# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Marcetta Darensbourg'
'Melissa L. Golden'
'Marilyn V. Rampersad'
'Joseph H. Reibenspies'

_publ_contact_author_name        'Prof Marcetta Darensbourg'
_publ_contact_author_address     
;
Department of Chemistry
Texas A & M University
College Station
TX
77843-3225
USA
;

_publ_contact_author_email       MARCETTA@MAIL.CHEM.TAMU.EDU

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Capture of Ni , Cu and Zn by Thiolate Sulfurs of an
N2S2Ni Complex: A role for a metallothiolate Ligand in the
Acetyl-coenzyme A Synthase Active Site
;

data_mr02
_database_code_CSD               211927

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C38 H80 Br2 Cu2 N6 Ni3 O2 S6'
_chemical_formula_weight         1308.47

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'
S S 0.1246 0.1234 '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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4/m

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

_cell_length_a                   26.1834(13)
_cell_length_b                   26.1834(13)
_cell_length_c                   15.5725(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10676.0(10)
_cell_formula_units_Z            8
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5392
_exptl_absorpt_coefficient_mu    3.592
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      110(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27161
_diffrn_reflns_av_R_equivalents  0.1329
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         24.99
_reflns_number_total             4799
_reflns_number_gt                3612
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4799
_refine_ls_number_parameters     276
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0519
_refine_ls_wR_factor_ref         0.1601
_refine_ls_wR_factor_gt          0.1447
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      5.347
_refine_ls_shift/su_max          0.113
_refine_ls_shift/su_mean         0.002

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 0.35373(12) 0.14787(13) 0.3699(2) 0.0313(11) Uani 1 1 d . . .
Ni1 Ni 0.45668(16) 0.10651(17) 0.5000 0.0212(12) Uani 1 2 d S . .
Ni2 Ni 0.33545(17) 0.25637(16) 0.5000 0.0233(12) Uani 1 2 d S . .
Ni3 Ni 0.27026(18) 0.07134(18) 0.5000 0.0319(14) Uani 1 2 d S . .
Br1 Br 0.35312(13) 0.15074(12) 0.20636(19) 0.0481(12) Uani 1 1 d . . .
S1 S 0.4050(3) 0.0780(3) 0.4028(5) 0.0369(18) Uani 1 1 d . . .
S2 S 0.3869(3) 0.2273(3) 0.4027(4) 0.0288(16) Uani 1 1 d . . .
S3 S 0.2694(3) 0.1302(3) 0.4025(6) 0.050(2) Uani 1 1 d . . .
N1 N 0.5071(9) 0.1247(9) 0.4104(12) 0.028(5) Uani 1 1 d . . .
N2 N 0.2915(9) 0.2874(9) 0.4096(13) 0.031(5) Uani 1 1 d . . .
N3 N 0.2640(10) 0.0177(10) 0.4099(15) 0.041(6) Uani 1 1 d . . .
C1 C 0.4495(12) 0.0770(12) 0.3146(19) 0.047(8) Uani 1 1 d . . .
H1A H 0.4699 0.0452 0.3161 0.057 Uiso 1 1 calc R . .
H1B H 0.4309 0.0784 0.2593 0.057 Uiso 1 1 calc R . .
C2 C 0.4837(11) 0.1222(11) 0.3231(17) 0.038(7) Uani 1 1 d . . .
H2A H 0.4637 0.1538 0.3126 0.045 Uiso 1 1 calc R . .
H2B H 0.5110 0.1203 0.2793 0.045 Uiso 1 1 calc R . .
C3 C 0.5487(10) 0.0851(11) 0.4179(15) 0.031(6) Uani 1 1 d D . .
H3A H 0.5822 0.1025 0.4136 0.038 Uiso 1 1 calc R A 1
H3B H 0.5459 0.0614 0.3687 0.038 Uiso 1 1 calc R A 1
C4 C 0.5477(18) 0.0543(19) 0.5000 0.031(16) Uani 0.79(13) 2 d SPD . 1
H4A H 0.5165 0.0329 0.5000 0.037 Uiso 1 2 calc SR . 1
H4B H 0.5774 0.0310 0.5000 0.037 Uiso 1 2 calc SR . 1
C4' C 0.579(6) 0.089(7) 0.5000 0.03(6) Uiso 0.21(13) 2 d SPD . 2
C5 C 0.5284(11) 0.1776(11) 0.4192(17) 0.037(7) Uani 1 1 d D . .
H5A H 0.5519 0.1841 0.3706 0.045 Uiso 1 1 calc R . 1
H5B H 0.5000 0.2024 0.4150 0.045 Uiso 1 1 calc R . 1
C6 C 0.5562(18) 0.187(2) 0.5000 0.034(17) Uani 0.76(13) 2 d SPD . 1
H6A H 0.5679 0.2226 0.5000 0.041 Uiso 1 2 calc SR . 1
H6B H 0.5870 0.1648 0.5000 0.041 Uiso 1 2 calc SR . 1
C6' C 0.521(6) 0.208(5) 0.5000 0.03(5) Uiso 0.24(13) 2 d SPD . 2
C7 C 0.3649(12) 0.2683(11) 0.3160(17) 0.040(7) Uani 1 1 d . . .
H7A H 0.3795 0.3030 0.3222 0.048 Uiso 1 1 calc R . .
H7B H 0.3755 0.2542 0.2598 0.048 Uiso 1 1 calc R . .
C8 C 0.3080(12) 0.2702(11) 0.3220(18) 0.041(7) Uani 1 1 d . . .
H8A H 0.2938 0.2360 0.3100 0.050 Uiso 1 1 calc R . .
H8B H 0.2946 0.2942 0.2782 0.050 Uiso 1 1 calc R . .
C9 C 0.2373(12) 0.2708(13) 0.419(2) 0.048(8) Uani 1 1 d . . .
H9A H 0.2362 0.2330 0.4178 0.058 Uiso 1 1 calc R . .
H9B H 0.2177 0.2833 0.3688 0.058 Uiso 1 1 calc R . .
C10 C 0.2111(17) 0.2890(17) 0.5000 0.051(12) Uani 1 2 d S . .
H10A H 0.2103 0.3268 0.5000 0.062 Uiso 1 2 calc SR . .
H10B H 0.1753 0.2768 0.5000 0.062 Uiso 1 2 calc SR . .
C11 C 0.2954(13) 0.3443(11) 0.4159(17) 0.040(7) Uani 1 1 d . . .
H11A H 0.2608 0.3592 0.4112 0.048 Uiso 1 1 calc R . .
H11B H 0.3160 0.3572 0.3672 0.048 Uiso 1 1 calc R . .
C12 C 0.3198(18) 0.3619(14) 0.5000 0.037(9) Uani 1 2 d S . .
H12A H 0.3201 0.3997 0.5000 0.045 Uiso 1 2 calc SR . .
H12B H 0.3558 0.3504 0.5000 0.045 Uiso 1 2 calc SR . .
C13 C 0.2485(15) 0.0907(17) 0.314(3) 0.076(13) Uani 1 1 d . . .
H13A H 0.2109 0.0868 0.3148 0.091 Uiso 1 1 calc R . .
H13B H 0.2582 0.1068 0.2583 0.091 Uiso 1 1 calc R . .
C14 C 0.2740(14) 0.0393(14) 0.322(2) 0.057(9) Uani 1 1 d . . .
H14A H 0.2606 0.0157 0.2782 0.069 Uiso 1 1 calc R . .
H14B H 0.3112 0.0430 0.3135 0.069 Uiso 1 1 calc R . .
C15 C 0.3033(14) -0.0238(12) 0.419(2) 0.048(8) Uani 1 1 d . . .
H15A H 0.3377 -0.0082 0.4186 0.057 Uiso 1 1 calc R . .
H15B H 0.3009 -0.0469 0.3687 0.057 Uiso 1 1 calc R . .
C16 C 0.297(2) -0.0550(16) 0.5000 0.055(13) Uani 1 2 d S . .
H16A H 0.2629 -0.0710 0.5000 0.066 Uiso 1 2 calc SR . .
H16B H 0.3228 -0.0828 0.5000 0.066 Uiso 1 2 calc SR . .
C17 C 0.2107(13) -0.0032(14) 0.416(2) 0.051(9) Uani 1 1 d . . .
H17A H 0.2120 -0.0407 0.4091 0.062 Uiso 1 1 calc R . .
H17B H 0.1902 0.0108 0.3679 0.062 Uiso 1 1 calc R . .
C18 C 0.1845(18) 0.010(2) 0.5000 0.063(15) Uani 1 2 d S . .
H18A H 0.1775 0.0467 0.5000 0.075 Uiso 1 2 calc SR . .
H18B H 0.1510 -0.0080 0.5000 0.075 Uiso 1 2 calc SR . .
O1E O 0.346(2) 0.4932(19) 0.5000 0.114(11) Uani 1 2 d SD . .
C1E C 0.325(2) 0.485(2) 0.3549(15) 0.114(11) Uani 1 1 d D . .
H1EA H 0.3211 0.5046 0.3019 0.171 Uiso 1 1 calc R . .
H1EB H 0.2922 0.4689 0.3696 0.171 Uiso 1 1 calc R . .
H1EC H 0.3507 0.4582 0.3464 0.171 Uiso 1 1 calc R . .
C2E C 0.341(3) 0.5189(13) 0.4251(18) 0.114(11) Uani 1 1 d D . .
H2EA H 0.3740 0.5350 0.4100 0.137 Uiso 1 1 calc R . .
H2EB H 0.3154 0.5464 0.4324 0.137 Uiso 1 1 calc R . .
O2E O 0.130(10) 0.903(10) 0.5000 0.091(14) Uani 0.15(6) 2 d SPD . 1
C3E C 0.136(11) 0.889(13) 0.349(5) 0.091(14) Uani 0.15(6) 1 d PD . 1
H3EA H 0.1200 0.8686 0.3028 0.136 Uiso 0.15(6) 1 calc PR . 1
H3EB H 0.1714 0.8780 0.3561 0.136 Uiso 0.15(6) 1 calc PR . 1
H3EC H 0.1347 0.9250 0.3336 0.136 Uiso 0.15(6) 1 calc PR . 1
C4E C 0.107(9) 0.880(10) 0.430(8) 0.091(14) Uani 0.15(6) 1 d PD . 1
H4EA H 0.0724 0.8940 0.4241 0.109 Uiso 0.15(6) 1 calc PR . 1
H4EB H 0.1047 0.8432 0.4411 0.109 Uiso 0.15(6) 1 calc PR . 1
O2E' O 0.1579(18) 0.8698(17) 0.5000 0.091(14) Uani 0.85 2 d SPD . 2
C3E' C 0.1191(18) 0.890(2) 0.362(3) 0.091(14) Uani 0.85 1 d PD . 2
H3ED H 0.1351 0.8809 0.3073 0.136 Uiso 0.85(6) 1 calc PR . 2
H3EE H 0.1147 0.9266 0.3661 0.136 Uiso 0.85(6) 1 calc PR . 2
H3EF H 0.0857 0.8728 0.3662 0.136 Uiso 0.85(6) 1 calc PR . 2
C4E' C 0.1481(16) 0.8740(17) 0.4250(12) 0.091(14) Uani 0.85 1 d PD . 2
H4EC H 0.1509 0.8375 0.4086 0.109 Uiso 0.85(6) 1 calc PR . 2
H4ED H 0.1808 0.8890 0.4055 0.109 Uiso 0.85(6) 1 calc PR . 2

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 0.0300(19) 0.0289(19) 0.035(2) -0.0003(13) -0.0083(13) 0.0041(13)
Ni1 0.016(2) 0.027(2) 0.020(2) 0.000 0.000 0.0038(18)
Ni2 0.025(2) 0.022(2) 0.023(2) 0.000 0.000 0.0058(18)
Ni3 0.021(2) 0.025(3) 0.049(3) 0.000 0.000 -0.0011(19)
Br1 0.060(2) 0.045(2) 0.040(2) -0.0116(13) -0.0168(14) 0.0177(15)
S1 0.033(4) 0.029(4) 0.049(4) -0.002(3) -0.021(3) 0.003(3)
S2 0.030(4) 0.029(4) 0.027(3) -0.004(3) 0.002(3) 0.003(3)
S3 0.028(4) 0.039(4) 0.082(6) 0.021(4) -0.010(4) 0.002(3)
N1 0.028(12) 0.035(12) 0.021(11) 0.001(9) 0.000(8) 0.009(10)
N2 0.037(13) 0.025(12) 0.031(12) 0.000(9) -0.009(9) 0.010(10)
N3 0.041(15) 0.036(14) 0.045(14) -0.001(11) -0.006(11) -0.014(12)
C1 0.054(19) 0.051(19) 0.036(16) -0.021(15) -0.018(14) 0.026(16)
C2 0.044(17) 0.052(18) 0.017(12) 0.000(12) 0.001(12) 0.018(14)
C3 0.025(14) 0.046(17) 0.023(13) -0.004(11) 0.001(10) 0.011(12)
C4 0.02(3) 0.04(3) 0.03(3) 0.000 0.000 0.01(2)
C5 0.034(15) 0.042(17) 0.036(16) 0.014(13) 0.008(12) 0.008(13)
C6 0.01(3) 0.03(3) 0.06(4) 0.000 0.000 0.00(2)
C7 0.07(2) 0.029(15) 0.024(14) -0.001(12) 0.006(13) 0.005(14)
C8 0.07(2) 0.030(15) 0.027(14) 0.000(12) -0.012(14) 0.012(14)
C9 0.038(17) 0.040(17) 0.07(2) -0.005(15) -0.019(15) 0.020(15)
C10 0.03(2) 0.04(2) 0.09(4) 0.000 0.000 0.015(19)
C11 0.06(2) 0.029(15) 0.034(15) 0.004(12) -0.004(13) 0.016(14)
C12 0.06(3) 0.022(19) 0.03(2) 0.000 0.000 0.005(18)
C13 0.06(2) 0.10(3) 0.07(3) 0.04(2) -0.04(2) -0.04(2)
C14 0.06(2) 0.06(2) 0.048(19) 0.002(17) -0.019(17) -0.025(18)
C15 0.05(2) 0.034(17) 0.06(2) -0.012(14) 0.006(15) -0.003(15)
C16 0.05(3) 0.02(2) 0.09(4) 0.000 0.000 -0.01(2)
C17 0.05(2) 0.042(19) 0.07(2) 0.000(15) -0.005(16) -0.022(16)
C18 0.03(2) 0.05(3) 0.11(4) 0.000 0.000 -0.02(2)
O1E 0.13(3) 0.09(2) 0.12(3) 0.000 0.000 0.02(2)
C1E 0.13(3) 0.09(2) 0.12(3) 0.000 0.000 0.02(2)
C2E 0.13(3) 0.09(2) 0.12(3) 0.000 0.000 0.02(2)
O2E 0.07(2) 0.041(13) 0.16(4) 0.000 0.000 -0.029(15)
C3E 0.07(2) 0.041(13) 0.16(4) 0.000 0.000 -0.029(15)
C4E 0.07(2) 0.041(13) 0.16(4) 0.000 0.000 -0.029(15)
O2E' 0.07(2) 0.041(13) 0.16(4) 0.000 0.000 -0.029(15)
C3E' 0.07(2) 0.041(13) 0.16(4) 0.000 0.000 -0.029(15)
C4E' 0.07(2) 0.041(13) 0.16(4) 0.000 0.000 -0.029(15)

_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 S2 2.310(7) . ?
Cu1 S3 2.313(9) . ?
Cu1 S1 2.326(8) . ?
Cu1 Br1 2.547(5) . ?
Ni1 N1 1.98(2) 11_556 ?
Ni1 N1 1.98(2) . ?
Ni1 S1 2.163(7) . ?
Ni1 S1 2.163(7) 11_556 ?
Ni2 N2 1.99(2) . ?
Ni2 N2 1.99(2) 11_556 ?
Ni2 S2 2.166(7) 11_556 ?
Ni2 S2 2.166(7) . ?
Ni3 N3 1.99(2) . ?
Ni3 N3 1.99(2) 11_556 ?
Ni3 S3 2.165(9) 11_556 ?
Ni3 S3 2.165(9) . ?
S1 C1 1.80(3) . ?
S2 C7 1.82(3) . ?
S3 C13 1.81(4) . ?
N1 C2 1.49(3) . ?
N1 C5 1.50(4) . ?
N1 C3 1.51(3) . ?
N2 C9 1.49(4) . ?
N2 C11 1.50(4) . ?
N2 C8 1.50(4) . ?
N3 C14 1.50(4) . ?
N3 C15 1.50(4) . ?
N3 C17 1.50(4) . ?
C1 C2 1.49(5) . ?
C3 C4' 1.51(8) . ?
C3 C4 1.51(4) . ?
C4 C3 1.51(4) 11_556 ?
C4' C3 1.51(8) 11_556 ?
C5 C6 1.47(4) . ?
C5 C6' 1.50(8) . ?
C6 C5 1.47(4) 11_556 ?
C6' C5 1.50(8) 11_556 ?
C7 C8 1.49(4) . ?
C9 C10 1.51(4) . ?
C10 C9 1.51(4) 11_556 ?
C11 C12 1.53(4) . ?
C12 C11 1.53(4) 11_556 ?
C13 C14 1.51(6) . ?
C15 C16 1.51(4) . ?
C16 C15 1.51(4) 11_556 ?
C17 C18 1.52(4) . ?
C18 C17 1.52(4) 11_556 ?
O1E C2E 1.353(5) 11_556 ?
O1E C2E 1.353(5) . ?
C1E C2E 1.474(5) . ?
O2E C4E 1.376(5) . ?
O2E C4E 1.376(5) 11_556 ?
C3E C4E 1.488(5) . ?
O2E' C4E' 1.200(11) . ?
O2E' C4E' 1.200(11) 11_556 ?
C3E' C4E' 1.303(11) . ?

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
S2 Cu1 S3 119.3(3) . . ?
S2 Cu1 S1 116.2(3) . . ?
S3 Cu1 S1 110.2(3) . . ?
S2 Cu1 Br1 101.4(2) . . ?
S3 Cu1 Br1 102.7(3) . . ?
S1 Cu1 Br1 104.3(2) . . ?
N1 Ni1 N1 89.6(13) 11_556 . ?
N1 Ni1 S1 173.5(7) 11_556 . ?
N1 Ni1 S1 90.4(7) . . ?
N1 Ni1 S1 90.4(7) 11_556 11_556 ?
N1 Ni1 S1 173.5(7) . 11_556 ?
S1 Ni1 S1 88.8(5) . 11_556 ?
N2 Ni2 N2 90.0(13) . 11_556 ?
N2 Ni2 S2 175.9(8) . 11_556 ?
N2 Ni2 S2 90.4(7) 11_556 11_556 ?
N2 Ni2 S2 90.4(7) . . ?
N2 Ni2 S2 175.9(8) 11_556 . ?
S2 Ni2 S2 88.8(4) 11_556 . ?
N3 Ni3 N3 89.6(14) . 11_556 ?
N3 Ni3 S3 174.7(8) . 11_556 ?
N3 Ni3 S3 90.4(8) 11_556 11_556 ?
N3 Ni3 S3 90.4(8) . . ?
N3 Ni3 S3 174.7(8) 11_556 . ?
S3 Ni3 S3 89.1(5) 11_556 . ?
C1 S1 Ni1 97.7(10) . . ?
C1 S1 Cu1 102.5(10) . . ?
Ni1 S1 Cu1 104.1(3) . . ?
C7 S2 Ni2 96.6(10) . . ?
C7 S2 Cu1 104.4(10) . . ?
Ni2 S2 Cu1 103.7(3) . . ?
C13 S3 Ni3 97.6(13) . . ?
C13 S3 Cu1 103.5(14) . . ?
Ni3 S3 Cu1 106.6(3) . . ?
C2 N1 C5 106(2) . . ?
C2 N1 C3 109.8(19) . . ?
C5 N1 C3 111(2) . . ?
C2 N1 Ni1 110.9(17) . . ?
C5 N1 Ni1 114.0(15) . . ?
C3 N1 Ni1 105.2(15) . . ?
C9 N2 C11 110(2) . . ?
C9 N2 C8 106(2) . . ?
C11 N2 C8 110(2) . . ?
C9 N2 Ni2 111.2(18) . . ?
C11 N2 Ni2 108.7(16) . . ?
C8 N2 Ni2 110.8(16) . . ?
C14 N3 C15 104(2) . . ?
C14 N3 C17 111(2) . . ?
C15 N3 C17 111(2) . . ?
C14 N3 Ni3 111.1(19) . . ?
C15 N3 Ni3 112.9(18) . . ?
C17 N3 Ni3 106.8(19) . . ?
C2 C1 S1 108.0(19) . . ?
C1 C2 N1 111(2) . . ?
N1 C3 C4' 114(6) . . ?
N1 C3 C4 115(2) . . ?
C4' C3 C4 48(6) . . ?
C3 C4 C3 115(4) 11_556 . ?
C3 C4' C3 116(10) . 11_556 ?
C6 C5 C6' 42(6) . . ?
C6 C5 N1 114(3) . . ?
C6' C5 N1 121(5) . . ?
C5 C6 C5 117(4) . 11_556 ?
C5 C6' C5 115(9) . 11_556 ?
C8 C7 S2 106.8(19) . . ?
C7 C8 N2 111(2) . . ?
N2 C9 C10 115(3) . . ?
C9 C10 C9 113(3) 11_556 . ?
N2 C11 C12 113(2) . . ?
C11 C12 C11 118(4) . 11_556 ?
C14 C13 S3 108(2) . . ?
N3 C14 C13 110(3) . . ?
N3 C15 C16 113(3) . . ?
C15 C16 C15 113(3) 11_556 . ?
N3 C17 C18 113(3) . . ?
C17 C18 C17 120(4) 11_556 . ?
C2E O1E C2E 119(5) 11_556 . ?
O1E C2E C1E 111.5(6) . . ?
C4E O2E C4E 104(10) . 11_556 ?
O2E C4E C3E 113.0(6) . . ?
C4E' O2E' C4E' 153(5) . 11_556 ?
O2E' C4E' C3E' 152(3) . . ?

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
N1 Ni1 S1 C1 -78(6) 11_556 . . . ?
N1 Ni1 S1 C1 12.8(12) . . . . ?
S1 Ni1 S1 C1 -160.8(10) 11_556 . . . ?
N1 Ni1 S1 Cu1 177(6) 11_556 . . . ?
N1 Ni1 S1 Cu1 -92.3(7) . . . . ?
S1 Ni1 S1 Cu1 94.1(3) 11_556 . . . ?
S2 Cu1 S1 C1 -79.7(11) . . . . ?
S3 Cu1 S1 C1 140.5(11) . . . . ?
Br1 Cu1 S1 C1 31.0(11) . . . . ?
S2 Cu1 S1 Ni1 21.7(4) . . . . ?
S3 Cu1 S1 Ni1 -118.1(4) . . . . ?
Br1 Cu1 S1 Ni1 132.3(3) . . . . ?
N2 Ni2 S2 C7 17.1(12) . . . . ?
N2 Ni2 S2 C7 -80(9) 11_556 . . . ?
S2 Ni2 S2 C7 -158.9(10) 11_556 . . . ?
N2 Ni2 S2 Cu1 -89.5(7) . . . . ?
N2 Ni2 S2 Cu1 174(9) 11_556 . . . ?
S2 Ni2 S2 Cu1 94.5(3) 11_556 . . . ?
S3 Cu1 S2 C7 -80.2(10) . . . . ?
S1 Cu1 S2 C7 143.8(10) . . . . ?
Br1 Cu1 S2 C7 31.4(10) . . . . ?
S3 Cu1 S2 Ni2 20.4(4) . . . . ?
S1 Cu1 S2 Ni2 -115.6(3) . . . . ?
Br1 Cu1 S2 Ni2 132.1(2) . . . . ?
N3 Ni3 S3 C13 12.9(17) . . . . ?
N3 Ni3 S3 C13 -77(8) 11_556 . . . ?
S3 Ni3 S3 C13 -161.8(14) 11_556 . . . ?
N3 Ni3 S3 Cu1 -93.7(8) . . . . ?
N3 Ni3 S3 Cu1 176(8) 11_556 . . . ?
S3 Ni3 S3 Cu1 91.6(4) 11_556 . . . ?
S2 Cu1 S3 C13 143.5(14) . . . . ?
S1 Cu1 S3 C13 -78.2(14) . . . . ?
Br1 Cu1 S3 C13 32.5(14) . . . . ?
S2 Cu1 S3 Ni3 -114.2(4) . . . . ?
S1 Cu1 S3 Ni3 24.2(5) . . . . ?
Br1 Cu1 S3 Ni3 134.9(3) . . . . ?
N1 Ni1 N1 C2 -173.9(13) 11_556 . . . ?
S1 Ni1 N1 C2 12.5(17) . . . . ?
S1 Ni1 N1 C2 95(6) 11_556 . . . ?
N1 Ni1 N1 C5 -54(2) 11_556 . . . ?
S1 Ni1 N1 C5 132.1(16) . . . . ?
S1 Ni1 N1 C5 -145(5) 11_556 . . . ?
N1 Ni1 N1 C3 67.5(18) 11_556 . . . ?
S1 Ni1 N1 C3 -106.1(15) . . . . ?
S1 Ni1 N1 C3 -23(7) 11_556 . . . ?
N2 Ni2 N2 C9 -58(2) 11_556 . . . ?
S2 Ni2 N2 C9 -154(9) 11_556 . . . ?
S2 Ni2 N2 C9 126.5(17) . . . . ?
N2 Ni2 N2 C11 64(2) 11_556 . . . ?
S2 Ni2 N2 C11 -33(10) 11_556 . . . ?
S2 Ni2 N2 C11 -111.8(18) . . . . ?
N2 Ni2 N2 C8 -175.2(14) 11_556 . . . ?
S2 Ni2 N2 C8 88(10) 11_556 . . . ?
S2 Ni2 N2 C8 8.9(18) . . . . ?
N3 Ni3 N3 C14 -172.0(17) 11_556 . . . ?
S3 Ni3 N3 C14 98(8) 11_556 . . . ?
S3 Ni3 N3 C14 13(2) . . . . ?
N3 Ni3 N3 C15 -56(2) 11_556 . . . ?
S3 Ni3 N3 C15 -146(8) 11_556 . . . ?
S3 Ni3 N3 C15 129.5(19) . . . . ?
N3 Ni3 N3 C17 67(2) 11_556 . . . ?
S3 Ni3 N3 C17 -23(9) 11_556 . . . ?
S3 Ni3 N3 C17 -107.7(19) . . . . ?
Ni1 S1 C1 C2 -37(2) . . . . ?
Cu1 S1 C1 C2 69.4(19) . . . . ?
S1 C1 C2 N1 52(3) . . . . ?
C5 N1 C2 C1 -165(2) . . . . ?
C3 N1 C2 C1 75(3) . . . . ?
Ni1 N1 C2 C1 -41(3) . . . . ?
C2 N1 C3 C4' 173(6) . . . . ?
C5 N1 C3 C4' 56(6) . . . . ?
Ni1 N1 C3 C4' -68(6) . . . . ?
C2 N1 C3 C4 -134(3) . . . . ?
C5 N1 C3 C4 109(3) . . . . ?
Ni1 N1 C3 C4 -15(3) . . . . ?
N1 C3 C4 C3 -55(5) . . . 11_556 ?
C4' C3 C4 C3 45(8) . . . 11_556 ?
N1 C3 C4' C3 57(13) . . . 11_556 ?
C4 C3 C4' C3 -46(8) . . . 11_556 ?
C2 N1 C5 C6 -177(3) . . . . ?
C3 N1 C5 C6 -57(3) . . . . ?
Ni1 N1 C5 C6 61(3) . . . . ?
C2 N1 C5 C6' 136(7) . . . . ?
C3 N1 C5 C6' -105(7) . . . . ?
Ni1 N1 C5 C6' 14(7) . . . . ?
C6' C5 C6 C5 53(8) . . . 11_556 ?
N1 C5 C6 C5 -57(5) . . . 11_556 ?
C6 C5 C6' C5 -50(7) . . . 11_556 ?
N1 C5 C6' C5 43(13) . . . 11_556 ?
Ni2 S2 C7 C8 -41.8(19) . . . . ?
Cu1 S2 C7 C8 64.3(19) . . . . ?
S2 C7 C8 N2 55(3) . . . . ?
C9 N2 C8 C7 -161(2) . . . . ?
C11 N2 C8 C7 80(3) . . . . ?
Ni2 N2 C8 C7 -40(3) . . . . ?
C11 N2 C9 C10 -55(3) . . . . ?
C8 N2 C9 C10 -174(3) . . . . ?
Ni2 N2 C9 C10 66(3) . . . . ?
N2 C9 C10 C9 -60(5) . . . 11_556 ?
C9 N2 C11 C12 108(3) . . . . ?
C8 N2 C11 C12 -136(3) . . . . ?
Ni2 N2 C11 C12 -14(3) . . . . ?
N2 C11 C12 C11 -56(5) . . . 11_556 ?
Ni3 S3 C13 C14 -38(3) . . . . ?
Cu1 S3 C13 C14 71(3) . . . . ?
C15 N3 C14 C13 -164(2) . . . . ?
C17 N3 C14 C13 77(3) . . . . ?
Ni3 N3 C14 C13 -42(3) . . . . ?
S3 C13 C14 N3 53(3) . . . . ?
C14 N3 C15 C16 -174(3) . . . . ?
C17 N3 C15 C16 -55(3) . . . . ?
Ni3 N3 C15 C16 65(3) . . . . ?
N3 C15 C16 C15 -62(5) . . . 11_556 ?
C14 N3 C17 C18 -138(3) . . . . ?
C15 N3 C17 C18 107(3) . . . . ?
Ni3 N3 C17 C18 -17(4) . . . . ?
N3 C17 C18 C17 -53(5) . . . 11_556 ?
C2E O1E C2E C1E -155(4) 11_556 . . . ?
C4E O2E C4E C3E -164(19) 11_556 . . . ?
C4E' O2E' C4E' C3E' 8(25) 11_556 . . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         2.018
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.136