# Supplementary Material (ESI) for Perkin Transactions
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 188/244
 
data_5xCa(ClO4)2
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C26 H34 Ca Cl2 N6 O16' 
_chemical_formula_weight          797.57 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0181   0.0091 
 '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'   0.0311   0.0180 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0492   0.0322 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.3639   0.7018 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ca'  'Ca'   0.3641   1.2855 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            orthorombic 
_symmetry_space_group_name_H-M    Pna2(1) 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, z+1/2' 
 'x+1/2, -y+1/2, z' 
 '-x+1/2, y+1/2, z+1/2' 
 
_cell_length_a                    23.1803(15) 
_cell_length_b                    10.1436(3) 
_cell_length_c                    14.6585(7) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3446.7(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     19 
_cell_measurement_theta_min       23.43 
_cell_measurement_theta_max       45.43 
 
_exptl_crystal_description        ? 
_exptl_crystal_colour             colourless 
_exptl_crystal_size_max           0.28 
_exptl_crystal_size_mid           0.21 
_exptl_crystal_size_min           0.21 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.537 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1656 
_exptl_absorpt_coefficient_mu     3.719 
_exptl_absorpt_correction_type    psi-scan 
_exptl_absorpt_correction_T_min   90.12 
_exptl_absorpt_correction_T_max   99.93 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      1.54178 
_diffrn_radiation_type            CuK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Enraf-Nonius MACH3'
_diffrn_measurement_method        EXPRESS 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  100 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         0.0 
_diffrn_reflns_number             2545 
_diffrn_reflns_av_R_equivalents   0.0000 
_diffrn_reflns_av_sigmaI/netI     0.0552 
_diffrn_reflns_limit_h_min        0 
_diffrn_reflns_limit_h_max        28 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        0 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        18 
_diffrn_reflns_theta_min          3.81 
_diffrn_reflns_theta_max          74.10 
_reflns_number_total              2545 
_reflns_number_gt                 2354 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        EXPRESS 
_computing_cell_refinement        EXPRESS 
_computing_data_reduction         MOLEN 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR 
and 
 goodness of fit S are based on F^2^, conventional R-factors R are based 
 on F, with F set to zero for negative F^2^. The threshold expression of 
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and 
is 
 not relevant to the choice of reflections for refinement.  R-factors 
based 
 on F^2^ are statistically about twice as large as those based on F, and 
R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+7.3980P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0076(6) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' 
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.01(3) 
_refine_ls_number_reflns          2545 
_refine_ls_number_parameters      461 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0859 
_refine_ls_R_factor_gt            0.0743 
_refine_ls_wR_factor_ref          0.1971 
_refine_ls_wR_factor_gt           0.1730 
_refine_ls_goodness_of_fit_ref    1.170 
_refine_ls_restrained_S_all       1.169 
_refine_ls_shift/su_max           0.008 
_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_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ca1 Ca 0.36976(8) 0.7542(2) 0.26158(19) 0.0321(5) Uani 1 d . . . 
Cl1 Cl 0.23837(13) 0.7302(3) 0.3950(2) 0.0544(8) Uani 1 d . . . 
Cl2 Cl 0.50847(12) 0.7643(3) 0.1474(2) 0.0535(8) Uani 1 d . . . 
O5 O 0.2790(4) 0.7725(10) 0.3319(8) 0.070(3) Uani 1 d . . . 
O6 O 0.2321(7) 0.5931(14) 0.3895(19) 0.174(10) Uani 1 d . . . 
O7 O 0.2641(12) 0.7426(18) 0.4791(11) 0.181(10) Uani 1 d . . . 
O8 O 0.1912(7) 0.792(3) 0.390(2) 0.251(16) Uani 1 d . . . 
O9 O 0.4569(4) 0.7150(12) 0.1886(10) 0.094(4) Uani 1 d . . . 
O10 O 0.5562(5) 0.7368(13) 0.2032(11) 0.099(4) Uani 1 d . . . 
O11 O 0.5137(9) 0.714(3) 0.0642(14) 0.238(14) Uani 1 d . . . 
O12 O 0.5031(7) 0.9073(14) 0.1493(18) 0.165(9) Uani 1 d . . . 
O1 O 0.3876(3) 1.5659(7) 0.3465(6) 0.048(2) Uani 1 d . . . 
O2 O 0.4168(3) 0.8828(7) 0.3693(6) 0.045(2) Uani 1 d . . . 
O3 O 0.5940(4) 1.1340(9) 0.4014(7) 0.053(2) Uani 1 d . . . 
O4 O 0.5796(4) 1.4135(9) 0.4237(6) 0.057(2) Uani 1 d . . . 
N1 N 0.4671(4) 1.4612(9) 0.3982(9) 0.052(3) Uani 1 d . . . 
H1 H 0.4826 1.3743 0.4191 0.062 Uiso 1 calc R . . 
N4 N 0.4161(3) 1.2282(8) 0.3858(6) 0.0338(19) Uani 1 d . . . 
N7 N 0.4866(4) 1.0286(9) 0.4061(9) 0.053(3) Uani 1 d . . . 
H7 H 0.4941 1.1219 0.4246 0.064 Uiso 1 calc R . . 
C2 C 0.4134(5) 1.4640(10) 0.3725(8) 0.039(2) Uani 1 d . . . 
C3 C 0.3822(4) 1.3369(11) 0.3775(8) 0.036(2) Uani 1 d . . . 
C5 C 0.3926(4) 1.1105(10) 0.3855(8) 0.036(2) Uani 1 d . . . 
C6 C 0.4336(5) 0.9977(12) 0.3880(8) 0.043(3) Uani 1 d . . . 
C8 C 0.3228(5) 1.3268(12) 0.3722(9) 0.047(3) Uani 1 d . . . 
H8 H 0.2982 1.4068 0.3641 0.056 Uiso 1 calc R . . 
C9 C 0.2986(5) 1.2027(12) 0.3784(10) 0.051(3) Uani 1 d . . . 
H9 H 0.2557 1.1928 0.3788 0.061 Uiso 1 calc R . . 
C10 C 0.3331(5) 1.0927(12) 0.3842(10) 0.050(3) Uani 1 d . . . 
H10 H 0.3158 1.0025 0.3873 0.060 Uiso 1 calc R . . 
C11 C 0.5364(5) 0.9408(12) 0.4022(12) 0.053(3) Uani 1 d . . . 
H11A H 0.5456 0.9153 0.3343 0.064 Uiso 1 calc R . . 
H11B H 0.5281 0.8541 0.4391 0.064 Uiso 1 calc R . . 
C12 C 0.5873(5) 1.0155(12) 0.4443(11) 0.056(3) Uani 1 d . . . 
H12A H 0.5797 1.0308 0.5141 0.067 Uiso 1 calc R . . 
H12B H 0.6251 0.9594 0.4374 0.067 Uiso 1 calc R . . 
C13 C 0.6348(6) 1.2188(14) 0.4441(13) 0.065(4) Uani 1 d . . . 
H13A H 0.6765 1.1795 0.4369 0.078 Uiso 1 calc R . . 
H13B H 0.6256 1.2262 0.5141 0.078 Uiso 1 calc R . . 
C14 C 0.6323(6) 1.3548(15) 0.4006(14) 0.071(4) Uani 1 d . . . 
H14A H 0.6667 1.4129 0.4244 0.085 Uiso 1 calc R . . 
H14B H 0.6359 1.3466 0.3294 0.085 Uiso 1 calc R . . 
C15 C 0.5645(6) 1.5242(13) 0.3682(11) 0.058(4) Uani 1 d . . . 
H15A H 0.5624 1.4963 0.2993 0.070 Uiso 1 calc R . . 
H15B H 0.5954 1.5991 0.3749 0.070 Uiso 1 calc R . . 
C16 C 0.5070(5) 1.5720(12) 0.3998(10) 0.050(3) Uani 1 d . . . 
H16A H 0.5102 1.6100 0.4662 0.060 Uiso 1 calc R . . 
H16B H 0.4921 1.6473 0.3566 0.060 Uiso 1 calc R . . 
O1' O 0.3476(4) -0.0613(7) 0.1811(6) 0.0447(19) Uani 1 d . . . 
O2' O 0.3268(3) 0.6240(7) 0.1539(6) 0.0430(19) Uani 1 d . . . 
O3' O 0.1464(4) 0.3929(10) 0.1115(8) 0.072(3) Uani 1 d . . . 
O4' O 0.1535(4) 0.1131(9) 0.1434(7) 0.061(2) Uani 1 d . . . 
N1' N 0.2663(5) 0.0509(10) 0.1479(10) 0.061(3) Uani 1 d . . . 
H1' H 0.2518 0.1406 0.1313 0.073 Uiso 1 calc R . . 
N4' N 0.3215(4) 0.2784(8) 0.1447(7) 0.0336(18) Uani 1 d . . . 
N7' N 0.2531(4) 0.4855(9) 0.1246(9) 0.052(3) Uani 1 d . . . 
H7' H 0.2441 0.3942 0.1030 0.062 Uiso 1 calc R . . 
C2' C 0.3223(4) 0.0412(11) 0.1601(8) 0.040(3) Uani 1 d . . . 
C3' C 0.3545(4) 0.1714(9) 0.1520(8) 0.034(2) Uani 1 d . . . 
C5' C 0.3473(5) 0.3958(9) 0.1393(8) 0.036(2) Uani 1 d . . . 
C6' C 0.3076(4) 0.5124(9) 0.1402(8) 0.034(2) Uani 1 d . . . 
C8' C 0.4132(5) 0.1752(11) 0.1539(9) 0.045(3) Uani 1 d . . . 
H8' H 0.4363 0.0926 0.1606 0.054 Uiso 1 calc R . . 
C9' C 0.4401(5) 0.2971(15) 0.1462(11) 0.058(4) Uani 1 d . . . 
H9' H 0.4832 0.3030 0.1465 0.070 Uiso 1 calc R . . 
C10' C 0.4070(5) 0.4110(11) 0.1380(9) 0.044(3) Uani 1 d . . . 
H10' H 0.4253 0.4998 0.1316 0.053 Uiso 1 calc R . . 
C11' C 0.2051(6) 0.5730(11) 0.1352(10) 0.053(3) Uani 1 d . . . 
H11C H 0.1955 0.6167 0.0721 0.064 Uiso 1 calc R . . 
H11D H 0.2162 0.6485 0.1810 0.064 Uiso 1 calc R . . 
C12' C 0.1531(6) 0.5031(14) 0.1697(13) 0.075(5) Uani 1 d . . . 
H12C H 0.1592 0.4729 0.2375 0.090 Uiso 1 calc R . . 
H12D H 0.1167 0.5645 0.1665 0.090 Uiso 1 calc R . . 
C13' C 0.0985(5) 0.3111(13) 0.1359(15) 0.079(5) Uani 1 d . . . 
H13C H 0.0600 0.3514 0.1108 0.095 Uiso 1 calc R . . 
H13D H 0.0953 0.3032 0.2071 0.095 Uiso 1 calc R . . 
C14' C 0.1093(5) 0.1778(13) 0.0941(14) 0.069(5) Uani 1 d . . . 
H14C H 0.0713 0.1213 0.0962 0.083 Uiso 1 calc R . . 
H14D H 0.1216 0.1887 0.0256 0.083 Uiso 1 calc R . . 
C15' C 0.1699(5) -0.0129(12) 0.1054(14) 0.066(4) Uani 1 d . . . 
H15C H 0.1780 -0.0048 0.0351 0.080 Uiso 1 calc R . . 
H15D H 0.1373 -0.0831 0.1157 0.080 Uiso 1 calc R . . 
C16' C 0.2230(6) -0.0500(12) 0.1552(14) 0.069(5) Uani 1 d . . . 
H16C H 0.2131 -0.0657 0.2242 0.083 Uiso 1 calc R . . 
H16D H 0.2392 -0.1386 0.1284 0.083 Uiso 1 calc R . . 
 
loop_ 
 _atom_site_aniso_label 
 _atom_site_aniso_U_11 
 _atom_site_aniso_U_22 
 _atom_site_aniso_U_33 
 _atom_site_aniso_U_23 
 _atom_site_aniso_U_13 
 _atom_site_aniso_U_12 
Ca1 0.0304(8) 0.0220(7) 0.0440(9) 0.0009(8) -0.0037(9) 0.0004(7) 
Cl1 0.0424(14) 0.065(2) 0.0558(18) 0.0078(18) 0.0149(13) 0.0003(13) 
Cl2 0.0372(13) 0.073(2) 0.0504(16) 0.0031(18) 0.0067(12) -0.0053(13) 
O5 0.066(6) 0.071(7) 0.074(7) 0.018(6) 0.034(5) 0.007(5) 
O6 0.123(12) 0.072(9) 0.33(3) 0.011(15) 0.041(17) -0.037(8) 
O7 0.32(3) 0.172(18) 0.054(8) -0.008(10) 0.029(13) -0.009(18) 
O8 0.096(11) 0.28(2) 0.38(4) 0.22(2) 0.119(17) 0.127(14) 
O9 0.052(5) 0.094(8) 0.136(12) -0.004(8) 0.036(7) -0.016(5) 
O10 0.055(6) 0.109(10) 0.133(11) 0.049(9) -0.020(7) 0.002(6) 
O11 0.161(17) 0.45(4) 0.102(13) -0.12(2) 0.068(13) -0.03(2) 
O12 0.109(10) 0.074(8) 0.31(3) 0.081(15) -0.026(14) -0.007(8) 
O1 0.046(4) 0.030(4) 0.067(6) -0.002(4) -0.008(4) 0.005(3) 
O2 0.046(4) 0.024(4) 0.066(6) -0.001(4) -0.007(4) -0.008(3) 
O3 0.054(5) 0.049(5) 0.057(5) 0.008(4) -0.006(4) -0.004(4) 
O4 0.052(5) 0.052(5) 0.068(6) 0.023(5) -0.003(4) -0.008(4) 
N1 0.050(5) 0.021(4) 0.085(8) 0.015(5) -0.011(6) -0.004(4) 
N4 0.033(4) 0.025(4) 0.043(5) -0.001(4) -0.009(4) -0.007(3) 
N7 0.051(6) 0.024(5) 0.084(8) -0.005(5) -0.013(6) 0.008(4) 
C2 0.043(5) 0.021(5) 0.051(7) -0.002(5) -0.007(5) 0.003(4) 
C3 0.036(5) 0.031(5) 0.040(6) -0.001(5) -0.002(4) 0.003(4) 
C5 0.038(5) 0.031(5) 0.039(6) 0.000(5) -0.004(5) -0.005(4) 
C6 0.052(6) 0.036(6) 0.039(6) -0.010(5) -0.008(6) -0.004(5) 
C8 0.044(6) 0.042(7) 0.054(8) 0.002(6) 0.006(6) 0.014(5) 
C9 0.035(6) 0.040(6) 0.077(9) -0.006(7) 0.011(6) -0.001(5) 
C10 0.043(6) 0.034(6) 0.073(9) 0.001(6) 0.008(6) -0.010(5) 
C11 0.042(6) 0.035(6) 0.083(10) 0.001(7) -0.002(7) -0.005(5) 
C12 0.045(6) 0.041(7) 0.081(10) -0.004(7) -0.010(7) 0.006(5) 
C13 0.047(7) 0.063(9) 0.086(10) 0.001(8) -0.023(7) 0.000(6) 
C14 0.055(8) 0.053(8) 0.104(13) 0.009(9) 0.009(9) -0.006(7) 
C15 0.062(8) 0.042(7) 0.072(9) 0.008(7) -0.009(7) -0.013(6) 
C16 0.036(5) 0.040(7) 0.074(9) -0.001(6) -0.005(6) 0.005(5) 
O1' 0.056(5) 0.032(4) 0.046(4) 0.007(3) 0.001(4) 0.008(4) 
O2' 0.060(5) 0.024(4) 0.045(4) -0.001(4) -0.009(4) -0.005(3) 
O3' 0.044(5) 0.066(7) 0.106(8) -0.021(6) 0.000(5) -0.009(5) 
O4' 0.057(5) 0.052(5) 0.073(6) -0.020(5) -0.010(5) 0.001(4) 
N1' 0.054(6) 0.030(5) 0.099(10) 0.021(6) -0.024(6) -0.011(4) 
N4' 0.036(4) 0.022(4) 0.043(5) 0.000(4) -0.001(4) 0.005(3) 
N7' 0.044(5) 0.027(5) 0.083(8) -0.020(5) -0.012(5) 0.006(4) 
C2' 0.030(5) 0.036(6) 0.053(7) 0.029(6) -0.002(5) -0.011(4) 
C3' 0.037(5) 0.027(5) 0.037(5) 0.003(5) 0.001(4) -0.003(4) 
C5' 0.053(6) 0.020(4) 0.035(5) -0.001(5) -0.005(5) -0.010(4) 
C6' 0.035(5) 0.015(4) 0.053(7) 0.001(5) -0.003(5) -0.003(4) 
C8' 0.055(7) 0.034(6) 0.045(6) -0.016(5) 0.008(5) -0.006(5) 
C9' 0.038(6) 0.064(9) 0.072(9) -0.008(8) 0.026(6) -0.007(6) 
C10' 0.048(6) 0.035(5) 0.049(7) -0.003(5) 0.009(5) -0.002(5) 
C11' 0.071(9) 0.030(6) 0.058(8) 0.004(6) -0.007(7) 0.011(6) 
C12' 0.059(8) 0.051(8) 0.116(15) -0.025(9) 0.004(9) 0.002(7) 
C13' 0.040(6) 0.053(8) 0.144(17) -0.014(11) 0.017(9) -0.004(6) 
C14' 0.032(6) 0.050(8) 0.126(14) -0.007(9) -0.010(8) -0.007(5) 
C15' 0.051(7) 0.037(6) 0.111(13) -0.020(8) 0.001(8) -0.014(5) 
C16' 0.071(9) 0.027(6) 0.110(14) -0.002(8) -0.015(9) -0.016(6) 
 
_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' 2.272(8) 1_565 ? 
Ca1 O2' 2.286(8) . ? 
Ca1 O1 2.317(8) 1_545 ? 
Ca1 O9 2.319(11) . ? 
Ca1 O2 2.321(8) . ? 
Ca1 O5 2.350(9) . ? 
Cl1 O8 1.261(13) . ? 
Cl1 O7 1.38(2) . ? 
Cl1 O5 1.387(9) . ? 
Cl1 O6 1.401(14) . ? 
Cl2 O11 1.329(18) . ? 
Cl2 O10 1.404(11) . ? 
Cl2 O9 1.431(10) . ? 
Cl2 O12 1.456(14) . ? 
O1 C2 1.253(13) . ? 
O1 Ca1 2.317(8) 1_565 ? 
O2 C6 1.259(13) . ? 
O3 C12 1.366(16) . ? 
O3 C13 1.424(16) . ? 
O4 C14 1.401(16) . ? 
O4 C15 1.430(15) . ? 
N1 C2 1.302(14) . ? 
N1 C16 1.455(14) . ? 
N4 C5 1.313(13) . ? 
N4 C3 1.359(13) . ? 
N7 C6 1.295(14) . ? 
N7 C11 1.459(15) . ? 
C2 C3 1.480(14) . ? 
C3 C8 1.383(15) . ? 
C5 C10 1.392(15) . ? 
C5 C6 1.488(16) . ? 
C8 C9 1.381(17) . ? 
C9 C10 1.375(16) . ? 
C11 C12 1.531(16) . ? 
C13 C14 1.52(2) . ? 
C15 C16 1.492(17) . ? 
O1' C2' 1.232(13) . ? 
O1' Ca1 2.272(8) 1_545 ? 
O2' C6' 1.233(12) . ? 
O3' C12' 1.415(17) . ? 
O3' C13' 1.431(16) . ? 
O4' C14' 1.415(17) . ? 
O4' C15' 1.445(15) . ? 
N1' C2' 1.316(14) . ? 
N1' C16' 1.437(16) . ? 
N4' C3' 1.332(13) . ? 
N4' C5' 1.335(12) . ? 
N7' C6' 1.313(13) . ? 
N7' C11' 1.433(14) . ? 
C2' C3' 1.521(13) . ? 
C3' C8' 1.361(16) . ? 
C5' C10' 1.394(16) . ? 
C5' C6' 1.498(14) . ? 
C8' C9' 1.389(17) . ? 
C9' C10' 1.392(18) . ? 
C11' C12' 1.485(19) . ? 
C13' C14' 1.51(2) . ? 
C15' C16' 1.48(2) . ? 
 
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 O2' 91.1(3) 1_565 . ? 
O1' Ca1 O1 177.1(3) 1_565 1_545 ? 
O2' Ca1 O1 88.4(3) . 1_545 ? 
O1' Ca1 O9 95.7(4) 1_565 . ? 
O2' Ca1 O9 87.8(4) . . ? 
O1 Ca1 O9 87.2(4) 1_545 . ? 
O1' Ca1 O2 89.8(3) 1_565 . ? 
O2' Ca1 O2 177.8(3) . . ? 
O1 Ca1 O2 90.8(3) 1_545 . ? 
O9 Ca1 O2 90.1(4) . . ? 
O1' Ca1 O5 87.7(3) 1_565 . ? 
O2' Ca1 O5 87.7(4) . . ? 
O1 Ca1 O5 89.4(3) 1_545 . ? 
O9 Ca1 O5 174.4(4) . . ? 
O2 Ca1 O5 94.4(4) . . ? 
O8 Cl1 O7 112.3(18) . . ? 
O8 Cl1 O5 113.5(10) . . ? 
O7 Cl1 O5 106.0(11) . . ? 
O8 Cl1 O6 113.5(15) . . ? 
O7 Cl1 O6 100.8(14) . . ? 
O5 Cl1 O6 109.9(11) . . ? 
O11 Cl2 O10 112.7(14) . . ? 
O11 Cl2 O9 109.2(11) . . ? 
O10 Cl2 O9 110.1(8) . . ? 
O11 Cl2 O12 114.2(17) . . ? 
O10 Cl2 O12 104.7(10) . . ? 
O9 Cl2 O12 105.5(10) . . ? 
Cl1 O5 Ca1 151.1(7) . . ? 
Cl2 O9 Ca1 149.7(8) . . ? 
C2 O1 Ca1 158.2(8) . 1_565 ? 
C6 O2 Ca1 144.5(8) . . ? 
C12 O3 C13 113.9(11) . . ? 
C14 O4 C15 114.3(11) . . ? 
C2 N1 C16 126.5(10) . . ? 
C5 N4 C3 119.9(9) . . ? 
C6 N7 C11 126.5(10) . . ? 
O1 C2 N1 124.2(10) . . ? 
O1 C2 C3 120.0(10) . . ? 
N1 C2 C3 115.7(9) . . ? 
N4 C3 C8 121.4(10) . . ? 
N4 C3 C2 115.4(9) . . ? 
C8 C3 C2 123.2(10) . . ? 
N4 C5 C10 121.9(10) . . ? 
N4 C5 C6 115.8(9) . . ? 
C10 C5 C6 122.3(10) . . ? 
O2 C6 N7 124.2(11) . . ? 
O2 C6 C5 120.6(10) . . ? 
N7 C6 C5 115.1(10) . . ? 
C9 C8 C3 117.9(11) . . ? 
C10 C9 C8 120.5(10) . . ? 
C9 C10 C5 118.2(10) . . ? 
N7 C11 C12 107.0(10) . . ? 
O3 C12 C11 109.8(11) . . ? 
O3 C13 C14 109.8(12) . . ? 
O4 C14 C13 108.5(12) . . ? 
O4 C15 C16 107.3(11) . . ? 
N1 C16 C15 108.1(10) . . ? 
C2' O1' Ca1 158.8(8) . 1_545 ? 
C6' O2' Ca1 143.1(8) . . ? 
C12' O3' C13' 113.1(12) . . ? 
C14' O4' C15' 113.8(11) . . ? 
C2' N1' C16' 128.8(12) . . ? 
C3' N4' C5' 118.3(9) . . ? 
C6' N7' C11' 126.9(10) . . ? 
O1' C2' N1' 124.4(10) . . ? 
O1' C2' C3' 121.3(9) . . ? 
N1' C2' C3' 114.2(9) . . ? 
N4' C3' C8' 123.5(9) . . ? 
N4' C3' C2' 115.6(9) . . ? 
C8' C3' C2' 120.9(9) . . ? 
N4' C5' C10' 123.0(10) . . ? 
N4' C5' C6' 115.4(9) . . ? 
C10' C5' C6' 121.5(8) . . ? 
O2' C6' N7' 124.5(9) . . ? 
O2' C6' C5' 120.3(9) . . ? 
N7' C6' C5' 115.2(8) . . ? 
C3' C8' C9' 118.2(11) . . ? 
C8' C9' C10' 119.9(11) . . ? 
C9' C10' C5' 117.0(10) . . ? 
N7' C11' C12' 111.8(10) . . ? 
O3' C12' C11' 105.2(13) . . ? 
O3' C13' C14' 106.9(12) . . ? 
O4' C14' C13' 109.2(14) . . ? 
O4' C15' C16' 104.7(12) . . ? 
N1' C16' C15' 111.3(12) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O8 Cl1 O5 Ca1 -176(2) . . . . ? 
O7 Cl1 O5 Ca1 60.7(18) . . . . ? 
O6 Cl1 O5 Ca1 -47(2) . . . . ? 
O1' Ca1 O5 Cl1 -176.3(16) 1_565 . . . ? 
O2' Ca1 O5 Cl1 92.5(16) . . . . ? 
O1 Ca1 O5 Cl1 4.1(16) 1_545 . . . ? 
O9 Ca1 O5 Cl1 57(6) . . . . ? 
O2 Ca1 O5 Cl1 -86.7(16) . . . . ? 
O11 Cl2 O9 Ca1 -127(2) . . . . ? 
O10 Cl2 O9 Ca1 109.0(19) . . . . ? 
O12 Cl2 O9 Ca1 -4(2) . . . . ? 
O1' Ca1 O9 Cl2 36.7(19) 1_565 . . . ? 
O2' Ca1 O9 Cl2 127.6(19) . . . . ? 
O1 Ca1 O9 Cl2 -143.9(19) 1_545 . . . ? 
O2 Ca1 O9 Cl2 -53.1(19) . . . . ? 
O5 Ca1 O9 Cl2 163(4) . . . . ? 
O1' Ca1 O2 C6 -6.8(14) 1_565 . . . ? 
O2' Ca1 O2 C6 106(8) . . . . ? 
O1 Ca1 O2 C6 176.1(13) 1_545 . . . ? 
O9 Ca1 O2 C6 88.9(14) . . . . ? 
O5 Ca1 O2 C6 -94.5(14) . . . . ? 
Ca1 O1 C2 N1 55(3) 1_565 . . . ? 
Ca1 O1 C2 C3 -126.8(18) 1_565 . . . ? 
C16 N1 C2 O1 -2(2) . . . . ? 
C16 N1 C2 C3 180.0(12) . . . . ? 
C5 N4 C3 C8 2.5(17) . . . . ? 
C5 N4 C3 C2 -176.1(11) . . . . ? 
O1 C2 C3 N4 165.5(11) . . . . ? 
N1 C2 C3 N4 -15.9(16) . . . . ? 
O1 C2 C3 C8 -13.1(18) . . . . ? 
N1 C2 C3 C8 165.5(12) . . . . ? 
C3 N4 C5 C10 -5.1(18) . . . . ? 
C3 N4 C5 C6 175.6(10) . . . . ? 
Ca1 O2 C6 N7 -123.3(14) . . . . ? 
Ca1 O2 C6 C5 53.3(19) . . . . ? 
C11 N7 C6 O2 5(2) . . . . ? 
C11 N7 C6 C5 -172.3(13) . . . . ? 
N4 C5 C6 O2 -165.4(11) . . . . ? 
C10 C5 C6 O2 15.4(19) . . . . ? 
N4 C5 C6 N7 11.6(17) . . . . ? 
C10 C5 C6 N7 -167.7(13) . . . . ? 
N4 C3 C8 C9 2.0(18) . . . . ? 
C2 C3 C8 C9 -179.5(12) . . . . ? 
C3 C8 C9 C10 -4(2) . . . . ? 
C8 C9 C10 C5 1(2) . . . . ? 
N4 C5 C10 C9 3(2) . . . . ? 
C6 C5 C10 C9 -177.6(12) . . . . ? 
C6 N7 C11 C12 -170.8(14) . . . . ? 
C13 O3 C12 C11 171.4(12) . . . . ? 
N7 C11 C12 O3 -54.1(16) . . . . ? 
C12 O3 C13 C14 -171.2(12) . . . . ? 
C15 O4 C14 C13 -163.6(12) . . . . ? 
O3 C13 C14 O4 68.7(18) . . . . ? 
C14 O4 C15 C16 178.4(12) . . . . ? 
C2 N1 C16 C15 -140.1(14) . . . . ? 
O4 C15 C16 N1 -53.9(14) . . . . ? 
O1' Ca1 O2' C6' -163.5(13) 1_565 . . . ? 
O1 Ca1 O2' C6' 13.6(13) 1_545 . . . ? 
O9 Ca1 O2' C6' 100.9(13) . . . . ? 
O2 Ca1 O2' C6' 84(9) . . . . ? 
O5 Ca1 O2' C6' -75.8(13) . . . . ? 
Ca1 O1' C2' N1' -55(3) 1_545 . . . ? 
Ca1 O1' C2' C3' 121.4(19) 1_545 . . . ? 
C16' N1' C2' O1' 0(3) . . . . ? 
C16' N1' C2' C3' -176.6(16) . . . . ? 
C5' N4' C3' C8' -0.2(18) . . . . ? 
C5' N4' C3' C2' 178.6(11) . . . . ? 
O1' C2' C3' N4' -168.8(12) . . . . ? 
N1' C2' C3' N4' 7.7(16) . . . . ? 
O1' C2' C3' C8' 10.1(18) . . . . ? 
N1' C2' C3' C8' -173.4(13) . . . . ? 
C3' N4' C5' C10' 2.0(18) . . . . ? 
C3' N4' C5' C6' -174.4(10) . . . . ? 
Ca1 O2' C6' N7' 114.6(14) . . . . ? 
Ca1 O2' C6' C5' -66.3(17) . . . . ? 
C11' N7' C6' O2' -11(2) . . . . ? 
C11' N7' C6' C5' 169.7(12) . . . . ? 
N4' C5' C6' O2' 165.5(12) . . . . ? 
C10' C5' C6' O2' -11.0(17) . . . . ? 
N4' C5' C6' N7' -15.4(15) . . . . ? 
C10' C5' C6' N7' 168.1(12) . . . . ? 
N4' C3' C8' C9' -1.2(19) . . . . ? 
C2' C3' C8' C9' -180.0(11) . . . . ? 
C3' C8' C9' C10' 1(2) . . . . ? 
C8' C9' C10' C5' 1(2) . . . . ? 
N4' C5' C10' C9' -2.3(19) . . . . ? 
C6' C5' C10' C9' 173.9(12) . . . . ? 
C6' N7' C11' C12' -143.5(15) . . . . ? 
C13' O3' C12' C11' 178.7(13) . . . . ? 
N7' C11' C12' O3' -50.7(17) . . . . ? 
C12' O3' C13' C14' -159.3(14) . . . . ? 
C15' O4' C14' C13' -176.3(12) . . . . ? 
O3' C13' C14' O4' 73.1(19) . . . . ? 
C14' O4' C15' C16' 169.4(13) . . . . ? 
C2' N1' C16' C15' -159.6(15) . . . . ? 
O4' C15' C16' N1' -55.5(19) . . . . ? 
 
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
N1 H1 O11  1.00 2.31 3.04(2) 129.5 2_675 
N7 H7 O11  1.00 2.65 3.49(3) 142.6 2_675 
N1' H1' O7  1.00 2.49 3.22(2) 130.3 4_544 
N7' H7' O7  1.00 2.39 3.28(2) 148.6 4_544 
C8 H8 O6  1.00 2.46 3.43(2) 164.0 1_565 
C15 H15B O8  1.05 2.49 3.495(18) 159.9 3_575 
 
_diffrn_measured_fraction_theta_max    0.696 
_diffrn_reflns_theta_full              74.10 
_diffrn_measured_fraction_theta_full   0.696 
_refine_diff_density_max    0.594 
_refine_diff_density_min   -0.975 
_refine_diff_density_rms    0.163