#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:07:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178491 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060253.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_4060253
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om034268l
_journal_year                    2004
_chemical_formula_sum            'C29 H61 B10 Li N O6 P'
_chemical_formula_weight         665.80
_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
_cell_angle_alpha                70.59(3)
_cell_angle_beta                 69.87(3)
_cell_angle_gamma                86.51(3)
_cell_formula_units_Z            2
_cell_length_a                   11.352(2)
_cell_length_b                   13.204(3)
_cell_length_c                   15.634(3)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     2071.4(7)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'ω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3902
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8532
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.35
_refine_ls_extinction_coef       0.029(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         3902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0908
_refine_ls_shift/su_max          0.127
_refine_ls_shift/su_mean         0.022
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1869P)²+0.1611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2465
_refine_ls_wR_factor_ref         0.2596
_reflns_number_gt                3425
_reflns_number_total             3902
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4060253
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
P1 P -0.10734(5) 0.18103(4) -0.28322(4) 0.07488(17) Uani 1 1 d . . .
N1 N 0.02907(16) 0.24339(12) -0.36736(11) 0.0839(6) Uani 1 1 d . . .
Li1 Li 0.3085(3) -0.2594(3) -0.1402(3) 0.0943(12) Uani 1 1 d . . .
O1 O 0.16632(17) -0.15793(14) -0.11111(15) 0.1342(8) Uani 1 1 d . . .
O2 O 0.1785(2) -0.35883(13) -0.00172(14) 0.1402(9) Uani 1 1 d . . .
O3 O 0.42202(16) -0.21684(13) -0.07634(11) 0.1140(6) Uani 1 1 d . . .
O4 O 0.42826(18) -0.13858(17) -0.26073(13) 0.1372(8) Uani 1 1 d . . .
O5 O 0.2335(2) -0.31689(18) -0.22410(15) 0.1785(9) Uani 1 1 d . . .
O6 O 0.4204(2) -0.39269(16) -0.16283(16) 0.1665(10) Uani 1 1 d . . .
C1 C -0.23206(19) 0.24252(14) -0.34067(13) 0.0756(6) Uani 1 1 d . . .
C2 C -0.3241(2) 0.16433(16) -0.35735(15) 0.0885(7) Uani 1 1 d . . .
H2 H -0.3034 0.0794 -0.3463 0.106 Uiso 1 1 calc R . .
B3 B -0.2258(3) 0.2581(2) -0.45597(18) 0.1014(10) Uani 1 1 d . . .
H3 H -0.1431 0.2411 -0.5106 0.122 Uiso 1 1 calc R . .
B4 B -0.2255(3) 0.3694(2) -0.41847(18) 0.0918(10) Uani 1 1 d . . .
H4 H -0.1426 0.4259 -0.4484 0.110 Uiso 1 1 calc R . .
B5 B -0.3226(2) 0.33550(18) -0.29722(18) 0.0835(9) Uani 1 1 d . . .
H5 H -0.3031 0.3704 -0.2483 0.100 Uiso 1 1 calc R . .
B6 B -0.3813(2) 0.20033(18) -0.25798(18) 0.0816(8) Uani 1 1 d . . .
H6 H -0.3995 0.1454 -0.1837 0.098 Uiso 1 1 calc R . .
B7 B -0.3807(3) 0.2274(3) -0.4472(2) 0.1201(12) Uani 1 1 d . . .
H7 H -0.3986 0.1905 -0.4954 0.144 Uiso 1 1 calc R . .
B8 B -0.3221(3) 0.3637(3) -0.4861(2) 0.1122(12) Uani 1 1 d . . .
H8 H -0.3024 0.4174 -0.5610 0.135 Uiso 1 1 calc R . .
B9 B -0.3831(3) 0.4117(2) -0.3879(2) 0.1016(11) Uani 1 1 d . . .
H9 H -0.4036 0.4966 -0.3986 0.122 Uiso 1 1 calc R . .
B10 B -0.4792(3) 0.3065(2) -0.2870(2) 0.1012(11) Uani 1 1 d . . .
H10 H -0.5617 0.3222 -0.2314 0.121 Uiso 1 1 calc R . .
B11 B -0.4755(3) 0.1950(2) -0.3258(2) 0.1002(10) Uani 1 1 d . . .
H11 H -0.5564 0.1363 -0.2952 0.120 Uiso 1 1 calc R . .
C11 C -0.11788(19) 0.04523(15) -0.27611(14) 0.0829(7) Uani 1 1 d . . .
B12 B -0.4790(3) 0.3239(2) -0.4048(2) 0.1132(12) Uani 1 1 d . . .
H12B H -0.5613 0.3511 -0.4262 0.136 Uiso 1 1 calc R . .
C12 C -0.0917(2) -0.00742(16) -0.34691(16) 0.0966(8) Uani 1 1 d . . .
H12A H -0.0611 0.0264 -0.4135 0.116 Uiso 1 1 calc R . .
C13 C -0.1192(2) -0.11643(16) -0.29998(19) 0.1129(10) Uani 1 1 d . . .
H13 H -0.1088 -0.1680 -0.3301 0.136 Uiso 1 1 calc R . .
C14 C -0.2074(2) -0.23229(19) -0.1205(2) 0.1193(11) Uani 1 1 d . . .
H14 H -0.2064 -0.2984 -0.1298 0.143 Uiso 1 1 calc R . .
C15 C -0.2499(2) -0.2266(2) -0.0297(2) 0.1332(12) Uani 1 1 d . . .
H15 H -0.2779 -0.2897 0.0226 0.160 Uiso 1 1 calc R . .
C16 C -0.2528(2) -0.1289(2) -0.01230(19) 0.1095(10) Uani 1 1 d . . .
H16 H -0.2829 -0.1275 0.0506 0.131 Uiso 1 1 calc R . .
C17 C -0.21119(19) -0.03570(18) -0.08846(15) 0.0865(7) Uani 1 1 d . . .
H17 H -0.2135 0.0294 -0.0772 0.104 Uiso 1 1 calc R . .
C18 C -0.16515(17) -0.03741(15) -0.18306(15) 0.0806(7) Uani 1 1 d . . .
C19 C -0.1651(2) -0.13739(17) -0.20025(18) 0.0972(9) Uani 1 1 d . . .
C21 C 0.2048(3) 0.1478(2) -0.4487(2) 0.1410(13) Uani 1 1 d . . .
H21A H 0.2351 0.1228 -0.5031 0.211 Uiso 1 1 calc R . .
H21B H 0.1760 0.0873 -0.3902 0.211 Uiso 1 1 calc R . .
H21C H 0.2715 0.1879 -0.4474 0.211 Uiso 1 1 calc R . .
C22 C 0.0970(2) 0.21940(17) -0.45729(15) 0.0945(8) Uani 1 1 d . . .
H22 H 0.0367 0.1787 -0.4675 0.113 Uiso 1 1 calc R . .
C23 C 0.1389(3) 0.3212(2) -0.54548(18) 0.1303(11) Uani 1 1 d . . .
H23A H 0.1763 0.3018 -0.6026 0.195 Uiso 1 1 calc R . .
H23B H 0.1994 0.3633 -0.5390 0.195 Uiso 1 1 calc R . .
H23C H 0.0674 0.3625 -0.5502 0.195 Uiso 1 1 calc R . .
C31 C 0.0313(2) 0.40389(17) -0.31923(17) 0.1098(9) Uani 1 1 d . . .
H31A H 0.0823 0.4470 -0.3050 0.165 Uiso 1 1 calc R . .
H31B H -0.0454 0.3791 -0.2652 0.165 Uiso 1 1 calc R . .
H31C H 0.0120 0.4462 -0.3754 0.165 Uiso 1 1 calc R . .
C32 C 0.1016(2) 0.30863(18) -0.33810(16) 0.0982(8) Uani 1 1 d . . .
H32 H 0.1786 0.3376 -0.3936 0.118 Uiso 1 1 calc R . .
C33 C 0.1425(2) 0.2409(2) -0.25521(17) 0.1164(10) Uani 1 1 d . . .
H33A H 0.1920 0.2852 -0.2409 0.175 Uiso 1 1 calc R . .
H33B H 0.1917 0.1845 -0.2728 0.175 Uiso 1 1 calc R . .
H33C H 0.0696 0.2099 -0.1993 0.175 Uiso 1 1 calc R . .
C41 C 0.1673(4) -0.4674(2) 0.0468(3) 0.1741(19) Uani 1 1 d . . .
H41A H 0.1425 -0.5045 0.0117 0.261 Uiso 1 1 calc R . .
H41B H 0.1050 -0.4824 0.1100 0.261 Uiso 1 1 calc R . .
H41C H 0.2466 -0.4913 0.0526 0.261 Uiso 1 1 calc R . .
C42 C 0.0607(3) -0.3128(3) 0.0219(3) 0.1668(18) Uani 1 1 d . . .
H42A H 0.0242 -0.3316 0.0916 0.200 Uiso 1 1 calc R . .
H42B H 0.0048 -0.3434 0.0007 0.200 Uiso 1 1 calc R . .
C43 C 0.0690(3) -0.1951(2) -0.0220(2) 0.1414(13) Uani 1 1 d . . .
H43A H -0.0101 -0.1722 -0.0308 0.170 Uiso 1 1 calc R . .
H43B H 0.0821 -0.1629 0.0217 0.170 Uiso 1 1 calc R . .
C44 C 0.1627(3) -0.0474(2) -0.1557(3) 0.1728(18) Uani 1 1 d . . .
H44A H 0.1946 -0.0305 -0.2246 0.259 Uiso 1 1 calc R . .
H44B H 0.2135 -0.0089 -0.1373 0.259 Uiso 1 1 calc R . .
H44C H 0.0776 -0.0269 -0.1359 0.259 Uiso 1 1 calc R . .
C51 C 0.3882(3) -0.2417(3) 0.02533(18) 0.1524(13) Uani 1 1 d . . .
H51A H 0.4615 -0.2600 0.0434 0.229 Uiso 1 1 calc R . .
H51B H 0.3270 -0.3015 0.0583 0.229 Uiso 1 1 calc R . .
H51C H 0.3532 -0.1804 0.0429 0.229 Uiso 1 1 calc R . .
C52 C 0.5367(3) -0.1204(3) -0.2370(3) 0.1599(16) Uani 1 1 d . . .
H52A H 0.5802 -0.0517 -0.2805 0.192 Uiso 1 1 calc R . .
H52B H 0.5948 -0.1765 -0.2442 0.192 Uiso 1 1 calc R . .
C53 C 0.4914(3) -0.1208(2) -0.1316(2) 0.1427(12) Uani 1 1 d . . .
H53A H 0.5625 -0.1160 -0.1119 0.171 Uiso 1 1 calc R . .
H53B H 0.4400 -0.0605 -0.1250 0.171 Uiso 1 1 calc R . .
C54 C 0.4612(4) -0.1167(4) -0.3581(2) 0.199(2) Uani 1 1 d . . .
H54A H 0.3867 -0.1116 -0.3748 0.299 Uiso 1 1 calc R . .
H54B H 0.5094 -0.1733 -0.3761 0.299 Uiso 1 1 calc R . .
H54C H 0.5107 -0.0497 -0.3918 0.299 Uiso 1 1 calc R . .
C61 C 0.5391(4) -0.4167(3) -0.1518(4) 0.257(3) Uani 1 1 d . . .
H61A H 0.5489 -0.4926 -0.1371 0.385 Uiso 1 1 calc R . .
H61B H 0.5439 -0.3951 -0.1001 0.385 Uiso 1 1 calc R . .
H61C H 0.6047 -0.3785 -0.2106 0.385 Uiso 1 1 calc R . .
C62 C 0.3942(5) -0.4333(3) -0.2247(3) 0.258(3) Uani 1 1 d . . .
H62A H 0.4019 -0.5105 -0.2040 0.310 Uiso 1 1 calc R . .
H62B H 0.4560 -0.4027 -0.2888 0.310 Uiso 1 1 calc R . .
C63 C 0.2687(5) -0.4114(3) -0.2299(3) 0.256(2) Uani 1 1 d . . .
H63A H 0.2674 -0.4156 -0.2903 0.307 Uiso 1 1 calc R . .
H63B H 0.2088 -0.4665 -0.1777 0.307 Uiso 1 1 calc R . .
C64 C 0.1257(3) -0.2787(4) -0.2514(3) 0.234(2) Uani 1 1 d . . .
H64A H 0.1531 -0.2355 -0.3185 0.350 Uiso 1 1 calc R . .
H64B H 0.0793 -0.2362 -0.2131 0.350 Uiso 1 1 calc R . .
H64C H 0.0729 -0.3390 -0.2407 0.350 Uiso 1 1 calc R . .
