# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


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# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_FO4582
_database_code_depnum_ccdc_archive 'CCDC 900418'
#TrackingRef 'chemcom.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C37 H59 B2 K N4 P2'
_chemical_formula_sum            'C37 H59 B2 K N4 P2'
_chemical_formula_weight         682.54

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'
N N 0.0061 0.0033 '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'
K K 0.2009 0.2494 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.1261(2)
_cell_length_b                   11.4604(4)
_cell_length_c                   18.7902(8)
_cell_angle_alpha                87.101(2)
_cell_angle_beta                 89.417(2)
_cell_angle_gamma                70.312(2)
_cell_volume                     2050.43(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12653
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         27.57
_reflns_number_total             9136
_reflns_number_gt                7613
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+5.9574P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9133
_refine_ls_number_parameters     455
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0836
_refine_ls_wR_factor_ref         0.1762
_refine_ls_wR_factor_gt          0.1640
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
K1 K 0.32490(8) 0.94660(7) 0.26526(4) 0.02451(17) Uani 1 1 d . . .
P1 P 0.18924(9) 0.57944(8) 0.24773(5) 0.02010(19) Uani 1 1 d . . .
P2 P 0.45650(9) 0.34355(8) 0.26730(5) 0.01949(18) Uani 1 1 d . . .
B1 B 0.2907(5) 0.6905(4) 0.2222(3) 0.0302(9) Uani 1 1 d . A .
H1B1 H 0.356(4) 0.654(4) 0.172(2) 0.039(12) Uiso 1 1 d . . .
H2B1 H 0.353(5) 0.691(4) 0.268(3) 0.044(13) Uiso 1 1 d . . .
H3B1 H 0.208(4) 0.782(4) 0.212(2) 0.036(11) Uiso 1 1 d . . .
B2 B 0.4928(5) 0.1778(4) 0.3100(2) 0.0273(9) Uani 1 1 d . A .
H1B2 H 0.604(4) 0.127(4) 0.313(2) 0.036(11) Uiso 1 1 d . . .
H2B2 H 0.449(4) 0.195(4) 0.367(2) 0.040(12) Uiso 1 1 d . . .
H3B2 H 0.432(5) 0.137(4) 0.274(3) 0.049(13) Uiso 1 1 d . . .
N1 N 0.5341(3) 0.9157(3) 0.15727(17) 0.0302(7) Uani 1 1 d . A .
N2 N 0.2229(3) 1.0621(3) 0.12797(16) 0.0299(7) Uani 1 1 d . A .
N3 N 0.0816(3) 1.0965(3) 0.34922(16) 0.0251(6) Uani 1 1 d . A .
N4 N 0.3466(3) 0.8895(3) 0.41288(16) 0.0263(6) Uani 1 1 d . A .
C1 C 0.2804(3) 0.4264(3) 0.27018(19) 0.0215(7) Uani 1 1 d . A .
H1A H 0.2238 0.3796 0.2871 0.026 Uiso 1 1 calc R . .
C2 C 0.0647(4) 0.5876(3) 0.17596(19) 0.0239(7) Uani 1 1 d . A .
C3 C -0.0215(4) 0.5149(4) 0.1803(2) 0.0338(9) Uani 1 1 d . . .
H3A H -0.0208 0.4651 0.2223 0.041 Uiso 1 1 calc R A .
C4 C -0.1081(4) 0.5147(4) 0.1237(3) 0.0412(10) Uani 1 1 d . A .
H4A H -0.1658 0.4643 0.1272 0.049 Uiso 1 1 calc R . .
C5 C -0.1110(5) 0.5868(5) 0.0627(2) 0.0461(11) Uani 1 1 d . . .
H5A H -0.1711 0.5868 0.0242 0.055 Uiso 1 1 calc R A .
C6 C -0.0271(5) 0.6586(5) 0.0576(2) 0.0533(13) Uani 1 1 d . A .
H6A H -0.0282 0.7080 0.0152 0.064 Uiso 1 1 calc R . .
C7 C 0.0598(5) 0.6595(4) 0.1143(2) 0.0395(10) Uani 1 1 d . . .
H7A H 0.1169 0.7105 0.1105 0.047 Uiso 1 1 calc R A .
C8 C 0.0718(4) 0.6433(3) 0.32133(19) 0.0225(7) Uani 1 1 d . A .
C9 C 0.1005(4) 0.5875(3) 0.39007(19) 0.0270(7) Uani 1 1 d . . .
H9A H 0.1783 0.5135 0.3981 0.032 Uiso 1 1 calc R A .
C10 C 0.0150(4) 0.6404(4) 0.4468(2) 0.0327(8) Uani 1 1 d . A .
H10A H 0.0355 0.6028 0.4934 0.039 Uiso 1 1 calc R . .
C11 C -0.0994(4) 0.7474(4) 0.4355(2) 0.0351(9) Uani 1 1 d . . .
H11A H -0.1576 0.7828 0.4742 0.042 Uiso 1 1 calc R A .
C12 C -0.1287(4) 0.8025(4) 0.3681(2) 0.0334(9) Uani 1 1 d . A .
H12A H -0.2079 0.8755 0.3604 0.040 Uiso 1 1 calc R . .
C13 C -0.0428(4) 0.7517(3) 0.3111(2) 0.0285(8) Uani 1 1 d . . .
H13A H -0.0628 0.7913 0.2649 0.034 Uiso 1 1 calc R A .
C14 C 0.5250(4) 0.3314(3) 0.17639(19) 0.0228(7) Uani 1 1 d . A .
C15 C 0.4365(4) 0.3793(3) 0.1177(2) 0.0266(7) Uani 1 1 d . . .
H15A H 0.3394 0.4215 0.1250 0.032 Uiso 1 1 calc R A .
C16 C 0.4885(4) 0.3660(4) 0.0489(2) 0.0342(9) Uani 1 1 d . A .
H16A H 0.4270 0.4000 0.0096 0.041 Uiso 1 1 calc R . .
C17 C 0.6283(5) 0.3039(4) 0.0372(2) 0.0387(10) Uani 1 1 d . . .
H17A H 0.6635 0.2947 -0.0100 0.046 Uiso 1 1 calc R A .
C18 C 0.7172(4) 0.2552(5) 0.0945(2) 0.0443(11) Uani 1 1 d . A .
H18A H 0.8140 0.2128 0.0867 0.053 Uiso 1 1 calc R . .
C19 C 0.6661(4) 0.2676(4) 0.1635(2) 0.0361(9) Uani 1 1 d . . .
H19A H 0.7281 0.2322 0.2025 0.043 Uiso 1 1 calc R A .
C20 C 0.5622(3) 0.4203(3) 0.31234(19) 0.0218(7) Uani 1 1 d . A .
C21 C 0.5665(4) 0.4101(4) 0.3861(2) 0.0337(9) Uani 1 1 d . . .
H21A H 0.5163 0.3644 0.4110 0.040 Uiso 1 1 calc R A .
C22 C 0.6439(5) 0.4665(4) 0.4238(2) 0.0429(11) Uani 1 1 d . A .
H22A H 0.6470 0.4585 0.4744 0.051 Uiso 1 1 calc R . .
C23 C 0.7159(4) 0.5337(4) 0.3882(3) 0.0394(10) Uani 1 1 d . . .
H23A H 0.7696 0.5713 0.4141 0.047 Uiso 1 1 calc R A .
C24 C 0.7101(5) 0.5464(4) 0.3150(3) 0.0443(11) Uani 1 1 d . A .
H24A H 0.7580 0.5945 0.2904 0.053 Uiso 1 1 calc R . .
C25 C 0.6345(4) 0.4890(4) 0.2767(2) 0.0381(9) Uani 1 1 d . . .
H25A H 0.6323 0.4967 0.2262 0.046 Uiso 1 1 calc R A .
C26 C 0.6680(6) 0.9131(6) 0.1847(4) 0.0488(15) Uani 0.786(5) 1 d P A 1
H26A H 0.7350 0.9023 0.1455 0.073 Uiso 0.786(5) 1 calc PR A 1
H26B H 0.7030 0.8440 0.2202 0.073 Uiso 0.786(5) 1 calc PR A 1
H26C H 0.6567 0.9914 0.2070 0.073 Uiso 0.786(5) 1 calc PR A 1
C27 C 0.5501(6) 0.8043(5) 0.1190(3) 0.0398(12) Uani 0.786(5) 1 d P A 1
H27A H 0.6219 0.7947 0.0823 0.060 Uiso 0.786(5) 1 calc PR A 1
H27B H 0.4606 0.8116 0.0965 0.060 Uiso 0.786(5) 1 calc PR A 1
H27C H 0.5784 0.7317 0.1525 0.060 Uiso 0.786(5) 1 calc PR A 1
C28 C 0.4761(5) 1.0293(5) 0.1080(3) 0.0321(11) Uani 0.786(5) 1 d P A 1
H28A H 0.4684 1.1036 0.1347 0.039 Uiso 0.786(5) 1 calc PR A 1
H28B H 0.5434 1.0250 0.0688 0.039 Uiso 0.786(5) 1 calc PR A 1
C26A C 0.637(2) 0.979(2) 0.1552(14) 0.0488(15) Uani 0.214(5) 1 d P A 2
H26D H 0.6959 0.9554 0.1131 0.073 Uiso 0.214(5) 1 calc PR A 2
H26E H 0.6956 0.9547 0.1982 0.073 Uiso 0.214(5) 1 calc PR A 2
H26F H 0.5884 1.0687 0.1529 0.073 Uiso 0.214(5) 1 calc PR A 2
C27A C 0.620(2) 0.7821(17) 0.1867(11) 0.0398(12) Uani 0.214(5) 1 d P A 2
H27D H 0.7059 0.7829 0.2098 0.048 Uiso 0.214(5) 1 calc PR A 2
H27E H 0.6443 0.7259 0.1473 0.048 Uiso 0.214(5) 1 calc PR A 2
H27F H 0.5633 0.7534 0.2215 0.048 Uiso 0.214(5) 1 calc PR A 2
C28A C 0.4626(19) 0.9157(17) 0.0998(10) 0.0321(11) Uani 0.214(5) 1 d P A 2
H28C H 0.4209 0.8493 0.1065 0.039 Uiso 0.214(5) 1 calc PR A 2
H28D H 0.5290 0.8936 0.0597 0.039 Uiso 0.214(5) 1 calc PR A 2
C29 C 0.3371(5) 1.0447(4) 0.0767(2) 0.0376(9) Uani 1 1 d . . .
H29A H 0.3114 1.1173 0.0423 0.045 Uiso 0.786(5) 1 calc PR A 1
H29B H 0.3455 0.9707 0.0496 0.045 Uiso 0.786(5) 1 calc PR A 1
H29C H 0.3723 1.1155 0.0768 0.045 Uiso 0.214(5) 1 calc PR A 2
H29D H 0.3030 1.0402 0.0280 0.045 Uiso 0.214(5) 1 calc PR A 2
C30 C 0.1121(5) 1.0231(5) 0.0988(3) 0.0493(12) Uani 1 1 d . . .
H30A H 0.0757 1.0721 0.0546 0.074 Uiso 1 1 calc R A .
H30B H 0.0361 1.0361 0.1334 0.074 Uiso 1 1 calc R . .
H30C H 0.1503 0.9350 0.0887 0.074 Uiso 1 1 calc R . .
C31 C 0.1657(5) 1.1912(4) 0.1464(2) 0.0406(10) Uani 1 1 d . . .
H31A H 0.1280 1.2435 0.1035 0.061 Uiso 1 1 calc R A .
H31B H 0.2400 1.2161 0.1670 0.061 Uiso 1 1 calc R . .
H31C H 0.0905 1.2008 0.1812 0.061 Uiso 1 1 calc R . .
C32 C -0.0520(4) 1.1013(4) 0.3177(2) 0.0413(10) Uani 1 1 d . . .
H32A H -0.1289 1.1425 0.3497 0.062 Uiso 1 1 calc R A .
H32B H -0.0508 1.0168 0.3108 0.062 Uiso 1 1 calc R . .
H32C H -0.0657 1.1479 0.2716 0.062 Uiso 1 1 calc R . .
C33 C 0.0822(4) 1.2234(4) 0.3546(2) 0.0339(9) Uani 1 1 d . . .
H33A H 0.0076 1.2680 0.3869 0.051 Uiso 1 1 calc R A .
H33B H 0.0662 1.2661 0.3074 0.051 Uiso 1 1 calc R . .
H33C H 0.1731 1.2210 0.3733 0.051 Uiso 1 1 calc R . .
C34 C 0.0986(4) 1.0324(4) 0.42010(19) 0.0283(8) Uani 1 1 d . . .
H34A H 0.0706 0.9579 0.4174 0.034 Uiso 1 1 calc R A .
H34B H 0.0346 1.0881 0.4537 0.034 Uiso 1 1 calc R . .
C35 C 0.2483(4) 0.9930(3) 0.44928(19) 0.0266(7) Uani 1 1 d . A .
H35A H 0.2817 1.0649 0.4448 0.032 Uiso 1 1 calc R . .
H35B H 0.2476 0.9690 0.5006 0.032 Uiso 1 1 calc R . .
C36 C 0.3191(5) 0.7741(4) 0.4303(3) 0.0440(11) Uani 1 1 d . . .
H36A H 0.3254 0.7571 0.4820 0.066 Uiso 1 1 calc R A .
H36B H 0.3887 0.7057 0.4069 0.066 Uiso 1 1 calc R . .
H36C H 0.2249 0.7822 0.4136 0.066 Uiso 1 1 calc R . .
C37 C 0.4905(4) 0.8757(4) 0.4337(2) 0.0391(10) Uani 1 1 d . . .
H37A H 0.5022 0.8577 0.4852 0.059 Uiso 1 1 calc R A .
H37B H 0.5089 0.9529 0.4211 0.059 Uiso 1 1 calc R . .
H37C H 0.5566 0.8074 0.4087 0.059 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
K1 0.0299(4) 0.0214(4) 0.0215(4) 0.0008(3) 0.0027(3) -0.0081(3)
P1 0.0205(4) 0.0165(4) 0.0249(4) -0.0012(3) 0.0021(3) -0.0084(3)
P2 0.0202(4) 0.0171(4) 0.0226(4) 0.0001(3) -0.0021(3) -0.0083(3)
B1 0.029(2) 0.0216(19) 0.042(3) -0.0005(18) 0.0054(19) -0.0119(17)
B2 0.028(2) 0.0193(18) 0.034(2) 0.0048(16) -0.0076(17) -0.0086(16)
N1 0.0271(16) 0.0298(16) 0.0324(17) -0.0062(13) 0.0059(13) -0.0072(13)
N2 0.0343(17) 0.0299(16) 0.0234(16) 0.0024(13) -0.0047(13) -0.0086(13)
N3 0.0240(15) 0.0266(15) 0.0264(16) 0.0033(12) -0.0003(12) -0.0113(12)
N4 0.0312(16) 0.0205(14) 0.0269(16) -0.0009(12) -0.0053(12) -0.0081(12)
C1 0.0204(16) 0.0171(15) 0.0284(18) 0.0029(13) -0.0028(13) -0.0089(13)
C2 0.0229(17) 0.0219(16) 0.0232(17) -0.0037(13) 0.0009(13) -0.0025(13)
C3 0.030(2) 0.034(2) 0.039(2) 0.0029(17) -0.0060(16) -0.0136(16)
C4 0.031(2) 0.042(2) 0.051(3) -0.011(2) -0.0112(19) -0.0124(18)
C5 0.032(2) 0.060(3) 0.037(2) -0.014(2) -0.0109(18) -0.003(2)
C6 0.053(3) 0.072(3) 0.030(2) 0.011(2) -0.009(2) -0.017(3)
C7 0.042(2) 0.046(2) 0.032(2) 0.0069(18) -0.0037(18) -0.018(2)
C8 0.0233(17) 0.0194(16) 0.0290(18) -0.0044(13) 0.0015(14) -0.0122(13)
C9 0.0277(18) 0.0298(18) 0.0258(18) -0.0048(15) -0.0003(14) -0.0123(15)
C10 0.038(2) 0.040(2) 0.0254(19) -0.0079(16) 0.0025(16) -0.0201(18)
C11 0.035(2) 0.042(2) 0.038(2) -0.0201(18) 0.0122(17) -0.0231(18)
C12 0.0281(19) 0.0289(19) 0.045(2) -0.0117(17) 0.0061(17) -0.0111(16)
C13 0.0299(19) 0.0260(18) 0.031(2) -0.0040(15) 0.0024(15) -0.0115(15)
C14 0.0237(17) 0.0190(16) 0.0285(18) -0.0027(13) -0.0002(14) -0.0108(13)
C15 0.0254(18) 0.0249(17) 0.0286(19) 0.0002(14) 0.0000(14) -0.0076(14)
C16 0.037(2) 0.036(2) 0.029(2) 0.0000(16) -0.0004(16) -0.0123(17)
C17 0.044(2) 0.045(2) 0.032(2) -0.0120(18) 0.0105(18) -0.021(2)
C18 0.026(2) 0.060(3) 0.044(3) -0.013(2) 0.0090(18) -0.010(2)
C19 0.0246(19) 0.044(2) 0.036(2) -0.0038(18) -0.0042(16) -0.0067(17)
C20 0.0190(16) 0.0154(15) 0.0308(18) -0.0015(13) -0.0047(13) -0.0053(12)
C21 0.047(2) 0.0278(19) 0.033(2) 0.0060(16) -0.0149(17) -0.0215(17)
C22 0.063(3) 0.029(2) 0.041(2) 0.0059(18) -0.026(2) -0.022(2)
C23 0.030(2) 0.0241(19) 0.067(3) -0.0082(19) -0.021(2) -0.0114(16)
C24 0.040(2) 0.047(3) 0.060(3) -0.011(2) 0.006(2) -0.032(2)
C25 0.040(2) 0.045(2) 0.041(2) -0.0065(19) 0.0042(18) -0.030(2)
C26 0.031(3) 0.055(4) 0.056(4) -0.015(3) -0.004(3) -0.006(3)
C27 0.042(3) 0.031(3) 0.043(3) -0.004(2) 0.011(2) -0.008(2)
C28 0.037(3) 0.031(2) 0.028(2) -0.0054(19) 0.013(2) -0.012(2)
C26A 0.031(3) 0.055(4) 0.056(4) -0.015(3) -0.004(3) -0.006(3)
C27A 0.042(3) 0.031(3) 0.043(3) -0.004(2) 0.011(2) -0.008(2)
C28A 0.037(3) 0.031(2) 0.028(2) -0.0054(19) 0.013(2) -0.012(2)
C29 0.046(2) 0.033(2) 0.031(2) 0.0005(17) 0.0087(18) -0.0099(18)
C30 0.050(3) 0.050(3) 0.051(3) 0.001(2) -0.011(2) -0.022(2)
C31 0.048(3) 0.035(2) 0.034(2) -0.0015(18) -0.0007(19) -0.0073(19)
C32 0.032(2) 0.052(3) 0.044(3) 0.011(2) -0.0118(18) -0.0212(19)
C33 0.041(2) 0.0288(19) 0.033(2) 0.0010(16) 0.0010(17) -0.0137(17)
C34 0.0313(19) 0.0320(19) 0.0256(18) 0.0031(15) 0.0048(15) -0.0168(16)
C35 0.0306(19) 0.0246(17) 0.0242(18) 0.0018(14) -0.0036(14) -0.0089(15)
C36 0.067(3) 0.0232(19) 0.045(3) 0.0013(18) -0.006(2) -0.020(2)
C37 0.033(2) 0.032(2) 0.049(3) -0.0056(18) -0.0087(18) -0.0058(17)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
K1 N4 2.811(3) . ?
K1 N1 2.865(3) . ?
K1 N2 2.874(3) . ?
K1 N3 2.975(3) . ?
K1 B1 3.213(4) . ?
K1 C27A 3.324(19) . ?
K1 H2B1 2.85(4) . ?
K1 H3B1 2.77(4) . ?
P1 C1 1.717(3) . ?
P1 C8 1.829(4) . ?
P1 C2 1.833(4) . ?
P1 B1 1.927(4) . ?
P2 C1 1.717(3) . ?
P2 C14 1.831(4) . ?
P2 C20 1.834(3) . ?
P2 B2 1.941(4) . ?
B1 H1B1 1.16(4) . ?
B1 H2B1 1.07(5) . ?
B1 H3B1 1.11(4) . ?
B2 H1B2 1.08(4) . ?
B2 H2B2 1.15(4) . ?
B2 H3B2 1.14(5) . ?
N1 C28A 1.306(19) . ?
N1 C26 1.446(6) . ?
N1 C27 1.458(6) . ?
N1 C26A 1.45(2) . ?
N1 C28 1.507(6) . ?
N1 C27A 1.560(19) . ?
N2 C31 1.454(5) . ?
N2 C30 1.461(5) . ?
N2 C29 1.466(5) . ?
N3 C33 1.465(5) . ?
N3 C32 1.465(5) . ?
N3 C34 1.471(4) . ?
N4 C36 1.461(5) . ?
N4 C35 1.462(5) . ?
N4 C37 1.467(5) . ?
C1 H1A 0.9500 . ?
C2 C7 1.379(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.385(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.374(7) . ?
C4 H4A 0.9500 . ?
C5 C6 1.367(7) . ?
C5 H5A 0.9500 . ?
C6 C7 1.392(6) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C13 1.391(5) . ?
C8 C9 1.400(5) . ?
C9 C10 1.395(5) . ?
C9 H9A 0.9500 . ?
C10 C11 1.383(6) . ?
C10 H10A 0.9500 . ?
C11 C12 1.374(6) . ?
C11 H11A 0.9500 . ?
C12 C13 1.396(5) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C19 1.394(5) . ?
C14 C15 1.395(5) . ?
C15 C16 1.387(5) . ?
C15 H15A 0.9500 . ?
C16 C17 1.375(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.379(6) . ?
C17 H17A 0.9500 . ?
C18 C19 1.387(6) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 C21 1.384(5) . ?
C20 C25 1.388(5) . ?
C21 C22 1.391(5) . ?
C21 H21A 0.9500 . ?
C22 C23 1.375(6) . ?
C22 H22A 0.9500 . ?
C23 C24 1.376(7) . ?
C23 H23A 0.9500 . ?
C24 C25 1.391(6) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.482(7) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C26A H26D 0.9800 . ?
C26A H26E 0.9800 . ?
C26A H26F 0.9800 . ?
C27A H27D 0.9800 . ?
C27A H27E 0.9800 . ?
C27A H27F 0.9800 . ?
C28A C29 1.634(19) . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 H29C 0.9900 . ?
C29 H29D 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.527(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?

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
N4 K1 N1 131.64(10) . . ?
N4 K1 N2 162.05(9) . . ?
N1 K1 N2 64.68(9) . . ?
N4 K1 N3 65.23(9) . . ?
N1 K1 N3 153.47(9) . . ?
N2 K1 N3 96.84(9) . . ?
N4 K1 B1 95.97(11) . . ?
N1 K1 B1 88.76(11) . . ?
N2 K1 B1 91.39(11) . . ?
N3 K1 B1 111.61(10) . . ?
N4 K1 C27A 109.6(4) . . ?
N1 K1 C27A 28.0(3) . . ?
N2 K1 C27A 88.2(4) . . ?
N3 K1 C27A 173.4(4) . . ?
B1 K1 C27A 72.3(4) . . ?
N4 K1 H2B1 79.7(10) . . ?
N1 K1 H2B1 92.0(9) . . ?
N2 K1 H2B1 109.8(10) . . ?
N3 K1 H2B1 112.9(9) . . ?
B1 K1 H2B1 19.2(9) . . ?
C27A K1 H2B1 69.0(10) . . ?
N4 K1 H3B1 104.6(9) . . ?
N1 K1 H3B1 95.7(9) . . ?
N2 K1 H3B1 77.9(9) . . ?
N3 K1 H3B1 98.8(9) . . ?
B1 K1 H3B1 19.6(9) . . ?
C27A K1 H3B1 86.3(9) . . ?
H2B1 K1 H3B1 37.3(12) . . ?
C1 P1 C8 107.93(16) . . ?
C1 P1 C2 108.90(16) . . ?
C8 P1 C2 101.87(16) . . ?
C1 P1 B1 119.46(18) . . ?
C8 P1 B1 108.54(18) . . ?
C2 P1 B1 108.72(19) . . ?
C1 P2 C14 112.57(16) . . ?
C1 P2 C20 112.13(16) . . ?
C14 P2 C20 103.16(16) . . ?
C1 P2 B2 109.96(17) . . ?
C14 P2 B2 108.97(18) . . ?
C20 P2 B2 109.82(17) . . ?
P1 B1 K1 141.6(2) . . ?
P1 B1 H1B1 107(2) . . ?
K1 B1 H1B1 111(2) . . ?
P1 B1 H2B1 106(2) . . ?
K1 B1 H2B1 61(2) . . ?
H1B1 B1 H2B1 114(3) . . ?
P1 B1 H3B1 105(2) . . ?
K1 B1 H3B1 57(2) . . ?
H1B1 B1 H3B1 113(3) . . ?
H2B1 B1 H3B1 111(3) . . ?
P2 B2 H1B2 111(2) . . ?
P2 B2 H2B2 104(2) . . ?
H1B2 B2 H2B2 110(3) . . ?
P2 B2 H3B2 103(2) . . ?
H1B2 B2 H3B2 114(3) . . ?
H2B2 B2 H3B2 115(3) . . ?
C28A N1 C26 145.1(9) . . ?
C28A N1 C27 56.7(8) . . ?
C26 N1 C27 110.5(4) . . ?
C28A N1 C26A 119.6(13) . . ?
C26 N1 C26A 35.3(10) . . ?
C27 N1 C26A 123.4(10) . . ?
C28A N1 C28 57.8(8) . . ?
C26 N1 C28 108.5(4) . . ?
C27 N1 C28 110.0(4) . . ?
C26A N1 C28 73.2(11) . . ?
C28A N1 C27A 112.6(11) . . ?
C26 N1 C27A 70.0(8) . . ?
C27 N1 C27A 56.5(8) . . ?
C26A N1 C27A 103.3(13) . . ?
C28 N1 C27A 161.9(8) . . ?
C28A N1 K1 101.6(8) . . ?
C26 N1 K1 113.2(3) . . ?
C27 N1 K1 110.3(3) . . ?
C26A N1 K1 123.9(10) . . ?
C28 N1 K1 104.1(2) . . ?
C27A N1 K1 92.6(7) . . ?
C31 N2 C30 109.9(3) . . ?
C31 N2 C29 110.6(3) . . ?
C30 N2 C29 110.4(3) . . ?
C31 N2 K1 100.1(2) . . ?
C30 N2 K1 113.8(3) . . ?
C29 N2 K1 111.7(2) . . ?
C33 N3 C32 108.9(3) . . ?
C33 N3 C34 110.5(3) . . ?
C32 N3 C34 109.4(3) . . ?
C33 N3 K1 111.0(2) . . ?
C32 N3 K1 111.7(2) . . ?
C34 N3 K1 105.3(2) . . ?
C36 N4 C35 111.0(3) . . ?
C36 N4 C37 109.9(3) . . ?
C35 N4 C37 109.4(3) . . ?
C36 N4 K1 111.0(2) . . ?
C35 N4 K1 108.8(2) . . ?
C37 N4 K1 106.7(2) . . ?
P2 C1 P1 130.9(2) . . ?
P2 C1 H1A 114.5 . . ?
P1 C1 H1A 114.5 . . ?
C7 C2 C3 118.0(4) . . ?
C7 C2 P1 121.1(3) . . ?
C3 C2 P1 120.8(3) . . ?
C4 C3 C2 120.5(4) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C5 C4 C3 120.4(4) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 H5A 120.1 . . ?
C4 C5 H5A 120.1 . . ?
C5 C6 C7 120.0(4) . . ?
C5 C6 H6A 120.0 . . ?
C7 C6 H6A 120.0 . . ?
C2 C7 C6 121.2(4) . . ?
C2 C7 H7A 119.4 . . ?
C6 C7 H7A 119.4 . . ?
C13 C8 C9 118.8(3) . . ?
C13 C8 P1 120.8(3) . . ?
C9 C8 P1 120.3(3) . . ?
C10 C9 C8 120.1(4) . . ?
C10 C9 H9A 119.9 . . ?
C8 C9 H9A 119.9 . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C12 C11 C10 119.9(4) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C11 C12 C13 120.4(4) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C8 C13 C12 120.5(4) . . ?
C8 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C19 C14 C15 117.9(3) . . ?
C19 C14 P2 120.8(3) . . ?
C15 C14 P2 121.2(3) . . ?
C16 C15 C14 120.8(3) . . ?
C16 C15 H15A 119.6 . . ?
C14 C15 H15A 119.6 . . ?
C17 C16 C15 120.5(4) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C18 119.5(4) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C17 C18 C19 120.5(4) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C18 C19 C14 120.8(4) . . ?
C18 C19 H19A 119.6 . . ?
C14 C19 H19A 119.6 . . ?
C21 C20 C25 119.1(3) . . ?
C21 C20 P2 117.2(3) . . ?
C25 C20 P2 123.7(3) . . ?
C20 C21 C22 120.4(4) . . ?
C20 C21 H21A 119.8 . . ?
C22 C21 H21A 119.8 . . ?
C23 C22 C21 120.2(4) . . ?
C23 C22 H22A 119.9 . . ?
C21 C22 H22A 119.9 . . ?
C22 C23 C24 119.9(4) . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C23 C24 C25 120.3(4) . . ?
C23 C24 H24A 119.9 . . ?
C25 C24 H24A 119.9 . . ?
C20 C25 C24 120.1(4) . . ?
C20 C25 H25A 119.9 . . ?
C24 C25 H25A 119.9 . . ?
N1 C26 H26A 109.5 . . ?
N1 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
N1 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N1 C27 H27A 109.5 . . ?
N1 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
N1 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C29 C28 N1 114.3(4) . . ?
C29 C28 H28A 108.7 . . ?
N1 C28 H28A 108.7 . . ?
C29 C28 H28B 108.7 . . ?
N1 C28 H28B 108.7 . . ?
H28A C28 H28B 107.6 . . ?
N1 C26A H26D 109.5 . . ?
N1 C26A H26E 109.5 . . ?
H26D C26A H26E 109.5 . . ?
N1 C26A H26F 109.5 . . ?
H26D C26A H26F 109.5 . . ?
H26E C26A H26F 109.5 . . ?
N1 C27A K1 59.4(6) . . ?
N1 C27A H27D 109.5 . . ?
K1 C27A H27D 114.6 . . ?
N1 C27A H27E 109.5 . . ?
K1 C27A H27E 135.7 . . ?
H27D C27A H27E 109.5 . . ?
N1 C27A H27F 109.5 . . ?
K1 C27A H27F 51.4 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
N1 C28A C29 116.9(12) . . ?
N1 C28A H28C 108.1 . . ?
C29 C28A H28C 108.1 . . ?
N1 C28A H28D 108.1 . . ?
C29 C28A H28D 108.1 . . ?
H28C C28A H28D 107.3 . . ?
N2 C29 C28 115.3(4) . . ?
N2 C29 C28A 108.1(7) . . ?
C28 C29 C28A 51.9(7) . . ?
N2 C29 H29A 108.5 . . ?
C28 C29 H29A 108.5 . . ?
C28A C29 H29A 143.4 . . ?
N2 C29 H29B 108.5 . . ?
C28 C29 H29B 108.5 . . ?
C28A C29 H29B 62.4 . . ?
H29A C29 H29B 107.5 . . ?
N2 C29 H29C 110.1 . . ?
C28 C29 H29C 59.3 . . ?
C28A C29 H29C 110.1 . . ?
H29A C29 H29C 53.7 . . ?
H29B C29 H29C 141.0 . . ?
N2 C29 H29D 110.1 . . ?
C28 C29 H29D 134.4 . . ?
C28A C29 H29D 110.1 . . ?
H29A C29 H29D 58.5 . . ?
H29B C29 H29D 50.9 . . ?
H29C C29 H29D 108.4 . . ?
N2 C30 H30A 109.5 . . ?
N2 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N2 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N2 C31 H31A 109.5 . . ?
N2 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N2 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 H32A 109.5 . . ?
N3 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N3 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
N3 C33 H33A 109.5 . . ?
N3 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
N3 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C34 C35 113.4(3) . . ?
N3 C34 H34A 108.9 . . ?
C35 C34 H34A 108.9 . . ?
N3 C34 H34B 108.9 . . ?
C35 C34 H34B 108.9 . . ?
H34A C34 H34B 107.7 . . ?
N4 C35 C34 113.5(3) . . ?
N4 C35 H35A 108.9 . . ?
C34 C35 H35A 108.9 . . ?
N4 C35 H35B 108.9 . . ?
C34 C35 H35B 108.9 . . ?
H35A C35 H35B 107.7 . . ?
N4 C36 H36A 109.5 . . ?
N4 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N4 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N4 C37 H37A 109.5 . . ?
N4 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N4 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.964
_diffrn_reflns_theta_full        27.57
_diffrn_measured_fraction_theta_full 0.964
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.076


data_FO3724
_database_code_depnum_ccdc_archive 'CCDC 900419'
#TrackingRef 'chemcom.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;

;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C150 H162 B12 Ba4 O P12'
_chemical_formula_sum            'C150 H162 B12 Ba4 O P12'
_chemical_formula_weight         3031.52

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'
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   24.6465(8)
_cell_length_b                   24.6465(9)
_cell_length_c                   35.3753(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     18609.8(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             6136
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           ?

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            33241
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.91
_diffrn_reflns_theta_max         27.46
_reflns_number_total             12177
_reflns_number_gt                6031
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       COLLECT
_computing_cell_refinement       DENZO
_computing_data_reduction        DENZO
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12176
_refine_ls_number_parameters     506
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1445
_refine_ls_R_factor_gt           0.0746
_refine_ls_wR_factor_ref         0.2311
_refine_ls_wR_factor_gt          0.2023
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000


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
Ba1 Ba 0.55469(2) 0.27678(2) 0.146538(10) 0.03909(17) Uani 1 1 d . . .
Ba2 Ba 0.6667 0.3333 0.245053(18) 0.0445(2) Uani 1 3 d S . .
P1 P 0.57647(10) 0.14724(9) 0.04431(5) 0.0465(5) Uani 1 1 d . . .
P2 P 0.43640(10) 0.10437(10) 0.05826(5) 0.0494(6) Uani 1 1 d . . .
P3 P 0.63359(11) 0.48333(11) 0.28546(5) 0.0542(6) Uani 1 1 d . . .
P4 P 0.54112(10) 0.35952(10) 0.25122(5) 0.0500(6) Uani 1 1 d . . .
O1 O 0.6667 0.3333 0.16529(18) 0.0364(19) Uani 1 3 d S . .
B1 B 0.6112(4) 0.2090(4) 0.0835(2) 0.058(3) Uani 1 1 d . . .
H1BA H 0.6011 0.2420 0.0785 0.087 Uiso 1 1 d R . .
H1BB H 0.6568 0.2271 0.0841 0.087 Uiso 1 1 d R . .
H1BC H 0.5935 0.1894 0.1079 0.087 Uiso 1 1 d R . .
B2 B 0.4505(4) 0.1666(4) 0.0959(2) 0.057(3) Uani 1 1 d . . .
H2BA H 0.4730 0.1622 0.1174 0.085 Uiso 1 1 d R . .
H2BB H 0.4101 0.1608 0.1045 0.085 Uiso 1 1 d R . .
H2BC H 0.4754 0.2085 0.0849 0.085 Uiso 1 1 d R . .
B3 B 0.6629(5) 0.4352(5) 0.3123(2) 0.068(3) Uani 1 1 d . . .
H3BA H 0.6796 0.4546 0.3369 0.102 Uiso 1 1 d R . .
H3BB H 0.6960 0.4341 0.2975 0.102 Uiso 1 1 d R . .
H3BC H 0.6281 0.3924 0.3159 0.102 Uiso 1 1 d R . .
B4 B 0.6402(5) 0.4480(4) 0.2098(2) 0.055(3) Uani 1 1 d . . .
H4BA H 0.6506 0.4837 0.1931 0.083 Uiso 1 1 d R . .
H4BB H 0.6211 0.4093 0.1949 0.083 Uiso 1 1 d R . .
H4BC H 0.6785 0.4537 0.2218 0.083 Uiso 1 1 d R . .
C1 C 0.4980(4) 0.0990(3) 0.04037(17) 0.051(2) Uani 1 1 d . . .
H1A H 0.4861 0.0625 0.0256 0.062 Uiso 1 1 calc R . .
C2 C 0.6121(4) 0.1863(3) -0.00046(18) 0.051(2) Uani 1 1 d . . .
C3 C 0.6682(5) 0.2423(4) -0.0024(2) 0.0773(13) Uani 1 1 d . . .
H3A H 0.6886 0.2629 0.0204 0.093 Uiso 1 1 calc R . .
C4 C 0.6957(5) 0.2694(4) -0.0373(2) 0.0773(13) Uani 1 1 d . . .
H4A H 0.7338 0.3084 -0.0381 0.093 Uiso 1 1 calc R . .
C5 C 0.6677(4) 0.2397(4) -0.0692(2) 0.0773(13) Uani 1 1 d . . .
H5A H 0.6889 0.2551 -0.0926 0.093 Uiso 1 1 calc R . .
C6 C 0.6086(5) 0.1868(4) -0.0691(2) 0.0773(13) Uani 1 1 d . . .
H6A H 0.5867 0.1699 -0.0921 0.093 Uiso 1 1 calc R . .
C7 C 0.5815(4) 0.1584(4) -0.0340(2) 0.0773(13) Uani 1 1 d . . .
H7A H 0.5425 0.1204 -0.0334 0.093 Uiso 1 1 calc R . .
C8 C 0.6142(5) 0.0981(4) 0.04719(17) 0.055(2) Uani 1 1 d . . .
C9 C 0.6795(4) 0.1259(4) 0.0452(2) 0.056(2) Uani 1 1 d . . .
H9A H 0.7051 0.1701 0.0429 0.067 Uiso 1 1 calc R . .
C10 C 0.7062(5) 0.0884(6) 0.0466(2) 0.080(3) Uani 1 1 d . . .
H10A H 0.7502 0.1070 0.0436 0.096 Uiso 1 1 calc R . .
C11 C 0.6708(6) 0.0248(6) 0.0523(2) 0.080(3) Uani 1 1 d . . .
H11A H 0.6900 -0.0001 0.0550 0.096 Uiso 1 1 calc R . .
C12 C 0.6075(6) -0.0014(5) 0.0539(2) 0.073(3) Uani 1 1 d . . .
H12A H 0.5828 -0.0456 0.0567 0.087 Uiso 1 1 calc R . .
C13 C 0.5769(4) 0.0333(4) 0.05163(17) 0.056(2) Uani 1 1 d . . .
H13A H 0.5326 0.0137 0.0531 0.067 Uiso 1 1 calc R . .
C14 C 0.3787(4) 0.0277(4) 0.0740(2) 0.060(2) Uani 1 1 d . . .
C15 C 0.3626(5) -0.0255(5) 0.0527(2) 0.079(3) Uani 1 1 d . . .
H15A H 0.3815 -0.0210 0.0287 0.095 Uiso 1 1 calc R . .
C16 C 0.3195(4) -0.0851(5) 0.0654(3) 0.0909(19) Uani 1 1 d . . .
H16A H 0.3089 -0.1203 0.0497 0.109 Uiso 1 1 calc R . .
C17 C 0.2921(5) -0.0938(5) 0.1001(3) 0.0909(19) Uani 1 1 d . . .
H17A H 0.2640 -0.1348 0.1091 0.109 Uiso 1 1 calc R . .
C18 C 0.3060(5) -0.0427(4) 0.1215(3) 0.0909(19) Uani 1 1 d . . .
H18A H 0.2861 -0.0479 0.1453 0.109 Uiso 1 1 calc R . .
C19 C 0.3496(5) 0.0177(4) 0.1087(2) 0.086(3) Uani 1 1 d . . .
H19A H 0.3592 0.0527 0.1244 0.104 Uiso 1 1 calc R . .
C20 C 0.3962(4) 0.1192(4) 0.0190(2) 0.053(2) Uani 1 1 d . . .
C21 C 0.3326(5) 0.0960(5) 0.0192(3) 0.086(3) Uani 1 1 d . . .
H21A H 0.3080 0.0710 0.0398 0.104 Uiso 1 1 calc R . .
C22 C 0.3043(6) 0.1088(6) -0.0102(4) 0.118(4) Uani 1 1 d . . .
H22A H 0.2600 0.0900 -0.0114 0.142 Uiso 1 1 calc R . .
C23 C 0.3422(7) 0.1500(6) -0.0385(3) 0.111(4) Uani 1 1 d . . .
H23A H 0.3235 0.1611 -0.0582 0.134 Uiso 1 1 calc R . .
C24 C 0.4052(6) 0.1743(5) -0.0381(3) 0.084(3) Uani 1 1 d . . .
H24A H 0.4307 0.2023 -0.0574 0.101 Uiso 1 1 calc R . .
C25 C 0.4310(5) 0.1580(4) -0.0097(2) 0.067(3) Uani 1 1 d . . .
H25A H 0.4750 0.1742 -0.0097 0.080 Uiso 1 1 calc R . .
C26 C 0.5910(4) 0.4439(3) 0.24236(18) 0.048(2) Uani 1 1 d . . .
H26A H 0.5655 0.4624 0.2331 0.057 Uiso 1 1 calc R . .
C27 C 0.6961(4) 0.5608(4) 0.2724(2) 0.062(2) Uani 1 1 d . . .
C28 C 0.6937(5) 0.5946(5) 0.2416(2) 0.068(2) Uani 1 1 d . . .
H28A H 0.6583 0.5756 0.2254 0.081 Uiso 1 1 calc R . .
C29 C 0.7403(6) 0.6538(6) 0.2338(3) 0.093(3) Uani 1 1 d . . .
H29A H 0.7372 0.6754 0.2124 0.111 Uiso 1 1 calc R . .
C30 C 0.7935(6) 0.6834(6) 0.2579(4) 0.101(4) Uani 1 1 d . . .
H30A H 0.8256 0.7254 0.2536 0.122 Uiso 1 1 calc R . .
C31 C 0.7974(6) 0.6484(6) 0.2883(3) 0.098(3) Uani 1 1 d . . .
H31A H 0.8340 0.6658 0.3035 0.117 Uiso 1 1 calc R . .
C32 C 0.7486(5) 0.5894(5) 0.2960(2) 0.071(3) Uani 1 1 d . . .
H32A H 0.7506 0.5677 0.3176 0.085 Uiso 1 1 calc R . .
C33 C 0.5853(4) 0.5016(4) 0.31535(18) 0.058(2) Uani 1 1 d . . .
C34 C 0.5597(5) 0.4669(5) 0.3480(2) 0.086(3) Uani 1 1 d . . .
H34A H 0.5662 0.4329 0.3538 0.103 Uiso 1 1 calc R . .
C35 C 0.5242(5) 0.4818(5) 0.3726(2) 0.085(3) Uani 1 1 d . . .
H35A H 0.5066 0.4579 0.3949 0.102 Uiso 1 1 calc R . .
C36 C 0.5155(4) 0.5294(5) 0.3644(2) 0.063(2) Uani 1 1 d . . .
H36A H 0.4938 0.5410 0.3818 0.076 Uiso 1 1 calc R . .
C37 C 0.5367(4) 0.5615(4) 0.3319(2) 0.069(3) Uani 1 1 d . . .
H37A H 0.5287 0.5946 0.3265 0.083 Uiso 1 1 calc R . .
C38 C 0.5704(4) 0.5472(4) 0.3059(2) 0.075(3) Uani 1 1 d . . .
H38A H 0.5827 0.5682 0.2823 0.090 Uiso 1 1 calc R . .
C39 C 0.4840(4) 0.3496(4) 0.28712(19) 0.058(2) Uani 1 1 d . . .
C40 C 0.4790(4) 0.3200(4) 0.3205(2) 0.071(3) Uani 1 1 d . . .
H40A H 0.5071 0.3050 0.3254 0.085 Uiso 1 1 calc R . .
C41 C 0.4345(5) 0.3108(5) 0.3480(2) 0.096(4) Uani 1 1 d . . .
H41A H 0.4327 0.2902 0.3710 0.115 Uiso 1 1 calc R . .
C42 C 0.3942(5) 0.3316(5) 0.3414(2) 0.081(3) Uani 1 1 d . . .
H42A H 0.3637 0.3257 0.3598 0.098 Uiso 1 1 calc R . .
C43 C 0.3973(4) 0.3616(4) 0.3076(2) 0.080(3) Uani 1 1 d . . .
H43A H 0.3692 0.3766 0.3028 0.096 Uiso 1 1 calc R . .
C44 C 0.4410(4) 0.3694(4) 0.2813(2) 0.068(3) Uani 1 1 d . . .
H44A H 0.4421 0.3892 0.2581 0.082 Uiso 1 1 calc R . .
C45 C 0.4901(4) 0.3317(4) 0.21026(18) 0.049(2) Uani 1 1 d . . .
C46 C 0.4465(4) 0.2667(4) 0.20966(19) 0.052(2) Uani 1 1 d . . .
H46A H 0.4435 0.2421 0.2311 0.062 Uiso 1 1 calc R . .
C47 C 0.4070(4) 0.2372(4) 0.1781(2) 0.061(2) Uani 1 1 d . . .
H47A H 0.3782 0.1934 0.1779 0.073 Uiso 1 1 calc R . .
C48 C 0.4119(4) 0.2749(5) 0.14713(19) 0.058(2) Uani 1 1 d . . .
H48A H 0.3859 0.2563 0.1257 0.070 Uiso 1 1 calc R . .
C49 C 0.4527(4) 0.3373(4) 0.14719(19) 0.054(2) Uani 1 1 d . . .
H49A H 0.4550 0.3618 0.1259 0.065 Uiso 1 1 calc R . .
C50 C 0.4918(4) 0.3660(4) 0.17845(19) 0.056(2) Uani 1 1 d . . .
H50A H 0.5201 0.4099 0.1779 0.067 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ba1 0.0487(3) 0.0487(3) 0.0176(2) -0.00009(18) 0.00059(16) 0.0226(3)
Ba2 0.0561(3) 0.0561(3) 0.0214(3) 0.000 0.000 0.02805(17)
P1 0.0624(15) 0.0506(12) 0.0208(8) -0.0031(8) 0.0013(9) 0.0240(12)
P2 0.0630(15) 0.0492(13) 0.0279(9) -0.0001(9) -0.0027(9) 0.0221(12)
P3 0.0705(16) 0.0771(17) 0.0268(10) -0.0090(10) 0.0030(10) 0.0456(14)
P4 0.0720(16) 0.0639(15) 0.0227(9) -0.0009(9) 0.0046(9) 0.0404(13)
O1 0.045(3) 0.045(3) 0.018(3) 0.000 0.000 0.0227(15)
B1 0.057(6) 0.059(6) 0.027(4) -0.002(4) 0.005(4) 0.005(5)
B2 0.068(7) 0.066(7) 0.035(5) -0.010(4) -0.010(4) 0.033(6)
B3 0.093(8) 0.096(9) 0.029(5) -0.007(5) -0.016(5) 0.059(7)
B4 0.087(8) 0.063(7) 0.024(4) -0.012(4) -0.001(4) 0.044(6)
C1 0.066(6) 0.051(5) 0.029(4) -0.013(3) -0.008(4) 0.023(5)
C2 0.077(6) 0.038(5) 0.027(4) -0.008(3) 0.000(3) 0.021(4)
C3 0.103(4) 0.074(3) 0.037(2) -0.0012(19) 0.016(2) 0.031(3)
C4 0.103(4) 0.074(3) 0.037(2) -0.0012(19) 0.016(2) 0.031(3)
C5 0.103(4) 0.074(3) 0.037(2) -0.0012(19) 0.016(2) 0.031(3)
C6 0.103(4) 0.074(3) 0.037(2) -0.0012(19) 0.016(2) 0.031(3)
C7 0.103(4) 0.074(3) 0.037(2) -0.0012(19) 0.016(2) 0.031(3)
C8 0.094(7) 0.044(5) 0.017(3) -0.007(3) -0.003(4) 0.026(5)
C9 0.060(6) 0.065(6) 0.042(4) -0.009(4) 0.002(4) 0.031(6)
C10 0.076(7) 0.139(11) 0.043(5) -0.011(6) 0.002(5) 0.067(8)
C11 0.127(11) 0.097(9) 0.059(6) -0.011(6) -0.008(6) 0.088(9)
C12 0.122(10) 0.070(7) 0.026(4) 0.000(4) -0.001(5) 0.048(8)
C13 0.072(6) 0.068(7) 0.024(4) -0.011(4) -0.003(4) 0.032(6)
C14 0.066(6) 0.053(6) 0.039(4) -0.004(4) -0.012(4) 0.012(5)
C15 0.102(8) 0.076(7) 0.053(5) -0.002(5) 0.004(5) 0.040(6)
C16 0.093(4) 0.070(4) 0.060(4) 0.006(3) 0.000(3) 0.004(4)
C17 0.093(4) 0.070(4) 0.060(4) 0.006(3) 0.000(3) 0.004(4)
C18 0.093(4) 0.070(4) 0.060(4) 0.006(3) 0.000(3) 0.004(4)
C19 0.121(9) 0.063(7) 0.049(5) -0.003(5) 0.006(5) 0.026(6)
C20 0.070(6) 0.043(5) 0.040(4) -0.010(4) -0.014(4) 0.024(5)
C21 0.078(8) 0.101(8) 0.081(7) 0.024(6) -0.013(6) 0.045(7)
C22 0.101(9) 0.138(12) 0.121(10) 0.037(9) -0.021(8) 0.063(9)
C23 0.131(12) 0.098(9) 0.099(9) 0.004(7) -0.053(9) 0.052(9)
C24 0.115(10) 0.079(8) 0.060(6) 0.026(5) -0.005(6) 0.050(8)
C25 0.108(8) 0.057(6) 0.043(5) 0.011(4) 0.005(5) 0.047(6)
C26 0.066(5) 0.062(5) 0.027(4) -0.005(3) -0.008(3) 0.040(5)
C27 0.064(6) 0.083(7) 0.041(5) -0.016(5) 0.014(4) 0.038(6)
C28 0.086(7) 0.073(7) 0.049(5) 0.003(5) 0.014(5) 0.043(6)
C29 0.094(9) 0.100(9) 0.084(8) 0.003(7) 0.037(7) 0.048(8)
C30 0.091(10) 0.088(9) 0.109(10) -0.017(8) 0.013(8) 0.034(8)
C31 0.084(9) 0.094(10) 0.093(9) -0.032(7) -0.001(7) 0.027(8)
C32 0.087(8) 0.068(7) 0.053(5) -0.022(5) 0.001(5) 0.035(6)
C33 0.083(6) 0.082(6) 0.022(4) -0.009(4) -0.003(4) 0.051(6)
C34 0.144(9) 0.134(9) 0.035(4) 0.003(5) 0.026(5) 0.110(8)
C35 0.139(10) 0.117(9) 0.040(5) 0.013(5) 0.024(5) 0.095(8)
C36 0.086(6) 0.111(7) 0.029(4) -0.003(4) 0.001(4) 0.076(6)
C37 0.094(7) 0.083(7) 0.053(5) 0.004(5) 0.002(5) 0.062(6)
C38 0.117(8) 0.096(7) 0.044(5) 0.006(5) 0.021(5) 0.077(7)
C39 0.102(7) 0.073(6) 0.028(4) 0.008(4) 0.012(4) 0.066(6)
C40 0.099(7) 0.097(7) 0.039(5) 0.011(4) 0.021(5) 0.067(6)
C41 0.144(10) 0.134(10) 0.049(6) 0.022(6) 0.030(6) 0.098(9)
C42 0.104(8) 0.116(8) 0.039(5) 0.005(5) 0.031(5) 0.065(7)
C43 0.102(8) 0.095(8) 0.054(6) -0.004(5) 0.016(5) 0.058(7)
C44 0.103(7) 0.090(7) 0.023(4) 0.009(4) 0.018(4) 0.057(6)
C45 0.065(6) 0.047(5) 0.024(4) -0.003(3) 0.010(3) 0.018(5)
C46 0.061(6) 0.075(6) 0.031(4) 0.007(4) 0.014(4) 0.042(5)
C47 0.069(6) 0.073(6) 0.039(4) 0.000(4) 0.006(4) 0.035(5)
C48 0.060(6) 0.096(7) 0.026(4) -0.012(4) -0.004(4) 0.045(6)
C49 0.081(7) 0.076(7) 0.028(4) -0.001(4) 0.005(4) 0.056(6)
C50 0.075(6) 0.070(6) 0.032(4) 0.007(4) 0.011(4) 0.043(5)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Ba1 O1 2.4805(18) . ?
Ba1 B4 3.036(8) 2_655 ?
Ba1 B2 3.195(8) . ?
Ba1 B1 3.285(8) 3_665 ?
Ba1 H1BA 2.9701 . ?
Ba1 H2BA 2.7217 . ?
Ba1 H2BC 2.8494 . ?
Ba2 O1 2.822(7) . ?
Ba2 P4 3.469(2) . ?
Ba2 P4 3.469(2) 2_655 ?
Ba2 P4 3.469(2) 3_665 ?
Ba2 H3BB 2.8883 . ?
Ba2 H4BC 2.9480 . ?
P1 C1 1.696(8) . ?
P1 C2 1.834(7) . ?
P1 C8 1.863(9) . ?
P1 B1 1.915(9) . ?
P2 C1 1.709(8) . ?
P2 C14 1.794(8) . ?
P2 C20 1.845(8) . ?
P2 B2 1.927(8) . ?
P3 C33 1.809(8) . ?
P3 C27 1.814(9) . ?
P3 C26 1.830(7) . ?
P3 B3 1.919(9) . ?
P4 C45 1.814(7) . ?
P4 C39 1.819(8) . ?
P4 C26 1.838(8) . ?
O1 Ba1 2.4805(18) 2_655 ?
O1 Ba1 2.4805(18) 3_665 ?
B1 Ba1 3.285(8) 2_655 ?
B1 H1BA 0.9800 . ?
B1 H1BB 0.9800 . ?
B1 H1BC 0.9800 . ?
B2 H2BA 0.9800 . ?
B2 H2BB 0.9800 . ?
B2 H2BC 0.9800 . ?
B3 H3BA 0.9800 . ?
B3 H3BB 0.9800 . ?
B3 H3BC 0.9800 . ?
B4 C26 1.638(10) . ?
B4 Ba1 3.036(8) 3_665 ?
B4 H4BA 0.9800 . ?
B4 H4BB 0.9800 . ?
B4 H4BC 0.9800 . ?
C1 H1A 0.9500 . ?
C2 C3 1.383(10) . ?
C2 C7 1.391(10) . ?
C3 C4 1.406(10) . ?
C3 H3A 0.9500 . ?
C4 C5 1.336(11) . ?
C4 H4A 0.9500 . ?
C5 C6 1.387(11) . ?
C5 H5A 0.9500 . ?
C6 C7 1.416(11) . ?
C6 H6A 0.9500 . ?
C7 H7A 0.9500 . ?
C8 C13 1.396(10) . ?
C8 C9 1.402(10) . ?
C9 C10 1.376(12) . ?
C9 H9A 0.9500 . ?
C10 C11 1.376(13) . ?
C10 H10A 0.9500 . ?
C11 C12 1.359(12) . ?
C11 H11A 0.9500 . ?
C12 C13 1.397(11) . ?
C12 H12A 0.9500 . ?
C13 H13A 0.9500 . ?
C14 C19 1.381(11) . ?
C14 C15 1.386(11) . ?
C15 C16 1.389(11) . ?
C15 H15A 0.9500 . ?
C16 C17 1.364(12) . ?
C16 H16A 0.9500 . ?
C17 C18 1.360(12) . ?
C17 H17A 0.9500 . ?
C18 C19 1.405(11) . ?
C18 H18A 0.9500 . ?
C19 H19A 0.9500 . ?
C20 C25 1.364(10) . ?
C20 C21 1.375(11) . ?
C21 C22 1.374(12) . ?
C21 H21A 0.9500 . ?
C22 C23 1.397(15) . ?
C22 H22A 0.9500 . ?
C23 C24 1.356(14) . ?
C23 H23A 0.9500 . ?
C24 C25 1.353(11) . ?
C24 H24A 0.9500 . ?
C25 H25A 0.9500 . ?
C26 H26A 1.0000 . ?
C27 C32 1.398(11) . ?
C27 C28 1.392(11) . ?
C28 C29 1.359(12) . ?
C28 H28A 0.9500 . ?
C29 C30 1.421(14) . ?
C29 H29A 0.9500 . ?
C30 C31 1.411(15) . ?
C30 H30A 0.9500 . ?
C31 C32 1.374(13) . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C34 1.387(10) . ?
C33 C38 1.387(10) . ?
C34 C35 1.406(11) . ?
C34 H34A 0.9500 . ?
C35 C36 1.327(11) . ?
C35 H35A 0.9500 . ?
C36 C37 1.344(10) . ?
C36 H36A 0.9500 . ?
C37 C38 1.398(10) . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 C40 1.362(9) . ?
C39 C44 1.386(11) . ?
C40 C41 1.396(11) . ?
C40 H40A 0.9500 . ?
C41 C42 1.347(12) . ?
C41 H41A 0.9500 . ?
C42 C43 1.388(11) . ?
C42 H42A 0.9500 . ?
C43 C44 1.361(10) . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
C45 C50 1.395(9) . ?
C45 C46 1.414(10) . ?
C46 C47 1.421(10) . ?
C46 H46A 0.9500 . ?
C47 C48 1.401(10) . ?
C47 H47A 0.9500 . ?
C48 C49 1.353(10) . ?
C48 H48A 0.9500 . ?
C49 C50 1.404(10) . ?
C49 H49A 0.9500 . ?
C50 H50A 0.9500 . ?

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
O1 Ba1 B4 79.9(2) . 2_655 ?
O1 Ba1 B2 145.42(19) . . ?
B4 Ba1 B2 95.6(2) 2_655 . ?
O1 Ba1 B1 84.7(2) . 3_665 ?
B4 Ba1 B1 164.6(2) 2_655 3_665 ?
B2 Ba1 B1 96.8(2) . 3_665 ?
O1 Ba1 H1BA 84.1 . . ?
B4 Ba1 H1BA 106.2 2_655 . ?
B2 Ba1 H1BA 64.0 . . ?
B1 Ba1 H1BA 71.5 3_665 . ?
O1 Ba1 H2BA 136.2 . . ?
B4 Ba1 H2BA 79.4 2_655 . ?
B2 Ba1 H2BA 16.7 . . ?
B1 Ba1 H2BA 112.1 3_665 . ?
H1BA Ba1 H2BA 65.5 . . ?
O1 Ba1 H2BC 141.1 . . ?
B4 Ba1 H2BC 112.6 2_655 . ?
B2 Ba1 H2BC 17.5 . . ?
B1 Ba1 H2BC 79.3 3_665 . ?
H1BA Ba1 H2BC 57.2 . . ?
H2BA Ba1 H2BC 33.3 . . ?
O1 Ba2 P4 93.61(3) . . ?
O1 Ba2 P4 93.61(3) . 2_655 ?
P4 Ba2 P4 119.608(7) . 2_655 ?
O1 Ba2 P4 93.61(3) . 3_665 ?
P4 Ba2 P4 119.608(7) . 3_665 ?
P4 Ba2 P4 119.608(7) 2_655 3_665 ?
O1 Ba2 H3BB 130.0 . . ?
P4 Ba2 H3BB 70.3 . . ?
P4 Ba2 H3BB 135.9 2_655 . ?
P4 Ba2 H3BB 59.9 3_665 . ?
O1 Ba2 H4BC 73.8 . . ?
P4 Ba2 H4BC 58.6 . . ?
P4 Ba2 H4BC 166.8 2_655 . ?
P4 Ba2 H4BC 66.4 3_665 . ?
H3BB Ba2 H4BC 57.2 . . ?
C1 P1 C2 112.1(3) . . ?
C1 P1 C8 108.3(4) . . ?
C2 P1 C8 97.2(3) . . ?
C1 P1 B1 121.1(4) . . ?
C2 P1 B1 107.5(4) . . ?
C8 P1 B1 107.9(4) . . ?
C1 P2 C14 107.4(4) . . ?
C1 P2 C20 108.8(4) . . ?
C14 P2 C20 102.8(4) . . ?
C1 P2 B2 120.3(4) . . ?
C14 P2 B2 110.9(4) . . ?
C20 P2 B2 105.2(4) . . ?
C33 P3 C27 101.8(4) . . ?
C33 P3 C26 110.2(4) . . ?
C27 P3 C26 107.9(4) . . ?
C33 P3 B3 111.2(4) . . ?
C27 P3 B3 113.1(5) . . ?
C26 P3 B3 112.1(4) . . ?
C45 P4 C39 99.4(4) . . ?
C45 P4 C26 103.7(3) . . ?
C39 P4 C26 107.9(4) . . ?
C45 P4 Ba2 113.2(2) . . ?
C39 P4 Ba2 136.1(3) . . ?
C26 P4 Ba2 92.6(2) . . ?
Ba1 O1 Ba1 113.13(12) 2_655 3_665 ?
Ba1 O1 Ba1 113.13(12) 2_655 . ?
Ba1 O1 Ba1 113.13(12) 3_665 . ?
Ba1 O1 Ba2 105.51(14) 2_655 . ?
Ba1 O1 Ba2 105.51(14) 3_665 . ?
Ba1 O1 Ba2 105.51(14) . . ?
P1 B1 Ba1 146.0(5) . 2_655 ?
P1 B1 H1BA 109.3 . . ?
Ba1 B1 H1BA 101.0 2_655 . ?
P1 B1 H1BB 109.5 . . ?
Ba1 B1 H1BB 43.5 2_655 . ?
H1BA B1 H1BB 109.5 . . ?
P1 B1 H1BC 109.6 . . ?
Ba1 B1 H1BC 73.0 2_655 . ?
H1BA B1 H1BC 109.5 . . ?
H1BB B1 H1BC 109.5 . . ?
P2 B2 Ba1 144.3(4) . . ?
P2 B2 H2BA 109.6 . . ?
Ba1 B2 H2BA 53.1 . . ?
P2 B2 H2BB 109.5 . . ?
Ba1 B2 H2BB 106.0 . . ?
H2BA B2 H2BB 109.5 . . ?
P2 B2 H2BC 109.4 . . ?
Ba1 B2 H2BC 60.9 . . ?
H2BA B2 H2BC 109.5 . . ?
H2BB B2 H2BC 109.5 . . ?
P3 B3 H3BA 109.6 . . ?
P3 B3 H3BB 109.4 . . ?
H3BA B3 H3BB 109.5 . . ?
P3 B3 H3BC 109.5 . . ?
H3BA B3 H3BC 109.5 . . ?
H3BB B3 H3BC 109.5 . . ?
C26 B4 Ba1 175.0(6) . 3_665 ?
C26 B4 H4BA 109.4 . . ?
Ba1 B4 H4BA 72.5 3_665 . ?
C26 B4 H4BB 109.7 . . ?
Ba1 B4 H4BB 65.4 3_665 . ?
H4BA B4 H4BB 109.5 . . ?
C26 B4 H4BC 109.4 . . ?
Ba1 B4 H4BC 73.8 3_665 . ?
H4BA B4 H4BC 109.5 . . ?
H4BB B4 H4BC 109.5 . . ?
P1 C1 P2 131.3(4) . . ?
P1 C1 H1A 114.3 . . ?
P2 C1 H1A 114.3 . . ?
C3 C2 C7 118.4(7) . . ?
C3 C2 P1 123.0(5) . . ?
C7 C2 P1 118.6(6) . . ?
C2 C3 C4 121.4(8) . . ?
C2 C3 H3A 119.3 . . ?
C4 C3 H3A 119.3 . . ?
C5 C4 C3 119.2(9) . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C4 C5 C6 121.7(8) . . ?
C4 C5 H5A 119.2 . . ?
C6 C5 H5A 119.2 . . ?
C5 C6 C7 118.7(8) . . ?
C5 C6 H6A 120.6 . . ?
C7 C6 H6A 120.6 . . ?
C2 C7 C6 119.9(8) . . ?
C2 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C13 C8 C9 120.3(8) . . ?
C13 C8 P1 119.5(7) . . ?
C9 C8 P1 120.2(6) . . ?
C10 C9 C8 119.1(9) . . ?
C10 C9 H9A 120.5 . . ?
C8 C9 H9A 120.5 . . ?
C9 C10 C11 121.8(9) . . ?
C9 C10 H10A 119.1 . . ?
C11 C10 H10A 119.1 . . ?
C12 C11 C10 118.1(9) . . ?
C12 C11 H11A 120.9 . . ?
C10 C11 H11A 120.9 . . ?
C11 C12 C13 123.3(9) . . ?
C11 C12 H12A 118.4 . . ?
C13 C12 H12A 118.4 . . ?
C8 C13 C12 117.3(8) . . ?
C8 C13 H13A 121.3 . . ?
C12 C13 H13A 121.3 . . ?
C19 C14 C15 116.0(8) . . ?
C19 C14 P2 122.1(7) . . ?
C15 C14 P2 121.9(7) . . ?
C16 C15 C14 122.0(9) . . ?
C16 C15 H15A 119.0 . . ?
C14 C15 H15A 119.0 . . ?
C17 C16 C15 120.9(9) . . ?
C17 C16 H16A 119.5 . . ?
C15 C16 H16A 119.5 . . ?
C18 C17 C16 118.7(9) . . ?
C18 C17 H17A 120.7 . . ?
C16 C17 H17A 120.7 . . ?
C17 C18 C19 120.5(9) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C14 C19 C18 121.9(8) . . ?
C14 C19 H19A 119.1 . . ?
C18 C19 H19A 119.1 . . ?
C25 C20 C21 118.8(8) . . ?
C25 C20 P2 119.2(7) . . ?
C21 C20 P2 121.8(7) . . ?
C20 C21 C22 120.3(10) . . ?
C20 C21 H21A 119.9 . . ?
C22 C21 H21A 119.9 . . ?
C21 C22 C23 118.5(11) . . ?
C21 C22 H22A 120.7 . . ?
C23 C22 H22A 120.7 . . ?
C24 C23 C22 121.1(10) . . ?
C24 C23 H23A 119.5 . . ?
C22 C23 H23A 119.5 . . ?
C25 C24 C23 118.7(10) . . ?
C25 C24 H24A 120.7 . . ?
C23 C24 H24A 120.7 . . ?
C24 C25 C20 122.5(9) . . ?
C24 C25 H25A 118.8 . . ?
C20 C25 H25A 118.8 . . ?
B4 C26 P3 110.1(5) . . ?
B4 C26 P4 104.3(5) . . ?
P3 C26 P4 109.9(4) . . ?
B4 C26 H26A 110.8 . . ?
P3 C26 H26A 110.8 . . ?
P4 C26 H26A 110.8 . . ?
C32 C27 C28 118.1(9) . . ?
C32 C27 P3 117.7(7) . . ?
C28 C27 P3 124.2(7) . . ?
C29 C28 C27 122.4(10) . . ?
C29 C28 H28A 118.8 . . ?
C27 C28 H28A 118.8 . . ?
C28 C29 C30 119.8(11) . . ?
C28 C29 H29A 120.1 . . ?
C30 C29 H29A 120.1 . . ?
C31 C30 C29 118.1(11) . . ?
C31 C30 H30A 121.0 . . ?
C29 C30 H30A 121.0 . . ?
C32 C31 C30 120.5(11) . . ?
C32 C31 H31A 119.7 . . ?
C30 C31 H31A 119.7 . . ?
C31 C32 C27 121.0(10) . . ?
C31 C32 H32A 119.5 . . ?
C27 C32 H32A 119.5 . . ?
C34 C33 C38 118.4(7) . . ?
C34 C33 P3 119.2(7) . . ?
C38 C33 P3 122.3(6) . . ?
C33 C34 C35 120.3(9) . . ?
C33 C34 H34A 119.8 . . ?
C35 C34 H34A 119.8 . . ?
C36 C35 C34 119.6(8) . . ?
C36 C35 H35A 120.2 . . ?
C34 C35 H35A 120.2 . . ?
C35 C36 C37 121.4(8) . . ?
C35 C36 H36A 119.3 . . ?
C37 C36 H36A 119.3 . . ?
C36 C37 C38 121.2(8) . . ?
C36 C37 H37A 119.4 . . ?
C38 C37 H37A 119.4 . . ?
C33 C38 C37 118.6(8) . . ?
C33 C38 H38A 120.7 . . ?
C37 C38 H38A 120.7 . . ?
C40 C39 C44 115.9(7) . . ?
C40 C39 P4 122.3(6) . . ?
C44 C39 P4 121.7(5) . . ?
C39 C40 C41 123.0(8) . . ?
C39 C40 H40A 118.5 . . ?
C41 C40 H40A 118.5 . . ?
C42 C41 C40 119.1(8) . . ?
C42 C41 H41A 120.4 . . ?
C40 C41 H41A 120.4 . . ?
C41 C42 C43 119.8(8) . . ?
C41 C42 H42A 120.1 . . ?
C43 C42 H42A 120.1 . . ?
C44 C43 C42 119.5(9) . . ?
C44 C43 H43A 120.2 . . ?
C42 C43 H43A 120.2 . . ?
C43 C44 C39 122.6(8) . . ?
C43 C44 H44A 118.7 . . ?
C39 C44 H44A 118.7 . . ?
C50 C45 C46 116.7(7) . . ?
C50 C45 P4 127.6(6) . . ?
C46 C45 P4 115.5(5) . . ?
C45 C46 C47 122.0(7) . . ?
C45 C46 H46A 119.0 . . ?
C47 C46 H46A 119.0 . . ?
C48 C47 C46 117.7(8) . . ?
C48 C47 H47A 121.2 . . ?
C46 C47 H47A 121.2 . . ?
C49 C48 C47 121.4(7) . . ?
C49 C48 H48A 119.3 . . ?
C47 C48 H48A 119.3 . . ?
C48 C49 C50 120.5(7) . . ?
C48 C49 H49A 119.7 . . ?
C50 C49 H49A 119.7 . . ?
C45 C50 C49 121.6(8) . . ?
C45 C50 H50A 119.2 . . ?
C49 C50 H50A 119.2 . . ?

_diffrn_measured_fraction_theta_max 0.858
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.858
_refine_diff_density_max         2.292
_refine_diff_density_min         -1.330
_refine_diff_density_rms         0.126



# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.002 5308 918 ' '
2 0.333 0.667 0.136 16 1 ' '
3 0.333 0.667 0.636 16 2 ' '
4 0.667 0.333 0.364 16 2 ' '
5 0.667 0.333 0.864 16 2 ' '
_platon_squeeze_details          
;
;
#=== END


# Attachment 'helmar_goerls.vcf'