# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#                                CCDC 
# 
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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
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
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#  data retrieval see:
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#  from this site to visualise CIF-encoded structures and 
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data_FO4996

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H33 N3'
_chemical_formula_sum            'C26 H33 N3'
_chemical_formula_weight         387.55

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   7.8983(2)
_cell_length_b                   33.9768(8)
_cell_length_c                   8.7134(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.311(1)
_cell_angle_gamma                90.00
_cell_volume                     2192.93(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    15947
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             840
_exptl_absorpt_coefficient_mu    0.069
_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            15947
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.40
_diffrn_reflns_theta_max         27.48
_reflns_number_total             4975
_reflns_number_gt                4591
_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 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 > 2sigma(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)+(0.0528P)²+0.7182P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4975
_refine_ls_number_parameters     394
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0399
_refine_ls_wR_factor_ref         0.1069
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_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
N1 N 0.55049(12) 0.08505(3) 0.49472(10) 0.01742(18) Uani 1 1 d . . .
H1N1 H 0.4548(19) 0.0768(4) 0.5153(16) 0.021(3) Uiso 1 1 d . . .
N2 N 0.68301(11) 0.13016(2) 0.38075(10) 0.01660(18) Uani 1 1 d . . .
C1 C 0.54008(13) 0.11919(3) 0.40631(11) 0.0157(2) Uani 1 1 d . . .
C2 C 0.35285(13) 0.13991(3) 0.35226(12) 0.0177(2) Uani 1 1 d . . .
N3 N 0.49815(12) 0.02712(3) 0.67777(11) 0.01948(19) Uani 1 1 d . . .
C3 C 0.27807(15) 0.14490(3) 0.16532(13) 0.0227(2) Uani 1 1 d . . .
H3C H 0.3598(18) 0.1611(4) 0.1276(16) 0.024(3) Uiso 1 1 d . . .
H3B H 0.2611(19) 0.1194(4) 0.1083(18) 0.031(4) Uiso 1 1 d . . .
H3A H 0.160(2) 0.1584(4) 0.1337(17) 0.028(3) Uiso 1 1 d . . .
C4 C 0.37479(15) 0.18077(3) 0.43189(14) 0.0215(2) Uani 1 1 d . . .
H4B H 0.4580(19) 0.1977(4) 0.3980(17) 0.027(3) Uiso 1 1 d . . .
H4C H 0.256(2) 0.1945(4) 0.3976(18) 0.031(4) Uiso 1 1 d . . .
H4A H 0.4205(19) 0.1790(4) 0.5519(18) 0.028(3) Uiso 1 1 d . . .
C5 C 0.21202(14) 0.11715(3) 0.40268(14) 0.0213(2) Uani 1 1 d . . .
H5C H 0.2473(18) 0.1146(4) 0.5238(17) 0.025(3) Uiso 1 1 d . . .
H5B H 0.1900(19) 0.0901(4) 0.3544(17) 0.027(3) Uiso 1 1 d . . .
H5A H 0.0963(19) 0.1322(4) 0.3634(17) 0.027(3) Uiso 1 1 d . . .
C6 C 0.69939(13) 0.06095(3) 0.57037(12) 0.0170(2) Uani 1 1 d . . .
C7 C 0.86848(15) 0.06417(3) 0.55802(14) 0.0234(2) Uani 1 1 d . . .
H7 H 0.8913(19) 0.0840(4) 0.4918(17) 0.029(3) Uiso 1 1 d . . .
C8 C 1.00758(16) 0.03754(4) 0.64178(16) 0.0290(3) Uani 1 1 d . . .
H8 H 1.125(2) 0.0402(5) 0.6282(18) 0.036(4) Uiso 1 1 d . . .
C9 C 0.98018(15) 0.00820(3) 0.73778(15) 0.0263(2) Uani 1 1 d . . .
H9 H 1.076(2) -0.0106(4) 0.7969(18) 0.032(4) Uiso 1 1 d . . .
C10 C 0.80888(14) 0.00396(3) 0.75395(12) 0.0190(2) Uani 1 1 d . . .
C11 C 0.77184(15) -0.02513(3) 0.85373(13) 0.0220(2) Uani 1 1 d . . .
H11 H 0.870(2) -0.0424(4) 0.9161(18) 0.031(4) Uiso 1 1 d . . .
C12 C 0.60337(16) -0.02765(3) 0.86266(14) 0.0244(2) Uani 1 1 d . . .
H12 H 0.573(2) -0.0469(5) 0.9311(19) 0.035(4) Uiso 1 1 d . . .
C13 C 0.46997(15) -0.00099(3) 0.77069(14) 0.0238(2) Uani 1 1 d . . .
H13 H 0.3497(19) -0.0028(4) 0.7737(16) 0.026(3) Uiso 1 1 d . . .
C14 C 0.66679(13) 0.03002(3) 0.66918(12) 0.0165(2) Uani 1 1 d . . .
C15 C 0.71914(13) 0.16304(3) 0.29974(12) 0.0166(2) Uani 1 1 d . . .
C16 C 0.70237(14) 0.15959(3) 0.13330(12) 0.0190(2) Uani 1 1 d . . .
C17 C 0.76298(15) 0.19056(3) 0.06061(14) 0.0246(2) Uani 1 1 d . . .
H17 H 0.753(2) 0.1884(4) -0.0555(18) 0.032(4) Uiso 1 1 d . . .
C18 C 0.84168(16) 0.22372(3) 0.14920(15) 0.0275(2) Uani 1 1 d . . .
H18 H 0.884(2) 0.2451(4) 0.0959(18) 0.035(4) Uiso 1 1 d . . .
C19 C 0.86216(15) 0.22631(3) 0.31370(15) 0.0248(2) Uani 1 1 d . . .
H19 H 0.9205(19) 0.2494(4) 0.3759(17) 0.027(3) Uiso 1 1 d . . .
C20 C 0.80335(14) 0.19637(3) 0.39228(13) 0.0193(2) Uani 1 1 d . . .
C21 C 0.62946(15) 0.12188(3) 0.03968(12) 0.0209(2) Uani 1 1 d . . .
H21 H 0.5508(19) 0.1092(4) 0.0926(17) 0.027(3) Uiso 1 1 d . . .
C22 C 0.5138(2) 0.12856(4) -0.13936(15) 0.0344(3) Uani 1 1 d . . .
H22C H 0.587(2) 0.1378(5) -0.205(2) 0.046(4) Uiso 1 1 d . . .
H22B H 0.415(2) 0.1488(5) -0.151(2) 0.048(5) Uiso 1 1 d . . .
H22A H 0.456(2) 0.1030(5) -0.193(2) 0.050(5) Uiso 1 1 d . . .
C23 C 0.78292(17) 0.09308(4) 0.05193(16) 0.0306(3) Uani 1 1 d . . .
H23A H 0.732(2) 0.0676(5) -0.009(2) 0.041(4) Uiso 1 1 d . . .
H23B H 0.853(2) 0.0863(5) 0.172(2) 0.041(4) Uiso 1 1 d . . .
H23C H 0.866(2) 0.1048(5) -0.002(2) 0.042(4) Uiso 1 1 d . . .
C24 C 0.83760(15) 0.19820(3) 0.57514(13) 0.0223(2) Uani 1 1 d . . .
H24 H 0.7427(18) 0.1821(4) 0.5956(16) 0.022(3) Uiso 1 1 d . . .
C25 C 1.02071(17) 0.17978(4) 0.67279(15) 0.0319(3) Uani 1 1 d . . .
H25C H 1.042(2) 0.1815(5) 0.792(2) 0.043(4) Uiso 1 1 d . . .
H25B H 1.120(2) 0.1953(5) 0.653(2) 0.046(4) Uiso 1 1 d . . .
H25A H 1.028(2) 0.1517(5) 0.6400(19) 0.039(4) Uiso 1 1 d . . .
C26 C 0.8257(2) 0.23988(4) 0.63664(18) 0.0345(3) Uani 1 1 d . . .
H26C H 0.929(2) 0.2562(5) 0.6324(19) 0.039(4) Uiso 1 1 d . . .
H26B H 0.829(2) 0.2383(5) 0.752(2) 0.039(4) Uiso 1 1 d . . .
H26A H 0.711(2) 0.2532(5) 0.569(2) 0.047(4) Uiso 1 1 d . . .


_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
N1 C1 1.3789(13) . ?
N1 C6 1.3965(12) . ?
N1 H1N1 0.881(14) . ?
N2 C1 1.2796(13) . ?
N2 C15 1.4027(12) . ?
C1 C2 1.5559(13) . ?
C2 C4 1.5348(14) . ?
C2 C3 1.5372(14) . ?
C2 C5 1.5386(14) . ?
N3 C13 1.3201(14) . ?
N3 C14 1.3633(13) . ?
C3 H3C 0.988(14) . ?
C3 H3B 0.985(15) . ?
C3 H3A 0.988(14) . ?
C4 H4B 0.991(15) . ?
C4 H4C 0.999(15) . ?
C4 H4A 0.983(15) . ?
C5 H5C 0.998(14) . ?
C5 H5B 1.002(14) . ?
C5 H5A 0.999(14) . ?
C6 C7 1.3809(15) . ?
C6 C14 1.4374(13) . ?
C7 C8 1.4146(15) . ?
C7 H7 0.944(14) . ?
C8 C9 1.3660(16) . ?
C8 H8 0.980(16) . ?
C9 C10 1.4155(15) . ?
C9 H9 0.989(15) . ?
C10 C11 1.4125(14) . ?
C10 C14 1.4190(14) . ?
C11 C12 1.3622(16) . ?
C11 H11 0.975(15) . ?
C12 C13 1.4094(16) . ?
C12 H12 0.968(16) . ?
C13 H13 0.962(14) . ?
C15 C16 1.4146(14) . ?
C15 C20 1.4153(14) . ?
C16 C17 1.3957(15) . ?
C16 C21 1.5207(14) . ?
C17 C18 1.3850(17) . ?
C17 H17 0.989(15) . ?
C18 C19 1.3883(17) . ?
C18 H18 0.979(15) . ?
C19 C20 1.3928(15) . ?
C19 H19 0.974(14) . ?
C20 C24 1.5221(15) . ?
C21 C22 1.5265(15) . ?
C21 C23 1.5324(15) . ?
C21 H21 0.991(14) . ?
C22 H22C 0.993(18) . ?
C22 H22B 1.016(18) . ?
C22 H22A 1.018(18) . ?
C23 H23A 1.022(16) . ?
C23 H23B 1.027(16) . ?
C23 H23C 1.012(17) . ?
C24 C26 1.5288(16) . ?
C24 C25 1.5339(16) . ?
C24 H24 0.993(13) . ?
C25 H25C 0.998(17) . ?
C25 H25B 1.008(18) . ?
C25 H25A 1.002(16) . ?
C26 H26C 0.997(16) . ?
C26 H26B 1.000(16) . ?
C26 H26A 1.001(18) . ?

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
C1 N1 C6 129.35(9) . . ?
C1 N1 H1N1 119.5(9) . . ?
C6 N1 H1N1 111.0(9) . . ?
C1 N2 C15 131.71(9) . . ?
N2 C1 N1 117.20(9) . . ?
N2 C1 C2 128.22(9) . . ?
N1 C1 C2 114.57(8) . . ?
C4 C2 C3 108.71(8) . . ?
C4 C2 C5 107.75(9) . . ?
C3 C2 C5 107.94(8) . . ?
C4 C2 C1 109.04(8) . . ?
C3 C2 C1 110.24(8) . . ?
C5 C2 C1 113.05(8) . . ?
C13 N3 C14 117.50(9) . . ?
C2 C3 H3C 111.1(8) . . ?
C2 C3 H3B 111.8(8) . . ?
H3C C3 H3B 108.3(12) . . ?
C2 C3 H3A 108.9(8) . . ?
H3C C3 H3A 108.1(11) . . ?
H3B C3 H3A 108.6(12) . . ?
C2 C4 H4B 111.8(8) . . ?
C2 C4 H4C 109.9(8) . . ?
H4B C4 H4C 107.1(12) . . ?
C2 C4 H4A 111.5(8) . . ?
H4B C4 H4A 108.4(12) . . ?
H4C C4 H4A 107.9(12) . . ?
C2 C5 H5C 112.4(8) . . ?
C2 C5 H5B 112.3(8) . . ?
H5C C5 H5B 108.1(11) . . ?
C2 C5 H5A 108.1(8) . . ?
H5C C5 H5A 107.0(11) . . ?
H5B C5 H5A 108.7(11) . . ?
C7 C6 N1 126.56(9) . . ?
C7 C6 C14 118.93(9) . . ?
N1 C6 C14 114.51(9) . . ?
C6 C7 C8 120.54(10) . . ?
C6 C7 H7 120.0(9) . . ?
C8 C7 H7 119.5(9) . . ?
C9 C8 C7 121.52(11) . . ?
C9 C8 H8 120.0(9) . . ?
C7 C8 H8 118.5(9) . . ?
C8 C9 C10 119.70(10) . . ?
C8 C9 H9 122.3(9) . . ?
C10 C9 H9 118.0(9) . . ?
C11 C10 C9 122.81(9) . . ?
C11 C10 C14 117.50(9) . . ?
C9 C10 C14 119.69(9) . . ?
C12 C11 C10 119.62(10) . . ?
C12 C11 H11 122.3(9) . . ?
C10 C11 H11 118.0(9) . . ?
C11 C12 C13 118.65(10) . . ?
C11 C12 H12 122.0(9) . . ?
C13 C12 H12 119.3(9) . . ?
N3 C13 C12 124.18(10) . . ?
N3 C13 H13 116.2(8) . . ?
C12 C13 H13 119.6(8) . . ?
N3 C14 C10 122.52(9) . . ?
N3 C14 C6 117.86(9) . . ?
C10 C14 C6 119.62(9) . . ?
N2 C15 C16 119.15(9) . . ?
N2 C15 C20 119.22(9) . . ?
C16 C15 C20 120.56(9) . . ?
C17 C16 C15 118.56(10) . . ?
C17 C16 C21 121.15(10) . . ?
C15 C16 C21 120.19(9) . . ?
C18 C17 C16 121.23(10) . . ?
C18 C17 H17 119.4(9) . . ?
C16 C17 H17 119.3(9) . . ?
C17 C18 C19 119.74(10) . . ?
C17 C18 H18 119.9(9) . . ?
C19 C18 H18 120.4(9) . . ?
C18 C19 C20 121.46(10) . . ?
C18 C19 H19 119.3(8) . . ?
C20 C19 H19 119.3(8) . . ?
C19 C20 C15 118.38(10) . . ?
C19 C20 C24 121.10(9) . . ?
C15 C20 C24 120.44(9) . . ?
C16 C21 C22 113.82(9) . . ?
C16 C21 C23 110.95(9) . . ?
C22 C21 C23 110.13(10) . . ?
C16 C21 H21 107.4(8) . . ?
C22 C21 H21 106.9(8) . . ?
C23 C21 H21 107.3(8) . . ?
C21 C22 H22C 111.9(10) . . ?
C21 C22 H22B 111.8(10) . . ?
H22C C22 H22B 107.8(14) . . ?
C21 C22 H22A 110.9(10) . . ?
H22C C22 H22A 105.3(14) . . ?
H22B C22 H22A 108.9(14) . . ?
C21 C23 H23A 110.0(9) . . ?
C21 C23 H23B 110.5(9) . . ?
H23A C23 H23B 108.3(13) . . ?
C21 C23 H23C 109.9(9) . . ?
H23A C23 H23C 107.3(13) . . ?
H23B C23 H23C 110.7(13) . . ?
C20 C24 C26 113.23(10) . . ?
C20 C24 C25 110.78(9) . . ?
C26 C24 C25 110.15(10) . . ?
C20 C24 H24 107.1(8) . . ?
C26 C24 H24 107.8(8) . . ?
C25 C24 H24 107.5(8) . . ?
C24 C25 H25C 109.9(9) . . ?
C24 C25 H25B 109.3(10) . . ?
H25C C25 H25B 106.9(14) . . ?
C24 C25 H25A 111.4(9) . . ?
H25C C25 H25A 110.3(13) . . ?
H25B C25 H25A 108.8(13) . . ?
C24 C26 H26C 110.6(9) . . ?
C24 C26 H26B 108.7(9) . . ?
H26C C26 H26B 109.2(13) . . ?
C24 C26 H26A 111.5(10) . . ?
H26C C26 H26A 108.1(13) . . ?
H26B C26 H26A 108.7(13) . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.041
_database_code_depnum_ccdc_archive 'CCDC 991548'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_FO5291

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H31 N3'
_chemical_formula_sum            'C22 H31 N3'
_chemical_formula_weight         337.50

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'


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

_cell_length_a                   14.0088(3)
_cell_length_b                   17.7217(4)
_cell_length_c                   8.4023(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.899(1)
_cell_angle_gamma                90.00
_cell_volume                     2033.31(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    12935
_cell_measurement_theta_min      2.30
_cell_measurement_theta_max      27.53

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.043
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.102
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             736
_exptl_absorpt_coefficient_mu    0.065
_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            12935
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0306
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.30
_diffrn_reflns_theta_max         27.53
_reflns_number_total             4660
_reflns_number_gt                3853
_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 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 > 2sigma(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)+(0.0812P)²+1.9028P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4660
_refine_ls_number_parameters     339
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0740
_refine_ls_wR_factor_ref         0.2023
_refine_ls_wR_factor_gt          0.1920
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.000
_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
N2 N 0.73467(12) 0.95038(10) 0.0665(2) 0.0288(4) Uani 1 1 d . . .
N1 N 0.74477(14) 0.83798(10) 0.2032(2) 0.0308(4) Uani 1 1 d . . .
H1N1 H 0.778(2) 0.8010(18) 0.244(4) 0.053(9) Uiso 1 1 d . . .
N3 N 0.63173(14) 0.76651(11) 0.2930(3) 0.0392(5) Uani 1 1 d . . .
C1 C 0.78759(15) 0.89393(11) 0.1339(3) 0.0284(4) Uani 1 1 d . A .
C2 C 0.89897(15) 0.88285(12) 0.1503(3) 0.0305(5) Uani 1 1 d . . .
C3 C 0.9257(3) 0.8784(2) -0.0133(4) 0.0394(9) Uani 0.680(4) 1 d P A 1
H3A H 0.9380 0.9294 -0.0497 0.059 Uiso 0.680(4) 1 calc PR A 1
H3B H 0.8717 0.8554 -0.0929 0.059 Uiso 0.680(4) 1 calc PR A 1
H3C H 0.9848 0.8477 -0.0039 0.059 Uiso 0.680(4) 1 calc PR A 1
C4 C 0.9549(2) 0.95056(18) 0.2506(4) 0.0338(8) Uani 0.680(4) 1 d P A 1
H4A H 0.9076 0.9845 0.2838 0.051 Uiso 0.680(4) 1 calc PR A 1
H4B H 0.9915 0.9783 0.1826 0.051 Uiso 0.680(4) 1 calc PR A 1
H4C H 1.0004 0.9312 0.3478 0.051 Uiso 0.680(4) 1 calc PR A 1
C5 C 0.9407(2) 0.81116(19) 0.2496(5) 0.0364(8) Uani 0.680(4) 1 d P A 1
H5A H 0.9581 0.8235 0.3662 0.055 Uiso 0.680(4) 1 calc PR A 1
H5B H 0.9992 0.7938 0.2145 0.055 Uiso 0.680(4) 1 calc PR A 1
H5C H 0.8911 0.7712 0.2305 0.055 Uiso 0.680(4) 1 calc PR A 1
C3A C 0.9053(7) 0.8064(5) 0.0542(16) 0.066(3) Uani 0.320(4) 1 d P A 2
H3AA H 0.8393 0.7863 0.0131 0.099 Uiso 0.320(4) 1 calc PR A 2
H3AB H 0.9446 0.7695 0.1280 0.099 Uiso 0.320(4) 1 calc PR A 2
H3AC H 0.9361 0.8161 -0.0377 0.099 Uiso 0.320(4) 1 calc PR A 2
C4A C 0.9430(5) 0.9421(5) 0.0607(10) 0.044(2) Uani 0.320(4) 1 d P A 2
H4AA H 0.9413 0.9910 0.1144 0.067 Uiso 0.320(4) 1 calc PR A 2
H4AB H 0.9053 0.9452 -0.0524 0.067 Uiso 0.320(4) 1 calc PR A 2
H4AC H 1.0110 0.9287 0.0617 0.067 Uiso 0.320(4) 1 calc PR A 2
C5A C 0.9422(6) 0.8783(8) 0.3182(11) 0.069(4) Uani 0.320(4) 1 d P A 2
H5AA H 0.9355 0.9269 0.3701 0.103 Uiso 0.320(4) 1 calc PR A 2
H5AB H 1.0117 0.8658 0.3330 0.103 Uiso 0.320(4) 1 calc PR A 2
H5AC H 0.9093 0.8390 0.3683 0.103 Uiso 0.320(4) 1 calc PR A 2
C6 C 0.64804(15) 0.83125(11) 0.2184(2) 0.0269(4) Uani 1 1 d . . .
C7 C 0.57651(16) 0.88402(11) 0.1669(3) 0.0307(5) Uani 1 1 d . . .
H7 H 0.5834 0.9290 0.1220 0.065(9) Uiso 1 1 d R . .
C8 C 0.48460(19) 0.86989(15) 0.1944(3) 0.0436(6) Uani 1 1 d . . .
H8 H 0.435(2) 0.9077(17) 0.161(4) 0.054(8) Uiso 1 1 d . . .
C9 C 0.46620(18) 0.80500(16) 0.2706(4) 0.0485(7) Uani 1 1 d . . .
H9 H 0.402(2) 0.7934(18) 0.292(4) 0.060(9) Uiso 1 1 d . . .
C10 C 0.54105(19) 0.75431(15) 0.3187(4) 0.0471(6) Uani 1 1 d . . .
H10 H 0.533(2) 0.7077(17) 0.379(3) 0.050(8) Uiso 1 1 d . . .
C11 C 0.75946(14) 1.01090(11) -0.0260(2) 0.0263(4) Uani 1 1 d . . .
C12 C 0.74780(15) 1.00219(12) -0.1961(3) 0.0306(5) Uani 1 1 d . . .
C13 C 0.76333(17) 1.06457(13) -0.2872(3) 0.0341(5) Uani 1 1 d . . .
H13 H 0.758(2) 1.0594(16) -0.400(3) 0.046(8) Uiso 1 1 d . . .
C14 C 0.78683(16) 1.13408(13) -0.2164(3) 0.0353(5) Uani 1 1 d . . .
H14 H 0.799(2) 1.1801(15) -0.285(3) 0.043(7) Uiso 1 1 d . . .
C15 C 0.79487(16) 1.14313(12) -0.0502(3) 0.0319(5) Uani 1 1 d . . .
H15 H 0.813(2) 1.1940(17) 0.003(4) 0.054(8) Uiso 1 1 d . . .
C16 C 0.78078(14) 1.08221(11) 0.0475(3) 0.0273(4) Uani 1 1 d . . .
C17 C 0.71374(18) 0.92795(13) -0.2801(3) 0.0374(5) Uani 1 1 d . . .
H17 H 0.724(2) 0.8880(16) -0.197(4) 0.048(8) Uiso 1 1 d . . .
C18 C 0.6039(2) 0.93127(18) -0.3537(5) 0.0593(8) Uani 1 1 d . . .
H18C H 0.567(2) 0.9391(18) -0.271(4) 0.054(9) Uiso 1 1 d . . .
H18B H 0.594(3) 0.974(2) -0.437(4) 0.076(11) Uiso 1 1 d . . .
H18A H 0.578(2) 0.882(2) -0.408(4) 0.070(10) Uiso 1 1 d . . .
C19 C 0.7704(3) 0.90594(19) -0.4085(4) 0.0561(8) Uani 1 1 d . . .
H19C H 0.753(2) 0.8516(17) -0.448(3) 0.049(8) Uiso 1 1 d . . .
H19B H 0.754(3) 0.939(2) -0.506(5) 0.086(12) Uiso 1 1 d . . .
H19A H 0.848(3) 0.9139(19) -0.365(4) 0.070(10) Uiso 1 1 d . . .
C20 C 0.78210(16) 1.09391(12) 0.2272(3) 0.0324(5) Uani 1 1 d . . .
H20 H 0.7880(17) 1.0464(14) 0.280(3) 0.030(6) Uiso 1 1 d . . .
C21 C 0.6834(3) 1.1258(2) 0.2430(4) 0.0622(10) Uani 1 1 d . . .
H21C H 0.682(2) 1.1367(18) 0.353(4) 0.062(9) Uiso 1 1 d . . .
H21B H 0.627(3) 1.092(2) 0.204(4) 0.066(10) Uiso 1 1 d . . .
H21A H 0.668(2) 1.173(2) 0.173(4) 0.070(10) Uiso 1 1 d . . .
C22 C 0.8658(3) 1.14404(17) 0.3153(4) 0.0553(8) Uani 1 1 d . . .
H22C H 0.867(2) 1.1483(17) 0.438(4) 0.055(8) Uiso 1 1 d . . .
H22B H 0.862(3) 1.198(2) 0.263(5) 0.089(12) Uiso 1 1 d . . .
H22A H 0.937(3) 1.123(2) 0.297(4) 0.081(11) Uiso 1 1 d . . .


_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
N2 C1 1.298(3) . ?
N2 C11 1.412(3) . ?
N1 C1 1.356(3) . ?
N1 C6 1.394(3) . ?
N1 H1N1 0.83(3) . ?
N3 C6 1.351(3) . ?
N3 C10 1.353(3) . ?
C1 C2 1.548(3) . ?
C2 C5A 1.408(9) . ?
C2 C4A 1.502(8) . ?
C2 C3 1.506(4) . ?
C2 C5 1.560(4) . ?
C2 C4 1.571(4) . ?
C2 C3A 1.590(9) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6 C7 1.368(3) . ?
C7 C8 1.381(3) . ?
C7 H7 0.8957 . ?
C8 C9 1.368(4) . ?
C8 H8 0.96(3) . ?
C9 C10 1.371(4) . ?
C9 H9 0.98(3) . ?
C10 H10 0.99(3) . ?
C11 C16 1.409(3) . ?
C11 C12 1.410(3) . ?
C12 C13 1.389(3) . ?
C12 C17 1.519(3) . ?
C13 C14 1.376(3) . ?
C13 H13 0.94(3) . ?
C14 C15 1.385(3) . ?
C14 H14 1.03(3) . ?
C15 C16 1.397(3) . ?
C15 H15 1.01(3) . ?
C16 C20 1.520(3) . ?
C17 C18 1.526(4) . ?
C17 C19 1.526(4) . ?
C17 H17 0.98(3) . ?
C18 H18C 0.96(3) . ?
C18 H18B 1.02(4) . ?
C18 H18A 1.01(4) . ?
C19 H19C 1.03(3) . ?
C19 H19B 0.99(4) . ?
C19 H19A 1.07(4) . ?
C20 C22 1.524(4) . ?
C20 C21 1.526(4) . ?
C20 H20 0.94(2) . ?
C21 H21C 0.95(3) . ?
C21 H21B 0.99(4) . ?
C21 H21A 1.01(4) . ?
C22 H22C 1.03(3) . ?
C22 H22B 1.05(4) . ?
C22 H22A 1.10(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N2 C11 129.70(17) . . ?
C1 N1 C6 129.34(19) . . ?
C1 N1 H1N1 120(2) . . ?
C6 N1 H1N1 111(2) . . ?
C6 N3 C10 118.2(2) . . ?
N2 C1 N1 119.13(19) . . ?
N2 C1 C2 127.09(18) . . ?
N1 C1 C2 113.75(18) . . ?
C5A C2 C4A 114.2(6) . . ?
C5A C2 C3 140.7(4) . . ?
C4A C2 C3 50.6(4) . . ?
C5A C2 C1 107.2(4) . . ?
C4A C2 C1 112.6(3) . . ?
C3 C2 C1 112.1(2) . . ?
C5A C2 C5 52.5(6) . . ?
C4A C2 C5 133.6(3) . . ?
C3 C2 C5 107.8(2) . . ?
C1 C2 C5 113.65(19) . . ?
C5A C2 C4 57.0(5) . . ?
C4A C2 C4 61.6(4) . . ?
C3 C2 C4 109.5(2) . . ?
C1 C2 C4 108.83(18) . . ?
C5 C2 C4 104.6(2) . . ?
C5A C2 C3A 113.5(7) . . ?
C4A C2 C3A 105.4(5) . . ?
C3 C2 C3A 55.8(4) . . ?
C1 C2 C3A 103.4(4) . . ?
C5 C2 C3A 61.4(5) . . ?
C4 C2 C3A 147.7(4) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C2 C3A H3AA 109.5 . . ?
C2 C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C2 C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C2 C4A H4AA 109.5 . . ?
C2 C4A H4AB 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
C2 C4A H4AC 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
C2 C5A H5AA 109.5 . . ?
C2 C5A H5AB 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
C2 C5A H5AC 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
N3 C6 C7 122.63(19) . . ?
N3 C6 N1 112.55(18) . . ?
C7 C6 N1 124.81(19) . . ?
C6 C7 C8 117.9(2) . . ?
C6 C7 H7 126.9 . . ?
C8 C7 H7 115.1 . . ?
C9 C8 C7 120.7(2) . . ?
C9 C8 H8 121.6(18) . . ?
C7 C8 H8 117.7(18) . . ?
C8 C9 C10 118.5(2) . . ?
C8 C9 H9 122.6(19) . . ?
C10 C9 H9 118.9(19) . . ?
N3 C10 C9 122.1(2) . . ?
N3 C10 H10 115.3(17) . . ?
C9 C10 H10 122.5(17) . . ?
C16 C11 C12 120.51(18) . . ?
C16 C11 N2 119.60(18) . . ?
C12 C11 N2 119.16(18) . . ?
C13 C12 C11 118.3(2) . . ?
C13 C12 C17 120.3(2) . . ?
C11 C12 C17 121.27(19) . . ?
C14 C13 C12 121.7(2) . . ?
C14 C13 H13 118.7(17) . . ?
C12 C13 H13 119.5(17) . . ?
C13 C14 C15 119.8(2) . . ?
C13 C14 H14 121.3(15) . . ?
C15 C14 H14 118.9(15) . . ?
C14 C15 C16 120.8(2) . . ?
C14 C15 H15 120.3(17) . . ?
C16 C15 H15 118.8(17) . . ?
C15 C16 C11 118.66(19) . . ?
C15 C16 C20 120.42(19) . . ?
C11 C16 C20 120.81(18) . . ?
C12 C17 C18 109.8(2) . . ?
C12 C17 C19 113.0(2) . . ?
C18 C17 C19 111.1(3) . . ?
C12 C17 H17 108.1(17) . . ?
C18 C17 H17 107.0(17) . . ?
C19 C17 H17 107.5(17) . . ?
C17 C18 H18C 111.4(19) . . ?
C17 C18 H18B 106(2) . . ?
H18C C18 H18B 112(3) . . ?
C17 C18 H18A 111.9(19) . . ?
H18C C18 H18A 105(3) . . ?
H18B C18 H18A 111(3) . . ?
C17 C19 H19C 110.0(16) . . ?
C17 C19 H19B 112(2) . . ?
H19C C19 H19B 107(3) . . ?
C17 C19 H19A 111.7(18) . . ?
H19C C19 H19A 113(2) . . ?
H19B C19 H19A 104(3) . . ?
C16 C20 C22 113.5(2) . . ?
C16 C20 C21 109.04(19) . . ?
C22 C20 C21 110.8(3) . . ?
C16 C20 H20 108.7(14) . . ?
C22 C20 H20 108.4(15) . . ?
C21 C20 H20 106.1(15) . . ?
C20 C21 H21C 112.3(19) . . ?
C20 C21 H21B 115(2) . . ?
H21C C21 H21B 105(3) . . ?
C20 C21 H21A 110(2) . . ?
H21C C21 H21A 110(3) . . ?
H21B C21 H21A 105(3) . . ?
C20 C22 H22C 111.7(17) . . ?
C20 C22 H22B 111(2) . . ?
H22C C22 H22B 110(3) . . ?
C20 C22 H22A 110.9(19) . . ?
H22C C22 H22A 110(3) . . ?
H22B C22 H22A 102(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.052
_database_code_depnum_ccdc_archive 'CCDC 991549'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_FO5335

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H40 K N3 O2'
_chemical_formula_sum            'C26 H40 K N3 O2'
_chemical_formula_weight         465.71

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'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   10.2690(1)
_cell_length_b                   24.2935(3)
_cell_length_c                   11.7753(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.840(1)
_cell_angle_gamma                90.00
_cell_volume                     2707.25(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    16968
_cell_measurement_theta_min      2.06
_cell_measurement_theta_max      27.51

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.074
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.042
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    0.221
_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            16968
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         2.06
_diffrn_reflns_theta_max         27.51
_reflns_number_total             6209
_reflns_number_gt                5265
_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 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 > 2sigma(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)+(0.0367P)²+1.5398P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6209
_refine_ls_number_parameters     449
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0424
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0955
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_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 0.05529(3) 0.563501(13) 0.08568(3) 0.02379(9) Uani 1 1 d . . .
O1 O 0.31237(14) 0.60691(5) 0.22985(14) 0.0468(4) Uani 1 1 d . . .
O2 O 0.09112(16) 0.62296(6) 0.30665(11) 0.0467(4) Uani 1 1 d . . .
N1 N 0.05678(13) 0.44311(5) 0.17572(11) 0.0194(2) Uani 1 1 d . . .
N3 N -0.15412(13) 0.48826(5) 0.07959(11) 0.0233(3) Uani 1 1 d . . .
N2 N 0.15767(12) 0.35795(5) 0.26892(11) 0.0195(2) Uani 1 1 d . . .
C1 C 0.15135(14) 0.41088(6) 0.26887(12) 0.0182(3) Uani 1 1 d . . .
C2 C 0.27364(17) 0.44079(6) 0.37061(14) 0.0260(3) Uani 1 1 d . . .
C3 C 0.3548(3) 0.40243(8) 0.4765(2) 0.0498(6) Uani 1 1 d . . .
H3C H 0.431(2) 0.4231(9) 0.542(2) 0.055(6) Uiso 1 1 d . . .
H3B H 0.398(3) 0.3689(11) 0.447(2) 0.073(8) Uiso 1 1 d . . .
H3A H 0.285(2) 0.3912(8) 0.5113(19) 0.038(6) Uiso 1 1 d . . .
C4 C 0.3734(2) 0.46157(8) 0.3092(2) 0.0397(4) Uani 1 1 d . . .
H4C H 0.454(2) 0.4827(9) 0.372(2) 0.051(6) Uiso 1 1 d . . .
H4B H 0.418(2) 0.4285(9) 0.286(2) 0.048(6) Uiso 1 1 d . . .
H4A H 0.320(3) 0.4873(10) 0.235(2) 0.065(7) Uiso 1 1 d . . .
C5 C 0.2210(2) 0.49066(7) 0.41886(17) 0.0342(4) Uani 1 1 d . . .
H5C H 0.303(2) 0.5114(8) 0.4772(18) 0.039(5) Uiso 1 1 d . . .
H5B H 0.167(2) 0.5156(9) 0.353(2) 0.046(6) Uiso 1 1 d . . .
H5A H 0.160(2) 0.4785(9) 0.466(2) 0.050(6) Uiso 1 1 d . . .
C6 C -0.06734(15) 0.45793(6) 0.17857(13) 0.0191(3) Uani 1 1 d . . .
C7 C -0.11409(17) 0.44560(6) 0.27558(14) 0.0247(3) Uani 1 1 d . . .
H7 H -0.0508(19) 0.4260(7) 0.3484(17) 0.029(5) Uiso 1 1 d . . .
C8 C -0.24417(19) 0.46212(7) 0.26791(17) 0.0331(4) Uani 1 1 d . . .
H8 H -0.275(2) 0.4524(8) 0.3342(19) 0.039(5) Uiso 1 1 d . . .
C9 C -0.33214(19) 0.49224(8) 0.16582(18) 0.0368(4) Uani 1 1 d . . .
H9 H -0.423(2) 0.5042(8) 0.1567(19) 0.045(6) Uiso 1 1 d . . .
C10 C -0.28081(17) 0.50406(7) 0.07670(16) 0.0309(4) Uani 1 1 d . . .
H10 H -0.338(2) 0.5253(8) 0.0036(18) 0.036(5) Uiso 1 1 d . . .
C11 C 0.06598(15) 0.32620(6) 0.16864(13) 0.0192(3) Uani 1 1 d . . .
C12 C -0.04726(15) 0.29723(6) 0.17946(13) 0.0217(3) Uani 1 1 d . . .
C13 C -0.12487(17) 0.26107(6) 0.08503(14) 0.0263(3) Uani 1 1 d . . .
H13 H -0.202(2) 0.2397(8) 0.0929(17) 0.037(5) Uiso 1 1 d . . .
C14 C -0.09308(18) 0.25347(6) -0.01739(15) 0.0285(3) Uani 1 1 d . . .
H14 H -0.1489(19) 0.2288(7) -0.0808(17) 0.030(5) Uiso 1 1 d . . .
C15 C 0.01960(17) 0.28180(6) -0.02714(14) 0.0263(3) Uani 1 1 d . . .
H15 H 0.0424(19) 0.2770(7) -0.0997(17) 0.031(5) Uiso 1 1 d . . .
C16 C 0.10180(16) 0.31794(6) 0.06554(13) 0.0222(3) Uani 1 1 d . . .
C17 C -0.07952(16) 0.30211(6) 0.29439(14) 0.0255(3) Uani 1 1 d . . .
H17 H -0.0321(19) 0.3348(8) 0.3387(17) 0.032(5) Uiso 1 1 d . . .
C18 C -0.23717(19) 0.30661(9) 0.2665(2) 0.0377(4) Uani 1 1 d . . .
H18C H -0.281(2) 0.3362(10) 0.210(2) 0.053(6) Uiso 1 1 d . . .
H18B H -0.255(2) 0.3140(9) 0.343(2) 0.047(6) Uiso 1 1 d . . .
H18A H -0.288(2) 0.2726(9) 0.230(2) 0.051(6) Uiso 1 1 d . . .
C19 C -0.0134(2) 0.25375(8) 0.38048(17) 0.0343(4) Uani 1 1 d . . .
H19C H -0.059(2) 0.2189(8) 0.3419(17) 0.033(5) Uiso 1 1 d . . .
H19B H -0.025(2) 0.2577(9) 0.462(2) 0.046(6) Uiso 1 1 d . . .
H19A H 0.090(2) 0.2520(9) 0.397(2) 0.049(6) Uiso 1 1 d . . .
C20 C 0.23247(17) 0.34575(7) 0.06085(15) 0.0270(3) Uani 1 1 d . . .
H20 H 0.2321(17) 0.3829(7) 0.0869(15) 0.020(4) Uiso 1 1 d . . .
C21 C 0.2363(2) 0.34735(8) -0.06750(18) 0.0366(4) Uani 1 1 d . . .
H21C H 0.247(2) 0.3112(9) -0.0982(19) 0.047(6) Uiso 1 1 d . . .
H21B H 0.323(2) 0.3689(9) -0.064(2) 0.050(6) Uiso 1 1 d . . .
H21A H 0.149(2) 0.3652(8) -0.1272(19) 0.042(5) Uiso 1 1 d . . .
C22 C 0.36672(19) 0.31769(9) 0.15079(19) 0.0370(4) Uani 1 1 d . . .
H22C H 0.367(2) 0.3181(8) 0.235(2) 0.039(5) Uiso 1 1 d . . .
H22B H 0.451(2) 0.3371(9) 0.1520(19) 0.046(6) Uiso 1 1 d . . .
H22A H 0.370(2) 0.2795(9) 0.1241(19) 0.046(6) Uiso 1 1 d . . .
C23 C 0.3897(3) 0.61467(11) 0.1542(3) 0.0659(7) Uani 1 1 d . . .
H23C H 0.389(3) 0.5774(14) 0.114(3) 0.096(10) Uiso 1 1 d . . .
H23B H 0.491(3) 0.6242(11) 0.207(3) 0.083(9) Uiso 1 1 d . . .
H23A H 0.343(3) 0.6439(11) 0.088(2) 0.063(7) Uiso 1 1 d . . .
C24 C 0.3016(3) 0.65614(8) 0.2900(2) 0.0520(6) Uani 1 1 d . . .
H24B H 0.248(2) 0.6840(8) 0.2288(18) 0.038(5) Uiso 1 1 d . . .
H24A H 0.398(3) 0.6698(9) 0.338(2) 0.058(7) Uiso 1 1 d . . .
C25 C 0.2298(3) 0.64367(9) 0.37521(19) 0.0591(7) Uani 1 1 d . . .
H25B H 0.286(2) 0.6162(10) 0.441(2) 0.056(6) Uiso 1 1 d . . .
H25A H 0.226(3) 0.6776(12) 0.419(2) 0.078(8) Uiso 1 1 d . . .
C26 C 0.0142(4) 0.61391(13) 0.3822(2) 0.0690(9) Uani 1 1 d . . .
H26B H -0.003(3) 0.6494(12) 0.413(3) 0.078(8) Uiso 1 1 d . . .
H26A H 0.069(3) 0.5896(11) 0.453(3) 0.072(8) Uiso 1 1 d . . .
H26C H -0.076(3) 0.5954(11) 0.334(3) 0.073(9) Uiso 1 1 d . . .


_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 O1 2.7358(13) . ?
K1 N3 2.8019(13) . ?
K1 N3 2.8164(13) 3_565 ?
K1 N1 2.8416(12) 3_565 ?
K1 O2 2.8721(13) . ?
K1 N1 3.1090(12) . ?
K1 C6 3.2044(14) 3_565 ?
K1 C6 3.2294(14) . ?
K1 C23 3.440(2) . ?
K1 C16 3.4408(14) 3_565 ?
K1 C24 3.5394(19) . ?
K1 K1 3.6196(6) 3_565 ?
O1 C24 1.416(2) . ?
O1 C23 1.417(3) . ?
O2 C26 1.418(3) . ?
O2 C25 1.429(3) . ?
N1 C6 1.3374(18) . ?
N1 C1 1.3901(18) . ?
N1 K1 2.8416(12) 3_565 ?
N3 C10 1.344(2) . ?
N3 C6 1.3744(18) . ?
N3 K1 2.8164(13) 3_565 ?
N2 C1 1.2875(18) . ?
N2 C11 1.4186(18) . ?
C1 C2 1.540(2) . ?
C2 C3 1.520(2) . ?
C2 C5 1.523(2) . ?
C2 C4 1.550(3) . ?
C3 H3C 0.99(2) . ?
C3 H3B 1.05(3) . ?
C3 H3A 0.99(2) . ?
C4 H4C 1.01(2) . ?
C4 H4B 1.01(2) . ?
C4 H4A 1.04(3) . ?
C5 H5C 0.99(2) . ?
C5 H5B 0.97(2) . ?
C5 H5A 1.02(2) . ?
C6 C7 1.432(2) . ?
C6 K1 3.2044(14) 3_565 ?
C7 C8 1.364(2) . ?
C7 H7 0.975(19) . ?
C8 C9 1.398(3) . ?
C8 H8 0.98(2) . ?
C9 C10 1.375(3) . ?
C9 H9 0.95(2) . ?
C10 H10 0.981(19) . ?
C11 C12 1.407(2) . ?
C11 C16 1.413(2) . ?
C12 C13 1.398(2) . ?
C12 C17 1.518(2) . ?
C13 C14 1.379(2) . ?
C13 H13 0.98(2) . ?
C14 C15 1.389(2) . ?
C14 H14 0.955(19) . ?
C15 C16 1.400(2) . ?
C15 H15 0.977(19) . ?
C16 C20 1.522(2) . ?
C16 K1 3.4408(14) 3_565 ?
C17 C18 1.526(2) . ?
C17 C19 1.528(2) . ?
C17 H17 0.971(19) . ?
C18 H18C 0.96(2) . ?
C18 H18B 1.00(2) . ?
C18 H18A 0.98(2) . ?
C19 H19C 0.989(19) . ?
C19 H19B 1.01(2) . ?
C19 H19A 1.01(2) . ?
C20 C21 1.528(2) . ?
C20 C22 1.534(2) . ?
C20 H20 0.955(17) . ?
C21 H21C 0.97(2) . ?
C21 H21B 1.02(2) . ?
C21 H21A 1.00(2) . ?
C22 H22C 0.98(2) . ?
C22 H22B 0.98(2) . ?
C22 H22A 0.98(2) . ?
C23 H23C 1.02(3) . ?
C23 H23B 1.01(3) . ?
C23 H23A 1.02(3) . ?
C24 C25 1.488(4) . ?
C24 H24B 0.99(2) . ?
C24 H24A 0.99(2) . ?
C25 H25B 1.02(2) . ?
C25 H25A 0.98(3) . ?
C26 H26B 0.98(3) . ?
C26 H26A 0.99(3) . ?
C26 H26C 0.98(3) . ?

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 K1 N3 144.44(4) . . ?
O1 K1 N3 94.65(4) . 3_565 ?
N3 K1 N3 99.78(3) . 3_565 ?
O1 K1 N1 125.55(4) . 3_565 ?
N3 K1 N1 87.21(4) . 3_565 ?
N3 K1 N1 47.88(3) 3_565 3_565 ?
O1 K1 O2 59.37(5) . . ?
N3 K1 O2 100.28(4) . . ?
N3 K1 O2 153.73(4) 3_565 . ?
N1 K1 O2 149.93(4) 3_565 . ?
O1 K1 N1 105.98(4) . . ?
N3 K1 N1 45.34(3) . . ?
N3 K1 N1 81.97(3) 3_565 . ?
N1 K1 N1 105.22(3) 3_565 . ?
O2 K1 N1 100.50(4) . . ?
O1 K1 C6 105.87(4) . 3_565 ?
N3 K1 C6 100.82(4) . 3_565 ?
N3 K1 C6 25.35(3) 3_565 3_565 ?
N1 K1 C6 24.63(3) 3_565 3_565 ?
O2 K1 C6 157.19(4) . 3_565 ?
N1 K1 C6 100.45(3) . 3_565 ?
O1 K1 C6 120.35(4) . . ?
N3 K1 C6 25.08(3) . . ?
N3 K1 C6 99.90(4) 3_565 . ?
N1 K1 C6 105.95(4) 3_565 . ?
O2 K1 C6 91.28(4) . . ?
N1 K1 C6 24.27(3) . . ?
C6 K1 C6 111.53(3) 3_565 . ?
O1 K1 C23 23.12(7) . . ?
N3 K1 C23 158.12(6) . . ?
N3 K1 C23 74.26(6) 3_565 . ?
N1 K1 C23 102.83(6) 3_565 . ?
O2 K1 C23 80.83(7) . . ?
N1 K1 C23 112.81(5) . . ?
C6 K1 C23 82.83(6) 3_565 . ?
C6 K1 C23 133.83(6) . . ?
O1 K1 C16 98.28(4) . 3_565 ?
N3 K1 C16 109.38(4) . 3_565 ?
N3 K1 C16 103.79(4) 3_565 3_565 ?
N1 K1 C16 64.87(3) 3_565 3_565 ?
O2 K1 C16 85.26(4) . 3_565 ?
N1 K1 C16 154.59(4) . 3_565 ?
C6 K1 C16 79.66(4) 3_565 3_565 ?
C6 K1 C16 132.37(4) . 3_565 ?
C23 K1 C16 92.50(6) . 3_565 ?
O1 K1 C24 21.59(5) . . ?
N3 K1 C24 140.45(5) . . ?
N3 K1 C24 113.55(5) 3_565 . ?
N1 K1 C24 130.87(5) 3_565 . ?
O2 K1 C24 42.09(6) . . ?
N1 K1 C24 117.30(4) . . ?
C6 K1 C24 118.47(5) 3_565 . ?
C6 K1 C24 122.99(5) . . ?
C23 K1 C24 39.29(7) . . ?
C16 K1 C24 83.53(4) 3_565 . ?
O1 K1 K1 133.86(3) . 3_565 ?
N3 K1 K1 50.07(3) . 3_565 ?
N3 K1 K1 49.72(3) 3_565 3_565 ?
N1 K1 K1 55.98(2) 3_565 3_565 ?
O2 K1 K1 146.71(3) . 3_565 ?
N1 K1 K1 49.25(2) . 3_565 ?
C6 K1 K1 56.09(3) 3_565 3_565 ?
C6 K1 K1 55.44(3) . 3_565 ?
C23 K1 K1 120.48(5) . 3_565 ?
C16 K1 K1 116.26(3) 3_565 3_565 ?
C24 K1 K1 155.19(4) . 3_565 ?
C24 O1 C23 111.95(18) . . ?
C24 O1 K1 113.09(12) . . ?
C23 O1 K1 107.59(15) . . ?
C26 O2 C25 112.1(2) . . ?
C26 O2 K1 125.74(17) . . ?
C25 O2 K1 115.98(13) . . ?
C6 N1 C1 120.84(12) . . ?
C6 N1 K1 93.05(8) . 3_565 ?
C1 N1 K1 133.47(9) . 3_565 ?
C6 N1 K1 82.92(8) . . ?
C1 N1 K1 135.11(9) . . ?
K1 N1 K1 74.78(3) 3_565 . ?
C10 N3 C6 118.50(13) . . ?
C10 N3 K1 122.68(10) . . ?
C6 N3 K1 95.13(8) . . ?
C10 N3 K1 135.63(10) . 3_565 ?
C6 N3 K1 93.31(8) . 3_565 ?
K1 N3 K1 80.22(3) . 3_565 ?
C1 N2 C11 121.70(12) . . ?
N2 C1 N1 125.63(13) . . ?
N2 C1 C2 116.43(12) . . ?
N1 C1 C2 117.19(12) . . ?
C3 C2 C5 110.01(16) . . ?
C3 C2 C1 111.76(13) . . ?
C5 C2 C1 111.42(13) . . ?
C3 C2 C4 109.33(17) . . ?
C5 C2 C4 108.03(14) . . ?
C1 C2 C4 106.13(13) . . ?
C2 C3 H3C 110.0(13) . . ?
C2 C3 H3B 111.6(14) . . ?
H3C C3 H3B 110.1(19) . . ?
C2 C3 H3A 104.7(12) . . ?
H3C C3 H3A 107.3(18) . . ?
H3B C3 H3A 112.8(19) . . ?
C2 C4 H4C 108.9(12) . . ?
C2 C4 H4B 108.3(12) . . ?
H4C C4 H4B 106.1(17) . . ?
C2 C4 H4A 111.0(13) . . ?
H4C C4 H4A 108.9(18) . . ?
H4B C4 H4A 113.5(18) . . ?
C2 C5 H5C 109.6(11) . . ?
C2 C5 H5B 112.1(13) . . ?
H5C C5 H5B 107.6(17) . . ?
C2 C5 H5A 110.5(12) . . ?
H5C C5 H5A 107.5(16) . . ?
H5B C5 H5A 109.4(17) . . ?
N1 C6 N3 115.69(13) . . ?
N1 C6 C7 125.56(13) . . ?
N3 C6 C7 118.74(13) . . ?
N1 C6 K1 62.32(7) . 3_565 ?
N3 C6 K1 61.34(7) . 3_565 ?
C7 C6 K1 153.11(10) . 3_565 ?
N1 C6 K1 72.82(8) . . ?
N3 C6 K1 59.79(7) . . ?
C7 C6 K1 137.04(10) . . ?
K1 C6 K1 68.47(3) 3_565 . ?
C8 C7 C6 120.57(15) . . ?
C8 C7 H7 120.2(11) . . ?
C6 C7 H7 119.2(11) . . ?
C7 C8 C9 120.03(16) . . ?
C7 C8 H8 119.1(12) . . ?
C9 C8 H8 120.9(12) . . ?
C10 C9 C8 117.03(16) . . ?
C10 C9 H9 120.3(13) . . ?
C8 C9 H9 122.6(13) . . ?
N3 C10 C9 125.10(16) . . ?
N3 C10 H10 114.9(11) . . ?
C9 C10 H10 120.0(11) . . ?
C12 C11 C16 120.45(13) . . ?
C12 C11 N2 120.10(13) . . ?
C16 C11 N2 118.85(13) . . ?
C13 C12 C11 118.57(14) . . ?
C13 C12 C17 120.26(14) . . ?
C11 C12 C17 121.06(13) . . ?
C14 C13 C12 121.63(15) . . ?
C14 C13 H13 119.0(11) . . ?
C12 C13 H13 119.3(11) . . ?
C13 C14 C15 119.59(14) . . ?
C13 C14 H14 119.6(11) . . ?
C15 C14 H14 120.8(11) . . ?
C14 C15 C16 121.06(15) . . ?
C14 C15 H15 120.3(11) . . ?
C16 C15 H15 118.7(11) . . ?
C15 C16 C11 118.67(14) . . ?
C15 C16 C20 121.56(14) . . ?
C11 C16 C20 119.68(13) . . ?
C15 C16 K1 95.84(9) . 3_565 ?
C11 C16 K1 95.72(8) . 3_565 ?
C20 C16 K1 81.51(8) . 3_565 ?
C12 C17 C18 113.24(14) . . ?
C12 C17 C19 109.70(13) . . ?
C18 C17 C19 111.02(14) . . ?
C12 C17 H17 107.8(11) . . ?
C18 C17 H17 109.0(11) . . ?
C19 C17 H17 105.7(11) . . ?
C17 C18 H18C 112.3(14) . . ?
C17 C18 H18B 111.4(12) . . ?
H18C C18 H18B 106.6(18) . . ?
C17 C18 H18A 111.7(13) . . ?
H18C C18 H18A 107.4(19) . . ?
H18B C18 H18A 107.2(18) . . ?
C17 C19 H19C 110.1(11) . . ?
C17 C19 H19B 111.6(12) . . ?
H19C C19 H19B 107.9(16) . . ?
C17 C19 H19A 108.9(12) . . ?
H19C C19 H19A 109.3(16) . . ?
H19B C19 H19A 109.0(17) . . ?
C16 C20 C21 114.13(14) . . ?
C16 C20 C22 110.26(14) . . ?
C21 C20 C22 109.45(14) . . ?
C16 C20 H20 107.1(10) . . ?
C21 C20 H20 107.4(10) . . ?
C22 C20 H20 108.2(10) . . ?
C20 C21 H21C 113.2(12) . . ?
C20 C21 H21B 109.3(12) . . ?
H21C C21 H21B 104.9(17) . . ?
C20 C21 H21A 110.2(12) . . ?
H21C C21 H21A 109.3(17) . . ?
H21B C21 H21A 109.8(17) . . ?
C20 C22 H22C 110.0(12) . . ?
C20 C22 H22B 110.2(12) . . ?
H22C C22 H22B 108.5(17) . . ?
C20 C22 H22A 109.3(12) . . ?
H22C C22 H22A 109.8(17) . . ?
H22B C22 H22A 108.9(17) . . ?
O1 C23 K1 49.29(10) . . ?
O1 C23 H23C 105.6(17) . . ?
K1 C23 H23C 75.1(17) . . ?
O1 C23 H23B 109.7(17) . . ?
K1 C23 H23B 157.3(16) . . ?
H23C C23 H23B 108(2) . . ?
O1 C23 H23A 111.2(14) . . ?
K1 C23 H23A 86.9(14) . . ?
H23C C23 H23A 110(2) . . ?
H23B C23 H23A 112(2) . . ?
O1 C24 C25 108.70(17) . . ?
O1 C24 K1 45.32(9) . . ?
C25 C24 K1 85.33(11) . . ?
O1 C24 H24B 110.1(11) . . ?
C25 C24 H24B 110.3(11) . . ?
K1 C24 H24B 83.6(11) . . ?
O1 C24 H24A 108.4(14) . . ?
C25 C24 H24A 109.3(14) . . ?
K1 C24 H24A 153.7(14) . . ?
H24B C24 H24A 110.0(17) . . ?
O2 C25 C24 109.68(16) . . ?
O2 C25 H25B 110.1(13) . . ?
C24 C25 H25B 111.7(13) . . ?
O2 C25 H25A 111.1(16) . . ?
C24 C25 H25A 108.3(16) . . ?
H25B C25 H25A 106(2) . . ?
O2 C26 H26B 109.0(16) . . ?
O2 C26 H26A 110.2(15) . . ?
H26B C26 H26A 110(2) . . ?
O2 C26 H26C 109.7(16) . . ?
H26B C26 H26C 110(2) . . ?
H26A C26 H26C 108(2) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.51
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.044
_database_code_depnum_ccdc_archive 'CCDC 991550'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_FO5076

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H64 Ca N6'
_chemical_formula_sum            'C52 H64 Ca N6'
_chemical_formula_weight         813.17

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'
Ca Ca 0.2262 0.3064 '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                   10.6116(3)
_cell_length_b                   12.0133(2)
_cell_length_c                   20.2597(4)
_cell_angle_alpha                79.156(1)
_cell_angle_beta                 77.228(1)
_cell_angle_gamma                66.909(1)
_cell_volume                     2302.16(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    14822
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      27.52

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.054
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.173
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             876
_exptl_absorpt_coefficient_mu    0.178
_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            14822
_diffrn_reflns_av_R_equivalents  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.50
_diffrn_reflns_theta_max         27.52
_reflns_number_total             10344
_reflns_number_gt                8689
_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 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 > 2sigma(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+2.9925P] 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       ?
_refine_ls_number_reflns         10344
_refine_ls_number_parameters     546
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1168
_refine_ls_wR_factor_gt          0.1072
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_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
Ca1 Ca 0.65457(4) 0.88448(3) 0.777204(19) 0.01683(9) Uani 1 1 d . . .
N1A N 0.65187(17) 0.79435(15) 0.89378(8) 0.0171(3) Uani 1 1 d . . .
N2A N 0.53483(17) 0.67036(15) 0.88410(8) 0.0193(3) Uani 1 1 d . . .
N3A N 0.76823(17) 0.96271(15) 0.84061(8) 0.0198(3) Uani 1 1 d . . .
C1A C 0.56614(19) 0.72970(17) 0.92152(9) 0.0162(4) Uani 1 1 d . . .
C2A C 0.4806(2) 0.74034(18) 0.99451(10) 0.0199(4) Uani 1 1 d . . .
C3A C 0.4760(2) 0.84910(19) 1.02551(11) 0.0247(4) Uani 1 1 d . . .
H3AA H 0.4126 0.8576 1.0691 0.037 Uiso 1 1 calc R . .
H3AB H 0.4431 0.9235 0.9943 0.037 Uiso 1 1 calc R . .
H3AC H 0.5692 0.8358 1.0329 0.037 Uiso 1 1 calc R . .
C4A C 0.3300(2) 0.7625(2) 0.98875(11) 0.0290(5) Uani 1 1 d . . .
H4AA H 0.2719 0.7735 1.0337 0.043 Uiso 1 1 calc R . .
H4AB H 0.3279 0.6922 0.9717 0.043 Uiso 1 1 calc R . .
H4AC H 0.2946 0.8357 0.9572 0.043 Uiso 1 1 calc R . .
C5A C 0.5330(2) 0.6218(2) 1.04228(11) 0.0278(5) Uani 1 1 d . . .
H5AA H 0.4630 0.6236 1.0832 0.042 Uiso 1 1 calc R . .
H5AB H 0.6197 0.6145 1.0554 0.042 Uiso 1 1 calc R . .
H5AC H 0.5496 0.5520 1.0187 0.042 Uiso 1 1 calc R . .
C6A C 0.75277(19) 0.79606(17) 0.92504(9) 0.0171(4) Uani 1 1 d . . .
C7A C 0.8134(2) 0.7108(2) 0.97691(11) 0.0245(4) Uani 1 1 d . . .
H7AA H 0.7830 0.6447 0.9937 0.029 Uiso 1 1 calc R . .
C8A C 0.9183(2) 0.7200(2) 1.00518(12) 0.0317(5) Uani 1 1 d . . .
H8AA H 0.9557 0.6604 1.0409 0.038 Uiso 1 1 calc R . .
C9A C 0.9678(2) 0.8120(2) 0.98276(12) 0.0311(5) Uani 1 1 d . . .
H9AA H 1.0357 0.8184 1.0040 0.037 Uiso 1 1 calc R . .
C10A C 0.9168(2) 0.8974(2) 0.92764(11) 0.0234(4) Uani 1 1 d . . .
C11A C 0.9665(2) 0.9923(2) 0.89877(12) 0.0297(5) Uani 1 1 d . . .
H11A H 1.0346 1.0028 0.9179 0.036 Uiso 1 1 calc R . .
C12A C 0.9171(2) 1.0688(2) 0.84356(12) 0.0290(5) Uani 1 1 d . . .
H12A H 0.9486 1.1337 0.8246 0.035 Uiso 1 1 calc R . .
C13A C 0.8188(2) 1.04944(19) 0.81537(11) 0.0250(4) Uani 1 1 d . . .
H13A H 0.7869 1.1013 0.7761 0.030 Uiso 1 1 calc R . .
C14A C 0.8125(2) 0.88777(18) 0.89739(10) 0.0184(4) Uani 1 1 d . . .
C15A C 0.5960(2) 0.67072(17) 0.81479(10) 0.0187(4) Uani 1 1 d . . .
C16A C 0.7410(2) 0.61530(17) 0.79331(10) 0.0199(4) Uani 1 1 d . . .
C17A C 0.7937(2) 0.62993(19) 0.72401(11) 0.0251(4) Uani 1 1 d . . .
H17A H 0.8908 0.5944 0.7091 0.030 Uiso 1 1 calc R . .
C18A C 0.7071(3) 0.6953(2) 0.67643(11) 0.0303(5) Uani 1 1 d . . .
H18A H 0.7453 0.7078 0.6299 0.036 Uiso 1 1 calc R . .
C19A C 0.5653(3) 0.7420(2) 0.69729(11) 0.0284(5) Uani 1 1 d . . .
H19A H 0.5063 0.7832 0.6643 0.034 Uiso 1 1 calc R . .
C20A C 0.5065(2) 0.73001(18) 0.76571(11) 0.0234(4) Uani 1 1 d . . .
C21A C 0.8361(2) 0.53476(18) 0.84308(11) 0.0219(4) Uani 1 1 d . . .
H21A H 0.7902 0.5586 0.8897 0.026 Uiso 1 1 calc R . .
C22A C 0.8503(2) 0.40288(19) 0.84226(12) 0.0278(5) Uani 1 1 d . . .
H22A H 0.7580 0.3975 0.8532 0.042 Uiso 1 1 calc R . .
H22B H 0.9071 0.3495 0.8761 0.042 Uiso 1 1 calc R . .
H22C H 0.8947 0.3775 0.7969 0.042 Uiso 1 1 calc R . .
C23A C 0.9783(2) 0.5474(2) 0.82846(13) 0.0312(5) Uani 1 1 d . . .
H23A H 0.9655 0.6332 0.8266 0.047 Uiso 1 1 calc R . .
H23B H 1.0289 0.5175 0.7847 0.047 Uiso 1 1 calc R . .
H23C H 1.0315 0.4994 0.8648 0.047 Uiso 1 1 calc R . .
C24A C 0.3496(2) 0.7758(2) 0.78860(12) 0.0303(5) Uani 1 1 d . . .
H24A H 0.3285 0.8169 0.8305 0.036 Uiso 1 1 calc R . .
C25A C 0.3010(3) 0.6670(3) 0.80792(16) 0.0455(7) Uani 1 1 d . . .
H25A H 0.3522 0.6094 0.8427 0.068 Uiso 1 1 calc R . .
H25B H 0.3185 0.6262 0.7674 0.068 Uiso 1 1 calc R . .
H25C H 0.2014 0.6962 0.8259 0.068 Uiso 1 1 calc R . .
C26A C 0.2694(3) 0.8689(3) 0.73520(15) 0.0462(7) Uani 1 1 d . . .
H26A H 0.3063 0.9344 0.7212 0.069 Uiso 1 1 calc R . .
H26B H 0.1709 0.9032 0.7548 0.069 Uiso 1 1 calc R . .
H26C H 0.2798 0.8286 0.6954 0.069 Uiso 1 1 calc R . .
N1B N 0.54462(16) 1.05421(14) 0.70200(8) 0.0168(3) Uani 1 1 d . . .
N2B N 0.41192(17) 1.27011(15) 0.67363(8) 0.0187(3) Uani 1 1 d . . .
N3B N 0.82597(17) 0.91584(16) 0.68272(9) 0.0210(3) Uani 1 1 d . . .
C1B C 0.44412(19) 1.16651(17) 0.71221(9) 0.0163(4) Uani 1 1 d . . .
C2B C 0.3518(2) 1.17694(18) 0.78323(10) 0.0185(4) Uani 1 1 d . . .
C3B C 0.3555(2) 1.2817(2) 0.81472(11) 0.0262(4) Uani 1 1 d . . .
H3BA H 0.2965 1.2889 0.8595 0.039 Uiso 1 1 calc R . .
H3BB H 0.3214 1.3579 0.7850 0.039 Uiso 1 1 calc R . .
H3BC H 0.4511 1.2654 0.8198 0.039 Uiso 1 1 calc R . .
C4B C 0.3931(2) 1.06169(19) 0.83365(10) 0.0230(4) Uani 1 1 d . . .
H4BA H 0.3254 1.0736 0.8758 0.034 Uiso 1 1 calc R . .
H4BB H 0.4854 1.0448 0.8437 0.034 Uiso 1 1 calc R . .
H4BC H 0.3948 0.9928 0.8137 0.034 Uiso 1 1 calc R . .
C5B C 0.2025(2) 1.2058(2) 0.77309(11) 0.0264(4) Uani 1 1 d . . .
H5BA H 0.1411 1.2146 0.8173 0.040 Uiso 1 1 calc R . .
H5BB H 0.1994 1.1394 0.7527 0.040 Uiso 1 1 calc R . .
H5BC H 0.1717 1.2819 0.7429 0.040 Uiso 1 1 calc R . .
C6B C 0.6146(2) 1.02867(17) 0.63625(10) 0.0172(4) Uani 1 1 d . . .
C7B C 0.5509(2) 1.05858(17) 0.57885(10) 0.0190(4) Uani 1 1 d . . .
H7BA H 0.4525 1.0944 0.5842 0.023 Uiso 1 1 calc R . .
C8B C 0.6273(2) 1.03755(18) 0.51323(10) 0.0231(4) Uani 1 1 d . . .
H8BA H 0.5798 1.0635 0.4752 0.028 Uiso 1 1 calc R . .
C9B C 0.7684(2) 0.98050(19) 0.50307(10) 0.0244(4) Uani 1 1 d . . .
H9BA H 0.8190 0.9694 0.4583 0.029 Uiso 1 1 calc R . .
C10B C 0.8382(2) 0.93821(18) 0.55997(10) 0.0220(4) Uani 1 1 d . . .
C11B C 0.9831(2) 0.8734(2) 0.55414(11) 0.0282(5) Uani 1 1 d . . .
H11B H 1.0375 0.8579 0.5105 0.034 Uiso 1 1 calc R . .
C12B C 1.0452(2) 0.8328(2) 0.61083(12) 0.0304(5) Uani 1 1 d . . .
H12B H 1.1428 0.7907 0.6071 0.037 Uiso 1 1 calc R . .
C13B C 0.9621(2) 0.8547(2) 0.67456(11) 0.0260(4) Uani 1 1 d . . .
H13B H 1.0053 0.8243 0.7140 0.031 Uiso 1 1 calc R . .
C14B C 0.7621(2) 0.96063(17) 0.62625(10) 0.0182(4) Uani 1 1 d . . .
C15B C 0.4762(2) 1.29767(17) 0.60808(10) 0.0191(4) Uani 1 1 d . . .
C16B C 0.3955(2) 1.33509(17) 0.55508(10) 0.0211(4) Uani 1 1 d . . .
C17B C 0.4570(2) 1.36215(18) 0.48906(10) 0.0246(4) Uani 1 1 d . . .
H17B H 0.4051 1.3838 0.4529 0.029 Uiso 1 1 calc R . .
C18B C 0.5920(2) 1.35815(19) 0.47522(10) 0.0267(5) Uani 1 1 d . . .
H18B H 0.6329 1.3754 0.4297 0.032 Uiso 1 1 calc R . .
C19B C 0.6674(2) 1.32885(18) 0.52780(11) 0.0244(4) Uani 1 1 d . . .
H19B H 0.7593 1.3286 0.5180 0.029 Uiso 1 1 calc R . .
C20B C 0.6117(2) 1.29972(17) 0.59488(10) 0.0217(4) Uani 1 1 d . . .
C21B C 0.2456(2) 1.34342(19) 0.57261(10) 0.0239(4) Uani 1 1 d . . .
H21B H 0.2426 1.2719 0.6064 0.029 Uiso 1 1 calc R . .
C22B C 0.1848(3) 1.3389(2) 0.51156(12) 0.0333(5) Uani 1 1 d . . .
H22D H 0.2440 1.2653 0.4898 0.050 Uiso 1 1 calc R . .
H22E H 0.1805 1.4109 0.4787 0.050 Uiso 1 1 calc R . .
H22F H 0.0911 1.3376 0.5272 0.050 Uiso 1 1 calc R . .
C23B C 0.1535(2) 1.4588(2) 0.60685(12) 0.0314(5) Uani 1 1 d . . .
H23D H 0.1911 1.4603 0.6466 0.047 Uiso 1 1 calc R . .
H23E H 0.0590 1.4590 0.6214 0.047 Uiso 1 1 calc R . .
H23F H 0.1515 1.5309 0.5744 0.047 Uiso 1 1 calc R . .
C24B C 0.6894(2) 1.2767(2) 0.65409(11) 0.0250(4) Uani 1 1 d . . .
H24B H 0.6674 1.2115 0.6874 0.030 Uiso 1 1 calc R . .
C25B C 0.6332(3) 1.3920(2) 0.69027(13) 0.0404(6) Uani 1 1 d . . .
H25D H 0.5319 1.4187 0.7020 0.061 Uiso 1 1 calc R . .
H25E H 0.6584 1.4566 0.6600 0.061 Uiso 1 1 calc R . .
H25F H 0.6735 1.3744 0.7319 0.061 Uiso 1 1 calc R . .
C26B C 0.8467(3) 1.2333(3) 0.63472(13) 0.0378(6) Uani 1 1 d . . .
H26D H 0.8807 1.1583 0.6130 0.057 Uiso 1 1 calc R . .
H26E H 0.8884 1.2174 0.6758 0.057 Uiso 1 1 calc R . .
H26F H 0.8723 1.2963 0.6029 0.057 Uiso 1 1 calc R . .


_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
Ca1 N1B 2.3645(16) . ?
Ca1 N1A 2.4049(16) . ?
Ca1 N3B 2.4167(17) . ?
Ca1 N3A 2.4530(17) . ?
Ca1 C15A 2.8046(19) . ?
Ca1 C20A 2.928(2) . ?
Ca1 C16A 2.9687(19) . ?
Ca1 C19A 3.073(2) . ?
Ca1 C17A 3.112(2) . ?
Ca1 C14B 3.1169(19) . ?
Ca1 C18A 3.145(2) . ?
N1A C6A 1.367(2) . ?
N1A C1A 1.382(2) . ?
N2A C1A 1.301(2) . ?
N2A C15A 1.411(3) . ?
N3A C13A 1.323(3) . ?
N3A C14A 1.368(3) . ?
C1A C2A 1.554(3) . ?
C2A C3A 1.533(3) . ?
C2A C5A 1.540(3) . ?
C2A C4A 1.541(3) . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C4A H4AA 0.9800 . ?
C4A H4AB 0.9800 . ?
C4A H4AC 0.9800 . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C6A C7A 1.394(3) . ?
C6A C14A 1.445(3) . ?
C7A C8A 1.407(3) . ?
C7A H7AA 0.9500 . ?
C8A C9A 1.366(3) . ?
C8A H8AA 0.9500 . ?
C9A C10A 1.412(3) . ?
C9A H9AA 0.9500 . ?
C10A C11A 1.416(3) . ?
C10A C14A 1.428(3) . ?
C11A C12A 1.365(3) . ?
C11A H11A 0.9500 . ?
C12A C13A 1.405(3) . ?
C12A H12A 0.9500 . ?
C13A H13A 0.9500 . ?
C15A C16A 1.417(3) . ?
C15A C20A 1.421(3) . ?
C16A C17A 1.397(3) . ?
C16A C21A 1.513(3) . ?
C17A C18A 1.389(3) . ?
C17A H17A 0.9500 . ?
C18A C19A 1.380(3) . ?
C18A H18A 0.9500 . ?
C19A C20A 1.394(3) . ?
C19A H19A 0.9500 . ?
C20A C24A 1.525(3) . ?
C21A C22A 1.535(3) . ?
C21A C23A 1.535(3) . ?
C21A H21A 1.0000 . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C23A H23A 0.9800 . ?
C23A H23B 0.9800 . ?
C23A H23C 0.9800 . ?
C24A C26A 1.533(3) . ?
C24A C25A 1.542(3) . ?
C24A H24A 1.0000 . ?
C25A H25A 0.9800 . ?
C25A H25B 0.9800 . ?
C25A H25C 0.9800 . ?
C26A H26A 0.9800 . ?
C26A H26B 0.9800 . ?
C26A H26C 0.9800 . ?
N1B C1B 1.371(2) . ?
N1B C6B 1.399(2) . ?
N2B C1B 1.302(2) . ?
N2B C15B 1.396(2) . ?
N3B C13B 1.327(3) . ?
N3B C14B 1.372(3) . ?
C1B C2B 1.547(3) . ?
C2B C3B 1.531(3) . ?
C2B C4B 1.530(3) . ?
C2B C5B 1.536(3) . ?
C3B H3BA 0.9800 . ?
C3B H3BB 0.9800 . ?
C3B H3BC 0.9800 . ?
C4B H4BA 0.9800 . ?
C4B H4BB 0.9800 . ?
C4B H4BC 0.9800 . ?
C5B H5BA 0.9800 . ?
C5B H5BB 0.9800 . ?
C5B H5BC 0.9800 . ?
C6B C7B 1.392(3) . ?
C6B C14B 1.441(3) . ?
C7B C8B 1.406(3) . ?
C7B H7BA 0.9500 . ?
C8B C9B 1.366(3) . ?
C8B H8BA 0.9500 . ?
C9B C10B 1.413(3) . ?
C9B H9BA 0.9500 . ?
C10B C11B 1.414(3) . ?
C10B C14B 1.419(3) . ?
C11B C12B 1.365(3) . ?
C11B H11B 0.9500 . ?
C12B C13B 1.399(3) . ?
C12B H12B 0.9500 . ?
C13B H13B 0.9500 . ?
C15B C20B 1.412(3) . ?
C15B C16B 1.418(3) . ?
C16B C17B 1.392(3) . ?
C16B C21B 1.518(3) . ?
C17B C18B 1.381(3) . ?
C17B H17B 0.9500 . ?
C18B C19B 1.383(3) . ?
C18B H18B 0.9500 . ?
C19B C20B 1.395(3) . ?
C19B H19B 0.9500 . ?
C20B C24B 1.527(3) . ?
C21B C22B 1.534(3) . ?
C21B C23B 1.536(3) . ?
C21B H21B 1.0000 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23B H23D 0.9800 . ?
C23B H23E 0.9800 . ?
C23B H23F 0.9800 . ?
C24B C26B 1.522(3) . ?
C24B C25B 1.534(3) . ?
C24B H24B 1.0000 . ?
C25B H25D 0.9800 . ?
C25B H25E 0.9800 . ?
C25B H25F 0.9800 . ?
C26B H26D 0.9800 . ?
C26B H26E 0.9800 . ?
C26B H26F 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
N1B Ca1 N1A 145.44(6) . . ?
N1B Ca1 N3B 70.76(6) . . ?
N1A Ca1 N3B 136.82(6) . . ?
N1B Ca1 N3A 104.25(6) . . ?
N1A Ca1 N3A 67.72(5) . . ?
N3B Ca1 N3A 83.26(6) . . ?
N1B Ca1 C15A 126.58(6) . . ?
N1A Ca1 C15A 61.06(5) . . ?
N3B Ca1 C15A 125.44(6) . . ?
N3A Ca1 C15A 126.45(6) . . ?
N1B Ca1 C20A 98.07(6) . . ?
N1A Ca1 C20A 85.14(6) . . ?
N3B Ca1 C20A 119.11(6) . . ?
N3A Ca1 C20A 152.86(6) . . ?
C15A Ca1 C20A 28.59(6) . . ?
N1B Ca1 C16A 138.88(6) . . ?
N1A Ca1 C16A 66.33(5) . . ?
N3B Ca1 C16A 101.38(6) . . ?
N3A Ca1 C16A 115.04(6) . . ?
C15A Ca1 C16A 28.23(6) . . ?
C20A Ca1 C16A 49.24(6) . . ?
N1B Ca1 C19A 84.37(6) . . ?
N1A Ca1 C19A 109.26(6) . . ?
N3B Ca1 C19A 92.92(6) . . ?
N3A Ca1 C19A 168.69(6) . . ?
C15A Ca1 C19A 48.39(6) . . ?
C20A Ca1 C19A 26.73(6) . . ?
C16A Ca1 C19A 55.19(6) . . ?
N1B Ca1 C17A 118.33(6) . . ?
N1A Ca1 C17A 91.77(6) . . ?
N3B Ca1 C17A 77.73(6) . . ?
N3A Ca1 C17A 123.18(6) . . ?
C15A Ca1 C17A 47.90(6) . . ?
C20A Ca1 C17A 55.02(6) . . ?
C16A Ca1 C17A 26.43(5) . . ?
C19A Ca1 C17A 45.51(6) . . ?
N1B Ca1 C14B 50.82(5) . . ?
N1A Ca1 C14B 161.21(6) . . ?
N3B Ca1 C14B 24.83(5) . . ?
N3A Ca1 C14B 102.47(5) . . ?
C15A Ca1 C14B 121.27(5) . . ?
C20A Ca1 C14B 103.57(6) . . ?
C16A Ca1 C14B 106.64(5) . . ?
C19A Ca1 C14B 77.11(6) . . ?
C17A Ca1 C14B 80.22(5) . . ?
N1B Ca1 C18A 93.71(6) . . ?
N1A Ca1 C18A 112.37(6) . . ?
N3B Ca1 C18A 73.61(6) . . ?
N3A Ca1 C18A 144.13(6) . . ?
C15A Ca1 C18A 55.77(6) . . ?
C20A Ca1 C18A 46.82(6) . . ?
C16A Ca1 C18A 46.75(6) . . ?
C19A Ca1 C18A 25.61(6) . . ?
C17A Ca1 C18A 25.65(6) . . ?
C14B Ca1 C18A 65.61(5) . . ?
C6A N1A C1A 123.83(16) . . ?
C6A N1A Ca1 115.64(12) . . ?
C1A N1A Ca1 119.78(12) . . ?
C1A N2A C15A 117.42(16) . . ?
C13A N3A C14A 118.94(18) . . ?
C13A N3A Ca1 124.47(14) . . ?
C14A N3A Ca1 114.13(12) . . ?
N2A C1A N1A 121.21(17) . . ?
N2A C1A C2A 114.76(16) . . ?
N1A C1A C2A 123.18(16) . . ?
C3A C2A C5A 110.62(17) . . ?
C3A C2A C4A 106.97(17) . . ?
C5A C2A C4A 107.30(17) . . ?
C3A C2A C1A 112.46(16) . . ?
C5A C2A C1A 111.95(17) . . ?
C4A C2A C1A 107.22(16) . . ?
C2A C3A H3AA 109.5 . . ?
C2A C3A H3AB 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
C2A C3A H3AC 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C2A C4A H4AA 109.5 . . ?
C2A C4A H4AB 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
C2A C4A H4AC 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
C2A C5A H5AA 109.5 . . ?
C2A C5A H5AB 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
C2A C5A H5AC 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
N1A C6A C7A 126.33(18) . . ?
N1A C6A C14A 117.09(17) . . ?
C7A C6A C14A 116.27(17) . . ?
C6A C7A C8A 121.9(2) . . ?
C6A C7A H7AA 119.0 . . ?
C8A C7A H7AA 119.0 . . ?
C9A C8A C7A 121.9(2) . . ?
C9A C8A H8AA 119.1 . . ?
C7A C8A H8AA 119.1 . . ?
C8A C9A C10A 119.12(19) . . ?
C8A C9A H9AA 120.4 . . ?
C10A C9A H9AA 120.4 . . ?
C9A C10A C11A 123.2(2) . . ?
C9A C10A C14A 119.62(19) . . ?
C11A C10A C14A 117.2(2) . . ?
C12A C11A C10A 120.4(2) . . ?
C12A C11A H11A 119.8 . . ?
C10A C11A H11A 119.8 . . ?
C11A C12A C13A 118.6(2) . . ?
C11A C12A H12A 120.7 . . ?
C13A C12A H12A 120.7 . . ?
N3A C13A C12A 123.5(2) . . ?
N3A C13A H13A 118.3 . . ?
C12A C13A H13A 118.3 . . ?
N3A C14A C10A 121.39(18) . . ?
N3A C14A C6A 117.82(17) . . ?
C10A C14A C6A 120.78(18) . . ?
N2A C15A C16A 122.55(17) . . ?
N2A C15A C20A 117.49(18) . . ?
C16A C15A C20A 119.95(18) . . ?
N2A C15A Ca1 107.01(11) . . ?
C16A C15A Ca1 82.33(11) . . ?
C20A C15A Ca1 80.55(12) . . ?
C17A C16A C15A 118.49(19) . . ?
C17A C16A C21A 120.22(19) . . ?
C15A C16A C21A 121.16(18) . . ?
C17A C16A Ca1 82.53(12) . . ?
C15A C16A Ca1 69.44(11) . . ?
C21A C16A Ca1 121.70(12) . . ?
C18A C17A C16A 121.5(2) . . ?
C18A C17A Ca1 78.49(12) . . ?
C16A C17A Ca1 71.04(11) . . ?
C18A C17A H17A 119.3 . . ?
C16A C17A H17A 119.3 . . ?
Ca1 C17A H17A 122.4 . . ?
C19A C18A C17A 119.5(2) . . ?
C19A C18A Ca1 74.27(12) . . ?
C17A C18A Ca1 75.86(12) . . ?
C19A C18A H18A 120.2 . . ?
C17A C18A H18A 120.2 . . ?
Ca1 C18A H18A 120.8 . . ?
C18A C19A C20A 121.5(2) . . ?
C18A C19A Ca1 80.12(13) . . ?
C20A C19A Ca1 70.84(11) . . ?
C18A C19A H19A 119.2 . . ?
C20A C19A H19A 119.2 . . ?
Ca1 C19A H19A 120.8 . . ?
C19A C20A C15A 118.7(2) . . ?
C19A C20A C24A 121.71(19) . . ?
C15A C20A C24A 119.60(19) . . ?
C19A C20A Ca1 82.43(13) . . ?
C15A C20A Ca1 70.86(11) . . ?
C24A C20A Ca1 118.00(13) . . ?
C16A C21A C22A 107.97(17) . . ?
C16A C21A C23A 113.31(18) . . ?
C22A C21A C23A 111.54(17) . . ?
C16A C21A H21A 107.9 . . ?
C22A C21A H21A 107.9 . . ?
C23A C21A H21A 107.9 . . ?
C21A C22A H22A 109.5 . . ?
C21A C22A H22B 109.5 . . ?
H22A C22A H22B 109.5 . . ?
C21A C22A H22C 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C21A C23A H23A 109.5 . . ?
C21A C23A H23B 109.5 . . ?
H23A C23A H23B 109.5 . . ?
C21A C23A H23C 109.5 . . ?
H23A C23A H23C 109.5 . . ?
H23B C23A H23C 109.5 . . ?
C20A C24A C26A 113.0(2) . . ?
C20A C24A C25A 109.70(19) . . ?
C26A C24A C25A 110.8(2) . . ?
C20A C24A H24A 107.7 . . ?
C26A C24A H24A 107.7 . . ?
C25A C24A H24A 107.7 . . ?
C24A C25A H25A 109.5 . . ?
C24A C25A H25B 109.5 . . ?
H25A C25A H25B 109.5 . . ?
C24A C25A H25C 109.5 . . ?
H25A C25A H25C 109.5 . . ?
H25B C25A H25C 109.5 . . ?
C24A C26A H26A 109.5 . . ?
C24A C26A H26B 109.5 . . ?
H26A C26A H26B 109.5 . . ?
C24A C26A H26C 109.5 . . ?
H26A C26A H26C 109.5 . . ?
H26B C26A H26C 109.5 . . ?
C1B N1B C6B 120.10(16) . . ?
C1B N1B Ca1 132.95(12) . . ?
C6B N1B Ca1 106.55(12) . . ?
C1B N2B C15B 128.36(17) . . ?
C13B N3B C14B 119.04(18) . . ?
C13B N3B Ca1 127.05(14) . . ?
C14B N3B Ca1 107.47(12) . . ?
N2B C1B N1B 132.22(18) . . ?
N2B C1B C2B 111.85(16) . . ?
N1B C1B C2B 115.90(16) . . ?
C3B C2B C4B 108.21(16) . . ?
C3B C2B C5B 109.00(17) . . ?
C4B C2B C5B 107.87(17) . . ?
C3B C2B C1B 109.38(16) . . ?
C4B C2B C1B 114.68(16) . . ?
C5B C2B C1B 107.59(16) . . ?
C2B C3B H3BA 109.5 . . ?
C2B C3B H3BB 109.5 . . ?
H3BA C3B H3BB 109.5 . . ?
C2B C3B H3BC 109.5 . . ?
H3BA C3B H3BC 109.5 . . ?
H3BB C3B H3BC 109.5 . . ?
C2B C4B H4BA 109.5 . . ?
C2B C4B H4BB 109.5 . . ?
H4BA C4B H4BB 109.5 . . ?
C2B C4B H4BC 109.5 . . ?
H4BA C4B H4BC 109.5 . . ?
H4BB C4B H4BC 109.5 . . ?
C2B C5B H5BA 109.5 . . ?
C2B C5B H5BB 109.5 . . ?
H5BA C5B H5BB 109.5 . . ?
C2B C5B H5BC 109.5 . . ?
H5BA C5B H5BC 109.5 . . ?
H5BB C5B H5BC 109.5 . . ?
C7B C6B N1B 124.66(18) . . ?
C7B C6B C14B 116.21(17) . . ?
N1B C6B C14B 119.04(17) . . ?
C6B C7B C8B 122.22(19) . . ?
C6B C7B H7BA 118.9 . . ?
C8B C7B H7BA 118.9 . . ?
C9B C8B C7B 121.32(19) . . ?
C9B C8B H8BA 119.3 . . ?
C7B C8B H8BA 119.3 . . ?
C8B C9B C10B 119.19(19) . . ?
C8B C9B H9BA 120.4 . . ?
C10B C9B H9BA 120.4 . . ?
C9B C10B C11B 122.72(19) . . ?
C9B C10B C14B 119.78(19) . . ?
C11B C10B C14B 117.49(19) . . ?
C12B C11B C10B 120.4(2) . . ?
C12B C11B H11B 119.8 . . ?
C10B C11B H11B 119.8 . . ?
C11B C12B C13B 118.5(2) . . ?
C11B C12B H12B 120.7 . . ?
C13B C12B H12B 120.7 . . ?
N3B C13B C12B 123.3(2) . . ?
N3B C13B H13B 118.3 . . ?
C12B C13B H13B 118.3 . . ?
N3B C14B C10B 121.07(18) . . ?
N3B C14B C6B 118.09(17) . . ?
C10B C14B C6B 120.82(18) . . ?
N3B C14B Ca1 47.70(10) . . ?
C10B C14B Ca1 154.43(14) . . ?
C6B C14B Ca1 74.78(11) . . ?
N2B C15B C20B 122.24(18) . . ?
N2B C15B C16B 117.35(18) . . ?
C20B C15B C16B 120.16(18) . . ?
C17B C16B C15B 118.7(2) . . ?
C17B C16B C21B 122.62(19) . . ?
C15B C16B C21B 118.65(17) . . ?
C18B C17B C16B 121.2(2) . . ?
C18B C17B H17B 119.4 . . ?
C16B C17B H17B 119.4 . . ?
C17B C18B C19B 119.76(19) . . ?
C17B C18B H18B 120.1 . . ?
C19B C18B H18B 120.1 . . ?
C18B C19B C20B 121.6(2) . . ?
C18B C19B H19B 119.2 . . ?
C20B C19B H19B 119.2 . . ?
C19B C20B C15B 118.30(19) . . ?
C19B C20B C24B 122.08(19) . . ?
C15B C20B C24B 119.55(18) . . ?
C16B C21B C22B 114.00(18) . . ?
C16B C21B C23B 110.63(18) . . ?
C22B C21B C23B 109.70(18) . . ?
C16B C21B H21B 107.4 . . ?
C22B C21B H21B 107.4 . . ?
C23B C21B H21B 107.4 . . ?
C21B C22B H22D 109.5 . . ?
C21B C22B H22E 109.5 . . ?
H22D C22B H22E 109.5 . . ?
C21B C22B H22F 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
C21B C23B H23D 109.5 . . ?
C21B C23B H23E 109.5 . . ?
H23D C23B H23E 109.5 . . ?
C21B C23B H23F 109.5 . . ?
H23D C23B H23F 109.5 . . ?
H23E C23B H23F 109.5 . . ?
C26B C24B C20B 114.80(18) . . ?
C26B C24B C25B 110.8(2) . . ?
C20B C24B C25B 109.13(18) . . ?
C26B C24B H24B 107.3 . . ?
C20B C24B H24B 107.3 . . ?
C25B C24B H24B 107.3 . . ?
C24B C25B H25D 109.5 . . ?
C24B C25B H25E 109.5 . . ?
H25D C25B H25E 109.5 . . ?
C24B C25B H25F 109.5 . . ?
H25D C25B H25F 109.5 . . ?
H25E C25B H25F 109.5 . . ?
C24B C26B H26D 109.5 . . ?
C24B C26B H26E 109.5 . . ?
H26D C26B H26E 109.5 . . ?
C24B C26B H26F 109.5 . . ?
H26D C26B H26F 109.5 . . ?
H26E C26B H26F 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.058
_database_code_depnum_ccdc_archive 'CCDC 991551'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  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.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_FO5366

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H76 Ca N6 O2, C4 H8 O'
_chemical_formula_sum            'C56 H84 Ca N6 O3'
_chemical_formula_weight         929.37

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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                   9.4797(4)
_cell_length_b                   13.3686(4)
_cell_length_c                   13.6570(5)
_cell_angle_alpha                99.978(2)
_cell_angle_beta                 105.794(2)
_cell_angle_gamma                109.907(2)
_cell_volume                     1496.72(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    240(2)
_cell_measurement_reflns_used    8979
_cell_measurement_theta_min      1.69
_cell_measurement_theta_max      26.02

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.052
_exptl_crystal_size_min          0.048
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             506
_exptl_absorpt_coefficient_mu    0.147
_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      240(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            8979
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         26.02
_reflns_number_total             5742
_reflns_number_gt                4949
_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 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 > 2sigma(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)+(0.1508P)²+1.2499P] 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       ?
_refine_ls_number_reflns         5742
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2605
_refine_ls_wR_factor_gt          0.2464
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.005
_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
Ca1 Ca 0.0000 0.0000 0.0000 0.0373(3) Uani 1 2 d S . .
O1 O 0.2501(3) 0.00058(19) 0.0933(2) 0.0590(6) Uani 1 1 d . B .
N1 N -0.1341(3) -0.20406(17) -0.05107(17) 0.0356(5) Uani 1 1 d . . .
N2 N -0.3108(3) -0.38663(18) -0.14888(18) 0.0390(5) Uani 1 1 d . . .
N3 N -0.1294(3) -0.10396(19) 0.10344(19) 0.0431(6) Uani 1 1 d . . .
C1 C -0.1949(3) -0.2948(2) -0.1385(2) 0.0336(6) Uani 1 1 d . . .
C2 C -0.1135(3) -0.2700(2) -0.2213(2) 0.0410(6) Uani 1 1 d . . .
C3 C -0.1766(5) -0.1951(3) -0.2769(3) 0.0589(9) Uani 1 1 d . . .
H3A H -0.2905 -0.2357 -0.3179 0.088 Uiso 1 1 calc R . .
H3B H -0.1196 -0.1729 -0.3240 0.088 Uiso 1 1 calc R . .
H3C H -0.1594 -0.1294 -0.2238 0.088 Uiso 1 1 calc R . .
C4 C -0.1443(5) -0.3734(3) -0.3076(3) 0.0643(10) Uani 1 1 d . . .
H4A H -0.2582 -0.4113 -0.3493 0.096 Uiso 1 1 calc R . .
H4B H -0.1086 -0.4233 -0.2742 0.096 Uiso 1 1 calc R . .
H4C H -0.0854 -0.3510 -0.3537 0.096 Uiso 1 1 calc R . .
C5 C 0.0673(4) -0.2092(3) -0.1651(3) 0.0555(8) Uani 1 1 d . . .
H5A H 0.1182 -0.1992 -0.2176 0.083 Uiso 1 1 calc R . .
H5B H 0.1065 -0.2525 -0.1236 0.083 Uiso 1 1 calc R . .
H5C H 0.0926 -0.1370 -0.1184 0.083 Uiso 1 1 calc R . .
C6 C -0.1783(3) -0.2075(2) 0.0368(2) 0.0344(6) Uani 1 1 d . . .
C7 C -0.2590(4) -0.3011(2) 0.0662(2) 0.0443(7) Uani 1 1 d . . .
H7A H -0.2933 -0.3734 0.0218 0.053 Uiso 1 1 calc R . .
C8 C -0.2872(4) -0.2855(3) 0.1607(3) 0.0523(8) Uani 1 1 d . . .
H8A H -0.3397 -0.3476 0.1808 0.063 Uiso 1 1 calc R . .
C9 C -0.2389(5) -0.1794(3) 0.2260(3) 0.0568(9) Uani 1 1 d . . .
H9A H -0.2586 -0.1677 0.2900 0.068 Uiso 1 1 calc R . .
C10 C -0.1614(4) -0.0923(3) 0.1937(3) 0.0538(8) Uani 1 1 d . . .
H10A H -0.1285 -0.0198 0.2372 0.065 Uiso 1 1 calc R . .
C11 C -0.3953(3) -0.4848(2) -0.2338(2) 0.0369(6) Uani 1 1 d . . .
C12 C -0.3478(3) -0.5741(2) -0.2337(2) 0.0415(6) Uani 1 1 d . . .
C13 C -0.4396(4) -0.6729(2) -0.3168(3) 0.0507(8) Uani 1 1 d . . .
H13A H -0.4084 -0.7326 -0.3182 0.061 Uiso 1 1 calc R . .
C14 C -0.5748(4) -0.6850(3) -0.3968(3) 0.0546(8) Uani 1 1 d . . .
H14A H -0.6324 -0.7511 -0.4535 0.066 Uiso 1 1 calc R . .
C15 C -0.6251(4) -0.5996(3) -0.3931(2) 0.0522(8) Uani 1 1 d . . .
H15A H -0.7198 -0.6092 -0.4463 0.063 Uiso 1 1 calc R . .
C16 C -0.5381(3) -0.4988(2) -0.3117(2) 0.0418(6) Uani 1 1 d . . .
C17 C -0.2062(4) -0.5646(3) -0.1423(3) 0.0538(8) Uani 1 1 d . . .
H17A H -0.1349 -0.4845 -0.1094 0.065 Uiso 1 1 calc R . .
C18 C -0.1057(5) -0.6233(4) -0.1769(4) 0.0801(13) Uani 1 1 d . . .
H18A H -0.0693 -0.5941 -0.2300 0.120 Uiso 1 1 calc R . .
H18B H -0.1711 -0.7027 -0.2068 0.120 Uiso 1 1 calc R . .
H18C H -0.0135 -0.6101 -0.1156 0.120 Uiso 1 1 calc R . .
C19 C -0.2645(5) -0.6079(3) -0.0572(3) 0.0698(11) Uani 1 1 d . . .
H19A H -0.3159 -0.5637 -0.0303 0.105 Uiso 1 1 calc R . .
H19B H -0.1735 -0.6024 0.0008 0.105 Uiso 1 1 calc R . .
H19C H -0.3409 -0.6851 -0.0884 0.105 Uiso 1 1 calc R . .
C20 C -0.6002(4) -0.4081(3) -0.3041(3) 0.0548(8) Uani 1 1 d . . .
H20A H -0.5045 -0.3363 -0.2747 0.066 Uiso 1 1 calc R . .
C21 C -0.7026(8) -0.4059(5) -0.4100(4) 0.1063(19) Uani 1 1 d . . .
H21A H -0.6423 -0.3988 -0.4574 0.159 Uiso 1 1 calc R . .
H21B H -0.7317 -0.3431 -0.3986 0.159 Uiso 1 1 calc R . .
H21C H -0.7992 -0.4744 -0.4415 0.159 Uiso 1 1 calc R . .
C22 C -0.6844(6) -0.4133(5) -0.2232(5) 0.0913(15) Uani 1 1 d . . .
H22A H -0.6123 -0.4101 -0.1558 0.137 Uiso 1 1 calc R . .
H22B H -0.7801 -0.4822 -0.2491 0.137 Uiso 1 1 calc R . .
H22C H -0.7143 -0.3507 -0.2133 0.137 Uiso 1 1 calc R . .
C23 C 0.2675(6) -0.0837(4) 0.1418(4) 0.0848(14) Uani 1 1 d . . .
H23A H 0.2452 -0.1509 0.0872 0.102 Uiso 0.50 1 calc PR A 1
H23B H 0.1910 -0.1032 0.1786 0.102 Uiso 0.50 1 calc PR A 1
H23C H 0.1941 -0.1584 0.0941 0.102 Uiso 0.50 1 calc PR A 2
H23D H 0.2478 -0.0741 0.2089 0.102 Uiso 0.50 1 calc PR A 2
C24 C 0.4319(11) -0.0407(9) 0.2178(9) 0.078(3) Uani 0.50 1 d P B 1
H24A H 0.4709 -0.0997 0.2208 0.093 Uiso 0.50 1 calc PR B 1
H24B H 0.4407 -0.0045 0.2894 0.093 Uiso 0.50 1 calc PR B 1
C25 C 0.5273(17) 0.0483(14) 0.1666(14) 0.097(4) Uani 0.50 1 d P B 1
H25A H 0.6203 0.1106 0.2218 0.116 Uiso 0.50 1 calc PR B 1
H25B H 0.5633 0.0131 0.1150 0.116 Uiso 0.50 1 calc PR B 1
C24A C 0.4351(18) -0.0647(13) 0.1600(13) 0.111(5) Uiso 0.50 1 d P B 2
H24C H 0.4550 -0.0827 0.0937 0.133 Uiso 0.50 1 calc PR B 2
H24D H 0.4745 -0.1036 0.2081 0.133 Uiso 0.50 1 calc PR B 2
C25A C 0.5083(16) 0.0751(13) 0.2185(12) 0.089(4) Uani 0.50 1 d P B 2
H25C H 0.4769 0.0946 0.2794 0.107 Uiso 0.50 1 calc PR B 2
H25D H 0.6243 0.1142 0.2366 0.107 Uiso 0.50 1 calc PR B 2
C26 C 0.4065(5) 0.0846(4) 0.1150(5) 0.0806(13) Uani 1 1 d . . .
H26A H 0.4207 0.1547 0.1614 0.097 Uiso 0.50 1 calc PR B 1
H26B H 0.4177 0.0971 0.0484 0.097 Uiso 0.50 1 calc PR B 1
H26C H 0.4053 0.1586 0.1248 0.097 Uiso 0.50 1 calc PR B 2
H26D H 0.4465 0.0694 0.0575 0.097 Uiso 0.50 1 calc PR B 2
O1T O 0.0880(16) -0.1674(12) -0.4780(11) 0.167(4) Uiso 0.50 1 d P . .
C1T C 0.1232(16) -0.2108(11) -0.5630(11) 0.111(4) Uiso 0.50 1 d P . .
H1TA H 0.0299 -0.2388 -0.6291 0.134 Uiso 0.50 1 calc PR . .
H1TB H 0.1539 -0.2721 -0.5519 0.134 Uiso 0.50 1 calc PR . .
C2T C 0.2631(18) -0.1150(13) -0.5685(13) 0.130(5) Uiso 0.50 1 d P . .
H2TA H 0.2540 -0.1149 -0.6417 0.156 Uiso 0.50 1 calc PR . .
H2TB H 0.3680 -0.1126 -0.5292 0.156 Uiso 0.50 1 calc PR . .
C3T C 0.225(2) -0.0216(15) -0.5100(13) 0.140(5) Uiso 0.50 1 d P . .
H3TA H 0.3236 0.0461 -0.4714 0.168 Uiso 0.50 1 calc PR . .
H3TB H 0.1495 -0.0037 -0.5611 0.168 Uiso 0.50 1 calc PR . .
C4T C 0.1602(17) -0.0624(12) -0.4423(11) 0.113(4) Uiso 0.50 1 d P . .
H4TA H 0.2447 -0.0416 -0.3729 0.135 Uiso 0.50 1 calc PR . .
H4TB H 0.0841 -0.0306 -0.4324 0.135 Uiso 0.50 1 calc PR . .


_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
Ca1 O1 2.363(2) . ?
Ca1 O1 2.363(2) 2 ?
Ca1 N3 2.428(2) . ?
Ca1 N3 2.428(2) 2 ?
Ca1 N1 2.458(2) . ?
Ca1 N1 2.458(2) 2 ?
Ca1 C6 2.925(3) . ?
Ca1 C6 2.925(3) 2 ?
O1 C26 1.435(4) . ?
O1 C23 1.436(5) . ?
N1 C1 1.370(3) . ?
N1 C6 1.376(3) . ?
N2 C1 1.292(3) . ?
N2 C11 1.400(3) . ?
N3 C10 1.344(4) . ?
N3 C6 1.363(3) . ?
C1 C2 1.554(4) . ?
C2 C5 1.518(4) . ?
C2 C4 1.535(4) . ?
C2 C3 1.537(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 H3C 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 H4C 0.9700 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 C7 1.415(4) . ?
C7 C8 1.383(4) . ?
C7 H7A 0.9400 . ?
C8 C9 1.384(5) . ?
C8 H8A 0.9400 . ?
C9 C10 1.364(5) . ?
C9 H9A 0.9400 . ?
C10 H10A 0.9400 . ?
C11 C16 1.405(4) . ?
C11 C12 1.412(4) . ?
C12 C13 1.396(4) . ?
C12 C17 1.515(4) . ?
C13 C14 1.377(5) . ?
C13 H13A 0.9400 . ?
C14 C15 1.378(5) . ?
C14 H14A 0.9400 . ?
C15 C16 1.398(4) . ?
C15 H15A 0.9400 . ?
C16 C20 1.518(5) . ?
C17 C19 1.534(5) . ?
C17 C18 1.539(5) . ?
C17 H17A 0.9900 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C18 H18C 0.9700 . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C19 H19C 0.9700 . ?
C20 C21 1.517(6) . ?
C20 C22 1.527(6) . ?
C20 H20A 0.9900 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 H21C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
C23 C24A 1.463(15) . ?
C23 C24 1.463(9) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C23 H23D 0.9800 . ?
C24 C25 1.619(19) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C25 C26 1.449(16) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C24A C25A 1.71(2) . ?
C24A H24C 0.9800 . ?
C24A H24D 0.9800 . ?
C25A C26 1.532(15) . ?
C25A H25C 0.9800 . ?
C25A H25D 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 H26D 0.9800 . ?
O1T C4T 1.266(17) . ?
O1T C1T 1.380(17) . ?
C1T C2T 1.528(19) . ?
C1T H1TA 0.9800 . ?
C1T H1TB 0.9800 . ?
C2T C3T 1.56(2) . ?
C2T H2TA 0.9800 . ?
C2T H2TB 0.9800 . ?
C3T C4T 1.337(19) . ?
C3T H3TA 0.9800 . ?
C3T H3TB 0.9800 . ?
C4T H4TA 0.9800 . ?
C4T H4TB 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
O1 Ca1 O1 180.0 . 2 ?
O1 Ca1 N3 91.75(9) . . ?
O1 Ca1 N3 88.25(9) 2 . ?
O1 Ca1 N3 88.25(9) . 2 ?
O1 Ca1 N3 91.75(9) 2 2 ?
N3 Ca1 N3 180.00(7) . 2 ?
O1 Ca1 N1 92.22(8) . . ?
O1 Ca1 N1 87.78(8) 2 . ?
N3 Ca1 N1 55.49(7) . . ?
N3 Ca1 N1 124.51(7) 2 . ?
O1 Ca1 N1 87.78(8) . 2 ?
O1 Ca1 N1 92.22(8) 2 2 ?
N3 Ca1 N1 124.51(7) . 2 ?
N3 Ca1 N1 55.49(7) 2 2 ?
N1 Ca1 N1 180.0 . 2 ?
O1 Ca1 C6 92.24(8) . . ?
O1 Ca1 C6 87.76(8) 2 . ?
N3 Ca1 C6 27.55(7) . . ?
N3 Ca1 C6 152.45(7) 2 . ?
N1 Ca1 C6 27.94(7) . . ?
N1 Ca1 C6 152.06(7) 2 . ?
O1 Ca1 C6 87.76(8) . 2 ?
O1 Ca1 C6 92.24(8) 2 2 ?
N3 Ca1 C6 152.45(7) . 2 ?
N3 Ca1 C6 27.55(7) 2 2 ?
N1 Ca1 C6 152.06(7) . 2 ?
N1 Ca1 C6 27.94(7) 2 2 ?
C6 Ca1 C6 180.0 . 2 ?
C26 O1 C23 109.0(3) . . ?
C26 O1 Ca1 126.9(2) . . ?
C23 O1 Ca1 124.0(2) . . ?
C1 N1 C6 122.8(2) . . ?
C1 N1 Ca1 140.04(17) . . ?
C6 N1 Ca1 95.26(15) . . ?
C1 N2 C11 130.4(2) . . ?
C10 N3 C6 120.0(2) . . ?
C10 N3 Ca1 143.0(2) . . ?
C6 N3 Ca1 96.97(16) . . ?
N2 C1 N1 121.8(2) . . ?
N2 C1 C2 126.3(2) . . ?
N1 C1 C2 111.8(2) . . ?
C5 C2 C4 107.0(3) . . ?
C5 C2 C3 109.0(3) . . ?
C4 C2 C3 108.0(3) . . ?
C5 C2 C1 109.8(2) . . ?
C4 C2 C1 114.7(2) . . ?
C3 C2 C1 108.3(2) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C6 N1 112.3(2) . . ?
N3 C6 C7 118.5(2) . . ?
N1 C6 C7 129.1(2) . . ?
N3 C6 Ca1 55.48(13) . . ?
N1 C6 Ca1 56.80(12) . . ?
C7 C6 Ca1 173.8(2) . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7A 120.2 . . ?
C6 C7 H7A 120.2 . . ?
C9 C8 C7 120.6(3) . . ?
C9 C8 H8A 119.7 . . ?
C7 C8 H8A 119.7 . . ?
C10 C9 C8 117.2(3) . . ?
C10 C9 H9A 121.4 . . ?
C8 C9 H9A 121.4 . . ?
N3 C10 C9 123.9(3) . . ?
N3 C10 H10A 118.0 . . ?
C9 C10 H10A 118.0 . . ?
N2 C11 C16 119.5(3) . . ?
N2 C11 C12 119.8(3) . . ?
C16 C11 C12 120.2(2) . . ?
C13 C12 C11 118.4(3) . . ?
C13 C12 C17 121.0(3) . . ?
C11 C12 C17 120.5(3) . . ?
C14 C13 C12 121.6(3) . . ?
C14 C13 H13A 119.2 . . ?
C12 C13 H13A 119.2 . . ?
C13 C14 C15 119.6(3) . . ?
C13 C14 H14A 120.2 . . ?
C15 C14 H14A 120.2 . . ?
C14 C15 C16 121.3(3) . . ?
C14 C15 H15A 119.4 . . ?
C16 C15 H15A 119.4 . . ?
C15 C16 C11 118.7(3) . . ?
C15 C16 C20 120.9(3) . . ?
C11 C16 C20 120.3(3) . . ?
C12 C17 C19 109.8(3) . . ?
C12 C17 C18 113.7(3) . . ?
C19 C17 C18 110.9(3) . . ?
C12 C17 H17A 107.4 . . ?
C19 C17 H17A 107.4 . . ?
C18 C17 H17A 107.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C21 C20 C16 114.7(3) . . ?
C21 C20 C22 112.5(4) . . ?
C16 C20 C22 109.8(3) . . ?
C21 C20 H20A 106.5 . . ?
C16 C20 H20A 106.5 . . ?
C22 C20 H20A 106.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O1 C23 C24A 102.5(7) . . ?
O1 C23 C24 108.6(5) . . ?
C24A C23 C24 32.2(6) . . ?
O1 C23 H23A 110.0 . . ?
C24A C23 H23A 83.4 . . ?
C24 C23 H23A 110.0 . . ?
O1 C23 H23B 110.0 . . ?
C24A C23 H23B 138.2 . . ?
C24 C23 H23B 110.0 . . ?
H23A C23 H23B 108.3 . . ?
O1 C23 H23C 111.3 . . ?
C24A C23 H23C 111.3 . . ?
C24 C23 H23C 131.6 . . ?
H23A C23 H23C 29.5 . . ?
H23B C23 H23C 80.8 . . ?
O1 C23 H23D 111.3 . . ?
C24A C23 H23D 111.3 . . ?
C24 C23 H23D 79.9 . . ?
H23A C23 H23D 131.3 . . ?
H23B C23 H23D 32.0 . . ?
H23C C23 H23D 109.2 . . ?
C23 C24 C25 101.1(8) . . ?
C23 C24 H24A 111.5 . . ?
C25 C24 H24A 111.6 . . ?
C23 C24 H24B 111.5 . . ?
C25 C24 H24B 111.5 . . ?
H24A C24 H24B 109.4 . . ?
C26 C25 C24 102.5(9) . . ?
C26 C25 H25A 111.3 . . ?
C24 C25 H25A 111.3 . . ?
C26 C25 H25B 111.3 . . ?
C24 C25 H25B 111.3 . . ?
H25A C25 H25B 109.2 . . ?
C23 C24A C25A 94.5(10) . . ?
C23 C24A H24C 112.8 . . ?
C25A C24A H24C 112.8 . . ?
C23 C24A H24D 112.8 . . ?
C25A C24A H24D 112.8 . . ?
H24C C24A H24D 110.3 . . ?
C26 C25A C24A 88.7(9) . . ?
C26 C25A H25C 113.9 . . ?
C24A C25A H25C 113.9 . . ?
C26 C25A H25D 113.9 . . ?
C24A C25A H25D 113.9 . . ?
H25C C25A H25D 111.1 . . ?
O1 C26 C25 109.1(7) . . ?
O1 C26 C25A 102.7(6) . . ?
C25 C26 C25A 32.2(6) . . ?
O1 C26 H26A 109.9 . . ?
C25 C26 H26A 109.9 . . ?
C25A C26 H26A 83.5 . . ?
O1 C26 H26B 109.9 . . ?
C25 C26 H26B 109.9 . . ?
C25A C26 H26B 138.2 . . ?
H26A C26 H26B 108.3 . . ?
O1 C26 H26C 111.2 . . ?
C25 C26 H26C 131.2 . . ?
C25A C26 H26C 111.2 . . ?
H26A C26 H26C 29.4 . . ?
H26B C26 H26C 80.8 . . ?
O1 C26 H26D 111.2 . . ?
C25 C26 H26D 79.8 . . ?
C25A C26 H26D 111.2 . . ?
H26A C26 H26D 131.3 . . ?
H26B C26 H26D 32.1 . . ?
H26C C26 H26D 109.1 . . ?
C4T O1T C1T 112.7(14) . . ?
O1T C1T C2T 105.9(12) . . ?
O1T C1T H1TA 110.6 . . ?
C2T C1T H1TA 110.6 . . ?
O1T C1T H1TB 110.6 . . ?
C2T C1T H1TB 110.6 . . ?
H1TA C1T H1TB 108.7 . . ?
C1T C2T C3T 94.8(12) . . ?
C1T C2T H2TA 112.8 . . ?
C3T C2T H2TA 112.8 . . ?
C1T C2T H2TB 112.8 . . ?
C3T C2T H2TB 112.8 . . ?
H2TA C2T H2TB 110.2 . . ?
C4T C3T C2T 105.9(14) . . ?
C4T C3T H3TA 110.6 . . ?
C2T C3T H3TA 110.5 . . ?
C4T C3T H3TB 110.6 . . ?
C2T C3T H3TB 110.5 . . ?
H3TA C3T H3TB 108.7 . . ?
O1T C4T C3T 110.2(14) . . ?
O1T C4T H4TA 109.6 . . ?
C3T C4T H4TA 109.6 . . ?
O1T C4T H4TB 109.6 . . ?
C3T C4T H4TB 109.6 . . ?
H4TA C4T H4TB 108.1 . . ?

_diffrn_measured_fraction_theta_max 0.974
_diffrn_reflns_theta_full        26.02
_diffrn_measured_fraction_theta_full 0.974
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.090

_database_code_depnum_ccdc_archive 'CCDC 991552'
