#------------------------------------------------------------------------------
#$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $
#$Revision: 32112 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/50/2005010.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_2005010
loop_
_publ_author_name
'Rabe, G. W.'
'Riede, J.'
'Schier, A.'
_publ_section_title
;
 [Li~2~(\m~3~-^<i>t^</i>Bu~2~ P)(\m~2~-^<i>t^</i>Bu~2~P)(thf)]~2~: a
 Redetermination
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1350
_journal_page_last               1352
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          '[Li4 (C8 H18 P)4 (C4 H8 O)2] , C6 H14'
_chemical_formula_sum            'C46 H102 Li4 O2 P4'
_chemical_formula_weight         838.98
_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_type_scat_source           IntTabIV
_cell_angle_alpha                90
_cell_angle_beta                 97.20(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.533(3)
_cell_length_b                   20.585(6)
_cell_length_c                   12.217(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213
_cell_measurement_theta_max      19
_cell_measurement_theta_min      15
_cell_volume                     2877.5(12)
_computing_cell_refinement       'CAD4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'SDP-Plus (Enraf-Nonius, 1988); CADSHEL (Kopf & R\"ubcke, 1993)'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL-Plus (Siemens, 1990)'
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6059
_diffrn_reflns_theta_max         27
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.16
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.968
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.307
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.004
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5740
_refine_ls_R_factor_obs          0.0552
_refine_ls_shift/esd_max         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'                    w = 1/[\s^2^(F) + 0.0001F^2^]'
_refine_ls_wR_factor_obs         0.1216
_reflns_number_observed          5740
_reflns_number_total             5759
_reflns_observed_criterion       I>2\s(I)
_[local]_cod_data_source_file    jz1099.cif
_[local]_cod_data_source_block   jz1099a
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_original_cell_volume        2877.5
_cod_database_code               2005010
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2+x,1/2-y,1/2+z
-x,-y,-z
1/2-x,1/2+y,1/2-z
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
P(1) .50280(7) .02005(4) .82926(6) .0337(2)
P(2) .27123(8) .14202(4) .95240(7) .0422(2)
C(10) .6393(3) .0567(2) .7831(2) .0438(8)
C(11) .7438(3) .0110(2) .7950(4) .0819(13)
C(12) .6226(3) .0822(2) .6651(3) .0682(11)
C(13) .6676(4) .1139(2) .8601(3) .0827(13)
C(20) .4341(3) -.0429(2) .7282(2) .0444(8)
C(21) .5219(4) -.0888(2) .6852(3) .0761(12)
C(22) .3582(3) -.0123(2) .6302(3) .0678(11)
C(23) .3546(3) -.0826(2) .7929(3) .0601(10)
C(30) .1124(3) .1198(2) .9149(3) .0555(9)
C(31) .1152(4) .0497(2) .8744(4) .0809(13)
C(32) .0410(4) .1190(2) 1.0110(4) .0822(13)
C(33) .0504(4) .1605(3) .8215(4) .100(2)
C(40) .2887(3) .2222(2) 1.0277(3) .0556(9)
C(41) .4184(4) .2354(2) 1.0380(4) .0805(13)
C(42) .2240(5) .2782(2) .9668(4) .089(2)
C(43) .2532(4) .2201(2) 1.1448(3) .0791(13)
Li(1) .4079(4) .0508(2) 1.0092(4) .0389(11)
Li(2) .3685(5) .1192(2) .7879(4) .0458(13)
O .3464(2) .17102(11) .6556(2) .0628(7)
C(1) .3127(6) .1589(2) .5445(3) .126(2)
C(2) .2827(6) .2216(3) .4890(4) .119(2)
C(3) .2777(5) .2673(2) .5770(5) .104(2)
C(4) .3502(7) .2393(2) .6696(4) .125(2)
C(5) 1.0170(6) .1122(3) .3281(5) .128(2)
C(6) .9882(6) .0817(3) .4301(6) .135(2)
C(7) 1.0140(5) .0159(3) .4474(4) .110(2)
H(111) .7277(3) -.0257(2) .7471(4) .080
H(112) .7586(3) -.0037(2) .8701(4) .080
H(113) .8112(3) .0336(2) .7758(4) .080
H(121) .6050(3) .0466(2) .6150(3) .080
H(122) .6932(3) .1031(2) .6496(3) .080
H(123) .5594(3) .1129(2) .6561(3) .080
H(131) .6782(4) .0991(2) .9352(3) .080
H(132) .6042(4) .1443(2) .8500(3) .080
H(133) .7379(4) .1346(2) .8434(3) .080
H(211) .5730(4) -.0646(2) .6441(3) .080
H(212) .4808(4) -.1209(2) .6383(3) .080
H(213) .5672(4) -.1099(2) .7464(3) .080
H(221) .4064(3) .0130(2) .5879(3) .080
H(222) .3006(3) .0152(2) .6568(3) .080
H(223) .3198(3) -.0458(2) .5845(3) .080
H(231) .4002(3) -.1026(2) .8550(3) .080
H(232) .3162(3) -.1157(2) .7462(3) .080
H(233) .2971(3) -.0546(2) .8184(3) .080
H(311) .1599(4) .0474(2) .8134(4) .080
H(312) .0368(4) .0354(2) .8512(4) .080
H(313) .1503(4) .0223(2) .9330(4) .080
H(321) .0370(4) .1622(2) 1.0399(4) .080
H(322) .0770(4) .0907(2) 1.0678(4) .080
H(323) -.0365(4) .1038(2) .9860(4) .080
H(331) .0476(4) .2050(3) .8449(4) .080
H(332) -.0278(4) .1446(3) .8023(4) .080
H(333) .0920(4) .1578(3) .7583(4) .080
H(411) .4603(4) .2003(2) 1.0765(4) .080
H(412) .4353(4) .2751(2) 1.0782(4) .080
H(413) .4420(4) .2395(2) .9657(4) .080
H(421) .1414(5) .2702(2) .9598(4) .080
H(422) .2482(5) .2822(2) .8947(4) .080
H(423) .2415(5) .3177(2) 1.0072(4) .080
H(431) .1710(4) .2116(2) 1.1405(3) .080
H(432) .2705(4) .2611(2) 1.1807(3) .080
H(433) .2959(4) .1863(2) 1.1862(3) .080
H(11) .3756(6) .1390(2) .5122(3) .150
H(12) .2461(6) .1305(2) .5360(3) .150
H(21) .2079(6) .2186(3) .4449(4) .150
H(22) .3408(6) .2338(3) .4430(4) .150
H(31) .3093(5) .3083(2) .5580(5) .150
H(32) .1990(5) .2733(2) .5931(5) .150
H(41) .3202(7) .2506(2) .7369(4) .150
H(42) .4291(7) .2547(2) .6722(4) .150
H(51) .9928(6) .1567(3) .3304(5) .150
H(52) .9760(6) .0915(3) .2642(5) .150
H(53) 1.0996(6) .1103(3) .3243(5) .150
H(61) .9055(6) .0857(3) .4317(6) .150
H(62) 1.0291(6) .1045(3) .4918(6) .150
H(71) 1.0995 .0072 .4454 .150
H(72) .9772 -.0115 .3860 .150
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C(10) P(1) C(20) 111.93(14) no
C(20) P(1) Li(1) 102.0(2) no
C(20) P(1) Li(2) 102.8(2) no
C(10) P(1) Li(1) 126.6(2) no
Li(1) P(1) Li(1) 70.5(2) no
C(30) P(2) C(40) 111.8(2) no
C(40) P(2) Li(2) 122.2(2) no
C(40) P(2) Li(1) 119.8(2) no
C(13) C(10) C(11) 108.3(3) no
C(11) C(10) C(12) 108.0(3) no
C(11) C(10) P(1) 113.8(2) no
C(10) C(11) H(111) 109.7(2) no
H(111) C(11) H(112) 109.5 no
H(111) C(11) H(113) 109.5 no
C(10) C(12) H(121) 109.3(2) no
H(121) C(12) H(122) 109.5 no
H(121) C(12) H(123) 109.5 no
C(10) P(1) Li(1) 100.8(2) no
C(10) P(1) Li(2) 97.3(2) no
Li(1) P(1) Li(2) 140.9(2) no
C(20) P(1) Li(1) 121.4(2) no
Li(2) P(1) Li(1) 70.9(2) no
C(30) P(2) Li(2) 106.4(2) no
C(30) P(2) Li(1) 116.4(2) no
Li(2) P(2) Li(1) 75.4(2) no
C(13) C(10) C(12) 108.1(3) no
C(13) C(10) P(1) 104.3(2) no
C(12) C(10) P(1) 114.1(2) no
C(10) C(11) H(112) 109.3(2) no
C(10) C(11) H(113) 109.4(2) no
H(112) C(11) H(113) 109.5 no
C(10) C(12) H(122) 109.3(2) no
C(10) C(12) H(123) 109.8(2) no
H(122) C(12) H(123) 109.5 no
C(10) C(13) H(131) 109.8(2) no
H(131) C(13) H(132) 109.5 no
H(131) C(13) H(133) 109.5 no
C(23) C(20) C(21) 108.4(3) no
C(21) C(20) C(22) 109.1(3) no
C(21) C(20) P(1) 114.0(2) no
C(20) C(21) H(211) 109.6(2) no
H(211) C(21) H(212) 109.5 no
H(211) C(21) H(213) 109.5 no
C(20) C(22) H(221) 109.4(2) no
H(221) C(22) H(222) 109.5 no
H(221) C(22) H(223) 109.5 no
C(20) C(23) H(231) 109.5(2) no
H(231) C(23) H(232) 109.5 no
H(231) C(23) H(233) 109.5 no
C(32) C(30) C(33) 109.7(3) no
C(33) C(30) C(31) 107.8(4) no
C(33) C(30) P(2) 113.5(3) no
C(30) C(31) H(311) 109.5(2) no
H(311) C(31) H(312) 109.5 no
H(311) C(31) H(313) 109.5 no
C(30) C(32) H(321) 109.3(2) no
H(321) C(32) H(322) 109.5 no
H(321) C(32) H(323) 109.5 no
C(30) C(33) H(331) 109.4(3) no
H(331) C(33) H(332) 109.5 no
H(331) C(33) H(333) 109.5 no
C(41) C(40) C(42) 109.0(4) no
C(42) C(40) C(43) 107.8(3) no
C(42) C(40) P(2) 114.2(3) no
C(40) C(41) H(411) 109.7(2) no
H(411) C(41) H(412) 109.5 no
H(411) C(41) H(413) 109.5 no
C(40) C(42) H(421) 109.6(2) no
H(421) C(42) H(422) 109.5 no
H(421) C(42) H(423) 109.5 no
C(40) C(43) H(431) 109.3(2) no
H(431) C(43) H(432) 109.5 no
H(431) C(43) H(433) 109.5 no
P(2) Li(1) P(1) 145.2(2) no
P(1) Li(1) P(1) 109.5(2) no
P(1) Li(1) Li(1) 56.1(2) no
P(2) Li(1) Li(2) 51.92(13) no
P(1) Li(1) Li(2) 53.34(13) no
O Li(2) P(2) 123.5(2) no
P(2) Li(2) P(1) 108.4(2) no
P(2) Li(2) Li(1) 52.73(13) no
C(1) O C(4) 107.3(3) no
C(4) O Li(2) 116.8(3) no
O C(1) H(11) 110.2(3) no
O C(1) H(12) 109.7(3) no
H(11) C(1) H(12) 109.5 no
C(3) C(2) H(21) 110.7(3) no
C(3) C(2) H(22) 111.3(4) no
H(21) C(2) H(22) 109.5 no
C(2) C(3) H(31) 110.0(3) no
C(2) C(3) H(32) 111.5(4) no
H(31) C(3) H(32) 109.5 no
O C(4) H(41) 109.5(2) no
O C(4) H(42) 110.3(3) no
H(41) C(4) H(42) 109.5 no
C(6) C(5) H(52) 111.1(4) no
C(6) C(5) H(53) 110.8(4) no
C(10) C(13) H(132) 109.0(2) no
C(10) C(13) H(133) 109.6(2) no
H(132) C(13) H(133) 109.5 no
C(23) C(20) C(22) 107.7(3) no
C(23) C(20) P(1) 105.0(2) no
C(22) C(20) P(1) 112.3(2) no
C(20) C(21) H(212) 109.4(2) no
C(20) C(21) H(213) 109.4(2) no
H(212) C(21) H(213) 109.5 no
C(20) C(22) H(222) 109.4(2) no
C(20) C(22) H(223) 109.7(2) no
H(222) C(22) H(223) 109.5 no
C(20) C(23) H(232) 109.5(2) no
C(20) C(23) H(233) 109.4(2) no
H(232) C(23) H(233) 109.5 no
C(32) C(30) C(31) 106.1(3) no
C(32) C(30) P(2) 114.8(3) no
C(31) C(30) P(2) 104.4(2) no
C(30) C(31) H(312) 109.2(2) no
C(30) C(31) H(313) 109.8(2) no
H(312) C(31) H(313) 109.5 no
C(30) C(32) H(322) 109.8(2) no
C(30) C(32) H(323) 109.3(2) no
H(322) C(32) H(323) 109.5 no
C(30) C(33) H(332) 109.5(2) no
C(30) C(33) H(333) 109.6(2) no
H(332) C(33) H(333) 109.5 no
C(41) C(40) C(43) 107.7(3) no
C(41) C(40) P(2) 104.0(2) no
C(43) C(40) P(2) 113.9(3) no
C(40) C(41) H(412) 109.3(2) no
C(40) C(41) H(413) 109.4(2) no
H(412) C(41) H(413) 109.5 no
C(40) C(42) H(422) 109.4(2) no
C(40) C(42) H(423) 109.4(2) no
H(422) C(42) H(423) 109.5 no
C(40) C(43) H(432) 109.7(2) no
C(40) C(43) H(433) 109.4(2) no
H(432) C(43) H(433) 109.5 no
P(2) Li(1) P(1) 105.2(2) no
P(2) Li(1) Li(1) 158.5(3) no
P(1) Li(1) Li(1) 53.40(14) no
P(1) Li(1) Li(2) 162.1(2) no
Li(1) Li(1) Li(2) 106.5(2) no
O Li(2) P(1) 128.1(2) no
O Li(2) Li(1) 174.0(3) no
P(1) Li(2) Li(1) 55.76(13) no
C(1) O Li(2) 135.4(3) no
O C(1) C(2) 108.2(4) no
C(2) C(1) H(11) 109.2(4) no
C(2) C(1) H(12) 110.1(4) no
C(3) C(2) C(1) 104.9(4) no
C(1) C(2) H(21) 110.0(4) no
C(1) C(2) H(22) 110.9(4) no
C(2) C(3) C(4) 104.7(4) no
C(4) C(3) H(31) 109.9(3) no
C(4) C(3) H(32) 111.2(3) no
O C(4) C(3) 107.2(4) no
C(3) C(4) H(41) 109.9(3) no
C(3) C(4) H(42) 110.5(3) no
C(6) C(5) H(51) 106.5(4) no
H(51) C(5) H(52) 109.5 no
H(51) C(5) H(53) 109.5 no
H(52) C(5) H(53) 109.5 no
C(7) C(6) H(61) 105.8(4) no
C(7) C(6) H(62) 106.3(4) no
H(61) C(6) H(62) 109.5 no
C(6) C(7) H(71) 111.1(6) no
C(6) C(7) H(72) 112.0(6) no
H(71) C(7) H(72) 102.1(5) no
C(7) C(6) C(5) 118.4(6) no
C(5) C(6) H(61) 108.2(4) no
C(5) C(6) H(62) 108.5(4) no
C(6) C(7) C(7) 118.9(7) no
C(7) C(7) H(71) 104.9(6) no
C(7) C(7) H(72) 106.3(7) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
P(1) C(10) 1.894(3) no
P(1) Li(1) 2.564(5) no
P(1) Li(1) 2.652(5) no
P(2) C(40) 1.888(4) no
P(2) Li(1) 2.493(5) no
C(10) C(11) 1.522(5) no
C(20) C(23) 1.523(4) no
C(20) C(22) 1.528(5) no
C(30) C(33) 1.521(5) no
C(40) C(41) 1.510(6) no
C(40) C(43) 1.537(5) no
Li(1) Li(1) 3.010(9) no
Li(2) O 1.926(5) no
O C(4) 1.417(5) no
C(2) C(3) 1.435(7) no
C(5) C(6) 1.470(7) no
C(7) C(7) 1.512(11) no
C(11) H(112) .96 no
C(12) H(121) .96 no
C(12) H(123) .96 no
C(13) H(132) .96 no
C(21) H(211) .96 no
C(21) H(213) .96 no
C(22) H(222) .96 no
C(23) H(231) .96 no
C(23) H(233) .96 no
C(31) H(312) .96 no
C(32) H(321) .96 no
C(32) H(323) .96 no
C(33) H(332) .96 no
C(41) H(411) .96 no
C(41) H(413) .96 no
C(42) H(422) .96 no
C(43) H(431) .96 no
C(43) H(433) .96 no
C(1) H(12) .96 no
C(2) H(22) .96 no
C(3) H(32) .96 no
C(4) H(42) .96 no
C(5) H(52) .96 no
C(6) H(61) .96 no
C(7) H(71) 1.006(6) no
P(1) C(20) 1.894(3) no
P(1) Li(2) 2.574(5) no
P(2) C(30) 1.888(4) no
P(2) Li(2) 2.466(5) no
C(10) C(13) 1.516(5) no
C(10) C(12) 1.524(4) no
C(20) C(21) 1.525(5) no
C(30) C(32) 1.516(5) no
C(30) C(31) 1.526(5) no
C(40) C(42) 1.517(5) no
Li(1) P(1) 2.564(5) no
Li(1) Li(2) 3.031(7) no
O C(1) 1.387(5) no
C(1) C(2) 1.480(6) no
C(3) C(4) 1.439(7) no
C(6) C(7) 1.398(8) no
C(11) H(111) .96 no
C(11) H(113) .96 no
C(12) H(122) .96 no
C(13) H(131) .96 no
C(13) H(133) .96 no
C(21) H(212) .96 no
C(22) H(221) .96 no
C(22) H(223) .96 no
C(23) H(232) .96 no
C(31) H(311) .96 no
C(31) H(313) .96 no
C(32) H(322) .96 no
C(33) H(331) .96 no
C(33) H(333) .96 no
C(41) H(412) .96 no
C(42) H(421) .96 no
C(42) H(423) .96 no
C(43) H(432) .96 no
C(1) H(11) .96 no
C(2) H(21) .96 no
C(3) H(31) .96 no
C(4) H(41) .96 no
C(5) H(51) .96 no
C(5) H(53) .96 no
C(6) H(62) .96 no
C(7) H(72) .991(6) no