)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Ni .80870(5) .69130(5) .19130(5) .0722(6) Uani d S 1 Ni
Cl1 .7878(2) .79346(13) .1199(2) .1112(10) Uani d . 1 Cl
P1 .88460(11) .61540(11) .11540(11) .0560(9) Uani d S 1 P
C11 .8359(4) .5758(4) .0345(4) .058(2) Uani d . 1 C
C12 .8477(4) .5025(5) .0093(4) .068(2) Uani d . 1 C
H12 .8806 .4712 .0359 .06(2) Uiso calc R 1 H
C13 .8115(5) .4749(6) -.0544(5) .085(3) Uani d . 1 C
H13 .8196 .4254 -.0705 .10(3) Uiso calc R 1 H
C14 .7635(6) .5217(6) -.0935(6) .099(3) Uani d . 1 C
H14 .7383 .5034 -.1360 .10(3) Uiso calc R 1 H
C15 .7520(6) .5947(7) -.0713(6) .107(3) Uani d . 1 C
H15 .7208 .6267 -.0990 .09(3) Uiso calc R 1 H
C16 .7874(5) .6198(5) -.0069(5) .085(3) Uani d . 1 C
H16 .7781 .6690 .0093 .05(2) Uiso calc R 1 H
N1 .6154(4) .3846(4) .1154(4) .071(3) Uani d S 1 N
C1 .650(2) .464(3) .099(3) .155(14) Uiso d P .33333 C
H1A .6860 .4755 .1387 .185 Uiso calc PR .33333 H
H1B .6784 .4607 .0518 .185 Uiso calc PR .33333 H
C2 .601(2) .524(2) .093(2) .146(15) Uiso d P .33333 C
H2A .6285 .5699 .0826 .219 Uiso calc PR .33333 H
H2B .5732 .5300 .1394 .219 Uiso calc PR .33333 H
H2C .5655 .5152 .0523 .219 Uiso calc PR .33333 H
C3 .660(2) .3057(18) .1048(17) .111(10) Uiso d P .33333 C
H3A .6611 .2927 .0515 .133 Uiso calc PR .33333 H
H3B .7120 .3122 .1215 .133 Uiso calc PR .33333 H
C4 .627(2) .247(2) .145(2) .128(13) Uiso d P .33333 C
H4A .6560 .2010 .1370 .191 Uiso calc PR .33333 H
H4B .5763 .2391 .1281 .191 Uiso calc PR .33333 H
H4C .6272 .2586 .1981 .191 Uiso calc PR .33333 H
C5 .5406(17) .3678(16) .0718(16) .089(8) Uiso d P .33333 C
H5A .5200 .3199 .0892 .107 Uiso calc PR .33333 H
H5B .5039 .4070 .0831 .107 Uiso calc PR .33333 H
C6 .5523(16) .3640(18) -.0126(18) .099(10) Uiso d P .33333 C
H6A .5176 .3282 -.0342 .149 Uiso calc PR .33333 H
H6B .6032 .3485 -.0232 .149 Uiso calc PR .33333 H
H6C .5435 .4131 -.0343 .149 Uiso calc PR .33333 H
C7 .609(2) .403(3) .194(2) .153(14) Uiso d P .33333 C
H7A .5773 .3642 .2162 .184 Uiso calc PR .33333 H
H7B .5799 .4496 .1963 .184 Uiso calc PR .33333 H
C8 .6715(17) .4139(19) .248(2) .108(11) Uiso d P .33333 C
H8A .6511 .4259 .2974 .162 Uiso calc PR .33333 H
H8B .7033 .4546 .2316 .162 Uiso calc PR .33333 H
H8C .7007 .3682 .2517 .162 Uiso calc PR .33333 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni .3333393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 '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_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Ni Cl1 12_656 114.61(6) yes
Cl1 Ni P1 . 103.65(8) yes
C11 P1 C11 12_656 104.7(3) yes
C11 P1 Ni . 113.9(2) yes
C16 C11 C12 . 116.9(7) no
C16 C11 P1 . 120.1(6) no
C12 C11 P1 . 122.9(6) no
C13 C12 C11 . 121.5(8) no
C13 C12 H12 . 119.3 no
C11 C12 H12 . 119.3 no
C14 C13 C12 . 118.9(9) no
C14 C13 H13 . 120.6 no
C12 C13 H13 . 120.6 no
C15 C14 C13 . 121.1(10) no
C15 C14 H14 . 119.4 no
C13 C14 H14 . 119.4 no
C14 C15 C16 . 118.5(9) no
C14 C15 H15 . 120.7 no
C16 C15 H15 . 120.7 no
C11 C16 C15 . 123.0(9) no
C11 C16 H16 . 118.5 no
C15 C16 H16 . 118.5 no
C7 N1 C5 . 117(2) no
C7 N1 C1 . 90(3) no
C5 N1 C1 . 114.4(18) no
C7 N1 C3 . 110(2) no
C5 N1 C3 . 101.1(16) no
C1 N1 C3 . 124(2) no
C2 C1 N1 . 117(3) no
C2 C1 H1A . 108.0 no
N1 C1 H1A . 108.0 no
C2 C1 H1B . 108.0 no
N1 C1 H1B . 108.0 no
H1A C1 H1B . 107.2 no
C1 C2 H2A . 109.5 no
C1 C2 H2B . 109.5 no
H2A C2 H2B . 109.5 no
C1 C2 H2C . 109.5 no
H2A C2 H2C . 109.5 no
H2B C2 H2C . 109.5 no
C4 C3 N1 . 113(3) no
C4 C3 H3A . 109.0 no
N1 C3 H3A . 109.0 no
C4 C3 H3B . 109.0 no
N1 C3 H3B . 109.0 no
H3A C3 H3B . 107.8 no
C3 C4 H4A . 109.5 no
C3 C4 H4B . 109.5 no
H4A C4 H4B . 109.5 no
C3 C4 H4C . 109.5 no
H4A C4 H4C . 109.5 no
H4B C4 H4C . 109.5 no
C6 C5 N1 . 112(2) no
C6 C5 H5A . 109.1 no
N1 C5 H5A . 109.1 no
C6 C5 H5B . 109.1 no
N1 C5 H5B . 109.1 no
H5A C5 H5B . 107.9 no
C5 C6 H6A . 109.5 no
C5 C6 H6B . 109.5 no
H6A C6 H6B . 109.5 no
C5 C6 H6C . 109.5 no
H6A C6 H6C . 109.5 no
H6B C6 H6C . 109.5 no
N1 C7 C8 . 127(3) no
N1 C7 H7A . 105.5 no
C8 C7 H7A . 105.5 no
N1 C7 H7B . 105.5 no
C8 C7 H7B . 105.5 no
H7A C7 H7B . 106.1 no
C7 C8 H8A . 109.5 no
C7 C8 H8B . 109.5 no
H8A C8 H8B . 109.5 no
C7 C8 H8C . 109.5 no
H8A C8 H8C . 109.5 no
H8B C8 H8C . 109.5 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Ni Cl1 2.233(2) yes
Ni P1 2.322(4) yes
P1 C11 1.809(7) yes
C11 C16 1.369(10) no
C11 C12 1.385(9) no
C12 C13 1.384(10) no
C12 H12 .93 no
C13 C14 1.372(11) no
C13 H13 .93 no
C14 C15 1.364(11) no
C14 H14 .93 no
C15 C16 1.371(11) no
C15 H15 .93 no
C16 H16 .93 no
N1 C7 1.44(4) no
N1 C5 1.56(3) no
N1 C1 1.56(4) no
N1 C3 1.61(3) no
C1 C2 1.38(5) no
C1 H1A .97 no
C1 H1B .97 no
C2 H2A .96 no
C2 H2B .96 no
C2 H2C .96 no
C3 C4 1.39(4) no
C3 H3A .97 no
C3 H3B .97 no
C4 H4A .96 no
C4 H4B .96 no
C4 H4C .96 no
C5 C6 1.51(4) no
C5 H5A .97 no
C5 H5B .97 no
C6 H6A .96 no
C6 H6B .96 no
C6 H6C .96 no
C7 C8 1.47(5) no
C7 H7A .97 no
C7 H7B .97 no
C8 H8A .96 no
C8 H8B .96 no
C8 H8C .96 no
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_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl1 Ni P1 C11 . -69.7(3) yes
Cl1 Ni P1 C11 7_664 50.3(3) yes
Cl1 Ni P1 C11 12_656 170.3(3) yes