#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:27:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179845 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/41/7014163.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_7014163
loop_
_publ_author_name
'Garcia, Felipe'
'Humphrey, Simon M.'
'Kowenicki, Richard A.'
'McPartlin, Mary'
'Wright, Dominic S.'
_publ_section_title
;
 Selective formation of the [PhP(H)-PPh]- anion in the reaction of
 PhPHLi with MeAlCl(2); synthesis and structure of the unusual tetramer
 [(PhP(H)-PPh)Li.thf]4.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              977
_journal_page_last               979
_journal_paper_doi               10.1039/b402295e
_journal_year                    2004
_chemical_formula_sum            'C64 H76 Li4 O4 P8'
_chemical_formula_weight         1184.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           114
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_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            2
_cell_length_a                   20.0636(6)
_cell_length_b                   20.0636(6)
_cell_length_c                   8.9176(2)
_cell_measurement_reflns_used    6725
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      20.60
_cell_measurement_theta_min      1.02
_cell_volume                     3589.76(17)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7923
_diffrn_reflns_theta_full        20.59
_diffrn_reflns_theta_max         20.59
_diffrn_reflns_theta_min         3.66
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         1801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0570
_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)+(0.1387P)²+3.8370P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1800
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                1679
_reflns_number_total             1801
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402295e.txt
_cod_data_source_block           mw0343
_cod_original_sg_symbol_H-M      P-42(1)c
_cod_database_code               7014163
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, z'
'x+1/2, -y+1/2, -z+1/2'
'-y, x, -z'
'y+1/2, x+1/2, z+1/2'
'y, -x, -z'
'-y+1/2, -x+1/2, z+1/2'
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
P1 P 0.93828(8) 0.89611(8) 0.8790(2) 0.0426(6) Uani 1 1 d . . .
P2 P 0.90215(9) 0.97599(8) 0.7420(2) 0.0437(6) Uani 1 1 d . . .
H2P H 0.9127 0.9550 0.6053 0.07(2) Uiso 1 1 d . . .
Li1 Li 0.9079(5) 0.9360(5) 1.1430(13) 0.047(3) Uani 1 1 d . . .
O1T O 0.8298(2) 0.8932(2) 1.2293(6) 0.0515(13) Uani 1 1 d . . .
C2T C 0.7836(5) 0.9278(4) 1.3156(11) 0.082(3) Uani 1 1 d . . .
H2T1 H 0.7668 0.9665 1.2583 0.098 Uiso 1 1 calc R . .
H2T2 H 0.8055 0.9447 1.4075 0.098 Uiso 1 1 calc R . .
C3T C 0.7291(5) 0.8857(5) 1.3562(16) 0.102(4) Uani 1 1 d . . .
H3T1 H 0.6861 0.9086 1.3378 0.122 Uiso 1 1 calc R . .
H3T2 H 0.7317 0.8734 1.4635 0.122 Uiso 1 1 calc R . .
C4T C 0.7351(4) 0.8253(4) 1.2597(13) 0.079(3) Uani 1 1 d . . .
H4T1 H 0.7247 0.7844 1.3174 0.095 Uiso 1 1 calc R . .
H4T2 H 0.7046 0.8281 1.1726 0.095 Uiso 1 1 calc R . .
C5T C 0.8069(4) 0.8251(3) 1.2092(9) 0.056(2) Uani 1 1 d . . .
H5T1 H 0.8336 0.7940 1.2708 0.067 Uiso 1 1 calc R . .
H5T2 H 0.8103 0.8117 1.1027 0.067 Uiso 1 1 calc R . .
C11 C 0.9024(3) 0.8180(3) 0.8091(8) 0.0375(16) Uani 1 1 d . . .
C12 C 0.8672(3) 0.8100(3) 0.6788(8) 0.0420(18) Uani 1 1 d . . .
H12 H 0.8587 0.8477 0.6172 0.050 Uiso 1 1 calc R . .
C13 C 0.8432(4) 0.7470(3) 0.6342(8) 0.0498(19) Uani 1 1 d . . .
H13 H 0.8190 0.7428 0.5431 0.060 Uiso 1 1 calc R . .
C14 C 0.8545(4) 0.6918(3) 0.7209(8) 0.0522(19) Uani 1 1 d . . .
H14 H 0.8383 0.6494 0.6909 0.063 Uiso 1 1 calc R . .
C15 C 0.8896(4) 0.6991(3) 0.8524(8) 0.0491(18) Uani 1 1 d . . .
H15 H 0.8983 0.6612 0.9132 0.059 Uiso 1 1 calc R . .
C16 C 0.9123(3) 0.7610(3) 0.8968(8) 0.0428(17) Uani 1 1 d . . .
H16 H 0.9353 0.7650 0.9895 0.051 Uiso 1 1 calc R . .
C21 C 0.8109(3) 0.9752(3) 0.7422(7) 0.0417(17) Uani 1 1 d . . .
C22 C 0.7773(4) 1.0208(3) 0.6455(8) 0.0517(18) Uani 1 1 d . . .
H22 H 0.8027 1.0476 0.5788 0.062 Uiso 1 1 calc R . .
C23 C 0.7108(4) 1.0267(4) 0.6464(10) 0.066(2) Uani 1 1 d . . .
H23 H 0.6895 1.0578 0.5817 0.080 Uiso 1 1 calc R . .
C24 C 0.6721(4) 0.9866(4) 0.7442(12) 0.075(3) Uani 1 1 d . . .
H24 H 0.6248 0.9889 0.7428 0.090 Uiso 1 1 calc R . .
C25 C 0.7045(4) 0.9441(4) 0.8413(10) 0.063(2) Uani 1 1 d . . .
H25 H 0.6794 0.9180 0.9099 0.076 Uiso 1 1 calc R . .
C26 C 0.7721(3) 0.9391(3) 0.8399(8) 0.0458(18) Uani 1 1 d . . .
H26 H 0.7932 0.9097 0.9085 0.055 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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
C11 P1 P2 108.2(2) . . ?
C11 P1 Li1 116.3(3) . 5_757 ?
P2 P1 Li1 102.8(3) . 5_757 ?
C11 P1 Li1 119.1(3) . . ?
P2 P1 Li1 102.1(2) . . ?
Li1 P1 Li1 106.2(4) 5_757 . ?
C21 P2 P1 109.4(2) . . ?
C21 P2 Li1 105.3(3) . 7_577 ?
P1 P2 Li1 110.6(3) . 7_577 ?
O1T Li1 P1 113.2(5) . 7_577 ?
O1T Li1 P1 114.7(5) . . ?
P1 Li1 P1 105.1(4) 7_577 . ?
O1T Li1 P2 116.4(5) . 5_757 ?
P1 Li1 P2 111.6(4) 7_577 5_757 ?
P1 Li1 P2 93.8(3) . 5_757 ?
C2T O1T C5T 109.0(6) . . ?
C2T O1T Li1 122.5(6) . . ?
C5T O1T Li1 128.4(5) . . ?
O1T C2T C3T 110.9(7) . . ?
C2T C3T C4T 105.8(8) . . ?
C5T C4T C3T 104.5(7) . . ?
O1T C5T C4T 105.3(6) . . ?
C12 C11 C16 116.8(6) . . ?
C12 C11 P1 126.2(5) . . ?
C16 C11 P1 116.9(5) . . ?
C11 C12 C13 121.4(6) . . ?
C14 C13 C12 120.6(7) . . ?
C15 C14 C13 118.7(6) . . ?
C14 C15 C16 120.6(7) . . ?
C11 C16 C15 121.9(6) . . ?
C26 C21 C22 117.1(6) . . ?
C26 C21 P2 124.8(5) . . ?
C22 C21 P2 117.8(5) . . ?
C23 C22 C21 121.6(8) . . ?
C22 C23 C24 119.9(7) . . ?
C25 C24 C23 118.6(7) . . ?
C24 C25 C26 120.7(8) . . ?
C21 C26 C25 122.1(7) . . ?
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
P1 C11 1.833(6) . ?
P1 P2 2.142(2) . ?
P1 Li1 2.542(10) 5_757 ?
P1 Li1 2.560(11) . ?
P2 C21 1.832(7) . ?
P2 Li1 2.634(11) 7_577 ?
Li1 O1T 1.945(11) . ?
Li1 P1 2.542(10) 7_577 ?
Li1 P2 2.634(11) 5_757 ?
O1T C2T 1.390(9) . ?
O1T C5T 1.453(8) . ?
C2T C3T 1.428(12) . ?
C3T C4T 1.492(13) . ?
C4T C5T 1.509(11) . ?
C11 C12 1.370(10) . ?
C11 C16 1.400(9) . ?
C12 C13 1.410(10) . ?
C13 C14 1.370(10) . ?
C14 C15 1.376(10) . ?
C15 C16 1.381(10) . ?
C21 C26 1.374(10) . ?
C21 C22 1.426(9) . ?
C22 C23 1.341(11) . ?
C23 C24 1.418(11) . ?
C24 C25 1.379(12) . ?
C25 C26 1.360(10) . ?
