data_shelxl 

 

_audit_creation_method            SHELXL 

_publ_section_references

;

Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A.

(1993) J. Appl. Cryst. 26, 343-350.

Sheldrick, G.M. SHELXL93. Program for crystal structure refinement.

University of Gottingen, Germany, 1993.

;

_chemical_formula_sum             'C42 H32 Cl6 O14' 

_chemical_formula_weight          973.38 

 

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' 

 'O'  'O'   0.0106   0.0060 

 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

 'Cl'  'Cl'   0.1484   0.1585 

 '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_Int_Tables_number            2

 

loop_ 

 _symmetry_equiv_pos_as_xyz 

 'x, y, z' 

 '-x, -y, -z' 

 

_cell_length_a                    12.104(4) 

_cell_length_b                    12.965(3) 

_cell_length_c                    15.309(4) 

_cell_angle_alpha                 76.681(2) 

_cell_angle_beta                  104.981(7) 

_cell_angle_gamma                 114.121(7) 

_cell_volume                      2096.9(10) 

_cell_formula_units_Z             2 

_cell_measurement_temperature     143(1) 

_exptl_crystal_size_max           0.48 

_exptl_crystal_size_mid           0.06 

_exptl_crystal_size_min           0.01 

_exptl_crystal_density_diffrn     1.542 

_exptl_crystal_F_000              996 

_exptl_absorpt_coefficient_mu     0.479 

_exptl_absorpt_correction_type    none

 

 

_diffrn_ambient_temperature       143(2) 

_diffrn_radiation_wavelength      0.71069 

_diffrn_radiation_type            MoK\a 

_diffrn_radiation_source          'rotating anode' 

_diffrn_radiation_monochromator   graphite 

_diffrn_measurement_device        'CCD area detector'

_diffrn_measurement_device_type   'Rigaku Mercury'

_diffrn_measurement_method        'phi oscillations'

_diffrn_reflns_number             12995 

_diffrn_reflns_av_R_equivalents   0.0326 

_diffrn_reflns_av_sigmaI/netI     0.0599 

_diffrn_reflns_limit_h_min        -11 

_diffrn_reflns_limit_h_max        14 

_diffrn_reflns_limit_k_min        -15 

_diffrn_reflns_limit_k_max        12 

_diffrn_reflns_limit_l_min        -18 

_diffrn_reflns_limit_l_max        15 

_diffrn_reflns_theta_min          2.53 

_diffrn_reflns_theta_max          25.35 

_reflns_number_total              7308 

_reflns_number_observed           5526 

_reflns_observed_criterion        >2sigma(I) 

 

_computing_structure_solution     'SIR92 (Altomare, 1993)' 

_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 

 

_refine_ls_structure_factor_coef  Fsqd  

_refine_ls_matrix_type            full 

_refine_ls_weighting_scheme 

 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+3.5407P] 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     ? 

_refine_ls_extinction_method      none 

_refine_ls_extinction_coef        ? 

_refine_ls_number_reflns          7307 

_refine_ls_number_parameters      565 

_refine_ls_number_restraints      0 

_refine_ls_R_factor_all           0.0999 

_refine_ls_R_factor_obs           0.0678 

_refine_ls_wR_factor_all          0.1171 

_refine_ls_wR_factor_obs          0.1079 

_refine_ls_goodness_of_fit_all    1.142 

_refine_ls_goodness_of_fit_obs    1.226 

_refine_ls_restrained_S_all       1.144 

_refine_ls_restrained_S_obs       1.226 

_refine_ls_shift/esd_max          0.000 

_refine_ls_shift/esd_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_thermal_displace_type 

 _atom_site_occupancy 

 _atom_site_calc_flag 

 _atom_site_refinement_flags 

 _atom_site_disorder_group 

C1 C 0.6907(3) -0.0528(3) 0.8553(2) 0.0154(7) Uani 1 d . . 

C2 C 0.6853(3) 0.0553(3) 0.8269(2) 0.0149(7) Uani 1 d . . 

C3 C 0.6650(3) 0.1063(3) 0.8900(2) 0.0149(7) Uani 1 d . . 

C4 C 0.6510(3) 0.0496(3) 0.9790(2) 0.0142(7) Uani 1 d . . 

C5 C 0.6421(3) 0.1078(3) 1.0451(2) 0.0148(7) Uani 1 d . . 

C6 C 0.6288(3) 0.0453(3) 1.1416(2) 0.0171(8) Uani 1 d . . 

C7 C 0.6328(3) -0.0698(3) 1.1634(2) 0.0162(7) Uani 1 d . . 

C8 C 0.6420(3) -0.1199(3) 1.0993(2) 0.0148(7) Uani 1 d . . 

H8 H 0.6396(3) -0.1944(3) 1.1145(2) 0.020 Uiso 1 calc R . 

C9 C 0.6558(3) -0.0617(3) 1.0069(2) 0.0139(7) Uani 1 d . . 

C10 C 0.6751(3) -0.1128(3) 0.9445(2) 0.0137(7) Uani 1 d . . 

C11 C 0.6911(3) -0.2259(3) 0.9679(2) 0.0132(7) Uani 1 d . . 

C12 C 0.8060(3) -0.2271(3) 1.0221(2) 0.0154(7) Uani 1 d . . 

C13 C 0.8370(3) -0.3235(3) 1.0401(2) 0.0169(8) Uani 1 d . . 

C14 C 0.7504(3) -0.4203(3) 1.0008(2) 0.0170(8) Uani 1 d . . 

C15 C 0.6367(3) -0.4221(3) 0.9487(2) 0.0147(7) Uani 1 d . . 

C16 C 0.5547(3) -0.5201(3) 0.9046(2) 0.0179(8) Uani 1 d . . 

C17 C 0.4308(3) -0.5191(3) 0.8467(2) 0.0187(8) Uani 1 d . . 

C18 C 0.4063(3) -0.4146(3) 0.8351(2) 0.0169(8) Uani 1 d . . 

C19 C 0.4873(3) -0.3238(3) 0.8757(2) 0.0152(7) Uani 1 d . . 

H19 H 0.4675(3) -0.2597(3) 0.8679(2) 0.020 Uiso 1 calc R . 

C20 C 0.6055(3) -0.3229(3) 0.9315(2) 0.0143(7) Uani 1 d . . 

C22 C 0.6647(4) -0.1089(3) 0.7077(2) 0.0279(9) Uani 1 d . . 

H22A H 0.7234(4) -0.0514(3) 0.6720(2) 0.037 Uiso 1 calc R . 

H22B H 0.5903(4) -0.0923(3) 0.6934(2) 0.037 Uiso 1 calc R . 

C23 C 0.6360(3) -0.2265(3) 0.6863(2) 0.0221(8) Uani 1 d . . 

C24 C 0.5300(4) -0.2782(3) 0.6258(3) 0.0350(10) Uani 1 d . . 

H24 H 0.4749(4) -0.2416(3) 0.5997(3) 0.047 Uiso 1 calc R . 

C25 C 0.5059(4) -0.3841(4) 0.6041(3) 0.0440(12) Uani 1 d . . 

H25 H 0.4353(4) -0.4179(4) 0.5627(3) 0.058 Uiso 1 calc R . 

C26 C 0.5858(5) -0.4393(4) 0.6433(3) 0.0504(13) Uani 1 d . . 

H26 H 0.5693(5) -0.5105(4) 0.6287(3) 0.067 Uiso 1 calc R . 

C27 C 0.6901(5) -0.3894(4) 0.7041(4) 0.0519(13) Uani 1 d . . 

H27 H 0.7436(5) -0.4276(4) 0.7313(4) 0.069 Uiso 1 calc R . 

C28 C 0.7164(4) -0.2826(3) 0.7252(3) 0.0348(10) Uani 1 d . . 

H28 H 0.7881(4) -0.2486(3) 0.7656(3) 0.046 Uiso 1 calc R . 

C29 C 0.7187(3) 0.1261(3) 0.7383(2) 0.0184(8) Uani 1 d . . 

C32 C 0.6626(4) 0.2441(4) 0.6081(3) 0.0407(11) Uani 1 d . . 

H32A H 0.7269(18) 0.3143(10) 0.6244(3) 0.061 Uiso 1 calc R . 

H32B H 0.5910(8) 0.2590(19) 0.5735(10) 0.061 Uiso 1 calc R . 

H32C H 0.6901(25) 0.2111(11) 0.5720(10) 0.061 Uiso 1 calc R . 

C37 C 0.6106(4) -0.2300(3) 1.2790(3) 0.0301(10) Uani 1 d . . 

H37A H 0.5984(24) -0.2529(7) 1.3412(6) 0.045 Uiso 1 calc R . 

H37B H 0.6842(10) -0.2379(5) 1.2743(17) 0.045 Uiso 1 calc R . 

H37C H 0.5413(14) -0.2775(4) 1.2404(11) 0.045 Uiso 1 calc R . 

C39 C 0.9660(3) -0.1154(3) 1.1367(2) 0.0224(8) Uani 1 d . . 

H39A H 1.0482(3) -0.0980(3) 1.1270(2) 0.030 Uiso 1 calc R . 

H39B H 0.9421(3) -0.1864(3) 1.1781(2) 0.030 Uiso 1 calc R . 

C40 C 0.9635(3) -0.0205(3) 1.1760(2) 0.0195(8) Uani 1 d . . 

C41 C 0.9759(4) -0.0277(3) 1.2697(3) 0.0274(9) Uani 1 d . . 

H41 H 0.9864(4) -0.0912(3) 1.3081(3) 0.036 Uiso 1 calc R . 

C42 C 0.9728(4) 0.0591(4) 1.3064(3) 0.0339(10) Uani 1 d . . 

H42 H 0.9820(4) 0.0539(4) 1.3692(3) 0.045 Uiso 1 calc R . 

C43 C 0.9562(4) 0.1532(3) 1.2497(3) 0.0341(10) Uani 1 d . . 

H43 H 0.9522(4) 0.2105(3) 1.2743(3) 0.045 Uiso 1 calc R . 

C44 C 0.9456(3) 0.1626(3) 1.1562(3) 0.0281(9) Uani 1 d . . 

H44 H 0.9356(3) 0.2265(3) 1.1180(3) 0.037 Uiso 1 calc R . 

C45 C 0.9502(3) 0.0761(3) 1.1202(3) 0.0226(8) Uani 1 d . . 

H45 H 0.9443(3) 0.0828(3) 1.0575(3) 0.030 Uiso 1 calc R . 

C46 C 0.9618(3) -0.3244(3) 1.0856(3) 0.0210(8) Uani 1 d . . 

C49 C 1.0697(4) -0.4284(4) 1.1926(3) 0.0438(12) Uani 1 d . . 

H49A H 1.0563(7) -0.4909(16) 1.2416(13) 0.066 Uiso 1 calc R . 

H49B H 1.1309(9) -0.3606(9) 1.2156(18) 0.066 Uiso 1 calc R . 

H49C H 1.0977(14) -0.4459(24) 1.1465(6) 0.066 Uiso 1 calc R . 

C54 C 0.2530(4) -0.3349(3) 0.7700(3) 0.0304(9) Uani 1 d . . 

H54A H 0.1700(9) -0.3565(9) 0.7364(15) 0.046 Uiso 1 calc R . 

H54B H 0.3052(15) -0.2681(7) 0.7369(15) 0.046 Uiso 1 calc R . 

H54C H 0.2555(22) -0.3187(15) 0.8287(3) 0.046 Uiso 1 calc R . 

O21 O 0.7156(2) -0.1091(2) 0.8034(2) 0.0197(5) Uani 1 d . . 

O30 O 0.6320(2) 0.1653(2) 0.6905(2) 0.0306(7) Uani 1 d . . 

O31 O 0.8135(2) 0.1462(2) 0.7150(2) 0.0296(6) Uani 1 d . . 

O33 O 0.6634(2) 0.2117(2) 0.8636(2) 0.0194(5) Uani 1 d . . 

H33 H 0.6501(37) 0.2324(14) 0.9053(10) 0.029 Uiso 1 calc R . 

O34 O 0.6451(2) 0.2070(2) 1.0279(2) 0.0225(6) Uani 1 d . . 

O35 O 0.6136(2) 0.0911(2) 1.1963(2) 0.0267(6) Uani 1 d . . 

O36 O 0.6221(2) -0.1134(2) 1.2511(2) 0.0219(6) Uani 1 d . . 

O38 O 0.8800(2) -0.1258(2) 1.0507(2) 0.0188(5) Uani 1 d . . 

O47 O 0.9558(2) -0.4102(2) 1.1534(2) 0.0311(7) Uani 1 d . . 

O48 O 1.0558(2) -0.2575(2) 1.0623(2) 0.0304(6) Uani 1 d . . 

O50 O 0.7836(2) -0.5105(2) 1.0123(2) 0.0258(6) Uani 1 d . . 

H50 H 0.7278(16) -0.5613(14) 0.9857(24) 0.039 Uiso 1 calc R . 

O51 O 0.5775(2) -0.6067(2) 0.9104(2) 0.0255(6) Uani 1 d . . 

O52 O 0.3578(2) -0.6037(2) 0.8134(2) 0.0278(6) Uani 1 d . . 

O53 O 0.2953(2) -0.4265(2) 0.7817(2) 0.0232(6) Uani 1 d . . 

C55 C 0.2547(4) -0.0292(3) 0.5742(3) 0.0331(10) Uani 1 d . . 

H55 H 0.2590(4) -0.0345(3) 0.6399(3) 0.044 Uiso 1 calc R . 

Cl1 Cl 0.22493(12) 0.09334(10) 0.51746(8) 0.0519(3) Uani 1 d . . 

Cl2 Cl 0.39625(12) -0.01955(13) 0.55604(10) 0.0616(4) Uani 1 d . . 

Cl3 Cl 0.13621(12) -0.15170(10) 0.53455(9) 0.0520(3) Uani 1 d . . 

C56 C -0.1727(4) -0.4309(3) 0.3931(3) 0.0316(10) Uani 1 d . . 

H56 H -0.2385(4) -0.4410(3) 0.3390(3) 0.042 Uiso 1 calc R . 

Cl4 Cl -0.03340(11) -0.33587(9) 0.35961(8) 0.0457(3) Uani 1 d . . 

Cl5 Cl -0.20895(13) -0.37558(11) 0.47185(9) 0.0579(4) Uani 1 d . . 

Cl6 Cl -0.16324(11) -0.56499(9) 0.44189(8) 0.0433(3) Uani 1 d . . 

 

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 

C1 0.010(2) 0.016(2) 0.018(2) -0.0058(14) 0.0003(15) 0.0033(14) 

C2 0.013(2) 0.013(2) 0.016(2) 0.0008(13) 0.0025(15) 0.0032(14) 

C3 0.009(2) 0.011(2) 0.021(2) -0.0019(14) -0.0006(15) 0.0027(13) 

C4 0.010(2) 0.015(2) 0.017(2) -0.0060(14) -0.0014(14) 0.0045(14) 

C5 0.010(2) 0.012(2) 0.021(2) -0.0039(14) 0.0013(15) 0.0031(13) 

C6 0.013(2) 0.017(2) 0.019(2) -0.0057(14) 0.003(2) 0.0021(14) 

C7 0.017(2) 0.015(2) 0.015(2) -0.0035(14) 0.0014(15) 0.0043(14) 

C8 0.017(2) 0.008(2) 0.019(2) -0.0009(13) 0.003(2) 0.0049(14) 

C9 0.009(2) 0.013(2) 0.017(2) -0.0019(13) -0.0005(14) 0.0023(13) 

C10 0.009(2) 0.011(2) 0.017(2) -0.0031(13) -0.0003(14) 0.0007(13) 

C11 0.015(2) 0.014(2) 0.014(2) -0.0004(13) 0.0068(15) 0.0073(14) 

C12 0.016(2) 0.016(2) 0.012(2) -0.0001(13) 0.0041(15) 0.0029(14) 

C13 0.015(2) 0.016(2) 0.019(2) 0.0012(14) 0.002(2) 0.0079(15) 

C14 0.020(2) 0.013(2) 0.020(2) 0.0001(14) 0.006(2) 0.0082(15) 

C15 0.015(2) 0.013(2) 0.016(2) 0.0000(13) 0.0049(15) 0.0048(14) 

C16 0.023(2) 0.016(2) 0.016(2) 0.0009(14) 0.005(2) 0.008(2) 

C17 0.020(2) 0.016(2) 0.019(2) -0.0060(14) 0.004(2) 0.003(2) 

C18 0.015(2) 0.014(2) 0.018(2) -0.0008(14) 0.000(2) 0.0047(14) 

C19 0.016(2) 0.014(2) 0.017(2) -0.0003(14) 0.003(2) 0.0082(15) 

C20 0.016(2) 0.013(2) 0.013(2) 0.0010(13) 0.0060(15) 0.0041(14) 

C22 0.044(3) 0.027(2) 0.013(2) -0.0036(15) 0.000(2) 0.015(2) 

C23 0.027(2) 0.022(2) 0.016(2) -0.0027(15) 0.009(2) 0.005(2) 

C24 0.039(3) 0.033(2) 0.028(2) -0.005(2) 0.004(2) 0.011(2) 

C25 0.046(3) 0.033(3) 0.039(3) -0.016(2) 0.001(2) -0.001(2) 

C26 0.070(4) 0.025(2) 0.056(3) -0.017(2) 0.019(3) 0.007(2) 

C27 0.063(4) 0.046(3) 0.062(3) -0.020(2) 0.010(3) 0.031(3) 

C28 0.029(2) 0.038(3) 0.042(3) -0.017(2) 0.003(2) 0.013(2) 

C29 0.021(2) 0.012(2) 0.021(2) -0.0020(14) 0.004(2) 0.0052(15) 

C32 0.061(3) 0.042(3) 0.021(2) 0.014(2) 0.010(2) 0.030(2) 

C37 0.053(3) 0.020(2) 0.019(2) 0.002(2) 0.011(2) 0.014(2) 

C39 0.018(2) 0.025(2) 0.021(2) -0.0037(15) -0.006(2) 0.009(2) 

C40 0.011(2) 0.019(2) 0.027(2) -0.0085(15) 0.000(2) 0.0031(14) 

C41 0.024(2) 0.035(2) 0.024(2) -0.003(2) 0.001(2) 0.014(2) 

C42 0.034(3) 0.047(3) 0.025(2) -0.010(2) 0.004(2) 0.017(2) 

C43 0.030(2) 0.036(2) 0.045(3) -0.019(2) 0.007(2) 0.014(2) 

C44 0.021(2) 0.023(2) 0.037(3) -0.008(2) 0.001(2) 0.007(2) 

C45 0.016(2) 0.027(2) 0.023(2) -0.006(2) 0.001(2) 0.006(2) 

C46 0.019(2) 0.014(2) 0.029(2) -0.004(2) 0.001(2) 0.006(2) 

C49 0.026(2) 0.036(2) 0.058(3) 0.008(2) -0.008(2) 0.018(2) 

C54 0.028(2) 0.024(2) 0.038(2) -0.008(2) -0.009(2) 0.015(2) 

O21 0.0290(15) 0.0223(13) 0.0128(13) -0.0021(10) 0.0035(11) 0.0148(11) 

O30 0.035(2) 0.040(2) 0.0189(14) 0.0114(12) 0.0062(13) 0.0240(14) 

O31 0.026(2) 0.032(2) 0.029(2) 0.0065(12) 0.0135(13) 0.0103(12) 

O33 0.0259(15) 0.0131(13) 0.0214(14) 0.0016(10) 0.0057(12) 0.0108(10) 

O34 0.030(2) 0.0166(14) 0.0251(15) -0.0051(10) 0.0030(12) 0.0123(11) 

O35 0.039(2) 0.0188(14) 0.027(2) -0.0083(11) 0.0112(13) 0.0101(12) 

O36 0.034(2) 0.0158(13) 0.0179(14) -0.0009(10) 0.0086(12) 0.0098(11) 

O38 0.0155(13) 0.0143(12) 0.0210(14) -0.0045(10) -0.0064(11) 0.0046(10) 

O47 0.0208(15) 0.0255(14) 0.038(2) 0.0077(12) -0.0026(13) 0.0105(12) 

O48 0.0176(15) 0.0275(15) 0.041(2) 0.0039(12) 0.0043(13) 0.0087(12) 

O50 0.027(2) 0.0188(14) 0.034(2) -0.0065(11) -0.0041(13) 0.0152(12) 

O51 0.031(2) 0.0162(14) 0.031(2) -0.0066(11) -0.0007(12) 0.0120(11) 

O52 0.026(2) 0.0203(14) 0.035(2) -0.0140(12) -0.0050(13) 0.0082(12) 

O53 0.0211(14) 0.0190(13) 0.0302(15) -0.0094(11) -0.0053(12) 0.0111(11) 

C55 0.037(3) 0.036(2) 0.026(2) -0.009(2) 0.004(2) 0.012(2) 

Cl1 0.0651(9) 0.0432(7) 0.0454(7) -0.0002(5) 0.0057(6) 0.0241(6) 

Cl2 0.0399(8) 0.0898(10) 0.0615(9) -0.0189(7) 0.0049(7) 0.0288(7) 

Cl3 0.0523(8) 0.0439(7) 0.0591(8) -0.0263(6) 0.0130(6) 0.0055(6) 

C56 0.030(2) 0.028(2) 0.028(2) -0.002(2) -0.005(2) 0.009(2) 

Cl4 0.0453(7) 0.0386(6) 0.0372(7) 0.0089(5) 0.0083(5) 0.0069(5) 

Cl5 0.0616(9) 0.0528(8) 0.0650(9) -0.0242(6) 0.0141(7) 0.0170(6) 

Cl6 0.0505(7) 0.0280(6) 0.0421(7) 0.0072(5) 0.0043(6) 0.0142(5) 

 

 

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 

C1 O21 1.351(4) . ? 

C1 C2 1.392(4) . ? 

C1 C10 1.424(5) . ? 

C2 C3 1.408(5) . ? 

C2 C29 1.500(5) . ? 

C3 O33 1.339(4) . ? 

C3 C4 1.407(5) . ? 

C4 C9 1.428(4) . ? 

C4 C5 1.442(4) . ? 

C5 O34 1.239(4) . ? 

C5 C6 1.526(5) . ? 

C6 O35 1.218(4) . ? 

C6 C7 1.471(5) . ? 

C7 C8 1.343(5) . ? 

C7 O36 1.349(4) . ? 

C8 C9 1.458(5) . ? 

C9 C10 1.394(5) . ? 

C10 C11 1.506(4) . ? 

C11 C20 1.388(5) . ? 

C11 C12 1.427(5) . ? 

C12 O38 1.349(4) . ? 

C12 C13 1.397(5) . ? 

C13 C14 1.407(5) . ? 

C13 C46 1.495(5) . ? 

C14 O50 1.346(4) . ? 

C14 C15 1.396(5) . ? 

C15 C20 1.434(4) . ? 

C15 C16 1.439(5) . ? 

C16 O51 1.241(4) . ? 

C16 C17 1.536(5) . ? 

C17 O52 1.215(4) . ? 

C17 C18 1.465(5) . ? 

C18 C19 1.345(5) . ? 

C18 O53 1.349(4) . ? 

C19 C20 1.461(5) . ? 

C22 O21 1.434(4) . ? 

C22 C23 1.514(5) . ? 

C23 C28 1.382(5) . ? 

C23 C24 1.386(5) . ? 

C24 C25 1.383(6) . ? 

C25 C26 1.369(7) . ? 

C26 C27 1.372(7) . ? 

C27 C28 1.384(6) . ? 

C29 O31 1.199(4) . ? 

C29 O30 1.328(4) . ? 

C32 O30 1.453(4) . ? 

C37 O36 1.431(4) . ? 

C39 O38 1.446(4) . ? 

C39 C40 1.503(5) . ? 

C40 C45 1.387(5) . ? 

C40 C41 1.388(5) . ? 

C41 C42 1.385(5) . ? 

C42 C43 1.380(6) . ? 

C43 C44 1.384(6) . ? 

C44 C45 1.385(5) . ? 

C46 O48 1.197(4) . ? 

C46 O47 1.328(4) . ? 

C49 O47 1.446(4) . ? 

C54 O53 1.434(4) . ? 

C55 Cl1 1.754(4) . ? 

C55 Cl3 1.755(4) . ? 

C55 Cl2 1.757(4) . ? 

C56 Cl4 1.756(4) . ? 

C56 Cl5 1.758(4) . ? 

C56 Cl6 1.764(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 

O21 C1 C2 124.0(3) . . ? 

O21 C1 C10 113.5(3) . . ? 

C2 C1 C10 122.5(3) . . ? 

C1 C2 C3 117.8(3) . . ? 

C1 C2 C29 123.0(3) . . ? 

C3 C2 C29 118.5(3) . . ? 

O33 C3 C4 121.2(3) . . ? 

O33 C3 C2 117.9(3) . . ? 

C4 C3 C2 120.8(3) . . ? 

C3 C4 C9 120.7(3) . . ? 

C3 C4 C5 119.8(3) . . ? 

C9 C4 C5 119.3(3) . . ? 

O34 C5 C4 123.4(3) . . ? 

O34 C5 C6 117.6(3) . . ? 

C4 C5 C6 119.0(3) . . ? 

O35 C6 C7 123.0(3) . . ? 

O35 C6 C5 119.5(3) . . ? 

C7 C6 C5 117.5(3) . . ? 

C8 C7 O36 128.1(3) . . ? 

C8 C7 C6 121.0(3) . . ? 

O36 C7 C6 110.9(3) . . ? 

C7 C8 C9 122.5(3) . . ? 

C10 C9 C4 118.7(3) . . ? 

C10 C9 C8 120.8(3) . . ? 

C4 C9 C8 120.5(3) . . ? 

C9 C10 C1 119.4(3) . . ? 

C9 C10 C11 123.6(3) . . ? 

C1 C10 C11 116.8(3) . . ? 

C20 C11 C12 120.1(3) . . ? 

C20 C11 C10 122.7(3) . . ? 

C12 C11 C10 116.9(3) . . ? 

O38 C12 C13 124.9(3) . . ? 

O38 C12 C11 112.9(3) . . ? 

C13 C12 C11 122.2(3) . . ? 

C12 C13 C14 117.1(3) . . ? 

C12 C13 C46 124.0(3) . . ? 

C14 C13 C46 118.2(3) . . ? 

O50 C14 C15 120.8(3) . . ? 

O50 C14 C13 117.2(3) . . ? 

C15 C14 C13 121.9(3) . . ? 

C14 C15 C20 120.5(3) . . ? 

C14 C15 C16 119.9(3) . . ? 

C20 C15 C16 119.4(3) . . ? 

O51 C16 C15 124.0(3) . . ? 

O51 C16 C17 117.2(3) . . ? 

C15 C16 C17 118.8(3) . . ? 

O52 C17 C18 123.1(3) . . ? 

O52 C17 C16 119.5(3) . . ? 

C18 C17 C16 117.5(3) . . ? 

C19 C18 O53 128.1(3) . . ? 

C19 C18 C17 121.5(3) . . ? 

O53 C18 C17 110.3(3) . . ? 

C18 C19 C20 122.0(3) . . ? 

C11 C20 C15 118.3(3) . . ? 

C11 C20 C19 121.2(3) . . ? 

C15 C20 C19 120.6(3) . . ? 

O21 C22 C23 107.1(3) . . ? 

C28 C23 C24 119.2(4) . . ? 

C28 C23 C22 120.4(4) . . ? 

C24 C23 C22 120.4(3) . . ? 

C25 C24 C23 120.3(4) . . ? 

C26 C25 C24 120.1(4) . . ? 

C25 C26 C27 120.0(4) . . ? 

C26 C27 C28 120.5(5) . . ? 

C23 C28 C27 119.9(4) . . ? 

O31 C29 O30 124.5(3) . . ? 

O31 C29 C2 123.7(3) . . ? 

O30 C29 C2 111.8(3) . . ? 

O38 C39 C40 107.3(3) . . ? 

C45 C40 C41 118.7(3) . . ? 

C45 C40 C39 121.1(3) . . ? 

C41 C40 C39 120.2(3) . . ? 

C42 C41 C40 120.5(4) . . ? 

C43 C42 C41 120.1(4) . . ? 

C42 C43 C44 120.2(4) . . ? 

C43 C44 C45 119.3(4) . . ? 

C44 C45 C40 121.2(4) . . ? 

O48 C46 O47 124.0(3) . . ? 

O48 C46 C13 124.1(3) . . ? 

O47 C46 C13 111.8(3) . . ? 

C1 O21 C22 122.0(3) . . ? 

C29 O30 C32 115.3(3) . . ? 

C7 O36 C37 116.9(3) . . ? 

C12 O38 C39 123.2(2) . . ? 

C46 O47 C49 115.8(3) . . ? 

C18 O53 C54 117.2(3) . . ? 

Cl1 C55 Cl3 110.2(2) . . ? 

Cl1 C55 Cl2 109.7(2) . . ? 

Cl3 C55 Cl2 109.9(2) . . ? 

Cl4 C56 Cl5 110.3(2) . . ? 

Cl4 C56 Cl6 110.5(2) . . ? 

Cl5 C56 Cl6 109.8(2) . . ? 


_diffrn_reflns_theta_full  25.35
_diffrn_measured_fraction_theta_full   0.949  

_refine_diff_density_max    0.314 

_refine_diff_density_min   -0.350 

_refine_diff_density_rms    0.064