#------------------------------------------------------------------------------
#$Date: 2016-03-21 06:07:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178491 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/02/4060263.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_4060263
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/om034268l
_journal_year                    2004
_chemical_formula_sum            'C29 H68 B12 Li N O6 P Y'
_chemical_formula_weight         783.38
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 130.7080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.6463(15)
_cell_length_b                   21.4575(12)
_cell_length_c                   20.0659(10)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     9349.7(9)
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'CCD area detector'
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.1175
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25121
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         ?
_exptl_absorpt_coefficient_mu    1.316
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7553
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.18
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.849
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8243
_refine_ls_number_restraints     81
_refine_ls_restrained_S_all      0.859
_refine_ls_R_factor_all          0.1336
_refine_ls_R_factor_gt           0.0556
_refine_ls_shift/su_max          0.066
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0727P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1316
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                3592
_reflns_number_total             8243
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4060263
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
Y1 Y 0.174454(7) 0.124834(9) 0.075741(10) 0.06480(6) Uani 1 1 d . . .
P1 P 0.210121(16) 0.27335(2) 0.20672(2) 0.05512(16) Uani 1 1 d . . .
N1 N 0.25193(5) 0.33761(6) 0.23449(7) 0.0635(5) Uani 1 1 d . . .
C1 C 0.26552(6) 0.20933(8) 0.28268(8) 0.0523(6) Uani 1 1 d . . .
C2 C 0.25426(6) 0.13834(7) 0.23719(9) 0.0561(6) Uani 1 1 d . . .
C3 C 0.29559(7) 0.34934(9) 0.22063(10) 0.0783(7) Uani 1 1 d . . .
H3A H 0.3066 0.3087 0.2121 0.094 Uiso 1 1 calc R . .
C4 C 0.26647(8) 0.38757(10) 0.13685(11) 0.1055(9) Uani 1 1 d . . .
H4A H 0.2295 0.3674 0.0875 0.158 Uiso 1 1 calc R . .
H4B H 0.2950 0.3906 0.1270 0.158 Uiso 1 1 calc R . .
H4C H 0.2568 0.4286 0.1437 0.158 Uiso 1 1 calc R . .
C5 C 0.35585(7) 0.37987(10) 0.30088(13) 0.1089(10) Uani 1 1 d . . .
H5A H 0.3737 0.3549 0.3522 0.163 Uiso 1 1 calc R . .
H5B H 0.3472 0.4208 0.3098 0.163 Uiso 1 1 calc R . .
H5C H 0.3842 0.3830 0.2907 0.163 Uiso 1 1 calc R . .
C6 C 0.23145(7) 0.39259(9) 0.25500(11) 0.0866(8) Uani 1 1 d . . .
H6A H 0.2571 0.4277 0.2646 0.104 Uiso 1 1 calc R . .
C7 C 0.16531(8) 0.41099(11) 0.17934(14) 0.1283(12) Uani 1 1 d . . .
H7A H 0.1600 0.4174 0.1274 0.193 Uiso 1 1 calc R . .
H7B H 0.1558 0.4488 0.1938 0.193 Uiso 1 1 calc R . .
H7C H 0.1382 0.3784 0.1689 0.193 Uiso 1 1 calc R . .
C8 C 0.24390(9) 0.38334(10) 0.34004(12) 0.1272(11) Uani 1 1 d . . .
H8A H 0.2864 0.3726 0.3860 0.191 Uiso 1 1 calc R . .
H8B H 0.2183 0.3503 0.3329 0.191 Uiso 1 1 calc R . .
H8C H 0.2349 0.4212 0.3552 0.191 Uiso 1 1 calc R . .
C11 C 0.18426(6) 0.24629(8) 0.10177(8) 0.0522(6) Uani 1 1 d . . .
C12 C 0.21434(6) 0.23235(8) 0.06861(9) 0.0631(6) Uani 1 1 d . . .
H12A H 0.2577 0.2416 0.0998 0.076 Uiso 1 1 calc R . .
C13 C 0.17235(6) 0.21378(9) -0.01849(9) 0.0703(7) Uani 1 1 d . . .
H13A H 0.1813 0.2080 -0.0577 0.084 Uiso 1 1 calc R . .
C14 C 0.05310(8) 0.20281(11) -0.12607(11) 0.0991(10) Uani 1 1 d . . .
H14A H 0.0480 0.1874 -0.1738 0.119 Uiso 1 1 calc R . .
C15 C 0.00414(9) 0.21293(12) -0.13211(12) 0.1122(11) Uani 1 1 d . . .
H15A H -0.0351 0.2047 -0.1850 0.135 Uiso 1 1 calc R . .
C16 C 0.01057(7) 0.23558(11) -0.06089(11) 0.1009(10) Uani 1 1 d . . .
H16A H -0.0245 0.2423 -0.0680 0.121 Uiso 1 1 calc R . .
C17 C 0.06658(6) 0.24788(9) 0.01793(10) 0.0784(8) Uani 1 1 d . . .
H17A H 0.0699 0.2625 0.0645 0.094 Uiso 1 1 calc R . .
C18 C 0.11980(6) 0.23832(8) 0.02850(9) 0.0601(7) Uani 1 1 d . . .
C19 C 0.11312(7) 0.21622(9) -0.04489(9) 0.0703(7) Uani 1 1 d . . .
C21 C 0.47613(8) 0.00082(13) 0.37878(12) 0.1578(13) Uani 1 1 d D . .
H21A H 0.4857 0.0139 0.4323 0.237 Uiso 1 1 calc R . .
H21B H 0.4902 -0.0412 0.3853 0.237 Uiso 1 1 calc R . .
H21C H 0.4324 0.0027 0.3313 0.237 Uiso 1 1 calc R . .
C22 C 0.54560(10) 0.08062(14) 0.42349(13) 0.1536(15) Uani 1 1 d D . .
H22A H 0.5749 0.0585 0.4786 0.184 Uiso 1 1 calc R . .
H22B H 0.5239 0.1103 0.4312 0.184 Uiso 1 1 calc R . .
C23 C 0.58102(12) 0.11649(17) 0.40118(16) 0.214(2) Uani 1 1 d D . .
H23A H 0.5718 0.1605 0.3977 0.257 Uiso 1 1 calc R . .
H23B H 0.6247 0.1114 0.4503 0.257 Uiso 1 1 calc R . .
C24 C 0.59575(9) 0.14104(13) 0.30573(14) 0.1544(14) Uani 1 1 d D . .
H24A H 0.6263 0.1659 0.3563 0.232 Uiso 1 1 calc R . .
H24B H 0.5643 0.1677 0.2586 0.232 Uiso 1 1 calc R . .
H24C H 0.6147 0.1181 0.2878 0.232 Uiso 1 1 calc R . .
C25 C 0.62473(9) -0.0384(2) 0.36844(15) 0.248(2) Uani 1 1 d D . .
H25A H 0.6437 -0.0775 0.3751 0.371 Uiso 1 1 calc R . .
H25B H 0.6288 -0.0309 0.4192 0.371 Uiso 1 1 calc R . .
H25C H 0.6445 -0.0055 0.3626 0.371 Uiso 1 1 calc R . .
C27 C 0.4179(2) 0.4099(3) 0.5585(3) 0.480(5) Uani 1 1 d D . .
H27A H 0.4029 0.3946 0.5026 0.720 Uiso 1 1 calc R . .
H27B H 0.4363 0.4501 0.5693 0.720 Uiso 1 1 calc R . .
H27C H 0.3843 0.4133 0.5581 0.720 Uiso 1 1 calc R . .
C28 C 0.49009(16) 0.3396(3) 0.6013(2) 0.524(3) Uani 1 1 d D . .
H28A H 0.5129 0.3685 0.5947 0.629 Uiso 1 1 calc R . .
H28B H 0.4613 0.3165 0.5471 0.629 Uiso 1 1 calc R . .
C29 C 0.54148(13) 0.2877(2) 0.69388(18) 0.315(2) Uani 1 1 d D . .
H29A H 0.5191 0.2504 0.6856 0.378 Uiso 1 1 calc R . .
H29B H 0.5749 0.2754 0.6957 0.378 Uiso 1 1 calc R . .
C30 C 0.61255(14) 0.2902(2) 0.8532(2) 0.308(3) Uani 1 1 d D . .
H30A H 0.6358 0.2606 0.8493 0.463 Uiso 1 1 calc R . .
H30B H 0.5957 0.2701 0.8762 0.463 Uiso 1 1 calc R . .
H30C H 0.6390 0.3237 0.8916 0.463 Uiso 1 1 calc R . .
C31 C 0.60955(8) 0.45884(17) 0.78486(17) 0.2434(17) Uani 1 1 d D . .
H31A H 0.6242 0.5008 0.7940 0.365 Uiso 1 1 calc R . .
H31B H 0.6015 0.4418 0.7340 0.365 Uiso 1 1 calc R . .
H31C H 0.6402 0.4341 0.8355 0.365 Uiso 1 1 calc R . .
C32 C 0.52828(10) 0.51639(15) 0.7505(2) 0.248(2) Uani 1 1 d D . .
H32A H 0.5134 0.5285 0.6930 0.297 Uiso 1 1 calc R . .
H32B H 0.5585 0.5470 0.7927 0.297 Uiso 1 1 calc R . .
B3 B 0.22674(8) 0.15328(10) 0.28995(11) 0.0666(8) Uani 1 1 d . . .
H3 H 0.1772 0.1556 0.2551 0.080 Uiso 1 1 calc R . .
B4 B 0.28019(9) 0.20218(11) 0.37887(12) 0.0761(9) Uani 1 1 d . . .
H4 H 0.2656 0.2364 0.4030 0.091 Uiso 1 1 calc R . .
B5 B 0.33876(9) 0.21919(12) 0.37658(12) 0.0785(10) Uani 1 1 d . . .
H5 H 0.3628 0.2643 0.3996 0.094 Uiso 1 1 calc R . .
B6 B 0.32100(8) 0.17916(10) 0.28462(12) 0.0666(8) Uani 1 1 d . . .
H6 H 0.3329 0.1982 0.2465 0.080 Uiso 1 1 calc R . .
B7 B 0.26438(9) 0.08241(11) 0.30609(12) 0.0790(10) Uani 1 1 d . . .
H7 H 0.2397 0.0376 0.2827 0.095 Uiso 1 1 calc R . .
B8 B 0.28109(9) 0.12219(12) 0.39714(12) 0.0840(9) Uani 1 1 d . . .
H8 H 0.2675 0.1038 0.4335 0.101 Uiso 1 1 calc R . .
B9 B 0.35109(10) 0.16225(12) 0.45035(14) 0.0937(12) Uani 1 1 d . . .
H9 H 0.3837 0.1698 0.5219 0.112 Uiso 1 1 calc R . .
B10 B 0.37642(10) 0.14780(12) 0.39103(15) 0.0915(12) Uani 1 1 d . . .
H10 H 0.4255 0.1462 0.4234 0.110 Uiso 1 1 calc R . .
B11 B 0.32256(9) 0.09853(11) 0.30340(13) 0.0795(10) Uani 1 1 d . . .
H11 H 0.3363 0.0643 0.2782 0.095 Uiso 1 1 calc R . .
B12 B 0.34109(10) 0.08817(13) 0.40459(14) 0.0918(11) Uani 1 1 d . . .
H12 H 0.3671 0.0474 0.4464 0.110 Uiso 1 1 calc R . .
B13 B 0.22174(11) 0.05161(14) 0.03858(15) 0.1126(12) Uani 1 1 d . . .
B14 B 0.08731(10) 0.07042(15) 0.05142(17) 0.1226(13) Uani 1 1 d . . .
O1 O 0.50520(6) 0.03993(8) 0.36068(7) 0.1271(7) Uani 1 1 d D . .
O2 O 0.57035(5) 0.10087(8) 0.32613(8) 0.1189(7) Uani 1 1 d D . .
O3 O 0.56403(6) -0.04040(8) 0.29540(9) 0.1268(8) Uani 1 1 d D . .
O4 O 0.46123(10) 0.36936(13) 0.62369(12) 0.2309(14) Uani 1 1 d D . .
O5 O 0.56479(8) 0.31392(13) 0.76984(11) 0.2459(12) Uani 1 1 d D . .
O6 O 0.55626(7) 0.45859(9) 0.77212(12) 0.1863(10) Uani 1 1 d D . .
Li1 Li 0.5000 0.0336(2) 0.2500 0.0724(17) Uani 1 2 d S . .
Li2 Li 0.5000 0.3829(3) 0.7500 0.098(2) Uani 1 2 d S . .
C26 C 0.54138(17) -0.09751(16) 0.2934(3) 0.310(4) Uani 1 1 d D . .
H26A H 0.5521 -0.1056 0.3494 0.372 Uiso 1 1 calc R . .
H26B H 0.5594 -0.1300 0.2828 0.372 Uiso 1 1 calc R . .
H13B H 0.2171(7) 0.0304(11) 0.0824(11) 0.162(9) Uiso 1 1 d . . .
H13C H 0.1729(6) 0.0714(10) -0.0136(9) 0.127(7) Uiso 1 1 d . . .
H14B H 0.1206(7) 0.1071(10) 0.0845(11) 0.144(8) Uiso 1 1 d . . .
H14C H 0.0842(7) 0.0773(10) -0.0086(10) 0.140(8) Uiso 1 1 d . . .
H13D H 0.2517(7) 0.0928(11) 0.0763(10) 0.142(8) Uiso 1 1 d . . .
H14D H 0.1252(6) 0.0417(9) 0.0826(9) 0.113(7) Uiso 1 1 d . . .
H13E H 0.2412(6) 0.0191(9) 0.0182(9) 0.124(7) Uiso 1 1 d . . .
H14E H 0.0525(6) 0.0441(9) 0.0365(9) 0.113(7) Uiso 1 1 d . . .
