 
data_03hur993
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C30 H54 P4'
_chemical_formula_weight          538.61
 
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'
 
_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                    8.913(5)
_cell_length_b                    13.389(8)
_cell_length_c                    14.059(8)
_cell_angle_alpha                 89.53(4)
_cell_angle_beta                  73.95(3)
_cell_angle_gamma                 77.08(3)
_cell_volume                      1569.0(16)
_cell_formula_units_Z             2
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        ?
_exptl_crystal_colour             ?
_exptl_crystal_size_max           0.20
_exptl_crystal_size_mid           0.18
_exptl_crystal_size_min           0.10
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.140
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              588
_exptl_absorpt_coefficient_mu     0.257
_exptl_absorpt_correction_type    none

 
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71069
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source         'rotating anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             4097
_diffrn_reflns_av_R_equivalents   0.0000
_diffrn_reflns_av_sigmaI/netI     0.3818
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        10
_diffrn_reflns_limit_k_min        -15
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        0
_diffrn_reflns_limit_l_max        16
_diffrn_reflns_theta_min          3.02
_diffrn_reflns_theta_max          24.96
_reflns_number_total              4097
_reflns_number_gt                 1244
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_refine_special_details
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² 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/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/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        0
_refine_ls_number_reflns          4097
_refine_ls_number_parameters      305
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.1586
_refine_ls_R_factor_gt            0.0653
_refine_ls_wR_factor_ref          0.1330
_refine_ls_wR_factor_gt           0.0956
_refine_ls_goodness_of_fit_ref    0.663
_refine_ls_restrained_S_all       0.663
_refine_ls_shift/su_max           0.028
_refine_ls_shift/su_mean          0.005
 
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
P2 P 0.8045(3) 0.22459(15) 0.65755(15) 0.0283(5) Uani 1 1 d . . .
P3 P 0.6923(3) 0.34673(15) 0.78016(15) 0.0293(5) Uani 1 1 d . . .
P1 P 0.6330(3) 0.08538(16) 0.60721(16) 0.0333(6) Uani 1 1 d . . .
P4 P 0.8722(3) 0.41607(15) 0.89570(15) 0.0312(6) Uani 1 1 d . . .
C1 C 0.8577(9) 0.0973(6) 0.7045(5) 0.030(2) Uani 1 1 d . . .
C2 C 0.7663(9) 0.0326(5) 0.6805(5) 0.0228(18) Uani 1 1 d . . .
C23 C 0.5124(9) 0.2455(5) 0.9374(5) 0.027(2) Uani 1 1 d . . .
C20 C 0.7702(9) 0.5549(5) 0.6734(5) 0.0314(19) Uiso 1 1 d . . .
H20A H 0.6985 0.5973 0.7318 0.047 Uiso 1 1 calc R . .
H20B H 0.7101 0.5141 0.6475 0.047 Uiso 1 1 calc R . .
H20C H 0.8136 0.5993 0.6223 0.047 Uiso 1 1 calc R . .
C3 C 0.6518(8) 0.2072(5) 0.6061(5) 0.0219(18) Uani 1 1 d . . .
C8 C 1.0114(10) 0.0764(6) 0.7374(6) 0.0320(19) Uiso 1 1 d . . .
C6 C 0.4437(9) 0.3739(5) 0.6203(5) 0.041(2) Uiso 1 1 d . . .
H6A H 0.3740 0.3440 0.6738 0.061 Uiso 1 1 calc R . .
H6B H 0.3788 0.4165 0.5825 0.061 Uiso 1 1 calc R . .
H6C H 0.4990 0.4163 0.6486 0.061 Uiso 1 1 calc R . .
C18 C 0.6627(9) 0.2959(5) 0.9003(5) 0.0282(19) Uiso 1 1 d . . .
C25 C 0.5570(10) 0.1319(6) 0.9545(6) 0.051(3) Uani 1 1 d . . .
H25A H 0.4595 0.1055 0.9755 0.077 Uiso 1 1 calc R . .
H25B H 0.6127 0.1220 1.0062 0.077 Uiso 1 1 calc R . .
H25C H 0.6277 0.0948 0.8929 0.077 Uiso 1 1 calc R . .
C17 C 0.7528(8) 0.3265(5) 0.9537(5) 0.0260(18) Uani 1 1 d . . .
C12 C 0.7692(11) -0.0823(5) 0.6960(6) 0.040(2) Uani 1 1 d . . .
C11 C 1.1388(9) -0.0140(5) 0.6716(6) 0.037(2) Uani 1 1 d . . .
H11A H 1.1673 0.0052 0.6026 0.055 Uiso 1 1 calc R . .
H11B H 1.0942 -0.0751 0.6758 0.055 Uiso 1 1 calc R . .
H11C H 1.2348 -0.0290 0.6951 0.055 Uiso 1 1 calc R . .
C21 C 1.0207(9) 0.4172(5) 0.6108(5) 0.042(2) Uani 1 1 d . . .
H21A H 1.0649 0.4619 0.5603 0.063 Uiso 1 1 calc R . .
H21B H 0.9603 0.3772 0.5841 0.063 Uiso 1 1 calc R . .
H21C H 1.1085 0.3705 0.6292 0.063 Uiso 1 1 calc R . .
C27 C 0.7699(10) 0.3095(6) 1.0582(6) 0.031(2) Uani 1 1 d . . .
C4 C 0.5715(10) 0.2852(6) 0.5494(6) 0.036(2) Uani 1 1 d . . .
C10 C 0.9837(9) 0.0539(5) 0.8470(5) 0.040(2) Uani 1 1 d . . .
H10A H 1.0857 0.0425 0.8637 0.061 Uiso 1 1 calc R . .
H10B H 0.9405 -0.0076 0.8597 0.061 Uiso 1 1 calc R . .
H10C H 0.9073 0.1124 0.8879 0.061 Uiso 1 1 calc R . .
C16 C 0.8403(8) 0.4130(5) 0.7842(5) 0.0175(16) Uani 1 1 d . . .
C19 C 0.9088(9) 0.4828(5) 0.7025(5) 0.0232(18) Uani 1 1 d . . .
C30 C 0.9470(10) 0.2936(6) 1.0593(6) 0.047(3) Uani 1 1 d . . .
H30A H 1.0158 0.2447 1.0048 0.071 Uiso 1 1 calc R . .
H30B H 0.9584 0.2667 1.1226 0.071 Uiso 1 1 calc R . .
H30C H 0.9787 0.3594 1.0512 0.071 Uiso 1 1 calc R . .
C26 C 0.3893(8) 0.3087(5) 1.0272(5) 0.032(2) Uani 1 1 d . . .
H26A H 0.2947 0.2793 1.0472 0.049 Uiso 1 1 calc R . .
H26B H 0.3574 0.3798 1.0096 0.049 Uiso 1 1 calc R . .
H26C H 0.4370 0.3075 1.0823 0.049 Uiso 1 1 calc R . .
C24 C 0.4188(9) 0.2570(6) 0.8572(5) 0.040(2) Uani 1 1 d . . .
H24A H 0.4886 0.2199 0.7953 0.059 Uiso 1 1 calc R . .
H24B H 0.3857 0.3298 0.8454 0.059 Uiso 1 1 calc R . .
H24C H 0.3237 0.2285 0.8806 0.059 Uiso 1 1 calc R . .
C13 C 0.6019(10) -0.0987(6) 0.7203(6) 0.051(3) Uani 1 1 d . . .
H13A H 0.6034 -0.1701 0.7368 0.077 Uiso 1 1 calc R . .
H13B H 0.5600 -0.0840 0.6629 0.077 Uiso 1 1 calc R . .
H13C H 0.5330 -0.0527 0.7770 0.077 Uiso 1 1 calc R . .
C15 C 0.8440(11) -0.1330(5) 0.7780(6) 0.045(2) Uani 1 1 d . . .
H15A H 0.7912 -0.0929 0.8411 0.067 Uiso 1 1 calc R . .
H15B H 0.9590 -0.1346 0.7590 0.067 Uiso 1 1 calc R . .
H15C H 0.8287 -0.2032 0.7852 0.067 Uiso 1 1 calc R . .
C7 C 0.4831(10) 0.2389(6) 0.4900(6) 0.051(3) Uani 1 1 d . . .
H7A H 0.5563 0.1793 0.4490 0.076 Uiso 1 1 calc R . .
H7B H 0.4435 0.2901 0.4472 0.076 Uiso 1 1 calc R . .
H7C H 0.3924 0.2172 0.5353 0.076 Uiso 1 1 calc R . .
C22 C 0.9989(9) 0.5512(5) 0.7379(5) 0.039(2) Uani 1 1 d . . .
H22A H 1.0418 0.5927 0.6837 0.058 Uiso 1 1 calc R . .
H22B H 1.0875 0.5088 0.7590 0.058 Uiso 1 1 calc R . .
H22C H 0.9258 0.5966 0.7939 0.058 Uiso 1 1 calc R . .
C28 C 0.7230(9) 0.2138(6) 1.1113(6) 0.047(3) Uani 1 1 d . . .
H28A H 0.6069 0.2211 1.1259 0.071 Uiso 1 1 calc R . .
H28B H 0.7537 0.2080 1.1732 0.071 Uiso 1 1 calc R . .
H28C H 0.7790 0.1519 1.0680 0.071 Uiso 1 1 calc R . .
C9 C 1.0882(9) 0.1685(5) 0.7226(5) 0.036(2) Uani 1 1 d . . .
H9A H 1.1177 0.1821 0.6520 0.055 Uiso 1 1 calc R . .
H9B H 1.1846 0.1537 0.7457 0.055 Uiso 1 1 calc R . .
H9C H 1.0118 0.2288 0.7604 0.055 Uiso 1 1 calc R . .
C29 C 0.6732(10) 0.4074(6) 1.1287(6) 0.045(2) Uani 1 1 d . . .
H29A H 0.7079 0.4682 1.0999 0.068 Uiso 1 1 calc R . .
H29B H 0.6931 0.3987 1.1938 0.068 Uiso 1 1 calc R . .
H29C H 0.5582 0.4161 1.1363 0.068 Uiso 1 1 calc R . .
C14 C 0.8734(9) -0.1444(5) 0.5946(5) 0.032(2) Uani 1 1 d . . .
H14A H 0.8700 -0.2169 0.6000 0.049 Uiso 1 1 calc R . .
H14B H 0.9848 -0.1381 0.5809 0.049 Uiso 1 1 calc R . .
H14C H 0.8298 -0.1166 0.5406 0.049 Uiso 1 1 calc R . .
C5 C 0.6914(9) 0.3362(5) 0.4736(5) 0.044(3) Uani 1 1 d . . .
H5A H 0.7498 0.3693 0.5087 0.066 Uiso 1 1 calc R . .
H5B H 0.6321 0.3878 0.4393 0.066 Uiso 1 1 calc R . .
H5C H 0.7677 0.2837 0.4251 0.066 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
P2 C3 1.766(7) . ?
P2 C1 1.833(7) . ?
P2 P3 2.238(3) . ?
P3 C16 1.760(6) . ?
P3 C18 1.789(7) . ?
P1 C3 1.676(6) . ?
P1 C2 1.806(7) . ?
P4 C16 1.671(6) . ?
P4 C17 1.820(7) . ?
C1 C2 1.414(9) . ?
C1 C8 1.531(10) . ?
C2 C12 1.547(8) . ?
C23 C25 1.520(9) . ?
C23 C26 1.533(9) . ?
C23 C24 1.566(9) . ?
C23 C18 1.592(9) . ?
C20 C19 1.538(9) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C3 C4 1.485(9) . ?
C8 C10 1.531(9) . ?
C8 C9 1.526(8) . ?
C8 C11 1.559(10) . ?
C6 C4 1.578(10) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C18 C17 1.365(9) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C17 C27 1.528(9) . ?
C12 C13 1.501(10) . ?
C12 C15 1.563(10) . ?
C12 C14 1.590(10) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C21 C19 1.531(9) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C27 C28 1.558(8) . ?
C27 C29 1.577(10) . ?
C27 C30 1.549(10) . ?
C4 C7 1.515(9) . ?
C4 C5 1.558(9) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C16 C19 1.554(7) . ?
C19 C22 1.513(8) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 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
C3 P2 C1 100.1(3) . . ?
C3 P2 P3 107.3(3) . . ?
C1 P2 P3 112.1(3) . . ?
C16 P3 C18 98.9(3) . . ?
C16 P3 P2 106.8(3) . . ?
C18 P3 P2 112.6(3) . . ?
C3 P1 C2 99.6(3) . . ?
C16 P4 C17 98.1(3) . . ?
C2 C1 C8 133.1(7) . . ?
C2 C1 P2 110.1(5) . . ?
C8 C1 P2 114.9(5) . . ?
C1 C2 C12 132.0(7) . . ?
C1 C2 P1 116.9(5) . . ?
C12 C2 P1 110.9(5) . . ?
C25 C23 C26 113.3(6) . . ?
C25 C23 C24 107.2(6) . . ?
C26 C23 C24 102.8(6) . . ?
C25 C23 C18 113.8(6) . . ?
C26 C23 C18 110.2(6) . . ?
C24 C23 C18 108.9(5) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C4 C3 P1 122.3(5) . . ?
C4 C3 P2 123.9(5) . . ?
P1 C3 P2 112.6(4) . . ?
C10 C8 C1 113.4(6) . . ?
C10 C8 C9 106.2(6) . . ?
C1 C8 C9 111.2(6) . . ?
C10 C8 C11 110.0(6) . . ?
C1 C8 C11 110.0(7) . . ?
C9 C8 C11 105.7(6) . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C17 C18 C23 129.0(6) . . ?
C17 C18 P3 113.0(5) . . ?
C23 C18 P3 116.3(5) . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C18 C17 C27 134.7(7) . . ?
C18 C17 P4 116.0(5) . . ?
C27 C17 P4 109.0(5) . . ?
C13 C12 C2 110.0(7) . . ?
C13 C12 C15 106.7(6) . . ?
C2 C12 C15 117.4(6) . . ?
C13 C12 C14 109.1(6) . . ?
C2 C12 C14 107.3(5) . . ?
C15 C12 C14 106.1(7) . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C27 C28 118.7(6) . . ?
C17 C27 C29 109.9(6) . . ?
C28 C27 C29 107.8(6) . . ?
C17 C27 C30 111.4(6) . . ?
C28 C27 C30 101.6(6) . . ?
C29 C27 C30 106.5(6) . . ?
C3 C4 C7 111.7(6) . . ?
C3 C4 C5 112.9(7) . . ?
C7 C4 C5 106.2(6) . . ?
C3 C4 C6 111.5(7) . . ?
C7 C4 C6 106.8(7) . . ?
C5 C4 C6 107.3(6) . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C19 C16 P4 121.0(5) . . ?
C19 C16 P3 124.5(5) . . ?
P4 C16 P3 113.2(3) . . ?
C22 C19 C20 106.2(6) . . ?
C22 C19 C21 109.2(6) . . ?
C20 C19 C21 109.2(6) . . ?
C22 C19 C16 112.3(6) . . ?
C20 C19 C16 109.6(6) . . ?
C21 C19 C16 110.2(5) . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C23 C26 H26A 109.5 . . ?
C23 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C23 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C27 C29 H29A 109.5 . . ?
C27 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C27 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
 
_diffrn_measured_fraction_theta_max    0.745
_diffrn_reflns_theta_full              24.96
_diffrn_measured_fraction_theta_full   0.745
_refine_diff_density_max    0.412
_refine_diff_density_min   -0.385
_refine_diff_density_rms    0.066
