#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:18:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178687 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/98/4079840.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_4079840
loop_
_publ_author_name
'Heuclin, Hadrien'
'Fustier-Boutignon, Marie'
'Ho, Samuel Ying-Fu'
'Goff, Xavier-Frédéric Le'
'Carenco, Sophie'
'So, Cheuk-Wai'
'Mézailles, Nicolas'
_publ_section_title
;
 Synthesis of Phosphorus(V)-Stabilized Geminal Dianions. The Cases of
 Mixed P═X/P→ BH3(X = S, O) and
 P═S/SiMe3Derivatives
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              498
_journal_paper_doi               10.1021/om300954a
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C58 H68 B2 Li2 O4 P4'
_chemical_formula_sum            'C58 H68 B2 Li2 O4 P4'
_chemical_formula_weight         988.50
_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                111.622(1)
_cell_angle_beta                 114.649(1)
_cell_angle_gamma                93.327(1)
_cell_formula_units_Z            1
_cell_length_a                   11.184(1)
_cell_length_b                   12.134(1)
_cell_length_c                   12.367(1)
_cell_measurement_reflns_used    5675
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1372.8(2)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega 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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18235
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.9820
_exptl_absorpt_correction_T_min  0.9645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1996)'
_exptl_crystal_colour            Block
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Colorless
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         6217
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0388
_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)+(0.0113P)²+0.9880P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                5401
_reflns_number_total             6217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300954a_si_002.cif
_cod_data_source_block           mf142
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P-1     '
_cod_database_code               4079840
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
P1 P 0.89393(4) 0.26293(3) 0.27436(3) 0.01851(9) Uani 1 1 d .
P2 P 0.65788(4) 0.19836(3) 0.32273(4) 0.02046(9) Uani 1 1 d .
O1 O 0.95855(10) 0.39342(9) 0.38267(10) 0.0220(2) Uani 1 1 d .
O2 O 0.83310(10) 0.59780(10) 0.32299(10) 0.0256(2) Uani 1 1 d .
C1 C 0.72888(14) 0.19982(14) 0.22324(14) 0.0223(3) Uani 1 1 d .
H1 H 0.6701 0.1616 0.1307 0.027 Uiso 1 1 calc R
C2 C 1.01319(15) 0.17633(13) 0.33228(14) 0.0208(3) Uani 1 1 d .
C3 C 1.15011(15) 0.22105(15) 0.37266(15) 0.0268(3) Uani 1 1 d .
H3 H 1.1776 0.2936 0.3673 0.032 Uiso 1 1 calc R
C4 C 1.24611(17) 0.16076(16) 0.42040(17) 0.0330(4) Uani 1 1 d .
H4 H 1.3388 0.1916 0.4471 0.040 Uiso 1 1 calc R
C5 C 1.20673(18) 0.05529(16) 0.42918(16) 0.0326(4) Uani 1 1 d .
H5 H 1.2726 0.0142 0.4626 0.039 Uiso 1 1 calc R
C6 C 1.07209(18) 0.00985(15) 0.38956(16) 0.0305(3) Uani 1 1 d .
H6 H 1.0455 -0.0624 0.3959 0.037 Uiso 1 1 calc R
C7 C 0.97483(16) 0.06963(14) 0.34022(15) 0.0259(3) Uani 1 1 d .
H7 H 0.8820 0.0373 0.3119 0.031 Uiso 1 1 calc R
C8 C 0.89729(14) 0.25141(14) 0.12550(14) 0.0219(3) Uani 1 1 d .
C9 C 0.89337(16) 0.13962(15) 0.03397(15) 0.0293(3) Uani 1 1 d .
H9 H 0.8945 0.0702 0.0524 0.035 Uiso 1 1 calc R
C10 C 0.88789(17) 0.12884(17) -0.08377(16) 0.0356(4) Uani 1 1 d .
H10 H 0.8846 0.0522 -0.1459 0.043 Uiso 1 1 calc R
C11 C 0.88720(17) 0.23000(18) -0.11061(16) 0.0354(4) Uani 1 1 d .
H11 H 0.8829 0.2227 -0.1914 0.042 Uiso 1 1 calc R
C12 C 0.89277(17) 0.34150(17) -0.01995(17) 0.0338(4) Uani 1 1 d .
H12 H 0.8934 0.4110 -0.0381 0.041 Uiso 1 1 calc R
C13 C 0.89753(16) 0.35266(15) 0.09801(16) 0.0274(3) Uani 1 1 d .
H13 H 0.9009 0.4296 0.1598 0.033 Uiso 1 1 calc R
C14 C 0.58647(14) 0.03986(14) 0.28119(14) 0.0232(3) Uani 1 1 d .
C15 C 0.59720(16) -0.05702(15) 0.18423(16) 0.0287(3) Uani 1 1 d .
H15 H 0.6456 -0.0409 0.1420 0.034 Uiso 1 1 calc R
C16 C 0.53771(17) -0.17741(16) 0.14838(18) 0.0361(4) Uani 1 1 d .
H16 H 0.5457 -0.2430 0.0821 0.043 Uiso 1 1 calc R
C17 C 0.46701(17) -0.20160(16) 0.20915(19) 0.0377(4) Uani 1 1 d .
H17 H 0.4266 -0.2838 0.1848 0.045 Uiso 1 1 calc R
C18 C 0.45506(17) -0.10609(17) 0.30550(18) 0.0345(4) Uani 1 1 d .
H18 H 0.4062 -0.1228 0.3471 0.041 Uiso 1 1 calc R
C19 C 0.51423(15) 0.01397(15) 0.34144(16) 0.0279(3) Uani 1 1 d .
H19 H 0.5056 0.0792 0.4076 0.033 Uiso 1 1 calc R
C20 C 0.50103(15) 0.24889(14) 0.26789(15) 0.0235(3) Uani 1 1 d .
C21 C 0.38916(16) 0.17370(16) 0.14613(16) 0.0307(4) Uani 1 1 d .
H21 H 0.3929 0.0945 0.0953 0.037 Uiso 1 1 calc R
C22 C 0.27264(17) 0.21374(18) 0.09876(19) 0.0380(4) Uani 1 1 d .
H22 H 0.1974 0.1621 0.0154 0.046 Uiso 1 1 calc R
C23 C 0.26538(18) 0.32782(19) 0.1719(2) 0.0398(4) Uani 1 1 d .
H23 H 0.1854 0.3549 0.1390 0.048 Uiso 1 1 calc R
C24 C 0.3745(2) 0.40302(18) 0.29337(19) 0.0401(4) Uani 1 1 d .
H24 H 0.3694 0.4817 0.3440 0.048 Uiso 1 1 calc R
C25 C 0.49230(17) 0.36356(16) 0.34169(17) 0.0314(4) Uani 1 1 d .
H25 H 0.5669 0.4153 0.4255 0.038 Uiso 1 1 calc R
C26 C 0.70605(15) 0.53367(15) 0.29952(15) 0.0271(3) Uani 1 1 d .
H26A H 0.6702 0.5919 0.3511 0.033 Uiso 1 1 calc R
H26B H 0.7224 0.4695 0.3315 0.033 Uiso 1 1 calc R
C27 C 0.60058(17) 0.47498(17) 0.15580(17) 0.0360(4) Uani 1 1 d .
H27A H 0.5773 0.5388 0.1257 0.054 Uiso 1 1 calc R
H27B H 0.5189 0.4278 0.1450 0.054 Uiso 1 1 calc R
H27C H 0.6370 0.4203 0.1035 0.054 Uiso 1 1 calc R
C28 C 0.82599(17) 0.70520(15) 0.29919(16) 0.0291(3) Uani 1 1 d .
H28A H 0.8994 0.7756 0.3766 0.035 Uiso 1 1 calc R
H28B H 0.7379 0.7246 0.2875 0.035 Uiso 1 1 calc R
C29 C 0.8400(2) 0.68624(19) 0.17802(19) 0.0439(5) Uani 1 1 d .
H29A H 0.9252 0.6632 0.1877 0.066 Uiso 1 1 calc R
H29B H 0.8406 0.7623 0.1672 0.066 Uiso 1 1 calc R
H29C H 0.7633 0.6209 0.1003 0.066 Uiso 1 1 calc R
B1 B 0.77773(18) 0.29055(18) 0.51042(17) 0.0272(4) Uani 1 1 d .
H1B H 0.8732(18) 0.2570(16) 0.5279(17) 0.033 Uiso 1 1 d .
H2B H 0.7266(18) 0.2712(16) 0.5637(17) 0.033 Uiso 1 1 d .
H3B H 0.7972(18) 0.3928(17) 0.5335(17) 0.033 Uiso 1 1 d .
Li1 Li 0.9982(3) 0.5652(2) 0.4358(2) 0.0262(5) Uani 1 1 d .
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'
B B 0.0013 0.0007 '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'
P P 0.1023 0.0942 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 P1 C1 118.14(7) . .
O1 P1 C8 110.83(6) . .
C1 P1 C8 104.49(7) . .
O1 P1 C2 104.17(6) . .
C1 P1 C2 114.84(7) . .
C8 P1 C2 103.53(7) . .
O1 P1 Li1 32.59(6) . 2_766
C1 P1 Li1 103.84(7) . 2_766
C8 P1 Li1 142.54(7) . 2_766
C2 P1 Li1 86.06(7) . 2_766
C1 P2 C14 109.52(7) . .
C1 P2 C20 107.84(7) . .
C14 P2 C20 99.68(7) . .
C1 P2 B1 115.03(8) . .
C14 P2 B1 111.43(8) . .
C20 P2 B1 112.22(8) . .
P1 O1 Li1 150.29(10) . .
P1 O1 Li1 122.38(10) . 2_766
Li1 O1 Li1 85.77(12) . 2_766
C28 O2 C26 113.99(12) . .
C28 O2 Li1 125.89(12) . .
C26 O2 Li1 116.53(12) . .
P1 C1 P2 126.47(9) . .
P1 C1 H1 116.8 . .
P2 C1 H1 116.8 . .
C7 C2 C3 118.79(14) . .
C7 C2 P1 123.18(11) . .
C3 C2 P1 118.02(11) . .
C4 C3 C2 120.73(15) . .
C4 C3 H3 119.6 . .
C2 C3 H3 119.6 . .
C3 C4 C5 119.88(16) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C6 C5 C4 120.12(15) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C7 120.19(15) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C2 C7 C6 120.28(15) . .
C2 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C13 C8 C9 119.05(14) . .
C13 C8 P1 120.42(12) . .
C9 C8 P1 120.47(12) . .
C10 C9 C8 120.61(16) . .
C10 C9 H9 119.7 . .
C8 C9 H9 119.7 . .
C11 C10 C9 119.89(16) . .
C11 C10 H10 120.1 . .
C9 C10 H10 120.1 . .
C12 C11 C10 119.98(15) . .
C12 C11 H11 120.0 . .
C10 C11 H11 120.0 . .
C11 C12 C13 120.36(16) . .
C11 C12 H12 119.8 . .
C13 C12 H12 119.8 . .
C8 C13 C12 120.10(15) . .
C8 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C19 118.66(14) . .
C15 C14 P2 120.57(12) . .
C19 C14 P2 120.69(12) . .
C14 C15 C16 120.64(16) . .
C14 C15 H15 119.7 . .
C16 C15 H15 119.7 . .
C17 C16 C15 120.04(17) . .
C17 C16 H16 120.0 . .
C15 C16 H16 120.0 . .
C16 C17 C18 119.97(16) . .
C16 C17 H17 120.0 . .
C18 C17 H17 120.0 . .
C17 C18 C19 120.12(16) . .
C17 C18 H18 119.9 . .
C19 C18 H18 119.9 . .
C18 C19 C14 120.56(16) . .
C18 C19 H19 119.7 . .
C14 C19 H19 119.7 . .
C25 C20 C21 118.70(15) . .
C25 C20 P2 121.56(12) . .
C21 C20 P2 119.66(12) . .
C22 C21 C20 120.55(17) . .
C22 C21 H21 119.7 . .
C20 C21 H21 119.7 . .
C23 C22 C21 120.35(17) . .
C23 C22 H22 119.8 . .
C21 C22 H22 119.8 . .
C22 C23 C24 119.95(16) . .
C22 C23 H23 120.0 . .
C24 C23 H23 120.0 . .
C23 C24 C25 120.10(17) . .
C23 C24 H24 120.0 . .
C25 C24 H24 120.0 . .
C20 C25 C24 120.36(16) . .
C20 C25 H25 119.8 . .
C24 C25 H25 119.8 . .
O2 C26 C27 113.11(13) . .
O2 C26 H26A 109.0 . .
C27 C26 H26A 109.0 . .
O2 C26 H26B 109.0 . .
C27 C26 H26B 109.0 . .
H26A C26 H26B 107.8 . .
C26 C27 H27A 109.5 . .
C26 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
C26 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
O2 C28 C29 111.12(14) . .
O2 C28 H28A 109.4 . .
C29 C28 H28A 109.4 . .
O2 C28 H28B 109.4 . .
C29 C28 H28B 109.4 . .
H28A C28 H28B 108.0 . .
C28 C29 H29A 109.5 . .
C28 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C28 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
P2 B1 Li1 112.83(10) . 2_766
P2 B1 H1B 104.4(9) . .
Li1 B1 H1B 60.0(9) 2_766 .
P2 B1 H2B 108.2(9) . .
Li1 B1 H2B 138.8(9) 2_766 .
H1B B1 H2B 113.3(13) . .
P2 B1 H3B 107.8(9) . .
Li1 B1 H3B 52.5(9) 2_766 .
H1B B1 H3B 112.0(13) . .
H2B B1 H3B 110.8(13) . .
O1 Li1 O1 94.23(12) . 2_766
O1 Li1 O2 106.23(13) . .
O1 Li1 O2 118.93(14) 2_766 .
O1 Li1 Li1 47.74(9) . 2_766
O1 Li1 Li1 46.49(9) 2_766 2_766
O2 Li1 Li1 124.21(18) . 2_766
O1 Li1 B1 128.02(14) . 2_766
O1 Li1 B1 96.57(11) 2_766 2_766
O2 Li1 B1 112.10(12) . 2_766
Li1 Li1 B1 122.20(16) 2_766 2_766
O1 Li1 P1 118.82(11) . 2_766
O1 Li1 P1 25.03(5) 2_766 2_766
O2 Li1 P1 111.57(11) . 2_766
Li1 Li1 P1 71.22(11) 2_766 2_766
B1 Li1 P1 77.61(8) 2_766 2_766
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.5232(10) .
P1 C1 1.7027(15) .
P1 C8 1.8107(15) .
P1 C2 1.8212(15) .
P1 Li1 3.041(3) 2_766
P2 C1 1.7246(15) .
P2 C14 1.8308(16) .
P2 C20 1.8308(15) .
P2 B1 1.9373(18) .
O1 Li1 1.900(3) .
O1 Li1 1.940(3) 2_766
O2 C28 1.4375(18) .
O2 C26 1.4388(18) .
O2 Li1 1.963(3) .
C1 H1 0.9500 .
C2 C7 1.391(2) .
C2 C3 1.398(2) .
C3 C4 1.385(2) .
C3 H3 0.9500 .
C4 C5 1.386(2) .
C4 H4 0.9500 .
C5 C6 1.379(2) .
C5 H5 0.9500 .
C6 C7 1.395(2) .
C6 H6 0.9500 .
C7 H7 0.9500 .
C8 C13 1.390(2) .
C8 C9 1.394(2) .
C9 C10 1.388(2) .
C9 H9 0.9500 .
C10 C11 1.384(3) .
C10 H10 0.9500 .
C11 C12 1.380(3) .
C11 H11 0.9500 .
C12 C13 1.392(2) .
C12 H12 0.9500 .
C13 H13 0.9500 .
C14 C15 1.390(2) .
C14 C19 1.397(2) .
C15 C16 1.392(2) .
C15 H15 0.9500 .
C16 C17 1.381(3) .
C16 H16 0.9500 .
C17 C18 1.384(3) .
C17 H17 0.9500 .
C18 C19 1.387(2) .
C18 H18 0.9500 .
C19 H19 0.9500 .
C20 C25 1.390(2) .
C20 C21 1.396(2) .
C21 C22 1.387(2) .
C21 H21 0.9500 .
C22 C23 1.376(3) .
C22 H22 0.9500 .
C23 C24 1.382(3) .
C23 H23 0.9500 .
C24 C25 1.396(2) .
C24 H24 0.9500 .
C25 H25 0.9500 .
C26 C27 1.509(2) .
C26 H26A 0.9900 .
C26 H26B 0.9900 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
C28 C29 1.506(2) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C29 H29A 0.9800 .
C29 H29B 0.9800 .
C29 H29C 0.9800 .
B1 Li1 2.651(3) 2_766
B1 H1B 1.129(18) .
B1 H2B 1.109(18) .
B1 H3B 1.151(18) .
Li1 O1 1.940(3) 2_766
Li1 Li1 2.614(5) 2_766
Li1 B1 2.651(3) 2_766
Li1 P1 3.041(3) 2_766
