# Copyright The Royal Society of Chemistry, 1999
# CCDC Number 186/1294

# The Influence of Linkage Mode Between Bipyridine Units in Oligobipyridine 
# Ligand on the Formation of Cu(I) and Cu(II) Helicates (Paper No 8/08550A).

data_C52H54Cl2Cu2N8O9 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C52 H54 Cl2 Cu2 N8 O9' 
_chemical_formula_weight          1133.01 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'Cu'  'Cu'   0.3201   1.2651 
 '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   '

loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    11.2999(7) 
_cell_length_b                    14.6693(15) 
_cell_length_c                    18.003(2) 
_cell_angle_alpha                 113.605(9) 
_cell_angle_beta                  95.520(10) 
_cell_angle_gamma                 103.020(7) 
_cell_volume                      2605.4(5) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used      28
_cell_measurement_theta_min        4.82
_cell_measurement_theta_max        9.99

_exptl_crystal_description       'prism'
_exptl_crystal_colour            'orange'
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.444 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              1172 
_exptl_absorpt_coefficient_mu     0.982 
_exptl_absorpt_correction_type   'empirical PSI-scan'
_exptl_absorpt_correction_T_min  0.5760
_exptl_absorpt_correction_T_max  0.6505

 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_standards_number            3
_diffrn_standards_interval_count  197
_diffrn_standards_decay_%        7.09
_diffrn_reflns_number             10307 
_diffrn_reflns_av_R_equivalents   0.0884 
_diffrn_reflns_av_sigmaI/netI     0.0771 
_diffrn_reflns_limit_h_min        -1 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -15 
_diffrn_reflns_limit_k_max        15 
_diffrn_reflns_limit_l_min        -21 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          1.89 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              8844 
_reflns_number_observed           5889 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection      'Siemens XSCANS'
_computing_cell_refinement      'Siemens XSCANS'
_computing_data_reduction       'Siemens SHELXTL'
_computing_structure_solution   'Siemens SHELXTL'
_computing_structure_refinement 'Siemens SHELXTL'
_computing_molecular_graphics   'Siemens SHELXTL'
_computing_publication_material 'Siemens SHELXTL'

_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     'riding model' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          8844 
_refine_ls_number_parameters      686 
_refine_ls_number_restraints      82 
_refine_ls_R_factor_all           0.0919 
_refine_ls_R_factor_obs           0.0588 
_refine_ls_wR_factor_all          0.1867 
_refine_ls_wR_factor_obs          0.1528 
_refine_ls_goodness_of_fit_all    1.046 
_refine_ls_goodness_of_fit_obs    1.067 
_refine_ls_restrained_S_all       1.060 
_refine_ls_restrained_S_obs       1.088 
_refine_ls_shift/esd_max          0.001 
_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 
Cu1 Cu 0.81017(4) 0.68899(4) 0.07792(3) 0.04966(13) Uani 1 d . . 
Cu2 Cu 0.87900(5) 0.72165(3) 0.53058(3) 0.05184(13) Uani 1 d . . 
N1 N 0.8349(3) 0.5758(2) -0.0227(2) 0.0460(8) Uani 1 d . . 
N2 N 1.0002(3) 0.7429(2) 0.0971(2) 0.0405(7) Uani 1 d . . 
N3 N 0.8980(3) 0.8058(2) 0.4664(2) 0.0416(7) Uani 1 d . . 
N4 N 0.7836(3) 0.8248(2) 0.5912(2) 0.0456(8) Uani 1 d . . 
N5 N 0.7202(3) 0.7965(2) 0.0795(2) 0.0456(8) Uani 1 d . . 
N6 N 0.7190(3) 0.6908(2) 0.1690(2) 0.0411(7) Uani 1 d . . 
N7 N 0.7604(3) 0.5738(2) 0.4879(2) 0.0437(7) Uani 1 d . . 
N8 N 0.9839(3) 0.6666(2) 0.5883(2) 0.0503(8) Uani 1 d . . 
C1 C 0.7474(4) 0.4914(3) -0.0779(3) 0.0617(12) Uani 1 d . . 
C2 C 0.7744(5) 0.4235(4) -0.1490(3) 0.075(2) Uani 1 d . . 
H2A H 0.7126(5) 0.3649(4) -0.1872(3) 0.090 Uiso 1 calc R . 
C3 C 0.8927(5) 0.4430(4) -0.1627(3) 0.0767(15) Uani 1 d . . 
H3A H 0.9116(5) 0.3983(4) -0.2107(3) 0.092 Uiso 1 calc R . 
C4 C 0.9827(4) 0.5289(4) -0.1053(3) 0.0696(14) Uani 1 d . . 
H4A H 1.0635(4) 0.5430(4) -0.1135(3) 0.083 Uiso 1 calc R . 
C5 C 0.9522(3) 0.5943(3) -0.0352(2) 0.0471(9) Uani 1 d . . 
C6 C 1.0456(3) 0.6877(3) 0.0319(2) 0.0482(10) Uani 1 d . . 
C7 C 1.1682(4) 0.7179(4) 0.0275(3) 0.0715(14) Uani 1 d . . 
H7A H 1.1975(4) 0.6780(4) -0.0174(3) 0.086 Uiso 1 calc R . 
C8 C 1.2469(4) 0.8079(4) 0.0903(3) 0.084(2) Uani 1 d . . 
H8A H 1.3286(4) 0.8325(4) 0.0868(3) 0.101 Uiso 1 calc R . 
C9 C 1.2026(4) 0.8599(4) 0.1574(3) 0.0729(15) Uani 1 d . . 
H9A H 1.2561(4) 0.9181(4) 0.2022(3) 0.087 Uiso 1 calc R . 
C10 C 1.0797(4) 0.8276(3) 0.1601(2) 0.0503(10) Uani 1 d . . 
C11 C 1.0263(4) 0.8799(3) 0.2340(2) 0.0510(10) Uani 1 d . . 
H11A H 0.9410(4) 0.8762(3) 0.2159(2) 0.061 Uiso 1 calc R . 
H11B H 1.0738(4) 0.9524(3) 0.2645(2) 0.061 Uiso 1 calc R . 
C12 C 1.0318(4) 0.8239(3) 0.2889(2) 0.0553(11) Uani 1 d . . 
H12A H 0.9994(4) 0.7498(3) 0.2539(2) 0.066 Uiso 1 calc R . 
H12B H 1.1185(4) 0.8377(3) 0.3123(2) 0.066 Uiso 1 calc R . 
C13 C 0.9600(3) 0.7947(3) 0.4054(2) 0.0444(9) Uani 1 d . . 
H13A H 1.0040(3) 0.7458(3) 0.3931(2) 0.053 Uiso 1 calc R . 
C14 C 0.9637(3) 0.8505(3) 0.3591(2) 0.0428(9) Uani 1 d . . 
C15 C 0.9005(4) 0.9262(3) 0.3802(2) 0.0480(10) Uani 1 d . . 
H15A H 0.9020(4) 0.9675(3) 0.3522(2) 0.058 Uiso 1 calc R . 
C16 C 0.8356(3) 0.9389(3) 0.4436(2) 0.0447(9) Uani 1 d . . 
H16A H 0.7932(3) 0.9889(3) 0.4581(2) 0.054 Uiso 1 calc R . 
C17 C 0.8339(3) 0.8782(3) 0.4847(2) 0.0388(8) Uani 1 d . . 
C18 C 0.7628(3) 0.8820(2) 0.5510(2) 0.0401(9) Uani 1 d . . 
C19 C 0.6761(4) 0.9363(3) 0.5686(2) 0.0510(10) Uani 1 d . . 
H19A H 0.6632(4) 0.9761(3) 0.5410(2) 0.061 Uiso 1 calc R . 
C20 C 0.6090(4) 0.9312(3) 0.6274(2) 0.0599(12) Uani 1 d . . 
H20A H 0.5488(4) 0.9660(3) 0.6385(2) 0.072 Uiso 1 calc R . 
C21 C 0.6305(4) 0.8746(3) 0.6697(2) 0.0527(11) Uani 1 d . . 
C22 C 0.7191(4) 0.8226(3) 0.6490(2) 0.0513(10) Uani 1 d . . 
H22A H 0.7346(4) 0.7838(3) 0.6770(2) 0.062 Uiso 1 calc R . 
C23 C 0.6200(5) 0.4743(4) -0.0591(3) 0.091(2) Uani 1 d . . 
H23A H 0.6205(5) 0.5297(4) -0.0072(3) 0.137 Uiso 1 calc R . 
H23B H 0.5959(5) 0.4092(4) -0.0557(3) 0.137 Uiso 1 calc R . 
H23C H 0.5619(5) 0.4730(4) -0.1024(3) 0.137 Uiso 1 calc R . 
C24 C 0.5593(5) 0.8647(4) 0.7347(3) 0.0742(14) Uani 1 d . . 
H24A H 0.5888(5) 0.8220(4) 0.7564(3) 0.111 Uiso 1 calc R . 
H24B H 0.4724(5) 0.8334(4) 0.7100(3) 0.111 Uiso 1 calc R . 
H24C H 0.5715(5) 0.9323(4) 0.7789(3) 0.111 Uiso 1 calc R . 
C25 C 0.7249(4) 0.8472(3) 0.0318(2) 0.0567(11) Uani 1 d . . 
H25A H 0.7628(4) 0.8251(3) -0.0132(2) 0.068 Uiso 1 calc R . 
C26 C 0.6771(4) 0.9307(3) 0.0450(2) 0.0582(11) Uani 1 d . . 
C27 C 0.6223(4) 0.9618(3) 0.1115(3) 0.0624(12) Uani 1 d . . 
H27A H 0.5904(4) 1.0181(3) 0.1241(3) 0.075 Uiso 1 calc R . 
C28 C 0.6146(4) 0.9080(3) 0.1608(2) 0.0541(10) Uani 1 d . . 
H28A H 0.5767(4) 0.9287(3) 0.2060(2) 0.065 Uiso 1 calc R . 
C29 C 0.6620(3) 0.8255(3) 0.1434(2) 0.0403(9) Uani 1 d . . 
C30 C 0.6559(3) 0.7636(3) 0.1911(2) 0.0391(9) Uani 1 d . . 
C31 C 0.5908(3) 0.7743(3) 0.2537(2) 0.0445(9) Uani 1 d . . 
H31A H 0.5452(3) 0.8220(3) 0.2672(2) 0.053 Uiso 1 calc R . 
C32 C 0.5932(4) 0.7148(3) 0.2961(2) 0.0501(10) Uani 1 d . . 
H32A H 0.5509(4) 0.7236(3) 0.3392(2) 0.060 Uiso 1 calc R . 
C33 C 0.6580(3) 0.6419(3) 0.2751(2) 0.0442(9) Uani 1 d . . 
C34 C 0.7178(3) 0.6327(3) 0.2100(2) 0.0456(9) Uani 1 d . . 
H34A H 0.7600(3) 0.5826(3) 0.1938(2) 0.055 Uiso 1 calc R . 
C35 C 0.6701(4) 0.5753(3) 0.3184(2) 0.0512(10) Uani 1 d . . 
H35A H 0.7579(4) 0.5849(3) 0.3354(2) 0.061 Uiso 1 calc R . 
H35B H 0.6336(4) 0.5033(3) 0.2785(2) 0.061 Uiso 1 calc R . 
C36 C 0.6118(4) 0.5931(3) 0.3945(2) 0.0499(10) Uani 1 d . . 
H36A H 0.6392(4) 0.6663(3) 0.4327(2) 0.060 Uiso 1 calc R . 
H36B H 0.5221(4) 0.5722(3) 0.3776(2) 0.060 Uiso 1 calc R . 
C37 C 0.6490(4) 0.5314(3) 0.4365(2) 0.0483(10) Uani 1 d . . 
C38 C 0.5737(5) 0.4352(3) 0.4213(3) 0.0666(13) Uani 1 d . . 
H38A H 0.4966(5) 0.4072(3) 0.3852(3) 0.080 Uiso 1 calc R . 
C39 C 0.6151(5) 0.3815(3) 0.4606(3) 0.0737(15) Uani 1 d . . 
H39A H 0.5652(5) 0.3169(3) 0.4519(3) 0.088 Uiso 1 calc R . 
C40 C 0.7295(5) 0.4228(3) 0.5125(3) 0.0681(13) Uani 1 d . . 
H40A H 0.7585(5) 0.3867(3) 0.5389(3) 0.082 Uiso 1 calc R . 
C41 C 0.8015(4) 0.5200(3) 0.5247(2) 0.0472(10) Uani 1 d . . 
C42 C 0.9259(4) 0.5715(3) 0.5809(2) 0.0489(9) Uani 1 d . . 
C43 C 0.9803(4) 0.5270(3) 0.6238(3) 0.0661(12) Uani 1 d . . 
H43A H 0.9407(4) 0.4608(3) 0.6176(3) 0.079 Uiso 1 calc R . 
C44 C 1.0946(5) 0.5825(4) 0.6759(3) 0.0830(15) Uani 1 d . . 
H44A H 1.1314(5) 0.5558(4) 0.7077(3) 0.100 Uiso 1 calc R . 
C45 C 1.1535(5) 0.6771(4) 0.6804(3) 0.0771(14) Uani 1 d . . 
H45A H 1.2325(5) 0.7133(4) 0.7134(3) 0.093 Uiso 1 calc R . 
C46 C 1.0974(4) 0.7190(4) 0.6368(3) 0.0660(12) Uani 1 d . . 
C47 C 0.6852(5) 0.9815(4) -0.0127(3) 0.087(2) Uani 1 d . . 
H47A H 0.7270(5) 0.9480(4) -0.0551(3) 0.130 Uiso 1 calc R . 
H47B H 0.7307(5) 1.0536(4) 0.0178(3) 0.130 Uiso 1 calc R . 
H47C H 0.6030(5) 0.9752(4) -0.0377(3) 0.130 Uiso 1 calc R . 
C48 C 1.1577(5) 0.8222(4) 0.6393(4) 0.091(2) Uani 1 d . . 
H48A H 1.1028(5) 0.8371(4) 0.6046(4) 0.137 Uiso 1 calc R . 
H48B H 1.2336(5) 0.8205(4) 0.6197(4) 0.137 Uiso 1 calc R . 
H48C H 1.1755(5) 0.8751(4) 0.6953(4) 0.137 Uiso 1 calc R . 
Cl1 Cl 0.32136(10) 0.78571(8) 0.40856(7) 0.0610(3) Uani 1 d . . 
O11 O 0.2097(4) 0.6987(3) 0.3672(3) 0.117(2) Uani 1 d . . 
O12 O 0.3558(3) 0.8261(3) 0.3524(2) 0.0947(10) Uani 1 d . . 
O13 O 0.2904(5) 0.8605(3) 0.4761(3) 0.1295(15) Uani 1 d . . 
O14 O 0.4164(3) 0.7520(3) 0.4363(2) 0.0895(10) Uani 1 d . . 
Cl2 Cl 1.39170(12) 0.69960(10) -0.12140(7) 0.0785(4) Uani 1 d D . 
O21 O 1.2762(3) 0.6220(3) -0.1508(2) 0.0946(13) Uani 1 d . . 
O22 O 1.4161(8) 0.7094(7) -0.1923(4) 0.122(3) Uani 0.455(6) d PDU 1 
O23 O 1.4717(8) 0.6473(7) -0.1037(8) 0.167(5) Uani 0.455(6) d PDU 1 
O24 O 1.4067(10) 0.7822(7) -0.0461(6) 0.160(6) Uani 0.455(6) d PDU 1 
O22' O 1.4345(9) 0.7243(9) -0.0393(4) 0.137(4) Uani 0.545(6) d PDU 2 
O23' O 1.3654(11) 0.7885(5) -0.1216(8) 0.177(5) Uani 0.545(6) d PDU 2 
O24' O 1.4803(7) 0.6776(10) -0.1675(6) 0.192(6) Uani 0.545(6) d PDU 2 
O1 O 0.8436(5) 0.7676(4) 0.8139(4) 0.170(2) Uani 1 d DU . 
C49 C 0.7034(7) 0.5933(6) 0.7484(5) 0.159(3) Uani 1 d DU . 
H49A H 0.6931(7) 0.5257(6) 0.7466(5) 0.238 Uiso 1 calc R . 
H49B H 0.7069(7) 0.5892(6) 0.6941(5) 0.238 Uiso 1 calc R . 
H49C H 0.6346(7) 0.6179(6) 0.7663(5) 0.238 Uiso 1 calc R . 
C50 C 0.8167(8) 0.6639(5) 0.8053(5) 0.173(3) Uani 1 d DU . 
H50A H 0.8129(8) 0.6654(5) 0.8593(5) 0.208 Uiso 1 calc R . 
H50B H 0.8850(8) 0.6368(5) 0.7872(5) 0.208 Uiso 1 calc R . 
C51 C 0.9707(7) 0.8302(6) 0.8537(6) 0.187(4) Uani 1 d DU . 
H51A H 1.0281(7) 0.7956(6) 0.8256(6) 0.224 Uiso 1 calc R . 
H51B H 0.9874(7) 0.8417(6) 0.9111(6) 0.224 Uiso 1 calc R . 
C52 C 0.9845(10) 0.9300(7) 0.8486(7) 0.233(5) Uani 1 d DU . 
H52B H 1.0678(10) 0.9741(7) 0.8743(7) 0.349 Uiso 1 calc R . 
H52C H 0.9272(10) 0.9634(7) 0.8768(7) 0.349 Uiso 1 calc R . 
H52D H 0.9673(10) 0.9174(7) 0.7915(7) 0.349 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 
Cu1 0.0491(2) 0.0558(3) 0.0468(2) 0.0190(2) 0.0220(2) 0.0214(2) 
Cu2 0.0636(3) 0.0468(2) 0.0577(2) 0.0309(2) 0.0162(2) 0.0224(2) 
N1 0.048(2) 0.049(2) 0.0353(14) 0.0125(12) 0.0136(12) 0.0123(14) 
N2 0.043(2) 0.0504(15) 0.0333(13) 0.0206(11) 0.0127(11) 0.0175(13) 
N3 0.050(2) 0.0376(14) 0.0409(14) 0.0191(11) 0.0140(12) 0.0143(13) 
N4 0.059(2) 0.0388(14) 0.0447(14) 0.0209(12) 0.0154(13) 0.0169(13) 
N5 0.045(2) 0.057(2) 0.0412(14) 0.0251(12) 0.0115(12) 0.0180(14) 
N6 0.0421(15) 0.0423(14) 0.0402(14) 0.0168(12) 0.0100(12) 0.0160(13) 
N7 0.058(2) 0.0380(13) 0.0457(14) 0.0232(11) 0.0199(13) 0.0206(13) 
N8 0.060(2) 0.055(2) 0.0470(15) 0.0275(13) 0.0130(14) 0.0257(15) 
C1 0.056(2) 0.062(2) 0.048(2) 0.010(2) 0.008(2) 0.008(2) 
C2 0.081(3) 0.060(3) 0.052(2) 0.001(2) 0.005(2) 0.011(2) 
C3 0.093(3) 0.068(3) 0.053(2) 0.003(2) 0.016(2) 0.036(3) 
C4 0.064(2) 0.082(3) 0.053(2) 0.010(2) 0.025(2) 0.032(2) 
C5 0.051(2) 0.055(2) 0.037(2) 0.0186(15) 0.016(2) 0.020(2) 
C6 0.045(2) 0.057(2) 0.045(2) 0.022(2) 0.018(2) 0.016(2) 
C7 0.054(2) 0.093(3) 0.054(2) 0.017(2) 0.028(2) 0.019(2) 
C8 0.055(3) 0.116(4) 0.056(2) 0.025(3) 0.019(2) -0.002(3) 
C9 0.056(3) 0.083(3) 0.052(2) 0.017(2) 0.010(2) -0.010(2) 
C10 0.057(2) 0.057(2) 0.038(2) 0.025(2) 0.013(2) 0.009(2) 
C11 0.065(2) 0.043(2) 0.040(2) 0.0156(15) 0.015(2) 0.010(2) 
C12 0.058(2) 0.063(2) 0.051(2) 0.024(2) 0.023(2) 0.023(2) 
C13 0.047(2) 0.046(2) 0.045(2) 0.0196(15) 0.016(2) 0.019(2) 
C14 0.047(2) 0.040(2) 0.039(2) 0.0168(14) 0.0109(15) 0.009(2) 
C15 0.057(2) 0.045(2) 0.045(2) 0.0222(15) 0.013(2) 0.014(2) 
C16 0.058(2) 0.039(2) 0.043(2) 0.0187(14) 0.018(2) 0.021(2) 
C17 0.045(2) 0.036(2) 0.034(2) 0.0138(13) 0.0069(14) 0.0118(15) 
C18 0.046(2) 0.031(2) 0.036(2) 0.0095(13) 0.0086(15) 0.0050(15) 
C19 0.062(2) 0.050(2) 0.050(2) 0.024(2) 0.018(2) 0.025(2) 
C20 0.066(2) 0.059(2) 0.059(2) 0.023(2) 0.026(2) 0.026(2) 
C21 0.063(2) 0.044(2) 0.045(2) 0.014(2) 0.020(2) 0.009(2) 
C22 0.064(2) 0.046(2) 0.046(2) 0.022(2) 0.017(2) 0.015(2) 
C23 0.060(3) 0.087(4) 0.085(3) 0.009(3) 0.016(3) -0.003(3) 
C24 0.095(3) 0.071(3) 0.065(2) 0.034(2) 0.040(2) 0.022(2) 
C25 0.058(2) 0.074(2) 0.045(2) 0.029(2) 0.021(2) 0.020(2) 
C26 0.062(2) 0.065(2) 0.065(2) 0.042(2) 0.015(2) 0.024(2) 
C27 0.073(3) 0.060(2) 0.069(2) 0.036(2) 0.020(2) 0.032(2) 
C28 0.061(2) 0.060(2) 0.052(2) 0.028(2) 0.022(2) 0.028(2) 
C29 0.040(2) 0.044(2) 0.039(2) 0.0189(14) 0.0088(14) 0.0144(15) 
C30 0.032(2) 0.045(2) 0.035(2) 0.0142(14) 0.0052(13) 0.0088(15) 
C31 0.048(2) 0.050(2) 0.043(2) 0.0209(15) 0.0178(15) 0.024(2) 
C32 0.058(2) 0.059(2) 0.043(2) 0.026(2) 0.023(2) 0.022(2) 
C33 0.044(2) 0.048(2) 0.042(2) 0.0209(14) 0.0086(15) 0.015(2) 
C34 0.050(2) 0.042(2) 0.051(2) 0.0201(15) 0.019(2) 0.021(2) 
C35 0.061(2) 0.057(2) 0.046(2) 0.027(2) 0.016(2) 0.025(2) 
C36 0.053(2) 0.059(2) 0.044(2) 0.027(2) 0.012(2) 0.018(2) 
C37 0.057(2) 0.046(2) 0.045(2) 0.0218(15) 0.014(2) 0.014(2) 
C38 0.074(3) 0.058(2) 0.059(2) 0.027(2) 0.008(2) 0.002(2) 
C39 0.097(4) 0.054(2) 0.065(2) 0.035(2) 0.005(2) 0.000(2) 
C40 0.097(3) 0.056(2) 0.064(2) 0.040(2) 0.014(2) 0.019(2) 
C41 0.069(2) 0.039(2) 0.039(2) 0.0184(14) 0.014(2) 0.020(2) 
C42 0.064(2) 0.050(2) 0.044(2) 0.0239(15) 0.021(2) 0.028(2) 
C43 0.087(3) 0.061(2) 0.065(2) 0.036(2) 0.009(2) 0.035(2) 
C44 0.099(3) 0.093(3) 0.086(3) 0.053(2) 0.016(3) 0.057(3) 
C45 0.067(3) 0.091(3) 0.080(3) 0.041(2) 0.005(2) 0.031(3) 
C46 0.056(2) 0.081(3) 0.068(2) 0.035(2) 0.011(2) 0.028(2) 
C47 0.110(4) 0.101(3) 0.088(3) 0.068(2) 0.037(3) 0.045(3) 
C48 0.060(3) 0.092(3) 0.109(4) 0.050(3) -0.012(3) -0.001(3) 
Cl1 0.0726(6) 0.0616(5) 0.0742(5) 0.0414(4) 0.0354(5) 0.0362(5) 
O11 0.105(3) 0.104(3) 0.135(3) 0.066(2) -0.004(3) 0.003(2) 
O12 0.126(3) 0.106(2) 0.117(2) 0.085(2) 0.069(2) 0.066(2) 
O13 0.212(4) 0.107(2) 0.123(3) 0.061(2) 0.113(3) 0.092(3) 
O14 0.076(2) 0.126(2) 0.119(2) 0.088(2) 0.038(2) 0.053(2) 
Cl2 0.0800(8) 0.0742(7) 0.0679(7) 0.0207(6) 0.0293(6) 0.0108(6) 
O21 0.082(2) 0.092(2) 0.078(2) 0.013(2) 0.029(2) 0.005(2) 
O22 0.079(5) 0.199(7) 0.141(5) 0.130(5) 0.046(4) 0.026(5) 
O23 0.151(8) 0.207(8) 0.184(9) 0.121(7) -0.019(7) 0.086(7) 
O24 0.109(7) 0.092(7) 0.159(9) -0.050(6) 0.073(6) -0.016(6) 
O22' 0.113(7) 0.178(9) 0.082(5) 0.038(6) -0.014(5) 0.023(7) 
O23' 0.225(10) 0.087(5) 0.186(10) 0.035(6) -0.013(9) 0.057(6) 
O24' 0.113(6) 0.184(10) 0.185(8) -0.012(7) 0.110(6) 0.008(6) 
O1 0.163(4) 0.163(4) 0.209(4) 0.122(3) -0.010(4) 0.034(4) 
C49 0.121(6) 0.170(6) 0.209(7) 0.119(6) 0.011(6) 0.027(5) 
C50 0.214(8) 0.172(6) 0.173(6) 0.108(5) 0.010(6) 0.079(6) 
C51 0.148(7) 0.218(8) 0.205(8) 0.107(7) 0.018(6) 0.051(7) 
C52 0.171(9) 0.204(9) 0.298(12) 0.152(8) -0.028(9) -0.039(8) 
 
_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 
Cu1 N1 2.004(3) . ? 
Cu1 N6 2.012(3) . ? 
Cu1 N5 2.052(3) . ? 
Cu1 N2 2.057(3) . ? 
Cu2 N3 1.994(3) . ? 
Cu2 N8 2.001(3) . ? 
Cu2 N7 2.061(3) . ? 
Cu2 N4 2.069(3) . ? 
N1 C1 1.331(5) . ? 
N1 C5 1.351(5) . ? 
N2 C10 1.345(4) . ? 
N2 C6 1.356(4) . ? 
N3 C13 1.335(5) . ? 
N3 C17 1.368(5) . ? 
N4 C22 1.332(5) . ? 
N4 C18 1.353(5) . ? 
N5 C25 1.340(5) . ? 
N5 C29 1.347(5) . ? 
N6 C34 1.331(5) . ? 
N6 C30 1.367(5) . ? 
N7 C37 1.338(5) . ? 
N7 C41 1.342(5) . ? 
N8 C46 1.342(5) . ? 
N8 C42 1.348(5) . ? 
C1 C2 1.383(6) . ? 
C1 C23 1.500(7) . ? 
C2 C3 1.371(7) . ? 
C3 C4 1.366(6) . ? 
C4 C5 1.377(5) . ? 
C5 C6 1.493(5) . ? 
C6 C7 1.376(6) . ? 
C7 C8 1.376(6) . ? 
C8 C9 1.358(6) . ? 
C9 C10 1.375(6) . ? 
C10 C11 1.506(5) . ? 
C11 C12 1.522(6) . ? 
C12 C14 1.506(5) . ? 
C13 C14 1.380(5) . ? 
C14 C15 1.400(5) . ? 
C15 C16 1.387(5) . ? 
C16 C17 1.366(5) . ? 
C17 C18 1.491(5) . ? 
C18 C19 1.379(5) . ? 
C19 C20 1.377(6) . ? 
C20 C21 1.374(6) . ? 
C21 C22 1.383(6) . ? 
C21 C24 1.519(6) . ? 
C25 C26 1.393(6) . ? 
C26 C27 1.363(6) . ? 
C26 C47 1.499(6) . ? 
C27 C28 1.401(6) . ? 
C28 C29 1.368(5) . ? 
C29 C30 1.473(5) . ? 
C30 C31 1.381(5) . ? 
C31 C32 1.374(6) . ? 
C32 C33 1.379(5) . ? 
C33 C34 1.385(5) . ? 
C33 C35 1.494(5) . ? 
C35 C36 1.531(5) . ? 
C36 C37 1.492(6) . ? 
C37 C38 1.376(6) . ? 
C38 C39 1.374(7) . ? 
C39 C40 1.368(7) . ? 
C40 C41 1.390(5) . ? 
C41 C42 1.486(5) . ? 
C42 C43 1.375(6) . ? 
C43 C44 1.376(6) . ? 
C44 C45 1.362(7) . ? 
C45 C46 1.363(7) . ? 
C46 C48 1.495(7) . ? 
Cl1 O12 1.406(4) . ? 
Cl1 O14 1.407(3) . ? 
Cl1 O13 1.412(4) . ? 
Cl1 O11 1.452(4) . ? 
Cl2 O24 1.372(6) . ? 
Cl2 O24' 1.374(6) . ? 
Cl2 O22' 1.379(6) . ? 
Cl2 O22 1.386(6) . ? 
Cl2 O23 1.399(6) . ? 
Cl2 O23' 1.402(6) . ? 
Cl2 O21 1.412(4) . ? 
O1 C50 1.423(7) . ? 
O1 C51 1.449(7) . ? 
C49 C50 1.436(7) . ? 
C51 C52 1.478(8) . ? 
 
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 
N1 Cu1 N6 134.04(12) . . ? 
N1 Cu1 N5 126.54(12) . . ? 
N6 Cu1 N5 81.16(12) . . ? 
N1 Cu1 N2 81.86(11) . . ? 
N6 Cu1 N2 123.43(11) . . ? 
N5 Cu1 N2 113.87(12) . . ? 
N3 Cu2 N8 138.99(13) . . ? 
N3 Cu2 N7 125.01(11) . . ? 
N8 Cu2 N7 81.99(12) . . ? 
N3 Cu2 N4 81.36(12) . . ? 
N8 Cu2 N4 123.07(12) . . ? 
N7 Cu2 N4 107.31(12) . . ? 
C1 N1 C5 119.7(3) . . ? 
C1 N1 Cu1 126.4(3) . . ? 
C5 N1 Cu1 113.8(2) . . ? 
C10 N2 C6 118.1(3) . . ? 
C10 N2 Cu1 129.2(3) . . ? 
C6 N2 Cu1 112.4(2) . . ? 
C13 N3 C17 117.7(3) . . ? 
C13 N3 Cu2 127.0(3) . . ? 
C17 N3 Cu2 115.3(2) . . ? 
C22 N4 C18 118.5(3) . . ? 
C22 N4 Cu2 127.6(3) . . ? 
C18 N4 Cu2 111.8(2) . . ? 
C25 N5 C29 118.3(3) . . ? 
C25 N5 Cu1 128.0(3) . . ? 
C29 N5 Cu1 113.2(2) . . ? 
C34 N6 C30 118.6(3) . . ? 
C34 N6 Cu1 127.5(2) . . ? 
C30 N6 Cu1 113.9(2) . . ? 
C37 N7 C41 119.0(3) . . ? 
C37 N7 Cu2 129.1(3) . . ? 
C41 N7 Cu2 111.7(2) . . ? 
C46 N8 C42 120.2(4) . . ? 
C46 N8 Cu2 125.8(3) . . ? 
C42 N8 Cu2 113.7(3) . . ? 
N1 C1 C2 120.8(4) . . ? 
N1 C1 C23 116.9(4) . . ? 
C2 C1 C23 122.3(4) . . ? 
C3 C2 C1 119.7(4) . . ? 
C4 C3 C2 119.3(4) . . ? 
C3 C4 C5 119.2(4) . . ? 
N1 C5 C4 121.2(3) . . ? 
N1 C5 C6 116.0(3) . . ? 
C4 C5 C6 122.7(4) . . ? 
N2 C6 C7 122.0(3) . . ? 
N2 C6 C5 115.1(3) . . ? 
C7 C6 C5 122.9(3) . . ? 
C6 C7 C8 119.2(4) . . ? 
C9 C8 C7 118.5(4) . . ? 
C8 C9 C10 120.7(4) . . ? 
N2 C10 C9 121.3(4) . . ? 
N2 C10 C11 115.5(3) . . ? 
C9 C10 C11 123.2(3) . . ? 
C10 C11 C12 108.1(3) . . ? 
C14 C12 C11 117.5(4) . . ? 
N3 C13 C14 124.7(3) . . ? 
C13 C14 C15 116.8(3) . . ? 
C13 C14 C12 118.0(3) . . ? 
C15 C14 C12 125.1(4) . . ? 
C16 C15 C14 119.2(4) . . ? 
C17 C16 C15 120.2(4) . . ? 
C16 C17 N3 121.4(3) . . ? 
C16 C17 C18 124.6(3) . . ? 
N3 C17 C18 114.1(3) . . ? 
N4 C18 C19 121.0(3) . . ? 
N4 C18 C17 116.0(3) . . ? 
C19 C18 C17 122.9(3) . . ? 
C20 C19 C18 119.4(4) . . ? 
C21 C20 C19 120.2(4) . . ? 
C20 C21 C22 117.1(4) . . ? 
C20 C21 C24 123.1(4) . . ? 
C22 C21 C24 119.7(4) . . ? 
N4 C22 C21 123.7(4) . . ? 
N5 C25 C26 124.6(4) . . ? 
C27 C26 C25 116.6(4) . . ? 
C27 C26 C47 122.8(4) . . ? 
C25 C26 C47 120.6(4) . . ? 
C26 C27 C28 119.3(4) . . ? 
C29 C28 C27 120.9(4) . . ? 
N5 C29 C28 120.2(4) . . ? 
N5 C29 C30 115.4(3) . . ? 
C28 C29 C30 124.4(3) . . ? 
N6 C30 C31 119.9(3) . . ? 
N6 C30 C29 115.6(3) . . ? 
C31 C30 C29 124.5(3) . . ? 
C32 C31 C30 120.3(4) . . ? 
C31 C32 C33 120.3(4) . . ? 
C32 C33 C34 116.5(4) . . ? 
C32 C33 C35 125.0(3) . . ? 
C34 C33 C35 118.5(3) . . ? 
N6 C34 C33 124.4(3) . . ? 
C33 C35 C36 117.5(3) . . ? 
C37 C36 C35 109.8(3) . . ? 
N7 C37 C38 122.3(4) . . ? 
N7 C37 C36 116.2(3) . . ? 
C38 C37 C36 121.5(4) . . ? 
C39 C38 C37 118.4(4) . . ? 
C40 C39 C38 120.3(4) . . ? 
C39 C40 C41 118.5(4) . . ? 
N7 C41 C40 121.5(4) . . ? 
N7 C41 C42 116.3(3) . . ? 
C40 C41 C42 122.2(4) . . ? 
N8 C42 C43 121.0(4) . . ? 
N8 C42 C41 115.7(3) . . ? 
C43 C42 C41 123.3(4) . . ? 
C42 C43 C44 118.6(4) . . ? 
C45 C44 C43 119.4(5) . . ? 
C44 C45 C46 120.5(5) . . ? 
N8 C46 C45 120.1(4) . . ? 
N8 C46 C48 117.1(4) . . ? 
C45 C46 C48 122.7(4) . . ? 
O12 Cl1 O14 111.1(2) . . ? 
O12 Cl1 O13 110.3(2) . . ? 
O14 Cl1 O13 110.7(3) . . ? 
O12 Cl1 O11 108.6(2) . . ? 
O14 Cl1 O11 109.5(2) . . ? 
O13 Cl1 O11 106.5(3) . . ? 
O24' Cl2 O22' 111.7(7) . . ? 
O24 Cl2 O22 124.1(7) . . ? 
O24 Cl2 O23 102.7(8) . . ? 
O22 Cl2 O23 106.6(7) . . ? 
O24' Cl2 O23' 108.8(9) . . ? 
O22' Cl2 O23' 105.6(7) . . ? 
O24 Cl2 O21 116.5(5) . . ? 
O24' Cl2 O21 115.6(4) . . ? 
O22' Cl2 O21 109.0(5) . . ? 
O22 Cl2 O21 102.8(4) . . ? 
O23 Cl2 O21 101.7(5) . . ? 
O23' Cl2 O21 105.5(5) . . ? 
C50 O1 C51 114.4(6) . . ? 
O1 C50 C49 115.3(7) . . ? 
O1 C51 C52 106.6(7) . . ? 
 
_refine_diff_density_max    0.603 
_refine_diff_density_min   -0.509 
_refine_diff_density_rms    0.131 
 
# = end

data_C48H47Cl3Cu2N8O14 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C48 H47 Cl3 Cu2 N8 O14' 
_chemical_formula_weight          1193.37 
_chemical_melting_point           ? 
_chemical_compound_source         ? 
 
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' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cu'  'Cu'   0.3201   1.2651 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 
 
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                    11.216(3) 
_cell_length_b                    21.616(4) 
_cell_length_c                    20.795(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  95.91(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      5014.6(20) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     25 
_cell_measurement_theta_min       4.85 
_cell_measurement_theta_max       12.45 
 
_exptl_crystal_description        'prism' 
_exptl_crystal_colour             'blue' 
_exptl_crystal_size_max           0.10 
_exptl_crystal_size_mid           0.05 
_exptl_crystal_size_min           0.05 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.581 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              2448 
_exptl_absorpt_coefficient_mu     1.084 
_exptl_absorpt_correction_type    'SADABS' 
_exptl_absorpt_correction_T_min   0.814270 
_exptl_absorpt_correction_T_max   1.00 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(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        'Siemens SMART CCD' 
_diffrn_measurement_method        '\w scans' 
_diffrn_standards_number          ? 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   ? 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             22769 
_diffrn_reflns_av_R_equivalents   0.0517 
_diffrn_reflns_av_sigmaI/netI     0.0735 
_diffrn_reflns_limit_h_min        -13 
_diffrn_reflns_limit_h_max        13 
_diffrn_reflns_limit_k_min        -24 
_diffrn_reflns_limit_k_max        25 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        24 
_diffrn_reflns_theta_min          1.36 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              8641 
_reflns_number_observed           5773 
_reflns_observed_criterion        >2sigma(I) 
 
_computing_data_collection        'Siemens SMART' 
_computing_cell_refinement        'Siemens SMART'
_computing_data_reduction         'Siemens SMART' 
_computing_structure_solution     'SHELXTL Version(Siemens, 1995)' 
_computing_structure_refinement   'SHELXTL Version(Siemens, 1995)'
_computing_molecular_graphics     'SHELXTL Version(Siemens, 1995)' 
_computing_publication_material   'SHELXTL Version(Siemens, 1995)' 

 
_refine_special_details 
; 
 Refinement on F^2^ for ALL reflections except for 273 with very negative F^2^ 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses 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 observed criterion 
 of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. 
 
 Hydrogen atoms of the oxyden atoms of the water molecule and hydroxyl group
 were found from the DIFMAP and refined using the riding model.

; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+11.1222P] 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     'riding model' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          8368 
_refine_ls_number_parameters      742 
_refine_ls_number_restraints      150 
_refine_ls_R_factor_all           0.1187 
_refine_ls_R_factor_obs           0.0712 
_refine_ls_wR_factor_all          0.1522 
_refine_ls_wR_factor_obs          0.1319 
_refine_ls_goodness_of_fit_all    1.064 
_refine_ls_goodness_of_fit_obs    1.144 
_refine_ls_restrained_S_all       1.066 
_refine_ls_restrained_S_obs       1.154 
_refine_ls_shift/esd_max          0.166 
_refine_ls_shift/esd_mean         0.004 
 
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 
Cu1 Cu 0.82366(2) -0.232850(12) 0.350821(13) 0.03679(7) Uani 1 d . . 
Cu2 Cu 0.61379(2) -0.266778(12) 0.648000(13) 0.03820(7) Uani 1 d . . 
O1 O 0.94784(14) -0.20552(7) 0.30133(7) 0.0531(5) Uani 1 d . . 
H1A H 0.94934(14) -0.22767(7) 0.26941(7) 0.080 Uiso 1 d R . 
H1B H 0.98124(14) -0.17981(7) 0.31224(7) 0.080 Uiso 1 d R . 
O2 O 0.48833(14) -0.24838(7) 0.70068(8) 0.0545(5) Uani 1 d . . 
H2A H 0.4624(15) -0.2135(5) 0.6922(9) 0.082 Uiso 1 calc R . 
N1 N 0.7151(2) -0.15875(8) 0.32150(9) 0.0412(6) Uani 1 d . . 
N2 N 0.87030(15) -0.16432(8) 0.42808(8) 0.0385(5) Uani 1 d . . 
N3 N 0.74796(15) -0.30066(8) 0.59988(9) 0.0395(5) Uani 1 d . . 
N4 N 0.5712(2) -0.35717(8) 0.64659(9) 0.0386(5) Uani 1 d . . 
N5 N 0.8913(2) -0.31943(8) 0.35585(9) 0.0390(5) Uani 1 d . . 
N6 N 0.6895(2) -0.27754(8) 0.39103(8) 0.0364(5) Uani 1 d . . 
N7 N 0.56104(15) -0.18817(7) 0.58692(8) 0.0355(5) Uani 1 d . . 
N8 N 0.7301(2) -0.19622(8) 0.68690(9) 0.0414(6) Uani 1 d . . 
C1 C 0.6429(2) -0.15850(11) 0.26607(13) 0.0530(8) Uani 1 d . . 
C2 C 0.5642(2) -0.10999(13) 0.2511(2) 0.0747(10) Uani 1 d . . 
H2B H 0.5128(2) -0.11060(13) 0.2130(2) 0.090 Uiso 1 calc R . 
C3 C 0.5627(3) -0.06150(15) 0.2926(2) 0.0889(12) Uani 1 d . . 
H3A H 0.5100(3) -0.02875(15) 0.2831(2) 0.107 Uiso 1 calc R . 
C4 C 0.6389(2) -0.06096(12) 0.3483(2) 0.0707(10) Uani 1 d . . 
H4A H 0.6389(2) -0.02761(12) 0.3766(2) 0.085 Uiso 1 calc R . 
C5 C 0.7158(2) -0.11010(10) 0.36255(12) 0.0454(7) Uani 1 d . . 
C6 C 0.8043(2) -0.11245(10) 0.41991(11) 0.0428(7) Uani 1 d . . 
C7 C 0.8244(2) -0.06200(11) 0.46168(13) 0.0593(9) Uani 1 d . . 
H7A H 0.7785(2) -0.02626(11) 0.45537(13) 0.071 Uiso 1 calc R . 
C8 C 0.9128(3) -0.06613(12) 0.51202(13) 0.0660(9) Uani 1 d . . 
H8A H 0.9259(3) -0.03362(12) 0.54118(13) 0.079 Uiso 1 calc R . 
C9 C 0.9817(2) -0.11846(12) 0.51916(12) 0.0619(9) Uani 1 d . . 
H9A H 1.0430(2) -0.12127(12) 0.55272(12) 0.074 Uiso 1 calc R . 
C10 C 0.9597(2) -0.16742(11) 0.47613(10) 0.0413(7) Uani 1 d . . 
C11 C 1.0384(2) -0.22330(12) 0.47989(11) 0.0482(7) Uani 1 d . . 
H11A H 1.1183(2) -0.21074(12) 0.47145(11) 0.058 Uiso 1 calc R . 
H11B H 1.0086(2) -0.25168(12) 0.44583(11) 0.058 Uiso 1 calc R . 
C12 C 1.0475(2) -0.25807(12) 0.54441(11) 0.0494(8) Uani 1 d . . 
H12A H 1.1154(2) -0.28603(12) 0.54611(11) 0.059 Uiso 1 calc R . 
H12B H 1.0634(2) -0.22837(12) 0.57921(11) 0.059 Uiso 1 calc R . 
C13 C 0.9377(2) -0.29466(11) 0.55601(11) 0.0409(7) Uani 1 d . . 
C14 C 0.8415(2) -0.26864(11) 0.58198(11) 0.0456(7) Uani 1 d . . 
H14A H 0.8413(2) -0.22594(11) 0.58750(11) 0.055 Uiso 1 calc R . 
C15 C 0.9318(2) -0.35819(12) 0.54461(12) 0.0550(8) Uani 1 d . . 
H15A H 0.9927(2) -0.37800(12) 0.52542(12) 0.066 Uiso 1 calc R . 
C16 C 0.8354(2) -0.39148(11) 0.56189(12) 0.0522(8) Uani 1 d . . 
H16A H 0.8303(2) -0.43373(11) 0.55361(12) 0.063 Uiso 1 calc R . 
C17 C 0.7464(2) -0.36218(10) 0.59151(11) 0.0374(6) Uani 1 d . . 
C18 C 0.6469(2) -0.39487(10) 0.61826(10) 0.0379(6) Uani 1 d . . 
C19 C 0.6310(2) -0.45794(10) 0.61740(12) 0.0509(8) Uani 1 d . . 
H19A H 0.6806(2) -0.48323(10) 0.59566(12) 0.061 Uiso 1 calc R . 
C20 C 0.5415(2) -0.48298(11) 0.64890(13) 0.0616(9) Uani 1 d . . 
H20A H 0.5330(2) -0.52575(11) 0.65008(13) 0.074 Uiso 1 calc R . 
C21 C 0.4637(2) -0.44630(11) 0.67891(11) 0.0455(7) Uani 1 d . . 
C22 C 0.4828(2) -0.38288(11) 0.67538(11) 0.0459(7) Uani 1 d . . 
H22A H 0.4305(2) -0.35678(11) 0.69432(11) 0.055 Uiso 1 calc R . 
C23 C 0.6525(3) -0.21181(13) 0.22113(14) 0.0708(10) Uani 1 d . . 
H23A H 0.7115(3) -0.24047(13) 0.23998(14) 0.106 Uiso 1 calc R . 
H23B H 0.6759(3) -0.19699(13) 0.18076(14) 0.106 Uiso 1 calc R . 
H23C H 0.5763(3) -0.23222(13) 0.21378(14) 0.106 Uiso 1 calc R . 
C24 C 0.3662(2) -0.47085(12) 0.71552(14) 0.0676(9) Uani 1 d . . 
H24A H 0.3234(2) -0.43698(12) 0.73223(14) 0.101 Uiso 1 calc R . 
H24B H 0.4005(2) -0.49607(12) 0.75068(14) 0.101 Uiso 1 calc R . 
H24C H 0.3121(2) -0.49529(12) 0.68719(14) 0.101 Uiso 1 calc R . 
C25 C 0.9940(2) -0.33852(12) 0.33567(11) 0.0506(8) Uani 1 d . . 
H25A H 1.0424(2) -0.30918(12) 0.31848(11) 0.061 Uiso 1 calc R . 
C26 C 1.0334(2) -0.39940(12) 0.33868(12) 0.0542(8) Uani 1 d . . 
C27 C 0.9602(2) -0.44164(11) 0.36416(12) 0.0570(8) Uani 1 d . . 
H27A H 0.9830(2) -0.48298(11) 0.36719(12) 0.068 Uiso 1 calc R . 
C28 C 0.8544(2) -0.42369(11) 0.38509(12) 0.0519(8) Uani 1 d . . 
H28A H 0.8054(2) -0.45263(11) 0.40246(12) 0.062 Uiso 1 calc R . 
C29 C 0.8202(2) -0.36240(10) 0.38042(10) 0.0386(7) Uani 1 d . . 
C30 C 0.7085(2) -0.33829(10) 0.40076(11) 0.0405(7) Uani 1 d . . 
C31 C 0.6254(2) -0.37497(11) 0.42851(12) 0.0521(8) Uani 1 d . . 
H31A H 0.6400(2) -0.41694(11) 0.43527(12) 0.063 Uiso 1 calc R . 
C32 C 0.5225(2) -0.34896(12) 0.44571(13) 0.0545(8) Uani 1 d . . 
H32A H 0.4671(2) -0.37330(12) 0.46444(13) 0.065 Uiso 1 calc R . 
C33 C 0.5001(2) -0.28667(11) 0.43551(11) 0.0430(7) Uani 1 d . . 
C34 C 0.5867(2) -0.25244(11) 0.40879(11) 0.0413(7) Uani 1 d . . 
H34A H 0.5741(2) -0.21023(11) 0.40267(11) 0.050 Uiso 1 calc R . 
C35 C 0.3861(2) -0.25753(12) 0.45362(11) 0.0491(8) Uani 1 d . . 
H35A H 0.3196(2) -0.28557(12) 0.44257(11) 0.059 Uiso 1 calc R . 
H35B H 0.3705(2) -0.21978(12) 0.42896(11) 0.059 Uiso 1 calc R . 
C36 C 0.3942(2) -0.24244(11) 0.52659(11) 0.0455(7) Uani 1 d . . 
H36A H 0.3138(2) -0.23825(11) 0.53930(11) 0.055 Uiso 1 calc R . 
H36B H 0.4325(2) -0.27671(11) 0.55073(11) 0.055 Uiso 1 calc R . 
C37 C 0.4623(2) -0.18481(11) 0.54396(11) 0.0438(7) Uani 1 d . . 
C38 C 0.4212(3) -0.12876(12) 0.51778(15) 0.0709(10) Uani 1 d . . 
H38A H 0.3534(3) -0.12725(12) 0.48800(15) 0.085 Uiso 1 calc R . 
C39 C 0.4813(3) -0.07621(13) 0.5363(2) 0.0846(11) Uani 1 d . . 
H39A H 0.4535(3) -0.03828(13) 0.5198(2) 0.101 Uiso 1 calc R . 
C40 C 0.5836(3) -0.07853(12) 0.57941(15) 0.0719(10) Uani 1 d . . 
H40A H 0.6262(3) -0.04279(12) 0.59155(15) 0.086 Uiso 1 calc R . 
C41 C 0.6205(2) -0.13584(10) 0.60401(12) 0.0450(7) Uani 1 d . . 
C42 C 0.7243(2) -0.14241(10) 0.65365(11) 0.0443(7) Uani 1 d . . 
C43 C 0.8118(2) -0.09776(12) 0.66562(14) 0.0610(9) Uani 1 d . . 
H43A H 0.8058(2) -0.06058(12) 0.64303(14) 0.073 Uiso 1 calc R . 
C44 C 0.9069(2) -0.10817(14) 0.71052(14) 0.0728(10) Uani 1 d . . 
H44A H 0.9677(2) -0.07893(14) 0.71777(14) 0.087 Uiso 1 calc R . 
C45 C 0.9118(2) -0.16243(14) 0.74488(14) 0.0703(10) Uani 1 d . . 
H45A H 0.9755(2) -0.16982(14) 0.77624(14) 0.084 Uiso 1 calc R . 
C46 C 0.8215(2) -0.20651(12) 0.73293(12) 0.0551(8) Uani 1 d . . 
C47 C 1.1498(2) -0.41636(14) 0.3131(2) 0.0899(11) Uani 1 d . . 
H47A H 1.1863(2) -0.37983(14) 0.2977(2) 0.135 Uiso 1 calc R . 
H47B H 1.1347(2) -0.44540(14) 0.2783(2) 0.135 Uiso 1 calc R . 
H47C H 1.2027(2) -0.43466(14) 0.3471(2) 0.135 Uiso 1 calc R . 
C48 C 0.8188(3) -0.26644(14) 0.76827(14) 0.0782(11) Uani 1 d . . 
H48A H 0.7487(3) -0.28936(14) 0.75210(14) 0.117 Uiso 1 calc R . 
H48B H 0.8167(3) -0.25856(14) 0.81357(14) 0.117 Uiso 1 calc R . 
H48C H 0.8892(3) -0.28998(14) 0.76189(14) 0.117 Uiso 1 calc R . 
Cl1 Cl 0.30789(7) 0.41620(3) 1.14395(4) 0.0708(2) Uani 1 d U . 
O11 O 0.3147(3) 0.35426(10) 1.12857(14) 0.1367(12) Uani 1 d U . 
O12 O 0.2543(3) 0.4298(2) 1.1991(2) 0.153(2) Uani 0.777(2) d PU 1 
O13 O 0.2538(3) 0.45121(15) 1.0926(2) 0.1459(14) Uani 0.777(2) d PU 1 
O14 O 0.4285(3) 0.4341(2) 1.1560(2) 0.161(2) Uani 0.777(2) d PU 1 
O12' O 0.3137(9) 0.4513(4) 1.0922(5) 0.092(3) Uani 0.223(2) d PU 2 
O13' O 0.3296(12) 0.4322(7) 1.2029(6) 0.150(4) Uani 0.223(2) d PU 2 
O14' O 0.1759(11) 0.4013(7) 1.1423(6) 0.141(4) Uani 0.223(2) d PU 2 
Cl2 Cl 1.26277(6) 0.07171(3) 0.97758(4) 0.0600(2) Uani 1 d U . 
O21 O 1.2139(7) 0.1230(3) 0.9470(3) 0.103(2) Uani 0.332(2) d PU 1 
O22 O 1.2727(8) 0.0881(3) 1.0427(4) 0.128(3) Uani 0.332(2) d PU 1 
O23 O 1.3570(6) 0.0462(3) 0.9581(4) 0.126(3) Uani 0.332(2) d PU 1 
O24 O 1.1829(4) 0.0203(2) 0.9704(3) 0.063(2) Uani 0.332(2) d PU 1 
O21' O 1.2943(3) 0.0864(2) 0.91449(14) 0.1069(13) Uani 0.668(2) d PU 2 
O22' O 1.2711(4) 0.1258(2) 1.0158(2) 0.127(2) Uani 0.668(2) d PU 2 
O23' O 1.3626(3) 0.03491(15) 1.0056(2) 0.0963(13) Uani 0.668(2) d PU 2 
O24' O 1.1515(3) 0.0396(2) 0.9776(2) 0.113(2) Uani 0.668(2) d PU 2 
Cl3 Cl 0.73983(6) 0.11761(3) 0.32173(3) 0.0557(2) Uani 1 d . . 
O31 O 0.6167(2) 0.10818(14) 0.30871(12) 0.1224(11) Uani 1 d . . 
O32 O 0.7948(2) 0.06815(11) 0.35605(13) 0.1220(10) Uani 1 d . . 
O33 O 0.7551(3) 0.17168(10) 0.35952(12) 0.1166(10) Uani 1 d . . 
O34 O 0.7933(2) 0.12655(11) 0.26231(10) 0.0916(8) 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 
Cu1 0.03854(13) 0.03639(14) 0.03614(14) -0.00063(13) 0.00720(11) -0.00222(12) 
Cu2 0.04504(14) 0.03011(13) 0.04222(14) 0.00415(13) 0.01785(12) 0.00371(12) 
O1 0.0667(9) 0.0505(9) 0.0462(9) -0.0133(8) 0.0250(8) -0.0171(8) 
O2 0.0662(9) 0.0433(9) 0.0605(9) 0.0102(8) 0.0378(8) 0.0142(8) 
N1 0.0432(10) 0.0391(10) 0.0412(11) 0.0063(9) 0.0042(9) -0.0017(9) 
N2 0.0387(9) 0.0440(10) 0.0344(10) -0.0021(9) 0.0115(8) -0.0051(8) 
N3 0.0384(9) 0.0386(10) 0.0431(11) 0.0007(9) 0.0119(8) 0.0031(8) 
N4 0.0407(10) 0.0326(9) 0.0428(10) 0.0013(9) 0.0054(9) -0.0021(8) 
N5 0.0366(9) 0.0416(10) 0.0385(10) 0.0016(9) 0.0025(8) 0.0013(8) 
N6 0.0385(9) 0.0383(10) 0.0322(9) 0.0007(8) 0.0022(8) -0.0015(8) 
N7 0.0400(9) 0.0317(9) 0.0364(10) 0.0071(8) 0.0116(8) 0.0008(8) 
N8 0.0383(10) 0.0464(11) 0.0399(10) -0.0068(9) 0.0061(9) 0.0001(9) 
C1 0.0487(14) 0.0487(14) 0.059(2) 0.0036(13) -0.0058(13) -0.0002(12) 
C2 0.064(2) 0.070(2) 0.084(2) 0.004(2) -0.024(2) 0.008(2) 
C3 0.075(2) 0.076(2) 0.110(3) -0.002(2) -0.021(2) 0.031(2) 
C4 0.075(2) 0.0448(14) 0.091(2) -0.011(2) 0.002(2) 0.0140(14) 
C5 0.0475(13) 0.0335(12) 0.0560(15) 0.0000(11) 0.0098(12) 0.0012(11) 
C6 0.0446(12) 0.0448(13) 0.0401(13) -0.0007(11) 0.0094(11) -0.0042(11) 
C7 0.082(2) 0.0393(13) 0.059(2) -0.0056(13) 0.0183(14) -0.0088(13) 
C8 0.093(2) 0.056(2) 0.051(2) -0.0139(13) 0.0147(15) -0.0190(15) 
C9 0.075(2) 0.070(2) 0.0409(14) -0.0034(14) 0.0056(13) -0.0237(14) 
C10 0.0402(12) 0.0530(13) 0.0311(12) -0.0048(11) 0.0061(10) -0.0119(11) 
C11 0.0352(11) 0.077(2) 0.0328(12) 0.0020(13) 0.0062(10) -0.0037(12) 
C12 0.0357(12) 0.071(2) 0.0409(13) 0.0006(13) 0.0007(11) -0.0010(12) 
C13 0.0338(11) 0.0570(14) 0.0319(12) -0.0028(11) 0.0034(10) 0.0062(11) 
C14 0.0482(12) 0.0409(12) 0.0497(13) -0.0022(12) 0.0146(11) 0.0036(11) 
C15 0.0415(13) 0.067(2) 0.057(2) -0.0077(14) 0.0073(12) 0.0192(12) 
C16 0.0479(13) 0.0433(13) 0.066(2) -0.0075(13) 0.0080(13) 0.0099(12) 
C17 0.0392(12) 0.0335(11) 0.0390(12) 0.0014(10) 0.0012(10) 0.0076(10) 
C18 0.0404(12) 0.0385(12) 0.0331(12) 0.0039(10) -0.0047(10) 0.0025(10) 
C19 0.0567(14) 0.0345(12) 0.061(2) -0.0032(12) 0.0059(13) 0.0057(11) 
C20 0.072(2) 0.0375(13) 0.074(2) 0.0022(14) 0.000(2) -0.0112(13) 
C21 0.0474(13) 0.0436(13) 0.0437(14) 0.0044(11) -0.0042(11) -0.0112(11) 
C22 0.0485(13) 0.0456(13) 0.0451(13) -0.0052(12) 0.0110(11) -0.0036(11) 
C23 0.071(2) 0.076(2) 0.061(2) -0.008(2) -0.017(2) -0.005(2) 
C24 0.064(2) 0.057(2) 0.083(2) 0.004(2) 0.0118(15) -0.0224(14) 
C25 0.0425(13) 0.0618(15) 0.0490(14) 0.0112(13) 0.0121(11) 0.0073(12) 
C26 0.0553(14) 0.0621(15) 0.0458(14) 0.0153(13) 0.0072(12) 0.0225(13) 
C27 0.069(2) 0.0433(13) 0.058(2) 0.0077(13) 0.0068(14) 0.0203(12) 
C28 0.0536(14) 0.0435(13) 0.060(2) 0.0069(12) 0.0115(13) 0.0014(12) 
C29 0.0418(12) 0.0429(12) 0.0297(11) -0.0014(10) -0.0029(10) -0.0035(10) 
C30 0.0422(12) 0.0434(12) 0.0353(12) 0.0013(11) 0.0018(10) -0.0046(11) 
C31 0.0501(14) 0.0419(13) 0.065(2) 0.0095(13) 0.0101(13) -0.0043(11) 
C32 0.0435(13) 0.0572(15) 0.063(2) 0.0076(13) 0.0087(12) -0.0109(12) 
C33 0.0377(12) 0.0573(14) 0.0340(12) -0.0012(11) 0.0036(10) -0.0054(11) 
C34 0.0416(12) 0.0429(13) 0.0387(12) 0.0024(11) 0.0012(10) 0.0030(10) 
C35 0.0342(12) 0.069(2) 0.0439(13) 0.0013(13) 0.0030(11) 0.0040(12) 
C36 0.0365(12) 0.0579(14) 0.0419(13) 0.0070(12) 0.0038(10) -0.0038(11) 
C37 0.0423(12) 0.0509(13) 0.0389(12) 0.0189(11) 0.0074(11) 0.0063(11) 
C38 0.068(2) 0.057(2) 0.086(2) 0.0318(15) -0.003(2) 0.0020(14) 
C39 0.088(2) 0.057(2) 0.106(2) 0.038(2) -0.001(2) 0.007(2) 
C40 0.087(2) 0.0364(13) 0.093(2) 0.0099(15) 0.009(2) -0.0126(14) 
C41 0.0422(12) 0.0373(12) 0.0576(14) 0.0078(11) 0.0147(11) 0.0038(10) 
C42 0.0526(13) 0.0364(12) 0.0472(13) -0.0077(11) 0.0211(11) -0.0056(11) 
C43 0.0624(15) 0.0485(14) 0.074(2) -0.0125(13) 0.0182(14) -0.0219(12) 
C44 0.056(2) 0.086(2) 0.077(2) -0.021(2) 0.0101(15) -0.0327(14) 
C45 0.0494(15) 0.094(2) 0.066(2) -0.017(2) -0.0010(14) -0.010(2) 
C46 0.0540(14) 0.067(2) 0.0451(14) -0.0012(13) 0.0085(12) 0.0032(13) 
C47 0.082(2) 0.090(2) 0.106(2) 0.034(2) 0.051(2) 0.043(2) 
C48 0.070(2) 0.100(2) 0.060(2) 0.014(2) -0.018(2) 0.009(2) 
Cl1 0.0818(5) 0.0518(4) 0.0757(5) -0.0049(4) -0.0063(4) 0.0098(4) 
O11 0.220(3) 0.0554(13) 0.140(2) 0.0040(15) 0.043(2) 0.019(2) 
O12 0.117(2) 0.208(3) 0.143(3) -0.062(3) 0.058(2) -0.003(2) 
O13 0.172(3) 0.091(2) 0.152(3) -0.014(2) -0.090(2) 0.045(2) 
O14 0.069(2) 0.262(4) 0.147(3) -0.040(3) -0.014(2) -0.043(2) 
O12' 0.102(6) 0.068(5) 0.109(6) 0.056(4) 0.032(5) 0.025(5) 
O13' 0.136(7) 0.208(8) 0.101(6) -0.063(7) -0.020(6) -0.006(7) 
O14' 0.114(7) 0.189(9) 0.118(8) -0.005(7) 0.010(7) -0.003(7) 
Cl2 0.0512(3) 0.0539(4) 0.0749(4) -0.0081(3) 0.0061(3) -0.0025(3) 
O21 0.171(5) 0.039(3) 0.091(4) -0.004(3) -0.020(4) 0.013(4) 
O22 0.184(6) 0.085(5) 0.099(5) -0.009(4) -0.061(5) -0.013(5) 
O23 0.084(4) 0.101(4) 0.197(6) -0.064(4) 0.030(4) -0.013(4) 
O24 0.050(3) 0.047(3) 0.094(4) 0.008(3) 0.021(3) -0.014(2) 
O21' 0.122(2) 0.147(3) 0.049(2) 0.032(2) -0.006(2) -0.059(2) 
O22' 0.162(3) 0.071(2) 0.154(3) -0.042(2) 0.051(3) -0.005(2) 
O23' 0.097(2) 0.074(2) 0.112(3) 0.026(2) -0.019(2) 0.012(2) 
O24' 0.067(2) 0.150(3) 0.123(3) 0.008(3) 0.004(2) -0.033(2) 
Cl3 0.0540(4) 0.0518(3) 0.0583(4) -0.0057(3) -0.0080(3) 0.0050(3) 
O31 0.0624(13) 0.201(3) 0.100(2) 0.018(2) -0.0134(13) -0.025(2) 
O32 0.136(2) 0.093(2) 0.131(2) 0.0434(15) -0.015(2) 0.0381(14) 
O33 0.183(2) 0.0721(13) 0.101(2) -0.0329(13) 0.045(2) -0.0277(15) 
O34 0.0916(14) 0.120(2) 0.0657(13) -0.0097(13) 0.0182(12) 0.0097(13) 
 
_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 
Cu1 O1 1.909(2) . ? 
Cu1 N5 2.018(2) . ? 
Cu1 N6 2.039(2) . ? 
Cu1 N1 2.066(2) . ? 
Cu1 N2 2.208(2) . ? 
Cu2 O2 1.912(2) . ? 
Cu2 N4 2.011(2) . ? 
Cu2 N3 2.028(2) . ? 
Cu2 N8 2.113(2) . ? 
Cu2 N7 2.167(2) . ? 
N1 C1 1.339(3) . ? 
N1 C5 1.354(3) . ? 
N2 C10 1.343(3) . ? 
N2 C6 1.345(3) . ? 
N3 C17 1.341(3) . ? 
N3 C14 1.341(3) . ? 
N4 C22 1.332(3) . ? 
N4 C18 1.355(3) . ? 
N5 C25 1.331(3) . ? 
N5 C29 1.358(3) . ? 
N6 C30 1.342(3) . ? 
N6 C34 1.359(3) . ? 
N7 C41 1.342(3) . ? 
N7 C37 1.351(3) . ? 
N8 C46 1.347(3) . ? 
N8 C42 1.351(3) . ? 
C1 C2 1.385(4) . ? 
C1 C23 1.495(4) . ? 
C2 C3 1.359(4) . ? 
C3 C4 1.367(4) . ? 
C4 C5 1.381(3) . ? 
C5 C6 1.472(3) . ? 
C6 C7 1.398(3) . ? 
C7 C8 1.368(4) . ? 
C8 C9 1.369(4) . ? 
C9 C10 1.391(3) . ? 
C10 C11 1.493(3) . ? 
C11 C12 1.532(3) . ? 
C12 C13 1.504(3) . ? 
C13 C14 1.376(3) . ? 
C13 C15 1.394(3) . ? 
C15 C16 1.377(3) . ? 
C16 C17 1.380(3) . ? 
C17 C18 1.477(3) . ? 
C18 C19 1.375(3) . ? 
C19 C20 1.366(4) . ? 
C20 C21 1.375(4) . ? 
C21 C22 1.391(3) . ? 
C21 C24 1.493(4) . ? 
C25 C26 1.387(4) . ? 
C26 C27 1.370(4) . ? 
C26 C47 1.505(4) . ? 
C27 C28 1.362(4) . ? 
C28 C29 1.380(3) . ? 
C29 C30 1.460(3) . ? 
C30 C31 1.393(3) . ? 
C31 C32 1.364(3) . ? 
C32 C33 1.382(3) . ? 
C33 C34 1.383(3) . ? 
C33 C35 1.507(3) . ? 
C35 C36 1.545(3) . ? 
C36 C37 1.487(3) . ? 
C37 C38 1.388(3) . ? 
C38 C39 1.356(4) . ? 
C39 C40 1.382(4) . ? 
C40 C41 1.387(3) . ? 
C41 C42 1.481(3) . ? 
C42 C43 1.381(3) . ? 
C43 C44 1.362(4) . ? 
C44 C45 1.371(4) . ? 
C45 C46 1.394(4) . ? 
C46 C48 1.491(4) . ? 
Cl1 O13' 1.273(13) . ? 
Cl1 O12' 1.324(10) . ? 
Cl1 O12 1.380(4) . ? 
Cl1 O11 1.380(2) . ? 
Cl1 O13 1.396(3) . ? 
Cl1 O14 1.405(3) . ? 
Cl1 O14' 1.512(13) . ? 
Cl2 O23 1.294(7) . ? 
Cl2 O21 1.366(6) . ? 
Cl2 O22 1.393(8) . ? 
Cl2 O22' 1.413(4) . ? 
Cl2 O24 1.426(5) . ? 
Cl2 O24' 1.429(4) . ? 
Cl2 O21' 1.429(3) . ? 
Cl2 O23' 1.446(3) . ? 
Cl3 O32 1.393(2) . ? 
Cl3 O31 1.394(2) . ? 
Cl3 O33 1.409(2) . ? 
Cl3 O34 1.441(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 Cu1 N5 91.36(7) . . ? 
O1 Cu1 N6 168.03(7) . . ? 
N5 Cu1 N6 80.14(7) . . ? 
O1 Cu1 N1 92.39(7) . . ? 
N5 Cu1 N1 160.28(7) . . ? 
N6 Cu1 N1 92.91(7) . . ? 
O1 Cu1 N2 93.05(7) . . ? 
N5 Cu1 N2 121.66(7) . . ? 
N6 Cu1 N2 98.57(7) . . ? 
N1 Cu1 N2 77.46(7) . . ? 
O2 Cu2 N4 91.31(7) . . ? 
O2 Cu2 N3 170.11(7) . . ? 
N4 Cu2 N3 80.16(7) . . ? 
O2 Cu2 N8 95.30(7) . . ? 
N4 Cu2 N8 147.48(7) . . ? 
N3 Cu2 N8 89.39(7) . . ? 
O2 Cu2 N7 90.01(7) . . ? 
N4 Cu2 N7 134.69(7) . . ? 
N3 Cu2 N7 99.53(7) . . ? 
N8 Cu2 N7 77.23(7) . . ? 
C1 N1 C5 120.2(2) . . ? 
C1 N1 Cu1 122.9(2) . . ? 
C5 N1 Cu1 116.81(14) . . ? 
C10 N2 C6 119.7(2) . . ? 
C10 N2 Cu1 127.65(15) . . ? 
C6 N2 Cu1 112.41(13) . . ? 
C17 N3 C14 118.4(2) . . ? 
C17 N3 Cu2 114.94(14) . . ? 
C14 N3 Cu2 126.30(15) . . ? 
C22 N4 C18 118.3(2) . . ? 
C22 N4 Cu2 125.8(2) . . ? 
C18 N4 Cu2 115.62(14) . . ? 
C25 N5 C29 117.9(2) . . ? 
C25 N5 Cu1 127.1(2) . . ? 
C29 N5 Cu1 114.94(14) . . ? 
C30 N6 C34 118.4(2) . . ? 
C30 N6 Cu1 114.41(14) . . ? 
C34 N6 Cu1 127.21(14) . . ? 
C41 N7 C37 118.7(2) . . ? 
C41 N7 Cu2 114.04(14) . . ? 
C37 N7 Cu2 125.83(14) . . ? 
C46 N8 C42 119.9(2) . . ? 
C46 N8 Cu2 123.2(2) . . ? 
C42 N8 Cu2 115.47(14) . . ? 
N1 C1 C2 120.8(2) . . ? 
N1 C1 C23 117.3(2) . . ? 
C2 C1 C23 121.9(2) . . ? 
C3 C2 C1 119.3(3) . . ? 
C2 C3 C4 119.9(3) . . ? 
C3 C4 C5 119.8(3) . . ? 
N1 C5 C4 119.9(2) . . ? 
N1 C5 C6 116.4(2) . . ? 
C4 C5 C6 123.7(2) . . ? 
N2 C6 C7 121.3(2) . . ? 
N2 C6 C5 116.6(2) . . ? 
C7 C6 C5 121.9(2) . . ? 
C8 C7 C6 118.8(2) . . ? 
C7 C8 C9 119.5(2) . . ? 
C8 C9 C10 119.9(2) . . ? 
N2 C10 C9 120.6(2) . . ? 
N2 C10 C11 118.1(2) . . ? 
C9 C10 C11 121.2(2) . . ? 
C10 C11 C12 115.4(2) . . ? 
C13 C12 C11 114.6(2) . . ? 
C14 C13 C15 116.4(2) . . ? 
C14 C13 C12 122.4(2) . . ? 
C15 C13 C12 121.1(2) . . ? 
N3 C14 C13 124.4(2) . . ? 
C16 C15 C13 119.7(2) . . ? 
C15 C16 C17 120.0(2) . . ? 
N3 C17 C16 120.8(2) . . ? 
N3 C17 C18 115.2(2) . . ? 
C16 C17 C18 123.9(2) . . ? 
N4 C18 C19 121.1(2) . . ? 
N4 C18 C17 114.0(2) . . ? 
C19 C18 C17 124.8(2) . . ? 
C20 C19 C18 119.2(2) . . ? 
C19 C20 C21 121.4(2) . . ? 
C20 C21 C22 115.9(2) . . ? 
C20 C21 C24 124.0(2) . . ? 
C22 C21 C24 120.1(2) . . ? 
N4 C22 C21 124.1(2) . . ? 
N5 C25 C26 124.1(2) . . ? 
C27 C26 C25 116.7(2) . . ? 
C27 C26 C47 123.4(2) . . ? 
C25 C26 C47 119.9(2) . . ? 
C28 C27 C26 120.7(2) . . ? 
C27 C28 C29 119.7(2) . . ? 
N5 C29 C28 120.9(2) . . ? 
N5 C29 C30 114.8(2) . . ? 
C28 C29 C30 124.3(2) . . ? 
N6 C30 C31 121.1(2) . . ? 
N6 C30 C29 115.7(2) . . ? 
C31 C30 C29 123.2(2) . . ? 
C32 C31 C30 119.6(2) . . ? 
C31 C32 C33 120.5(2) . . ? 
C32 C33 C34 117.3(2) . . ? 
C32 C33 C35 121.0(2) . . ? 
C34 C33 C35 121.8(2) . . ? 
N6 C34 C33 123.1(2) . . ? 
C33 C35 C36 111.6(2) . . ? 
C37 C36 C35 113.1(2) . . ? 
N7 C37 C38 121.5(2) . . ? 
N7 C37 C36 118.8(2) . . ? 
C38 C37 C36 119.6(2) . . ? 
C39 C38 C37 119.0(3) . . ? 
C38 C39 C40 120.6(3) . . ? 
C39 C40 C41 117.9(2) . . ? 
N7 C41 C40 122.2(2) . . ? 
N7 C41 C42 115.9(2) . . ? 
C40 C41 C42 121.8(2) . . ? 
N8 C42 C43 120.9(2) . . ? 
N8 C42 C41 115.6(2) . . ? 
C43 C42 C41 123.5(2) . . ? 
C44 C43 C42 120.0(2) . . ? 
C43 C44 C45 119.0(3) . . ? 
C44 C45 C46 120.2(2) . . ? 
N8 C46 C45 120.0(2) . . ? 
N8 C46 C48 116.1(2) . . ? 
C45 C46 C48 123.9(2) . . ? 
O13' Cl1 O12' 127.4(8) . . ? 
O13' Cl1 O11 118.5(7) . . ? 
O12' Cl1 O11 111.0(4) . . ? 
O12 Cl1 O11 116.0(2) . . ? 
O12 Cl1 O13 109.1(2) . . ? 
O11 Cl1 O13 112.2(2) . . ? 
O12 Cl1 O14 106.7(2) . . ? 
O11 Cl1 O14 103.5(2) . . ? 
O13 Cl1 O14 108.8(2) . . ? 
O13' Cl1 O14' 99.8(8) . . ? 
O12' Cl1 O14' 103.5(7) . . ? 
O11 Cl1 O14' 82.3(6) . . ? 
O23 Cl2 O21 120.1(5) . . ? 
O23 Cl2 O22 115.3(5) . . ? 
O21 Cl2 O22 103.5(4) . . ? 
O23 Cl2 O24 99.2(4) . . ? 
O21 Cl2 O24 111.5(4) . . ? 
O22 Cl2 O24 106.7(4) . . ? 
O22' Cl2 O24' 114.2(2) . . ? 
O22' Cl2 O21' 108.9(2) . . ? 
O24' Cl2 O21' 114.0(2) . . ? 
O22' Cl2 O23' 103.0(2) . . ? 
O24' Cl2 O23' 111.9(2) . . ? 
O21' Cl2 O23' 103.7(2) . . ? 
O32 Cl3 O31 111.4(2) . . ? 
O32 Cl3 O33 109.2(2) . . ? 
O31 Cl3 O33 106.9(2) . . ? 
O32 Cl3 O34 109.9(2) . . ? 
O31 Cl3 O34 110.16(14) . . ? 
O33 Cl3 O34 109.25(15) . . ? 
 
_refine_diff_density_max    0.393 
_refine_diff_density_min   -0.305 
_refine_diff_density_rms    0.070