# Electronic supplementary material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009


data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Zhiquan Pan'
_publ_contact_author_email       ZHIQPAN@163.COM

_publ_section_title              
;
Hexamine Copper(II) Coordination Polymers: Synthesis,
Structure and Magnetic Properties
;
loop_
_publ_author_name
'Zhiquan Pan'
'Zheng-Wu Bai'
'Lei Chen'
'Rong Chen'
'Xue-Lei Hu'
'Qi-Mao Huang'
'Zheng-He Peng'
;
Y.Song
;
'Hong Zhou'

# Attachment 'complex 1.cif'

data_050613cm
_database_code_depnum_ccdc_archive 'CCDC 697699'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'4(C31 H76 Br2 Cu4 N12 O3), 12(Cl O4), 9(H4 O2), 4(Br)'
_chemical_formula_sum            'C124 H324 Br12 Cl12 Cu16 N48 O70'
_chemical_formula_weight         6009.27

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'
Br Br -0.2901 2.4595 '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 '
_symmetry_space_group_name_Hall  '-P 2yn'

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

_cell_length_a                   14.1105(8)
_cell_length_b                   18.4033(10)
_cell_length_c                   21.9209(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.0580(10)
_cell_angle_gamma                90.00
_cell_volume                     5604.9(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4759
_cell_measurement_theta_min      2.01
_cell_measurement_theta_max      25.47

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3052
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.41
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            30289
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         26.00
_reflns_number_total             11007
_reflns_number_gt                7772
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.06P)²+1.85P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         11007
_refine_ls_number_parameters     640
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1289
_refine_ls_wR_factor_gt          0.1234
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 1.03743(5) 0.73530(3) 0.44748(3) 0.04821(16) Uani 1 1 d . . .
Br2 Br 0.53290(5) 0.72220(3) 0.61778(3) 0.04851(16) Uani 1 1 d . . .
Br3 Br 0.75518(4) 0.53746(3) 0.50927(3) 0.03534(12) Uani 1 1 d . . .
C1 C 0.8392(5) 0.6065(3) 0.3548(3) 0.0447(14) Uani 1 1 d . . .
H1A H 0.8039 0.5610 0.3489 0.054 Uiso 1 1 calc R . .
H1B H 0.9034 0.5958 0.3769 0.054 Uiso 1 1 calc R . .
C2 C 0.8465(5) 0.6383(3) 0.2920(3) 0.0456(15) Uani 1 1 d . . .
H2A H 0.8790 0.6036 0.2695 0.055 Uiso 1 1 calc R . .
H2B H 0.7820 0.6452 0.2688 0.055 Uiso 1 1 calc R . .
C3 C 0.8994(4) 0.7097(3) 0.2948(3) 0.0323(12) Uani 1 1 d . . .
H3A H 0.9617 0.7035 0.3212 0.039 Uiso 1 1 calc R . .
H3B H 0.9110 0.7211 0.2535 0.039 Uiso 1 1 calc R . .
C4 C 0.9143(4) 0.8381(3) 0.3124(3) 0.0418(14) Uani 1 1 d . . .
H4A H 0.9779 0.8276 0.3355 0.050 Uiso 1 1 calc R . .
H4B H 0.9205 0.8428 0.2692 0.050 Uiso 1 1 calc R . .
C5 C 0.8834(5) 0.9094(3) 0.3336(3) 0.0507(17) Uani 1 1 d . . .
H5A H 0.8176 0.9185 0.3135 0.061 Uiso 1 1 calc R . .
H5B H 0.9235 0.9471 0.3205 0.061 Uiso 1 1 calc R . .
C6 C 0.8890(4) 0.9144(3) 0.4031(3) 0.0387(13) Uani 1 1 d . . .
H6A H 0.9546 0.9052 0.4234 0.046 Uiso 1 1 calc R . .
H6B H 0.8719 0.9632 0.4139 0.046 Uiso 1 1 calc R . .
C7 C 1.0669(4) 0.8816(3) 0.5769(3) 0.0362(12) Uani 1 1 d . . .
H7A H 1.0542 0.9307 0.5896 0.043 Uiso 1 1 calc R . .
H7B H 1.0646 0.8817 0.5324 0.043 Uiso 1 1 calc R . .
C8 C 1.1665(4) 0.8580(3) 0.6093(3) 0.0442(15) Uani 1 1 d . . .
H8A H 1.2137 0.8927 0.5999 0.053 Uiso 1 1 calc R . .
H8B H 1.1684 0.8586 0.6537 0.053 Uiso 1 1 calc R . .
C9 C 1.1939(4) 0.7829(3) 0.5901(3) 0.0350(12) Uani 1 1 d . . .
H9A H 1.1875 0.7825 0.5453 0.042 Uiso 1 1 calc R . .
H9B H 1.2616 0.7756 0.6068 0.042 Uiso 1 1 calc R . .
C10 C 1.1857(4) 0.6543(3) 0.5848(3) 0.0349(12) Uani 1 1 d . . .
H10A H 1.2533 0.6536 0.6033 0.042 Uiso 1 1 calc R . .
H10B H 1.1820 0.6595 0.5404 0.042 Uiso 1 1 calc R . .
C11 C 1.1424(4) 0.5817(3) 0.5970(3) 0.0371(13) Uani 1 1 d . . .
H11A H 1.1375 0.5788 0.6405 0.044 Uiso 1 1 calc R . .
H11B H 1.1854 0.5433 0.5884 0.044 Uiso 1 1 calc R . .
C12 C 1.0439(5) 0.5692(3) 0.5584(3) 0.0493(15) Uani 1 1 d . . .
H12A H 1.0479 0.5735 0.5148 0.059 Uiso 1 1 calc R . .
H12B H 1.0226 0.5203 0.5656 0.059 Uiso 1 1 calc R . .
C13 C 0.6941(4) 0.8701(3) 0.7062(3) 0.0375(13) Uani 1 1 d . . .
H13A H 0.6289 0.8714 0.6832 0.045 Uiso 1 1 calc R . .
H13B H 0.7197 0.9191 0.7082 0.045 Uiso 1 1 calc R . .
C14 C 0.6934(5) 0.8421(3) 0.7714(3) 0.0431(14) Uani 1 1 d . . .
H14A H 0.6565 0.8754 0.7923 0.052 Uiso 1 1 calc R . .
H14B H 0.7589 0.8419 0.7941 0.052 Uiso 1 1 calc R . .
C15 C 0.6513(4) 0.7662(3) 0.7732(3) 0.0398(13) Uani 1 1 d . . .
H15A H 0.6400 0.7573 0.8150 0.048 Uiso 1 1 calc R . .
H15B H 0.5892 0.7656 0.7461 0.048 Uiso 1 1 calc R . .
C16 C 0.6535(4) 0.6373(3) 0.7646(3) 0.0351(12) Uani 1 1 d . . .
H16A H 0.5887 0.6431 0.7417 0.042 Uiso 1 1 calc R . .
H16B H 0.6489 0.6341 0.8081 0.042 Uiso 1 1 calc R . .
C17 C 0.6927(4) 0.5658(3) 0.7455(2) 0.0354(12) Uani 1 1 d . . .
H17A H 0.6583 0.5262 0.7612 0.042 Uiso 1 1 calc R . .
H17B H 0.7600 0.5619 0.7644 0.042 Uiso 1 1 calc R . .
C18 C 0.6838(4) 0.5579(3) 0.6757(2) 0.0327(11) Uani 1 1 d . . .
H18A H 0.7041 0.5096 0.6659 0.039 Uiso 1 1 calc R . .
H18B H 0.6170 0.5639 0.6563 0.039 Uiso 1 1 calc R . .
C19 C 0.4800(4) 0.6016(3) 0.4745(3) 0.0450(14) Uani 1 1 d . . .
H19A H 0.4800 0.5916 0.5180 0.054 Uiso 1 1 calc R . .
H19B H 0.4891 0.5559 0.4542 0.054 Uiso 1 1 calc R . .
C20 C 0.3840(4) 0.6344(3) 0.4456(3) 0.0450(15) Uani 1 1 d . . .
H20A H 0.3847 0.6435 0.4021 0.054 Uiso 1 1 calc R . .
H20B H 0.3337 0.5991 0.4480 0.054 Uiso 1 1 calc R . .
C21 C 0.3595(4) 0.7027(3) 0.4745(3) 0.0371(13) Uani 1 1 d . . .
H21A H 0.3657 0.6944 0.5187 0.045 Uiso 1 1 calc R . .
H21B H 0.2923 0.7133 0.4589 0.045 Uiso 1 1 calc R . .
C22 C 0.3766(4) 0.8296(3) 0.4980(3) 0.0365(12) Uani 1 1 d . . .
H22A H 0.3775 0.8143 0.5404 0.044 Uiso 1 1 calc R . .
H22B H 0.3097 0.8357 0.4790 0.044 Uiso 1 1 calc R . .
C23 C 0.4248(4) 0.9028(3) 0.4996(3) 0.0407(14) Uani 1 1 d . . .
H23A H 0.3851 0.9384 0.5160 0.049 Uiso 1 1 calc R . .
H23B H 0.4291 0.9171 0.4576 0.049 Uiso 1 1 calc R . .
C24 C 0.5244(5) 0.9039(3) 0.5383(3) 0.0445(15) Uani 1 1 d . . .
H24A H 0.5483 0.9534 0.5419 0.053 Uiso 1 1 calc R . .
H24B H 0.5215 0.8862 0.5796 0.053 Uiso 1 1 calc R . .
C25 C 0.7516(4) 0.7850(3) 0.2826(2) 0.0316(11) Uani 1 1 d . . .
H25A H 0.7230 0.8260 0.3005 0.038 Uiso 1 1 calc R . .
H25B H 0.7129 0.7425 0.2872 0.038 Uiso 1 1 calc R . .
C26 C 0.7475(4) 0.7995(3) 0.2133(2) 0.0294(11) Uani 1 1 d . . .
H26A H 0.7650 0.8496 0.2072 0.035 Uiso 1 1 calc R . .
H26B H 0.7932 0.7684 0.1976 0.035 Uiso 1 1 calc R . .
C27 C 0.6467(4) 0.7850(3) 0.1777(2) 0.0326(12) Uani 1 1 d . . .
H27A H 0.6234 0.7398 0.1924 0.039 Uiso 1 1 calc R . .
H27B H 0.6044 0.8236 0.1867 0.039 Uiso 1 1 calc R . .
C28 C 0.8083(4) 0.7026(3) 0.7932(3) 0.0357(12) Uani 1 1 d . . .
H28A H 0.8421 0.7464 0.7849 0.043 Uiso 1 1 calc R . .
H28B H 0.8427 0.6616 0.7797 0.043 Uiso 1 1 calc R . .
C29 C 0.8119(4) 0.6965(3) 0.8632(2) 0.0307(12) Uani 1 1 d . . .
H29A H 0.7664 0.7304 0.8759 0.037 Uiso 1 1 calc R . .
H29B H 0.7935 0.6478 0.8733 0.037 Uiso 1 1 calc R . .
C30 C 0.9131(4) 0.7132(3) 0.8982(3) 0.0361(12) Uani 1 1 d . . .
H30A H 0.9541 0.6716 0.8949 0.043 Uiso 1 1 calc R . .
H30B H 0.9389 0.7540 0.8783 0.043 Uiso 1 1 calc R . .
C31 C 0.7924(5) 0.7377(3) 0.5311(4) 0.0502(17) Uani 1 1 d . . .
Cl2 Cl 0.02199(11) 0.87281(9) 0.77962(8) 0.0478(4) Uani 1 1 d . . .
Cl3 Cl 0.58371(10) 0.96430(8) 0.33841(7) 0.0432(3) Uani 1 1 d . . .
Cl11 Cl 0.81595(11) 0.98522(8) 0.57669(8) 0.0439(3) Uani 1 1 d . . .
Cu1 Cu 0.84047(5) 0.75663(3) 0.41082(3) 0.03085(15) Uani 1 1 d . . .
Cu2 Cu 0.99606(5) 0.72807(4) 0.56717(4) 0.03890(17) Uani 1 1 d . . .
Cu3 Cu 0.72262(5) 0.71753(4) 0.66178(3) 0.03436(15) Uani 1 1 d . . .
Cu4 Cu 0.56293(5) 0.75163(4) 0.50276(4) 0.04022(17) Uani 1 1 d . . .
N1 N 0.7907(4) 0.6557(3) 0.3926(2) 0.0384(11) Uani 1 1 d . . .
H1C H 0.7905 0.6336 0.4292 0.046 Uiso 1 1 calc R . .
H1D H 0.7289 0.6595 0.3737 0.046 Uiso 1 1 calc R . .
N2 N 0.8506(3) 0.7731(2) 0.3181(2) 0.0322(10) Uani 1 1 d . . .
N3 N 0.8244(3) 0.8621(2) 0.4256(2) 0.0332(10) Uani 1 1 d . . .
H3C H 0.7637 0.8741 0.4085 0.040 Uiso 1 1 calc R . .
H3D H 0.8298 0.8685 0.4667 0.040 Uiso 1 1 calc R . .
N4 N 0.9925(3) 0.8320(2) 0.5925(2) 0.0363(11) Uani 1 1 d . . .
H4C H 0.9347 0.8501 0.5755 0.044 Uiso 1 1 calc R . .
H4D H 0.9959 0.8332 0.6339 0.044 Uiso 1 1 calc R . .
N5 N 1.1405(3) 0.7199(2) 0.6082(2) 0.0303(9) Uani 1 1 d . . .
N6 N 0.9724(3) 0.6223(2) 0.5740(2) 0.0361(11) Uani 1 1 d . . .
H6C H 0.9650 0.6135 0.6133 0.043 Uiso 1 1 calc R . .
H6D H 0.9157 0.6124 0.5496 0.043 Uiso 1 1 calc R . .
N7 N 0.7539(4) 0.8222(2) 0.6743(2) 0.0397(11) Uani 1 1 d . . .
H7C H 0.8146 0.8249 0.6954 0.048 Uiso 1 1 calc R . .
H7D H 0.7544 0.8415 0.6367 0.048 Uiso 1 1 calc R . .
N8 N 0.7098(3) 0.7045(3) 0.7552(2) 0.0360(10) Uani 1 1 d . . .
N9 N 0.7434(3) 0.6125(2) 0.6507(2) 0.0321(10) Uani 1 1 d . . .
H9C H 0.7371 0.6044 0.6097 0.039 Uiso 1 1 calc R . .
H9D H 0.8051 0.6030 0.6672 0.039 Uiso 1 1 calc R . .
N10 N 0.5604(3) 0.6517(2) 0.4687(2) 0.0354(11) Uani 1 1 d . . .
H10C H 0.5627 0.6556 0.4281 0.043 Uiso 1 1 calc R . .
H10D H 0.6152 0.6297 0.4866 0.043 Uiso 1 1 calc R . .
N11 N 0.4175(3) 0.7694(2) 0.4650(2) 0.0295(9) Uani 1 1 d . . .
N12 N 0.5914(3) 0.8576(2) 0.5098(2) 0.0375(11) Uani 1 1 d . . .
H12C H 0.6509 0.8631 0.5320 0.045 Uiso 1 1 calc R . .
H12D H 0.5927 0.8748 0.4715 0.045 Uiso 1 1 calc R . .
O1 O 0.8651(3) 0.7394(2) 0.50549(18) 0.0366(9) Uani 1 1 d . . .
O2 O 0.8008(3) 0.7295(2) 0.58764(19) 0.0414(9) Uani 1 1 d . . .
O3 O 0.7119(3) 0.7435(2) 0.49720(19) 0.0417(10) Uani 1 1 d . . .
O4 O 1.1121(3) 0.57596(19) 0.39211(16) 0.0328(8) Uani 1 1 d . . .
H4H H 1.0928 0.6156 0.4056 0.039 Uiso 1 1 d R . .
H4F H 1.1632 0.5622 0.4157 0.049 Uiso 1 1 d R . .
O5 O 0.4362(3) 0.9559(2) 0.1867(2) 0.0454(10) Uani 1 1 d . . .
H5D H 0.4560 0.9874 0.1636 0.068 Uiso 1 1 d R . .
H5F H 0.4706 0.9575 0.2226 0.054 Uiso 1 1 d R . .
O6 O 0.1044(5) 0.0598(4) 0.8461(3) 0.0393(19) Uani 0.50 1 d P . .
H6H H 0.0550 0.0327 0.8390 0.047 Uiso 0.50 1 d PR . .
H6E H 0.0864 0.1034 0.8379 0.047 Uiso 0.50 1 d PR . .
O11 O 0.8962(3) 0.9874(2) 0.6245(2) 0.0550(12) Uani 1 1 d . . .
O12 O 0.7339(3) 1.0075(2) 0.6029(2) 0.0528(12) Uani 1 1 d . . .
O13 O 0.8241(3) 1.0272(2) 0.5258(2) 0.0551(12) Uani 1 1 d . . .
O14 O 0.7997(3) 0.9106(2) 0.5573(2) 0.0507(11) Uani 1 1 d . . .
O21 O 0.0721(3) 0.8298(3) 0.8279(2) 0.0564(12) Uani 1 1 d . . .
O22 O 0.0869(3) 0.9095(3) 0.7507(2) 0.0580(12) Uani 1 1 d . . .
O23 O -0.0267(3) 0.8236(3) 0.7341(2) 0.0561(12) Uani 1 1 d . . .
O24 O -0.0463(3) 0.9127(2) 0.8016(2) 0.0562(12) Uani 1 1 d . . .
O31 O 0.6174(4) 0.9150(3) 0.3823(2) 0.0571(12) Uani 1 1 d . . .
O32 O 0.6136(3) 0.9493(3) 0.2830(2) 0.0559(12) Uani 1 1 d . . .
O33 O 0.4859(4) 0.9671(3) 0.3319(2) 0.0588(12) Uani 1 1 d . . .
O34 O 0.6186(4) 1.0307(3) 0.3546(2) 0.0588(13) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Cu1 2.7828(7) . ?
Br1 Cu2 2.7889(8) . ?
Br2 Cu3 2.6838(7) . ?
Br2 Cu4 2.6839(8) . ?
C1 N1 1.475(6) . ?
C1 C2 1.516(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.506(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.490(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.483(9) . ?
C4 N2 1.514(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.515(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N3 1.470(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N4 1.475(5) . ?
C7 C8 1.523(8) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.514(8) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N5 1.475(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N5 1.498(5) . ?
C10 C11 1.512(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.514(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N6 1.487(6) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 N7 1.478(5) . ?
C13 C14 1.520(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C15 1.522(8) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N8 1.497(5) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N8 1.504(5) . ?
C16 C17 1.513(8) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.522(7) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 N9 1.475(5) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N10 1.485(6) . ?
C19 C20 1.517(8) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.475(6) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 N11 1.510(6) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 N11 1.493(7) . ?
C22 C23 1.507(8) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.509(8) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 N12 1.489(7) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 N2 1.492(7) . ?
C25 C26 1.533(7) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.521(7) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 N5 1.512(7) 4_575 ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 N8 1.490(7) . ?
C28 C29 1.531(8) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.530(7) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N11 1.489(7) 4_676 ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C31 O2 1.234(8) . ?
C31 O3 1.249(8) . ?
C31 O1 1.252(8) . ?
Cl2 O24 1.364(5) . ?
Cl2 O22 1.379(5) . ?
Cl2 O21 1.408(5) . ?
Cl2 O23 1.431(5) . ?
Cl3 O34 1.342(5) . ?
Cl3 O31 1.348(5) . ?
Cl3 O33 1.364(5) . ?
Cl3 O32 1.381(5) . ?
Cl11 O13 1.377(5) . ?
Cl11 O11 1.402(5) . ?
Cl11 O12 1.438(4) . ?
Cl11 O14 1.444(5) . ?
Cu1 N3 1.987(4) . ?
Cu1 N1 2.001(5) . ?
Cu1 O1 2.068(4) . ?
Cu1 N2 2.085(4) . ?
Cu2 N6 1.984(4) . ?
Cu2 N4 1.995(5) . ?
Cu2 N5 2.085(4) . ?
Cu2 O1 2.101(4) . ?
Cu3 N9 1.977(4) . ?
Cu3 N7 1.985(5) . ?
Cu3 N8 2.101(5) . ?
Cu3 O2 2.129(5) . ?
Cu4 N10 1.983(4) . ?
Cu4 N12 1.992(4) . ?
Cu4 N11 2.100(4) . ?
Cu4 O3 2.132(4) . ?
N1 H1C 0.9000 . ?
N1 H1D 0.9000 . ?
N3 H3C 0.9000 . ?
N3 H3D 0.9000 . ?
N4 H4C 0.9000 . ?
N4 H4D 0.9000 . ?
N5 C27 1.512(7) 4_676 ?
N6 H6C 0.9000 . ?
N6 H6D 0.9000 . ?
N7 H7C 0.9000 . ?
N7 H7D 0.9000 . ?
N9 H9C 0.9000 . ?
N9 H9D 0.9000 . ?
N10 H10C 0.9000 . ?
N10 H10D 0.9000 . ?
N11 C30 1.489(7) 4_575 ?
N12 H12C 0.9000 . ?
N12 H12D 0.9000 . ?
O4 H4H 0.8499 . ?
O4 H4F 0.8500 . ?
O5 H5D 0.8499 . ?
O5 H5F 0.8501 . ?
O6 H6H 0.8500 . ?
O6 H6E 0.8502 . ?

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
Cu1 Br1 Cu2 85.17(2) . . ?
Cu3 Br2 Cu4 91.88(2) . . ?
N1 C1 C2 112.6(4) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C1 114.3(5) . . ?
C3 C2 H2A 108.7 . . ?
C1 C2 H2A 108.7 . . ?
C3 C2 H2B 108.7 . . ?
C1 C2 H2B 108.7 . . ?
H2A C2 H2B 107.6 . . ?
N2 C3 C2 116.2(4) . . ?
N2 C3 H3A 108.2 . . ?
C2 C3 H3A 108.2 . . ?
N2 C3 H3B 108.2 . . ?
C2 C3 H3B 108.2 . . ?
H3A C3 H3B 107.4 . . ?
C5 C4 N2 117.5(4) . . ?
C5 C4 H4A 107.9 . . ?
N2 C4 H4A 107.9 . . ?
C5 C4 H4B 107.9 . . ?
N2 C4 H4B 107.9 . . ?
H4A C4 H4B 107.2 . . ?
C4 C5 C6 113.7(5) . . ?
C4 C5 H5A 108.8 . . ?
C6 C5 H5A 108.8 . . ?
C4 C5 H5B 108.8 . . ?
C6 C5 H5B 108.8 . . ?
H5A C5 H5B 107.7 . . ?
N3 C6 C5 111.8(4) . . ?
N3 C6 H6A 109.3 . . ?
C5 C6 H6A 109.3 . . ?
N3 C6 H6B 109.3 . . ?
C5 C6 H6B 109.3 . . ?
H6A C6 H6B 107.9 . . ?
N4 C7 C8 110.6(4) . . ?
N4 C7 H7A 109.5 . . ?
C8 C7 H7A 109.5 . . ?
N4 C7 H7B 109.5 . . ?
C8 C7 H7B 109.5 . . ?
H7A C7 H7B 108.1 . . ?
C9 C8 C7 113.0(5) . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8B 109.0 . . ?
C7 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
N5 C9 C8 118.4(4) . . ?
N5 C9 H9A 107.7 . . ?
C8 C9 H9A 107.7 . . ?
N5 C9 H9B 107.7 . . ?
C8 C9 H9B 107.7 . . ?
H9A C9 H9B 107.1 . . ?
N5 C10 C11 116.2(4) . . ?
N5 C10 H10A 108.2 . . ?
C11 C10 H10A 108.2 . . ?
N5 C10 H10B 108.2 . . ?
C11 C10 H10B 108.2 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 C12 113.3(5) . . ?
C10 C11 H11A 108.9 . . ?
C12 C11 H11A 108.9 . . ?
C10 C11 H11B 108.9 . . ?
C12 C11 H11B 108.9 . . ?
H11A C11 H11B 107.7 . . ?
N6 C12 C11 111.4(4) . . ?
N6 C12 H12A 109.3 . . ?
C11 C12 H12A 109.3 . . ?
N6 C12 H12B 109.3 . . ?
C11 C12 H12B 109.3 . . ?
H12A C12 H12B 108.0 . . ?
N7 C13 C14 109.9(4) . . ?
N7 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
N7 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C13 C14 C15 113.7(5) . . ?
C13 C14 H14A 108.8 . . ?
C15 C14 H14A 108.8 . . ?
C13 C14 H14B 108.8 . . ?
C15 C14 H14B 108.8 . . ?
H14A C14 H14B 107.7 . . ?
N8 C15 C14 117.0(4) . . ?
N8 C15 H15A 108.1 . . ?
C14 C15 H15A 108.1 . . ?
N8 C15 H15B 108.1 . . ?
C14 C15 H15B 108.1 . . ?
H15A C15 H15B 107.3 . . ?
N8 C16 C17 116.7(4) . . ?
N8 C16 H16A 108.1 . . ?
C17 C16 H16A 108.1 . . ?
N8 C16 H16B 108.1 . . ?
C17 C16 H16B 108.1 . . ?
H16A C16 H16B 107.3 . . ?
C16 C17 C18 113.0(5) . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
N9 C18 C17 110.8(4) . . ?
N9 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
N9 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
N10 C19 C20 110.9(4) . . ?
N10 C19 H19A 109.5 . . ?
C20 C19 H19A 109.5 . . ?
N10 C19 H19B 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 108.1 . . ?
C21 C20 C19 114.8(5) . . ?
C21 C20 H20A 108.6 . . ?
C19 C20 H20A 108.6 . . ?
C21 C20 H20B 108.6 . . ?
C19 C20 H20B 108.6 . . ?
H20A C20 H20B 107.5 . . ?
C20 C21 N11 117.4(4) . . ?
C20 C21 H21A 108.0 . . ?
N11 C21 H21A 108.0 . . ?
C20 C21 H21B 108.0 . . ?
N11 C21 H21B 108.0 . . ?
H21A C21 H21B 107.2 . . ?
N11 C22 C23 117.6(5) . . ?
N11 C22 H22A 107.9 . . ?
C23 C22 H22A 107.9 . . ?
N11 C22 H22B 107.9 . . ?
C23 C22 H22B 107.9 . . ?
H22A C22 H22B 107.2 . . ?
C22 C23 C24 113.4(5) . . ?
C22 C23 H23A 108.9 . . ?
C24 C23 H23A 108.9 . . ?
C22 C23 H23B 108.9 . . ?
C24 C23 H23B 108.9 . . ?
H23A C23 H23B 107.7 . . ?
N12 C24 C23 110.7(5) . . ?
N12 C24 H24A 109.5 . . ?
C23 C24 H24A 109.5 . . ?
N12 C24 H24B 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 108.1 . . ?
N2 C25 C26 114.4(4) . . ?
N2 C25 H25A 108.7 . . ?
C26 C25 H25A 108.7 . . ?
N2 C25 H25B 108.7 . . ?
C26 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C27 C26 C25 110.4(4) . . ?
C27 C26 H26A 109.6 . . ?
C25 C26 H26A 109.6 . . ?
C27 C26 H26B 109.6 . . ?
C25 C26 H26B 109.6 . . ?
H26A C26 H26B 108.1 . . ?
N5 C27 C26 114.3(4) 4_575 . ?
N5 C27 H27A 108.7 4_575 . ?
C26 C27 H27A 108.7 . . ?
N5 C27 H27B 108.7 4_575 . ?
C26 C27 H27B 108.7 . . ?
H27A C27 H27B 107.6 . . ?
N8 C28 C29 115.2(4) . . ?
N8 C28 H28A 108.5 . . ?
C29 C28 H28A 108.5 . . ?
N8 C28 H28B 108.5 . . ?
C29 C28 H28B 108.5 . . ?
H28A C28 H28B 107.5 . . ?
C30 C29 C28 110.7(4) . . ?
C30 C29 H29A 109.5 . . ?
C28 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 108.1 . . ?
N11 C30 C29 114.3(4) 4_676 . ?
N11 C30 H30A 108.7 4_676 . ?
C29 C30 H30A 108.7 . . ?
N11 C30 H30B 108.7 4_676 . ?
C29 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
O2 C31 O3 121.7(7) . . ?
O2 C31 O1 120.8(6) . . ?
O3 C31 O1 117.5(7) . . ?
O24 Cl2 O22 117.8(3) . . ?
O24 Cl2 O21 109.3(3) . . ?
O22 Cl2 O21 109.5(3) . . ?
O24 Cl2 O23 107.7(3) . . ?
O22 Cl2 O23 105.4(3) . . ?
O21 Cl2 O23 106.5(3) . . ?
O34 Cl3 O31 110.9(3) . . ?
O34 Cl3 O33 108.1(3) . . ?
O31 Cl3 O33 108.9(3) . . ?
O34 Cl3 O32 105.1(3) . . ?
O31 Cl3 O32 111.7(3) . . ?
O33 Cl3 O32 112.0(3) . . ?
O13 Cl11 O11 114.7(3) . . ?
O13 Cl11 O12 110.5(3) . . ?
O11 Cl11 O12 107.1(3) . . ?
O13 Cl11 O14 109.1(3) . . ?
O11 Cl11 O14 108.2(3) . . ?
O12 Cl11 O14 106.9(3) . . ?
N3 Cu1 N1 153.2(2) . . ?
N3 Cu1 O1 89.47(17) . . ?
N1 Cu1 O1 92.84(17) . . ?
N3 Cu1 N2 92.63(18) . . ?
N1 Cu1 N2 91.24(18) . . ?
O1 Cu1 N2 166.59(18) . . ?
N3 Cu1 Br1 103.16(14) . . ?
N1 Cu1 Br1 102.98(15) . . ?
O1 Cu1 Br1 72.79(11) . . ?
N2 Cu1 Br1 93.84(13) . . ?
N6 Cu2 N4 155.0(2) . . ?
N6 Cu2 N5 93.51(18) . . ?
N4 Cu2 N5 91.09(18) . . ?
N6 Cu2 O1 90.29(17) . . ?
N4 Cu2 O1 91.28(17) . . ?
N5 Cu2 O1 165.65(16) . . ?
N6 Cu2 Br1 100.55(15) . . ?
N4 Cu2 Br1 103.65(15) . . ?
N5 Cu2 Br1 93.45(12) . . ?
O1 Cu2 Br1 72.23(11) . . ?
N9 Cu3 N7 158.8(2) . . ?
N9 Cu3 N8 92.74(18) . . ?
N7 Cu3 N8 91.75(19) . . ?
N9 Cu3 O2 84.27(17) . . ?
N7 Cu3 O2 82.69(18) . . ?
N8 Cu3 O2 154.19(17) . . ?
N9 Cu3 Br2 98.46(13) . . ?
N7 Cu3 Br2 101.69(15) . . ?
N8 Cu3 Br2 95.97(13) . . ?
O2 Cu3 Br2 109.84(11) . . ?
N10 Cu4 N12 158.0(2) . . ?
N10 Cu4 N11 92.52(18) . . ?
N12 Cu4 N11 92.75(18) . . ?
N10 Cu4 O3 82.35(17) . . ?
N12 Cu4 O3 83.40(17) . . ?
N11 Cu4 O3 153.34(17) . . ?
N10 Cu4 Br2 99.83(14) . . ?
N12 Cu4 Br2 100.84(16) . . ?
N11 Cu4 Br2 95.62(12) . . ?
O3 Cu4 Br2 111.02(11) . . ?
C1 N1 Cu1 120.1(3) . . ?
C1 N1 H1C 107.3 . . ?
Cu1 N1 H1C 107.3 . . ?
C1 N1 H1D 107.3 . . ?
Cu1 N1 H1D 107.3 . . ?
H1C N1 H1D 106.9 . . ?
C3 N2 C25 112.5(4) . . ?
C3 N2 C4 105.9(3) . . ?
C25 N2 C4 110.9(3) . . ?
C3 N2 Cu1 109.5(2) . . ?
C25 N2 Cu1 108.2(3) . . ?
C4 N2 Cu1 109.8(2) . . ?
C6 N3 Cu1 119.4(3) . . ?
C6 N3 H3C 107.5 . . ?
Cu1 N3 H3C 107.5 . . ?
C6 N3 H3D 107.5 . . ?
Cu1 N3 H3D 107.5 . . ?
H3C N3 H3D 107.0 . . ?
C7 N4 Cu2 118.4(3) . . ?
C7 N4 H4C 107.7 . . ?
Cu2 N4 H4C 107.7 . . ?
C7 N4 H4D 107.7 . . ?
Cu2 N4 H4D 107.7 . . ?
H4C N4 H4D 107.1 . . ?
C9 N5 C10 105.8(3) . . ?
C9 N5 C27 112.1(3) . 4_676 ?
C10 N5 C27 110.1(3) . 4_676 ?
C9 N5 Cu2 109.5(2) . . ?
C10 N5 Cu2 110.6(2) . . ?
C27 N5 Cu2 108.6(3) 4_676 . ?
C12 N6 Cu2 119.9(3) . . ?
C12 N6 H6C 107.3 . . ?
Cu2 N6 H6C 107.3 . . ?
C12 N6 H6D 107.3 . . ?
Cu2 N6 H6D 107.3 . . ?
H6C N6 H6D 106.9 . . ?
C13 N7 Cu3 120.8(3) . . ?
C13 N7 H7C 107.1 . . ?
Cu3 N7 H7C 107.1 . . ?
C13 N7 H7D 107.1 . . ?
Cu3 N7 H7D 107.1 . . ?
H7C N7 H7D 106.8 . . ?
C28 N8 C15 112.0(4) . . ?
C28 N8 C16 111.6(4) . . ?
C15 N8 C16 105.0(3) . . ?
C28 N8 Cu3 108.4(3) . . ?
C15 N8 Cu3 108.4(3) . . ?
C16 N8 Cu3 111.4(3) . . ?
C18 N9 Cu3 121.0(3) . . ?
C18 N9 H9C 107.1 . . ?
Cu3 N9 H9C 107.1 . . ?
C18 N9 H9D 107.1 . . ?
Cu3 N9 H9D 107.1 . . ?
H9C N9 H9D 106.8 . . ?
C19 N10 Cu4 120.5(3) . . ?
C19 N10 H10C 107.2 . . ?
Cu4 N10 H10C 107.2 . . ?
C19 N10 H10D 107.2 . . ?
Cu4 N10 H10D 107.2 . . ?
H10C N10 H10D 106.8 . . ?
C30 N11 C22 111.4(4) 4_575 . ?
C30 N11 C21 112.3(4) 4_575 . ?
C22 N11 C21 105.8(4) . . ?
C30 N11 Cu4 106.9(3) 4_575 . ?
C22 N11 Cu4 111.0(3) . . ?
C21 N11 Cu4 109.6(3) . . ?
C24 N12 Cu4 117.2(4) . . ?
C24 N12 H12C 108.0 . . ?
Cu4 N12 H12C 108.0 . . ?
C24 N12 H12D 108.0 . . ?
Cu4 N12 H12D 108.0 . . ?
H12C N12 H12D 107.2 . . ?
C31 O1 Cu1 116.5(4) . . ?
C31 O1 Cu2 114.0(4) . . ?
Cu1 O1 Cu2 129.49(19) . . ?
C31 O2 Cu3 144.0(4) . . ?
C31 O3 Cu4 140.9(5) . . ?
H4H O4 H4F 109.5 . . ?
H5D O5 H5F 109.5 . . ?
H6H O6 H6E 108.0 . . ?

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 H1C Br3 0.90 2.60 3.461(5) 160.0 .
N3 H3C O31 0.90 2.18 3.068(7) 169.6 .
N7 H7D O14 0.90 2.33 3.197(7) 161.2 .
N10 H10D Br3 0.90 2.59 3.451(4) 161.6 .
N12 H12C O14 0.90 2.25 3.100(6) 156.7 .
N12 H12D O31 0.90 2.17 3.067(7) 172.1 .
N10 H10D Br3 0.90 2.59 3.451(4) 161.6 .
N12 H12C O14 0.90 2.25 3.100(6) 156.7 .
O5 H5F O32 0.85 2.22 2.982(6) 149.8 .
O5 H5F O33 0.85 2.37 3.143(7) 150.8 .
O5 H5F Cl3 0.85 2.76 3.605(4) 179.3 .
N12 H12D O31 0.90 2.17 3.067(7) 172.1 .
O4 H4H Br1 0.85 2.56 3.410(3) 179.1 .
O4 H4H Br1 0.85 2.56 3.410(3) 179.1 .
N9 H9C Br3 0.90 2.57 3.425(4) 157.9 .
N3 H3D O14 0.90 2.24 3.101(6) 159.8 .
N6 H6D Br3 0.90 2.67 3.511(4) 156.5 .
N4 H4C O14 0.90 2.18 3.058(6) 164.5 .
N1 H1D O21 0.90 2.27 3.174(7) 178.8 4_675
N10 H10C O21 0.90 2.24 3.140(7) 177.4 4_675
N9 H9D O5 0.90 2.12 2.976(6) 158.2 4_676
N6 H6C O5 0.90 2.15 2.980(6) 153.3 4_676
N7 H7C O23 0.90 2.25 3.144(7) 170.6 1_655
N4 H4D O23 0.90 2.28 3.166(7) 167.7 1_655
O4 H4F Br3 0.85 2.59 3.335(3) 146.3 3_766
O5 H5D O4 0.85 2.16 2.815(6) 133.8 2_655
#O6 H6E Br2 0.85 3.02 3.721(8) 141.0 2_546

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.118

# Attachment 'cif_and_check_for_complex_2.cif'

data_0906et
_database_code_depnum_ccdc_archive 'CCDC 697700'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C11 H30 Cl3 Cu2 N6), 2(Cl O4), H4 O2 '
_chemical_formula_sum            'C22 H64 Cl8 Cu4 N12 O10'
_chemical_formula_weight         1194.61

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           Orthorhombic
_symmetry_space_group_name_H-M   'Pnma '
_symmetry_space_group_name_Hall  '-P 2ac 2n '

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

_cell_length_a                   11.1759(7)
_cell_length_b                   8.5562(5)
_cell_length_c                   23.4528(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2242.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    3359
_cell_measurement_theta_min      2.13
_cell_measurement_theta_max      25.24

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    2.408
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Apex CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11726
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2361
_reflns_number_gt                2027
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.

There is solvent disorder present in the structure.
The O5 atmom is disordered over a site of symmetry,
its occupation factor is 0.5.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.06P)²+1.99P] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2361
_refine_ls_number_parameters     181
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1104
_refine_ls_wR_factor_gt          0.1072
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.2117(3) -0.0273(4) 0.53775(17) 0.0404(8) Uani 1 1 d . . .
H1C H 0.2389 -0.0532 0.5759 0.049 Uiso 1 1 calc R . .
H1D H 0.1732 -0.1189 0.5216 0.049 Uiso 1 1 calc R . .
C2 C 0.1248(3) 0.1049(4) 0.54036(15) 0.0363(8) Uani 1 1 d . . .
H2A H 0.0872 0.1190 0.5034 0.044 Uiso 1 1 calc R . .
H2B H 0.0627 0.0820 0.5680 0.044 Uiso 1 1 calc R . .
C3 C 0.2230(4) 0.2500 0.61859(19) 0.0316(10) Uani 1 2 d S . .
H3A H 0.2721 0.3413 0.6259 0.038 Uiso 0.50 1 calc PR . .
H3B H 0.2721 0.1587 0.6259 0.038 Uiso 0.50 1 calc PR . .
C4 C 0.1199(4) 0.2500 0.6611(2) 0.0382(12) Uani 1 2 d S . .
H4C H 0.0704 0.1580 0.6556 0.046 Uiso 0.50 1 calc PR . .
H4D H 0.0704 0.3420 0.6556 0.046 Uiso 0.50 1 calc PR . .
C5 C 0.1729(5) 0.2500 0.7214(2) 0.0454(13) Uani 1 2 d S . .
H5A H 0.2235 0.1586 0.7255 0.055 Uiso 0.50 1 calc PR . .
H5B H 0.2235 0.3414 0.7255 0.055 Uiso 0.50 1 calc PR . .
C6 C 0.0120(4) 0.1059(5) 0.77041(16) 0.0426(9) Uani 1 1 d . . .
H6A H -0.0227 0.0859 0.7332 0.051 Uiso 1 1 calc R . .
H6B H -0.0527 0.1183 0.7976 0.051 Uiso 1 1 calc R . .
C7 C 0.0897(4) -0.0286(5) 0.78765(16) 0.0431(9) Uani 1 1 d . . .
H7A H 0.0404 -0.1183 0.7970 0.052 Uiso 1 1 calc R . .
H7B H 0.1420 -0.0573 0.7563 0.052 Uiso 1 1 calc R . .
Cl1 Cl 0.47159(13) 0.2500 0.42764(5) 0.0445(3) Uani 1 2 d S . .
Cl2 Cl 0.50615(11) 0.2500 0.57977(5) 0.0370(3) Uani 1 2 d S . .
Cl3 Cl 0.33036(11) 0.2500 0.90591(6) 0.0435(3) Uani 1 2 d S . .
Cl4 Cl 0.44529(12) 0.7500 0.85326(6) 0.0431(3) Uani 1 2 d S . .
Cu1 Cu 0.34130(5) 0.2500 0.50526(3) 0.03099(18) Uani 1 2 d S . .
Cu2 Cu 0.17710(5) 0.2500 0.84406(3) 0.03481(19) Uani 1 2 d S . .
N1 N 0.1622(3) 0.0171(4) 0.83779(15) 0.0425(8) Uani 1 1 d . . .
H1A H 0.237(4) -0.019(5) 0.8373(18) 0.051 Uiso 1 1 d . . .
H1B H 0.132(4) -0.021(5) 0.869(2) 0.051 Uiso 1 1 d . . .
N2 N 0.0843(3) 0.2500 0.76840(17) 0.0328(9) Uani 1 2 d S . .
N3 N 0.1892(3) 0.2500 0.55697(17) 0.0310(9) Uani 1 2 d S . .
N4 N 0.3141(3) 0.0186(4) 0.50215(15) 0.0425(8) Uani 1 1 d . . .
H4A H 0.302(4) -0.005(5) 0.466(2) 0.051 Uiso 1 1 d . . .
H4B H 0.380(4) -0.030(6) 0.5145(18) 0.051 Uiso 1 1 d . . .
O1 O 0.3760(4) 0.7500 0.90116(18) 0.0534(10) Uani 1 2 d S . .
O2 O 0.3802(5) 0.8036(6) 0.8060(2) 0.0530(16) Uani 0.50 1 d P . .
O3 O 0.5565(5) 0.8282(7) 0.8486(3) 0.0564(15) Uani 0.50 1 d P . .
O4 O 0.4461(5) 0.5966(7) 0.8509(2) 0.0522(14) Uani 0.50 1 d P . .
O5 O 0.8041(6) 0.8321(8) 0.8244(3) 0.0557(16) Uani 0.50 1 d P A -1
H5C H 0.809(8) 0.824(11) 0.784(4) 0.067 Uiso 0.50 1 d P B -1
H5D H 0.742(9) 0.826(12) 0.823(5) 0.067 Uiso 0.50 1 d P C -1


_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
C1 N4 1.470(5) . ?
C1 C2 1.492(5) . ?
C1 H1C 0.9700 . ?
C1 H1D 0.9700 . ?
C2 N3 1.487(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N3 1.494(6) . ?
C3 C4 1.524(7) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.533(7) . ?
C4 H4C 0.9700 . ?
C4 H4D 0.9700 . ?
C5 N2 1.482(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N2 1.475(4) . ?
C6 C7 1.498(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.480(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
Cl1 Cu1 2.3310(14) . ?
Cl2 Cu1 2.5392(13) . ?
Cl2 Cu2 2.6155(13) 6_657 ?
Cl3 Cu2 2.2445(14) . ?
Cl4 O4 1.314(6) 7_575 ?
Cl4 O4 1.314(6) . ?
Cl4 O1 1.365(4) . ?
Cl4 O2 1.403(5) 7_575 ?
Cl4 O2 1.403(5) . ?
Cl4 O3 1.416(6) . ?
Cl4 O3 1.416(6) 7_575 ?
Cu1 N4 2.004(4) . ?
Cu1 N4 2.004(4) 7_565 ?
Cu1 N3 2.088(4) . ?
Cu2 N1 2.005(4) . ?
Cu2 N1 2.005(4) 7_565 ?
Cu2 N2 2.055(4) . ?
Cu2 Cl2 2.6155(13) 6_557 ?
N1 H1A 0.90(5) . ?
N1 H1B 0.86(5) . ?
N2 C6 1.475(4) 7_565 ?
N3 C2 1.487(4) 7_565 ?
N4 H4A 0.87(5) . ?
N4 H4B 0.89(5) . ?
O2 O2 0.918(11) 7_575 ?
O2 O4 1.544(8) 7_575 ?
O3 O3 1.338(12) 7_575 ?
O3 O4 1.393(8) 7_575 ?
O4 O3 1.393(8) 7_575 ?
O4 O2 1.544(8) 7_575 ?
O5 H5C 0.94(10) . ?
O5 H5D 0.70(10) . ?

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
N4 C1 C2 109.1(3) . . ?
N4 C1 H1C 109.9 . . ?
C2 C1 H1C 109.9 . . ?
N4 C1 H1D 109.9 . . ?
C2 C1 H1D 109.9 . . ?
H1C C1 H1D 108.3 . . ?
N3 C2 C1 109.2(3) . . ?
N3 C2 H2A 109.8 . . ?
C1 C2 H2A 109.8 . . ?
N3 C2 H2B 109.8 . . ?
C1 C2 H2B 109.8 . . ?
H2A C2 H2B 108.3 . . ?
N3 C3 C4 116.2(4) . . ?
N3 C3 H3A 108.2 . . ?
C4 C3 H3A 108.2 . . ?
N3 C3 H3B 108.2 . . ?
C4 C3 H3B 108.2 . . ?
H3A C3 H3B 107.4 . . ?
C3 C4 C5 108.1(4) . . ?
C3 C4 H4C 110.1 . . ?
C5 C4 H4C 110.1 . . ?
C3 C4 H4D 110.1 . . ?
C5 C4 H4D 110.1 . . ?
H4C C4 H4D 108.4 . . ?
N2 C5 C4 115.3(4) . . ?
N2 C5 H5A 108.4 . . ?
C4 C5 H5A 108.4 . . ?
N2 C5 H5B 108.4 . . ?
C4 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
N2 C6 C7 109.4(3) . . ?
N2 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
N2 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.2 . . ?
N1 C7 C6 109.2(3) . . ?
N1 C7 H7A 109.8 . . ?
C6 C7 H7A 109.8 . . ?
N1 C7 H7B 109.8 . . ?
C6 C7 H7B 109.8 . . ?
H7A C7 H7B 108.3 . . ?
Cu1 Cl2 Cu2 179.59(5) . 6_657 ?
O4 Cl4 O4 175.1(5) 7_575 . ?
O4 Cl4 O1 92.2(3) 7_575 . ?
O4 Cl4 O1 92.2(3) . . ?
O4 Cl4 O2 107.3(4) 7_575 7_575 ?
O4 Cl4 O2 69.1(3) . 7_575 ?
O1 Cl4 O2 110.9(3) . 7_575 ?
O4 Cl4 O2 69.1(3) 7_575 . ?
O4 Cl4 O2 107.3(4) . . ?
O1 Cl4 O2 110.9(3) . . ?
O4 Cl4 O3 61.2(4) 7_575 . ?
O4 Cl4 O3 117.6(4) . . ?
O1 Cl4 O3 124.2(3) . . ?
O2 Cl4 O3 123.3(4) 7_575 . ?
O2 Cl4 O3 103.9(3) . . ?
O4 Cl4 O3 117.6(4) 7_575 7_575 ?
O4 Cl4 O3 61.2(4) . 7_575 ?
O1 Cl4 O3 124.2(3) . 7_575 ?
O2 Cl4 O3 103.9(3) 7_575 7_575 ?
O2 Cl4 O3 123.3(3) . 7_575 ?
O3 Cl4 O3 56.4(5) . 7_575 ?
N4 Cu1 N4 162.0(2) . 7_565 ?
N4 Cu1 N3 84.12(10) . . ?
N4 Cu1 N3 84.12(10) 7_565 . ?
N4 Cu1 Cl1 93.80(9) . . ?
N4 Cu1 Cl1 93.80(9) 7_565 . ?
N3 Cu1 Cl1 164.16(12) . . ?
N4 Cu1 Cl2 97.77(12) . . ?
N4 Cu1 Cl2 97.77(12) 7_565 . ?
N3 Cu1 Cl2 101.01(12) . . ?
Cl1 Cu1 Cl2 94.83(5) . . ?
N1 Cu2 N1 167.3(2) . 7_565 ?
N1 Cu2 N2 83.95(10) . . ?
N1 Cu2 N2 83.95(10) 7_565 . ?
N1 Cu2 Cl3 96.37(10) . . ?
N1 Cu2 Cl3 96.37(10) 7_565 . ?
N2 Cu2 Cl3 160.56(12) . . ?
N1 Cu2 Cl2 89.38(11) . 6_557 ?
N1 Cu2 Cl2 89.38(11) 7_565 6_557 ?
N2 Cu2 Cl2 102.78(11) . 6_557 ?
Cl3 Cu2 Cl2 96.67(5) . 6_557 ?
C7 N1 Cu2 111.5(2) . . ?
C7 N1 H1A 114(3) . . ?
Cu2 N1 H1A 105(3) . . ?
C7 N1 H1B 110(3) . . ?
Cu2 N1 H1B 110(3) . . ?
H1A N1 H1B 104(4) . . ?
C6 N2 C6 113.4(4) . 7_565 ?
C6 N2 C5 113.0(2) . . ?
C6 N2 C5 113.0(2) 7_565 . ?
C6 N2 Cu2 104.4(2) . . ?
C6 N2 Cu2 104.4(2) 7_565 . ?
C5 N2 Cu2 107.8(3) . . ?
C2 N3 C2 113.2(4) . 7_565 ?
C2 N3 C3 112.1(2) . . ?
C2 N3 C3 112.1(2) 7_565 . ?
C2 N3 Cu1 104.0(2) . . ?
C2 N3 Cu1 104.0(2) 7_565 . ?
C3 N3 Cu1 110.9(3) . . ?
C1 N4 Cu1 111.2(2) . . ?
C1 N4 H4A 111(3) . . ?
Cu1 N4 H4A 107(3) . . ?
C1 N4 H4B 109(3) . . ?
Cu1 N4 H4B 109(3) . . ?
H4A N4 H4B 110(4) . . ?
O2 O2 Cl4 70.9(2) 7_575 . ?
O2 O2 O4 123.6(3) 7_575 7_575 ?
Cl4 O2 O4 52.7(3) . 7_575 ?
O3 O3 O4 117.5(3) 7_575 7_575 ?
O3 O3 Cl4 61.8(3) 7_575 . ?
O4 O3 Cl4 55.8(3) 7_575 . ?
Cl4 O4 O3 63.0(4) . 7_575 ?
Cl4 O4 O2 58.2(3) . 7_575 ?
O3 O4 O2 98.1(5) 7_575 7_575 ?
H5C O5 H5D 91(10) . . ?

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 H1A O2 0.90(5) 2.32(5) 3.135(6) 151(4) 1_545
N1 H1A O4 0.90(5) 2.44(5) 3.333(7) 171(4) 7_565
N1 H1B Cl1 0.86(5) 2.66(5) 3.449(4) 152(4) 2
N4 H4A Cl3 0.87(5) 2.93(5) 3.603(4) 135(4) 2_554
N4 H4B Cl1 0.89(5) 2.85(5) 3.706(4) 160(4) 5_656
O5 H5C O2 0.94(10) 2.27(10) 3.183(9) 163(8) 6_657
O5 H5C O2 0.94(10) 2.51(10) 3.379(9) 153(8) 4_566
O5 H5D O3 0.70(10) 2.16(10) 2.825(9) 161(12) .
O5 H5D O3 0.70(10) 2.53(10) 3.140(9) 148(11) 7_575

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.085

# Attachment 'complex 3.cif'

data_050930em
_database_code_depnum_ccdc_archive 'CCDC 697701'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' C6 H16 Cl Cu N3, Cl O4 '
_chemical_formula_sum            'C6 H16 Cl2 Cu N3 O4'
_chemical_formula_weight         328.66

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'
Cu Cu 0.3201 1.2651 '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           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c '
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   6.8456(6)
_cell_length_b                   12.0195(11)
_cell_length_c                   14.6950(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.473(2)
_cell_angle_gamma                90.00
_cell_volume                     1195.92(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    292(2)
_cell_measurement_reflns_used    3027
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      28.26

_exptl_crystal_description       needle
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.825
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             672
_exptl_absorpt_coefficient_mu    2.276
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_correction_T_min  0.4630
_exptl_absorpt_correction_T_max  0.7412
_exptl_absorpt_process_details   'SADABS, BRUKR'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      292(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7931
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2711
_reflns_number_gt                2316
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0400P)²+0.6362P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr.
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2711
_refine_ls_number_parameters     145
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0878
_refine_ls_wR_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.63152(4) 0.60728(2) 0.44295(2) 0.02987(12) Uani 1 1 d . . .
N1 N 0.6636(3) 0.77652(16) 0.42126(14) 0.0300(4) Uani 1 1 d . . .
N2 N 0.4610(4) 0.60952(18) 0.32212(17) 0.0392(5) Uani 1 1 d . . .
H2A H 0.5166 0.5677 0.2821 0.047 Uiso 1 1 calc R . .
H2B H 0.3431 0.5794 0.3279 0.047 Uiso 1 1 calc R . .
N3 N 0.8674(4) 0.62473(19) 0.53735(18) 0.0439(6) Uani 1 1 d . . .
H3A H 0.8414 0.5976 0.5914 0.053 Uiso 1 1 calc R . .
H3B H 0.9683 0.5854 0.5207 0.053 Uiso 1 1 calc R . .
Cl1 Cl 0.63756(9) 0.41081(5) 0.44516(5) 0.03580(16) Uani 1 1 d . . .
C1 C 0.6139(5) 0.7904(2) 0.32081(19) 0.0436(7) Uani 1 1 d . . .
H1A H 0.7235 0.7656 0.2910 0.052 Uiso 1 1 calc R . .
H1B H 0.5903 0.8684 0.3062 0.052 Uiso 1 1 calc R . .
C2 C 0.4312(5) 0.7234(2) 0.2856(2) 0.0479(7) Uani 1 1 d . . .
H2C H 0.3159 0.7565 0.3060 0.058 Uiso 1 1 calc R . .
H2D H 0.4106 0.7220 0.2189 0.058 Uiso 1 1 calc R . .
C3 C 0.9251(4) 0.7430(2) 0.5487(2) 0.0456(7) Uani 1 1 d . . .
H3C H 1.0652 0.7494 0.5709 0.055 Uiso 1 1 calc R . .
H3D H 0.8525 0.7790 0.5924 0.055 Uiso 1 1 calc R . .
C4 C 0.8765(4) 0.7957(2) 0.4556(2) 0.0397(6) Uani 1 1 d . . .
H4A H 0.9035 0.8749 0.4599 0.048 Uiso 1 1 calc R . .
H4B H 0.9571 0.7633 0.4135 0.048 Uiso 1 1 calc R . .
C5 C 0.5331(4) 0.84541(19) 0.47258(18) 0.0314(5) Uani 1 1 d . . .
H5A H 0.5433 0.8170 0.5349 0.038 Uiso 1 1 calc R . .
H5B H 0.3974 0.8354 0.4437 0.038 Uiso 1 1 calc R . .
C6 C 0.5776(4) 0.9690(2) 0.47748(19) 0.0327(6) Uani 1 1 d . . .
H6A H 0.5791 0.9978 0.4159 0.039 Uiso 1 1 calc R . .
H6B H 0.7071 0.9812 0.5128 0.039 Uiso 1 1 calc R . .
Cl2 Cl 0.94758(10) 0.51206(5) 0.23435(5) 0.03844(17) Uani 1 1 d . . .
O1 O 1.0015(4) 0.5686(2) 0.32045(16) 0.0612(6) Uani 1 1 d . . .
O2 O 0.7494(4) 0.5402(3) 0.19836(19) 0.0920(10) Uani 1 1 d . . .
O3 O 1.0748(4) 0.5443(2) 0.17053(17) 0.0623(6) Uani 1 1 d . . .
O4 O 0.9639(5) 0.3955(2) 0.2503(2) 0.0807(9) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 N2 1.976(2) . ?
Cu1 N3 1.979(2) . ?
Cu1 N1 2.076(2) . ?
Cu1 Cl1 2.3620(7) . ?
Cu1 Cl1 2.6526(7) 3_666 ?
N1 C1 1.475(3) . ?
N1 C4 1.489(3) . ?
N1 C5 1.500(3) . ?
N2 C2 1.473(3) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?
N3 C3 1.478(3) . ?
N3 H3A 0.9000 . ?
N3 H3B 0.9000 . ?
Cl1 Cu1 2.6525(7) 3_666 ?
C1 C2 1.513(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2C 0.9700 . ?
C2 H2D 0.9700 . ?
C3 C4 1.499(4) . ?
C3 H3C 0.9700 . ?
C3 H3D 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.517(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C6 1.526(5) 3_676 ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
Cl2 O4 1.422(2) . ?
Cl2 O2 1.423(3) . ?
Cl2 O3 1.425(2) . ?
Cl2 O1 1.436(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
N2 Cu1 N3 160.29(11) . . ?
N2 Cu1 N1 84.86(9) . . ?
N3 Cu1 N1 84.83(9) . . ?
N2 Cu1 Cl1 91.88(7) . . ?
N3 Cu1 Cl1 94.91(7) . . ?
N1 Cu1 Cl1 168.50(6) . . ?
N2 Cu1 Cl1 100.71(8) . 3_666 ?
N3 Cu1 Cl1 98.26(8) . 3_666 ?
N1 Cu1 Cl1 105.92(6) . 3_666 ?
Cl1 Cu1 Cl1 85.52(2) . 3_666 ?
C1 N1 C4 113.1(2) . . ?
C1 N1 C5 112.0(2) . . ?
C4 N1 C5 111.7(2) . . ?
C1 N1 Cu1 104.52(15) . . ?
C4 N1 Cu1 102.72(14) . . ?
C5 N1 Cu1 112.31(15) . . ?
C2 N2 Cu1 111.84(17) . . ?
C2 N2 H2A 109.2 . . ?
Cu1 N2 H2A 109.2 . . ?
C2 N2 H2B 109.2 . . ?
Cu1 N2 H2B 109.2 . . ?
H2A N2 H2B 107.9 . . ?
C3 N3 Cu1 110.95(17) . . ?
C3 N3 H3A 109.4 . . ?
Cu1 N3 H3A 109.4 . . ?
C3 N3 H3B 109.4 . . ?
Cu1 N3 H3B 109.4 . . ?
H3A N3 H3B 108.0 . . ?
Cu1 Cl1 Cu1 94.48(2) . 3_666 ?
N1 C1 C2 109.8(2) . . ?
N1 C1 H1A 109.7 . . ?
C2 C1 H1A 109.7 . . ?
N1 C1 H1B 109.7 . . ?
C2 C1 H1B 109.7 . . ?
H1A C1 H1B 108.2 . . ?
N2 C2 C1 107.9(2) . . ?
N2 C2 H2C 110.1 . . ?
C1 C2 H2C 110.1 . . ?
N2 C2 H2D 110.1 . . ?
C1 C2 H2D 110.1 . . ?
H2C C2 H2D 108.4 . . ?
N3 C3 C4 106.5(2) . . ?
N3 C3 H3C 110.4 . . ?
C4 C3 H3C 110.4 . . ?
N3 C3 H3D 110.4 . . ?
C4 C3 H3D 110.4 . . ?
H3C C3 H3D 108.6 . . ?
N1 C4 C3 108.6(2) . . ?
N1 C4 H4A 110.0 . . ?
C3 C4 H4A 110.0 . . ?
N1 C4 H4B 110.0 . . ?
C3 C4 H4B 110.0 . . ?
H4A C4 H4B 108.4 . . ?
N1 C5 C6 115.8(2) . . ?
N1 C5 H5A 108.3 . . ?
C6 C5 H5A 108.3 . . ?
N1 C5 H5B 108.3 . . ?
C6 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
C5 C6 C6 110.5(3) . 3_676 ?
C5 C6 H6A 109.5 . . ?
C6 C6 H6A 109.5 3_676 . ?
C5 C6 H6B 109.5 . . ?
C6 C6 H6B 109.5 3_676 . ?
H6A C6 H6B 108.1 . . ?
O4 Cl2 O2 110.1(2) . . ?
O4 Cl2 O3 109.62(16) . . ?
O2 Cl2 O3 109.44(17) . . ?
O4 Cl2 O1 108.48(16) . . ?
O2 Cl2 O1 108.81(17) . . ?
O3 Cl2 O1 110.40(16) . . ?

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
N2 Cu1 N1 C1 -21.50(17) . . . . ?
N3 Cu1 N1 C1 141.67(18) . . . . ?
Cl1 Cu1 N1 C1 52.5(4) . . . . ?
Cl1 Cu1 N1 C1 -121.19(16) 3_666 . . . ?
N2 Cu1 N1 C4 -139.77(17) . . . . ?
N3 Cu1 N1 C4 23.40(17) . . . . ?
Cl1 Cu1 N1 C4 -65.8(4) . . . . ?
Cl1 Cu1 N1 C4 120.53(15) 3_666 . . . ?
N2 Cu1 N1 C5 100.10(18) . . . . ?
N3 Cu1 N1 C5 -96.73(18) . . . . ?
Cl1 Cu1 N1 C5 174.1(2) . . . . ?
Cl1 Cu1 N1 C5 0.40(17) 3_666 . . . ?
N3 Cu1 N2 C2 -63.8(4) . . . . ?
N1 Cu1 N2 C2 -5.1(2) . . . . ?
Cl1 Cu1 N2 C2 -174.03(19) . . . . ?
Cl1 Cu1 N2 C2 100.18(19) 3_666 . . . ?
N2 Cu1 N3 C3 64.4(4) . . . . ?
N1 Cu1 N3 C3 5.7(2) . . . . ?
Cl1 Cu1 N3 C3 174.1(2) . . . . ?
Cl1 Cu1 N3 C3 -99.7(2) 3_666 . . . ?
N2 Cu1 Cl1 Cu1 -100.60(8) . . . 3_666 ?
N3 Cu1 Cl1 Cu1 97.93(8) . . . 3_666 ?
N1 Cu1 Cl1 Cu1 -173.9(3) . . . 3_666 ?
Cl1 Cu1 Cl1 Cu1 0.0 3_666 . . 3_666 ?
C4 N1 C1 C2 155.0(2) . . . . ?
C5 N1 C1 C2 -77.8(3) . . . . ?
Cu1 N1 C1 C2 44.0(2) . . . . ?
Cu1 N2 C2 C1 30.3(3) . . . . ?
N1 C1 C2 N2 -50.2(3) . . . . ?
Cu1 N3 C3 C4 -33.7(3) . . . . ?
C1 N1 C4 C3 -160.8(2) . . . . ?
C5 N1 C4 C3 71.9(2) . . . . ?
Cu1 N1 C4 C3 -48.7(2) . . . . ?
N3 C3 C4 N1 55.9(3) . . . . ?
C1 N1 C5 C6 -75.4(3) . . . . ?
C4 N1 C5 C6 52.6(3) . . . . ?
Cu1 N1 C5 C6 167.39(17) . . . . ?
N1 C5 C6 C6 174.2(3) . . . 3_676 ?

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
N3 H3B Cl1 0.90 2.67 3.388(3) 137.2 3_766
N3 H3A O1 0.90 2.53 3.165(3) 127.8 3_766
N3 H3A O4 0.90 2.51 3.173(4) 131.3 3_766
N2 H2B Cl2 0.90 2.96 3.749(2) 146.9 1_455
N2 H2B O1 0.90 2.33 3.180(4) 157.9 1_455
N2 H2A O2 0.90 2.18 2.993(4) 150.4 .

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.074

# Attachment 'complex 4.cif'

data_1019
_database_code_depnum_ccdc_archive 'CCDC 697702'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C7 H18 Cl2 Cu N3 O4'
_chemical_formula_sum            'C7 H18 Cl2 Cu N3 O4'
_chemical_formula_weight         342.68

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)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   7.1450(14)
_cell_length_b                   13.486(3)
_cell_length_c                   14.077(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.77(2)
_cell_angle_gamma                90.00
_cell_volume                     1340.6(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    291(2)
_cell_measurement_reflns_used    735
_cell_measurement_theta_min      2.11
_cell_measurement_theta_max      18.72

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_absorpt_coefficient_mu    2.034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_process_details   'SADABS; Bruker, 2000'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      291(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Smart Aepex CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            2638
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2638
_reflns_number_gt                1657
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  SHELXTL
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.04P)²] where P=(Fo²+2Fc²)/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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2638
_refine_ls_number_parameters     166
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0900
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.0976
_refine_ls_wR_factor_gt          0.0943
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0028(7) 1.0073(4) 0.9465(3) 0.0522(11) Uani 1 1 d . . .
H1A H 0.0348 1.0747 0.9346 0.063 Uiso 1 1 calc R . .
H1B H -0.1317 0.9982 0.9144 0.063 Uiso 1 1 calc R . .
C2 C 0.1322(6) 0.9325(3) 0.9024(3) 0.0495(11) Uani 1 1 d . . .
H2A H 0.2615 0.9377 0.9350 0.059 Uiso 1 1 calc R . .
H2B H 0.0893 0.8646 0.9064 0.059 Uiso 1 1 calc R . .
C3 C 0.1156(7) 0.9670(3) 0.7964(3) 0.0557(12) Uani 1 1 d . . .
H3A H -0.0081 0.9479 0.7631 0.067 Uiso 1 1 calc R . .
H3B H 0.1222 1.0388 0.7955 0.067 Uiso 1 1 calc R . .
C4 C 0.4470(6) 0.9853(3) 0.7684(3) 0.0499(11) Uani 1 1 d . . .
H4A H 0.4702 0.9997 0.8367 0.060 Uiso 1 1 calc R . .
H4B H 0.5519 0.9462 0.7526 0.060 Uiso 1 1 calc R . .
C5 C 0.4302(6) 1.0785(4) 0.7127(3) 0.0500(10) Uani 1 1 d . . .
H5A H 0.5481 1.1154 0.7237 0.060 Uiso 1 1 calc R . .
H5B H 0.3301 1.1198 0.7307 0.060 Uiso 1 1 calc R . .
C6 C 0.2992(6) 0.8219(3) 0.7692(3) 0.0465(10) Uani 1 1 d . . .
H6A H 0.3093 0.8121 0.8381 0.056 Uiso 1 1 calc R . .
H6B H 0.4149 0.7992 0.7480 0.056 Uiso 1 1 calc R . .
C7 C 0.1174(6) 0.7658(3) 0.7127(3) 0.0430(9) Uani 1 1 d . . .
H7A H 0.0058 0.7823 0.7409 0.052 Uiso 1 1 calc R . .
H7B H 0.1361 0.6946 0.7169 0.052 Uiso 1 1 calc R . .
Cl1 Cl 0.13432(14) 0.93174(7) 0.41895(8) 0.0445(2) Uani 1 1 d . . .
Cl2 Cl 0.58570(15) 0.73462(8) 0.55629(8) 0.0475(3) Uani 1 1 d . . .
Cu1 Cu 0.19329(8) 0.93644(4) 0.59425(4) 0.04900(19) Uani 1 1 d . . .
N1 N 0.2603(5) 0.9274(3) 0.7430(3) 0.0537(10) Uani 1 1 d . . .
N2 N 0.3842(6) 1.0476(3) 0.6091(3) 0.0566(10) Uani 1 1 d . . .
H2C H 0.491(8) 1.027(4) 0.588(4) 0.068 Uiso 1 1 d . . .
H2D H 0.337(8) 1.100(4) 0.573(4) 0.068 Uiso 1 1 d . . .
N3 N 0.0892(7) 0.8012(3) 0.5999(3) 0.0536(10) Uani 1 1 d . . .
H3C H -0.035(8) 0.801(4) 0.575(4) 0.064 Uiso 1 1 d . . .
H3D H 0.150(7) 0.759(4) 0.565(4) 0.064 Uiso 1 1 d . . .
O11 O 0.6582(4) 0.7309(2) 0.4656(2) 0.0510(7) Uani 1 1 d . . .
O12 O 0.5477(4) 0.8374(2) 0.57986(19) 0.0414(6) Uani 1 1 d . . .
O13 O 0.7260(4) 0.6941(2) 0.6314(2) 0.0470(8) Uani 1 1 d . . .
O14 O 0.4113(4) 0.6778(2) 0.5513(2) 0.0446(7) Uani 1 1 d . . .


_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C1 1.513(9) 3_577 ?
C1 C2 1.586(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.549(6) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.469(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.478(6) . ?
C4 N1 1.540(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N2 1.505(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.485(6) . ?
C6 C7 1.606(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N3 1.641(6) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
Cl1 Cu1 2.4399(13) . ?
Cl2 O13 1.448(3) . ?
Cl2 O11 1.450(3) . ?
Cl2 O14 1.455(3) . ?
Cl2 O12 1.461(3) . ?
Cu1 N3 1.976(4) . ?
Cu1 N2 2.016(4) . ?
Cu1 N1 2.079(4) . ?
N2 H2C 0.90(6) . ?
N2 H2D 0.90(5) . ?
N3 H3C 0.90(5) . ?
N3 H3D 0.90(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 C1 C2 112.5(5) 3_577 . ?
C1 C1 H1A 109.1 3_577 . ?
C2 C1 H1A 109.1 . . ?
C1 C1 H1B 109.1 3_577 . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C1 103.0(4) . . ?
C3 C2 H2A 111.2 . . ?
C1 C2 H2A 111.2 . . ?
C3 C2 H2B 111.2 . . ?
C1 C2 H2B 111.2 . . ?
H2A C2 H2B 109.1 . . ?
N1 C3 C2 115.3(4) . . ?
N1 C3 H3A 108.4 . . ?
C2 C3 H3A 108.4 . . ?
N1 C3 H3B 108.4 . . ?
C2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C5 C4 N1 108.1(3) . . ?
C5 C4 H4A 110.1 . . ?
N1 C4 H4A 110.1 . . ?
C5 C4 H4B 110.1 . . ?
N1 C4 H4B 110.1 . . ?
H4A C4 H4B 108.4 . . ?
C4 C5 N2 105.5(4) . . ?
C4 C5 H5A 110.6 . . ?
N2 C5 H5A 110.6 . . ?
C4 C5 H5B 110.6 . . ?
N2 C5 H5B 110.6 . . ?
H5A C5 H5B 108.8 . . ?
N1 C6 C7 102.8(3) . . ?
N1 C6 H6A 111.2 . . ?
C7 C6 H6A 111.2 . . ?
N1 C6 H6B 111.2 . . ?
C7 C6 H6B 111.2 . . ?
H6A C6 H6B 109.1 . . ?
C6 C7 N3 108.3(3) . . ?
C6 C7 H7A 110.0 . . ?
N3 C7 H7A 110.0 . . ?
C6 C7 H7B 110.0 . . ?
N3 C7 H7B 110.0 . . ?
H7A C7 H7B 108.4 . . ?
O13 Cl2 O11 109.24(18) . . ?
O13 Cl2 O14 109.23(17) . . ?
O11 Cl2 O14 110.93(19) . . ?
O13 Cl2 O12 108.90(17) . . ?
O11 Cl2 O12 109.65(18) . . ?
O14 Cl2 O12 108.87(17) . . ?
N3 Cu1 N2 159.24(19) . . ?
N3 Cu1 N1 86.32(17) . . ?
N2 Cu1 N1 83.74(17) . . ?
N3 Cu1 Cl1 90.49(13) . . ?
N2 Cu1 Cl1 97.69(13) . . ?
N1 Cu1 Cl1 174.11(11) . . ?
C3 N1 C6 109.9(4) . . ?
C3 N1 C4 110.4(4) . . ?
C6 N1 C4 107.7(3) . . ?
C3 N1 Cu1 115.0(3) . . ?
C6 N1 Cu1 108.2(3) . . ?
C4 N1 Cu1 105.3(3) . . ?
C5 N2 Cu1 110.5(3) . . ?
C5 N2 H2C 110(3) . . ?
Cu1 N2 H2C 110(3) . . ?
C5 N2 H2D 110(4) . . ?
Cu1 N2 H2D 110(4) . . ?
H2C N2 H2D 108(5) . . ?
C7 N3 Cu1 108.4(3) . . ?
C7 N3 H3C 110(4) . . ?
Cu1 N3 H3C 110(3) . . ?
C7 N3 H3D 110(4) . . ?
Cu1 N3 H3D 110(4) . . ?
H3C N3 H3D 108(5) . . ?

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
N2 H2C O12 0.90(6) 2.60(5) 3.116(5) 117(4) .
N2 H2C Cl1 0.90(6) 2.75(6) 3.533(5) 146(4) 3_676
N2 H2D O11 0.90(5) 2.35(6) 3.166(6) 151(5) 3_676
N2 H2D O12 0.90(5) 2.56(6) 3.179(5) 126(4) 3_676
N3 H3C O13 0.90(5) 2.46(5) 3.061(5) 125(4) 1_455
N3 H3C Cl2 0.90(5) 2.83(5) 3.668(5) 155(4) 1_455
N3 H3D O14 0.90(5) 2.20(5) 3.003(5) 148(5) .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.084


