#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/60/7016096.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7016096
loop_
_publ_author_name
'Lü, Xue'
'Chen, Xi'
'Ren, Zhi-Gang'
'Lang, Jian-Ping'
'Liu, Dong'
'Sun, Zhen-Rong'
_publ_section_title
;
 Four [Tp*W(μ(3)-S)(3)Cu(3)(μ(3)-Br)]-based clusters: synthesis,
 structural characterization and third-order NLO properties.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7983
_journal_page_last               7992
_journal_paper_doi               10.1039/c1dt10230c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety
'(C21 H34 B Br2 Cu3 N18 S3 W), 0.5(C4 H10 O), (C2 H3 N)'
_chemical_formula_sum            'C25 H42 B Br2 Cu3 N19 O0.5 S3 W'
_chemical_formula_weight         1258.06
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2011-05-13 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.09(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.683(4)
_cell_length_b                   22.969(5)
_cell_length_c                   25.060(5)
_cell_measurement_reflns_used    13726
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.4700
_cell_measurement_theta_min      3.0144
_cell_volume                     9619(4)
_computing_cell_refinement       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_collection       'CrystalClear, Ver. 1.30 (Rigaku/MSC, 2001)'
_computing_data_reduction
'CrystalStructure, Ver. 3.60 (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_sigmaI/netI    0.0661
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37439
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.526
_exptl_absorpt_correction_T_max  0.4045
_exptl_absorpt_correction_T_min  0.1687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication.'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         10972
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0666P)²+33.1173P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1459
_reflns_number_gt                9137
_reflns_number_total             10972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10230c.txt
_cod_data_source_block           ss
_cod_original_cell_volume        9619(3)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C25 H42 B Br2 Cu3 N19 O0.50 S3 W'
_cod_database_code               7016096
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
W1 W 0.363988(7) 0.941213(6) 0.340261(5) 0.02415(3) Uani 1 1 d . . .
Br1 Br 0.24094(2) 0.810854(19) 0.176281(14) 0.04029(10) Uani 1 1 d . . .
Cu1 Cu 0.31242(2) 0.85872(2) 0.260511(16) 0.03298(11) Uani 1 1 d . . .
S1 S 0.37646(4) 0.89196(4) 0.42277(3) 0.02685(19) Uani 1 1 d . . .
C1 C 0.5757(2) 0.91444(19) 0.44234(19) 0.0527(14) Uani 1 1 d . . .
H1A H 0.5405 0.8970 0.4605 0.079 Uiso 1 1 calc R . .
H1B H 0.6299 0.9154 0.4687 0.079 Uiso 1 1 calc R . .
H1C H 0.5744 0.8916 0.4095 0.079 Uiso 1 1 calc R . .
C2 C 0.5486(2) 0.97487(17) 0.42451(15) 0.0363(10) Uani 1 1 d . . .
C3 C 0.5980(2) 1.02401(19) 0.44273(16) 0.0418(11) Uani 1 1 d . . .
H3 H 0.6514 1.0244 0.4669 0.050 Uiso 1 1 calc R . .
C4 C 0.5528(2) 1.07071(16) 0.41812(14) 0.0334(9) Uani 1 1 d . . .
C5 C 0.5737(2) 1.13457(18) 0.42273(18) 0.0492(12) Uani 1 1 d . . .
H5A H 0.5547 1.1522 0.3855 0.074 Uiso 1 1 calc R . .
H5B H 0.6314 1.1390 0.4384 0.074 Uiso 1 1 calc R . .
H5C H 0.5487 1.1535 0.4472 0.074 Uiso 1 1 calc R . .
C6 C 0.3321(3) 0.9592(2) 0.18214(14) 0.0529(13) Uani 1 1 d . . .
H6A H 0.3764 0.9319 0.1936 0.079 Uiso 1 1 calc R . .
H6B H 0.3233 0.9714 0.1435 0.079 Uiso 1 1 calc R . .
H6C H 0.2842 0.9405 0.1846 0.079 Uiso 1 1 calc R . .
C7 C 0.3513(2) 1.01105(17) 0.22010(15) 0.0405(10) Uani 1 1 d . . .
C8 C 0.3566(3) 1.06741(19) 0.20244(16) 0.0490(12) Uani 1 1 d . . .
H8 H 0.3489 1.0791 0.1651 0.059 Uiso 1 1 calc R . .
C9 C 0.3748(2) 1.10310(18) 0.24824(16) 0.0437(11) Uani 1 1 d . . .
C10 C 0.3863(3) 1.16838(19) 0.25290(19) 0.0579(14) Uani 1 1 d . . .
H10A H 0.3447 1.1856 0.2652 0.087 Uiso 1 1 calc R . .
H10B H 0.3832 1.1842 0.2164 0.087 Uiso 1 1 calc R . .
H10C H 0.4382 1.1772 0.2801 0.087 Uiso 1 1 calc R . .
C11 C 0.2000(2) 0.96771(18) 0.40769(17) 0.0513(11) Uani 1 1 d . . .
H11A H 0.1708 0.9513 0.3711 0.077 Uiso 1 1 calc R . .
H11B H 0.1624 0.9817 0.4256 0.077 Uiso 1 1 calc R . .
H11C H 0.2339 0.9380 0.4312 0.077 Uiso 1 1 calc R . .
C12 C 0.2506(2) 1.01725(17) 0.40037(14) 0.0355(9) Uani 1 1 d . . .
C13 C 0.2433(2) 1.07351(18) 0.41713(16) 0.0406(10) Uani 1 1 d . . .
H13 H 0.2066 1.0867 0.4344 0.049 Uiso 1 1 calc R . .
C14 C 0.2987(2) 1.10654(17) 0.40427(15) 0.0375(10) Uani 1 1 d . . .
C15 C 0.3156(3) 1.16982(19) 0.4125(2) 0.0616(14) Uani 1 1 d . . .
H15A H 0.3729 1.1759 0.4288 0.092 Uiso 1 1 calc R . .
H15B H 0.2891 1.1854 0.4377 0.092 Uiso 1 1 calc R . .
H15C H 0.2958 1.1896 0.3764 0.092 Uiso 1 1 calc R . .
C16 C 0.16437(18) 0.81429(16) 0.42004(13) 0.0296(8) Uani 1 1 d . . .
C17 C 0.03270(18) 0.79084(16) 0.38199(14) 0.0317(9) Uani 1 1 d . . .
C18 C 0.10493(16) 0.80888(15) 0.32436(13) 0.0250(8) Uani 1 1 d . . .
C19 C 0.58279(18) 0.77051(16) 0.40798(14) 0.0316(9) Uani 1 1 d . . .
C20 C 0.62986(18) 0.72053(16) 0.48973(13) 0.0304(8) Uani 1 1 d . . .
C21 C 0.49836(18) 0.74637(15) 0.45790(13) 0.0277(8) Uani 1 1 d . . .
N1 N 0.47666(15) 0.99097(13) 0.39124(12) 0.0301(7) Uani 1 1 d . . .
B1 B 0.4052(2) 1.08574(18) 0.35531(17) 0.0321(10) Uani 1 1 d . . .
H1 H 0.4171 1.1279 0.3597 0.038 Uiso 1 1 calc R . .
N2 N 0.47963(16) 1.05091(13) 0.38757(12) 0.0307(8) Uani 1 1 d . . .
Cu2 Cu 0.42805(2) 0.83447(2) 0.370405(16) 0.03021(10) Uani 1 1 d . . .
S2 S 0.44107(4) 0.88787(4) 0.29908(3) 0.0283(2) Uani 1 1 d . . .
Br2 Br 0.31207(2) 0.755972(17) 0.323110(16) 0.03730(10) Uani 1 1 d . . .
N3 N 0.36516(17) 1.01150(13) 0.27660(11) 0.0317(7) Uani 1 1 d . . .
Cu3 Cu 0.26430(2) 0.86031(2) 0.356209(16) 0.02955(10) Uani 1 1 d . . .
S3 S 0.23528(4) 0.92432(4) 0.28436(3) 0.0284(2) Uani 1 1 d . . .
N4 N 0.38048(17) 1.06944(13) 0.29383(12) 0.0326(8) Uani 1 1 d . . .
N5 N 0.31011(15) 1.01532(13) 0.37724(12) 0.0317(8) Uani 1 1 d . . .
N6 N 0.33828(17) 1.07095(13) 0.37907(12) 0.0314(8) Uani 1 1 d . . .
N7 N 0.17060(15) 0.82273(13) 0.36811(10) 0.0274(7) Uani 1 1 d . . .
N8 N 0.09623(15) 0.79843(14) 0.42953(11) 0.0318(8) Uani 1 1 d . . .
N9 N 0.03405(15) 0.79317(13) 0.32908(11) 0.0308(7) Uani 1 1 d . . .
N10 N 0.22903(16) 0.82031(16) 0.46533(12) 0.0417(9) Uani 1 1 d . . .
H10D H 0.2260 0.8141 0.4988 0.050 Uiso 1 1 calc R . .
H10E H 0.2744 0.8305 0.4615 0.050 Uiso 1 1 calc R . .
N11 N -0.03804(15) 0.77989(16) 0.38903(12) 0.0405(9) Uani 1 1 d . . .
H11D H -0.0805 0.7747 0.3597 0.049 Uiso 1 1 calc R . .
H11E H -0.0414 0.7780 0.4229 0.049 Uiso 1 1 calc R . .
N12 N 0.10867(15) 0.81162(14) 0.27206(11) 0.0323(8) Uani 1 1 d . . .
H12A H 0.0666 0.8035 0.2433 0.039 Uiso 1 1 calc R . .
H12B H 0.1531 0.8216 0.2667 0.039 Uiso 1 1 calc R . .
N13 N 0.50854(15) 0.77609(13) 0.41318(11) 0.0292(7) Uani 1 1 d . . .
N14 N 0.64445(15) 0.74528(13) 0.44594(11) 0.0299(7) Uani 1 1 d . . .
N15 N 0.55686(15) 0.71776(13) 0.49642(11) 0.0291(7) Uani 1 1 d . . .
N16 N 0.59380(17) 0.79214(16) 0.36244(12) 0.0447(9) Uani 1 1 d . . .
H16A H 0.6405 0.7896 0.3580 0.054 Uiso 1 1 calc R . .
H16B H 0.5544 0.8090 0.3367 0.054 Uiso 1 1 calc R . .
N17 N 0.69095(16) 0.69465(14) 0.52944(11) 0.0339(8) Uani 1 1 d . . .
H17A H 0.7384 0.6944 0.5262 0.041 Uiso 1 1 calc R . .
H17B H 0.6830 0.6782 0.5584 0.041 Uiso 1 1 calc R . .
N18 N 0.42631(16) 0.74677(14) 0.46378(12) 0.0383(8) Uani 1 1 d . . .
H18A H 0.4185 0.7287 0.4921 0.046 Uiso 1 1 calc R . .
H18B H 0.3870 0.7651 0.4393 0.046 Uiso 1 1 calc R . .
N19 N 0.2267(5) 0.8458(4) 0.5792(3) 0.088(2) Uani 0.50 1 d PD . .
C26 C 0.1389(5) 0.8933(5) 0.6300(3) 0.088(2) Uani 0.50 1 d PD . .
H26A H 0.1424 0.8608 0.6554 0.132 Uiso 0.50 1 calc PR . .
H26B H 0.0832 0.9011 0.6090 0.132 Uiso 0.50 1 calc PR . .
H26C H 0.1628 0.9275 0.6517 0.132 Uiso 0.50 1 calc PR . .
C27 C 0.1846(5) 0.8781(6) 0.5879(3) 0.088(2) Uani 0.50 1 d PD . .
C29 C 0.1283(6) 0.1498(8) 0.2756(4) 0.133(3) Uiso 0.50 1 d PD . .
H29A H 0.0939 0.1605 0.2381 0.200 Uiso 0.50 1 calc PR . .
H29B H 0.1526 0.1122 0.2741 0.200 Uiso 0.50 1 calc PR . .
H29C H 0.1699 0.1789 0.2895 0.200 Uiso 0.50 1 calc PR . .
N20 N 0.0428(5) 0.1373(6) 0.3446(4) 0.133(3) Uiso 0.50 1 d PD . .
C28 C 0.0814(6) 0.1463(8) 0.3132(4) 0.133(3) Uiso 0.50 1 d PD . .
O1 O 0.0673(6) 1.0348(4) 0.6048(4) 0.104(2) Uani 0.50 1 d P . .
C23 C 0.0370(9) 1.0611(5) 0.6432(6) 0.104(2) Uani 0.50 1 d P . .
H23A H 0.0751 1.0902 0.6651 0.125 Uiso 0.50 1 calc PR . .
H23B H -0.0132 1.0810 0.6230 0.125 Uiso 0.50 1 calc PR . .
C25 C 0.0808(9) 1.0659(6) 0.5640(6) 0.104(2) Uani 0.50 1 d P . .
H25A H 0.1152 1.0987 0.5821 0.125 Uiso 0.50 1 calc PR . .
H25B H 0.0295 1.0825 0.5409 0.125 Uiso 0.50 1 calc PR . .
C24 C 0.1162(8) 1.0389(6) 0.5263(6) 0.104(2) Uani 0.50 1 d P . .
H24A H 0.1739 1.0434 0.5411 0.156 Uiso 0.50 1 calc PR . .
H24B H 0.0958 1.0571 0.4895 0.156 Uiso 0.50 1 calc PR . .
H24C H 0.1028 0.9978 0.5229 0.156 Uiso 0.50 1 calc PR . .
C22 C 0.0243(8) 1.0227(5) 0.6768(6) 0.104(2) Uani 0.50 1 d P . .
H22A H -0.0163 0.9956 0.6553 0.156 Uiso 0.50 1 calc PR . .
H22B H 0.0060 1.0419 0.7048 0.156 Uiso 0.50 1 calc PR . .
H22C H 0.0735 1.0018 0.6955 0.156 Uiso 0.50 1 calc PR . .
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'
B B 0.0013 0.0007 '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'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 W1 S3 85.76(7) . . ?
N3 W1 N5 81.76(11) . . ?
S3 W1 N5 84.92(7) . . ?
N3 W1 N1 80.28(10) . . ?
S3 W1 N1 159.80(7) . . ?
N5 W1 N1 78.72(10) . . ?
N3 W1 S1 163.35(7) . . ?
S3 W1 S1 104.54(4) . . ?
N5 W1 S1 86.11(8) . . ?
N1 W1 S1 86.21(8) . . ?
N3 W1 S2 85.48(8) . . ?
S3 W1 S2 104.54(3) . . ?
N5 W1 S2 163.52(8) . . ?
N1 W1 S2 88.92(8) . . ?
S1 W1 S2 104.07(3) . . ?
N3 W1 Cu3 138.95(7) . . ?
S3 W1 Cu3 53.20(3) . . ?
N5 W1 Cu3 94.25(8) . . ?
N1 W1 Cu3 139.26(7) . . ?
S1 W1 Cu3 53.14(3) . . ?
S2 W1 Cu3 102.22(3) . . ?
N3 W1 Cu1 93.30(7) . . ?
S3 W1 Cu1 52.83(3) . . ?
N5 W1 Cu1 137.75(6) . . ?
N1 W1 Cu1 142.04(8) . . ?
S1 W1 Cu1 103.35(3) . . ?
S2 W1 Cu1 53.18(3) . . ?
Cu3 W1 Cu1 62.76(2) . . ?
N3 W1 Cu2 137.80(8) . . ?
S3 W1 Cu2 105.07(3) . . ?
N5 W1 Cu2 138.87(8) . . ?
N1 W1 Cu2 95.06(7) . . ?
S1 W1 Cu2 52.79(3) . . ?
S2 W1 Cu2 52.38(2) . . ?
Cu3 W1 Cu2 64.232(19) . . ?
Cu1 W1 Cu2 65.01(2) . . ?
S3 Cu1 S2 107.56(4) . . ?
S3 Cu1 Br1 111.03(3) . . ?
S2 Cu1 Br1 133.85(4) . . ?
S3 Cu1 W1 54.25(3) . . ?
S2 Cu1 W1 54.87(3) . . ?
Br1 Cu1 W1 161.85(2) . . ?
S3 Cu1 Cu3 51.66(3) . . ?
S2 Cu1 Cu3 100.09(4) . . ?
Br1 Cu1 Cu3 123.49(2) . . ?
W1 Cu1 Cu3 58.481(16) . . ?
S3 Cu1 Br2 107.49(3) . . ?
S2 Cu1 Br2 101.17(3) . . ?
Br1 Cu1 Br2 90.56(2) . . ?
W1 Cu1 Br2 103.71(2) . . ?
Cu3 Cu1 Br2 58.647(17) . . ?
S3 Cu1 Cu2 100.24(3) . . ?
S2 Cu1 Cu2 49.64(3) . . ?
Br1 Cu1 Cu2 140.30(3) . . ?
W1 Cu1 Cu2 57.75(2) . . ?
Cu3 Cu1 Cu2 60.34(2) . . ?
Br2 Cu1 Cu2 56.113(15) . . ?
Cu2 S1 Cu3 78.81(3) . . ?
Cu2 S1 W1 72.74(3) . . ?
Cu3 S1 W1 72.02(3) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 110.3(3) . . ?
N1 C2 C1 126.7(3) . . ?
C3 C2 C1 123.0(3) . . ?
C4 C3 C2 105.9(3) . . ?
C4 C3 H3 127.1 . . ?
C2 C3 H3 127.1 . . ?
N2 C4 C3 107.7(3) . . ?
N2 C4 C5 122.5(3) . . ?
C3 C4 C5 129.7(3) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C7 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 C8 108.6(3) . . ?
N3 C7 C6 126.7(3) . . ?
C8 C7 C6 124.7(3) . . ?
C9 C8 C7 108.5(4) . . ?
C9 C8 H8 125.8 . . ?
C7 C8 H8 125.8 . . ?
N4 C9 C8 107.4(4) . . ?
N4 C9 C10 122.0(4) . . ?
C8 C9 C10 130.6(4) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 C13 108.9(3) . . ?
N5 C12 C11 127.3(3) . . ?
C13 C12 C11 123.8(4) . . ?
C14 C13 C12 107.7(4) . . ?
C14 C13 H13 126.1 . . ?
C12 C13 H13 126.1 . . ?
N6 C14 C13 107.2(3) . . ?
N6 C14 C15 122.9(4) . . ?
C13 C14 C15 129.9(4) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N10 C16 N8 116.4(3) . . ?
N10 C16 N7 119.2(3) . . ?
N8 C16 N7 124.3(3) . . ?
N9 C17 N11 117.2(3) . . ?
N9 C17 N8 126.1(3) . . ?
N11 C17 N8 116.7(3) . . ?
N12 C18 N9 116.4(3) . . ?
N12 C18 N7 118.8(3) . . ?
N9 C18 N7 124.8(3) . . ?
N16 C19 N14 117.9(3) . . ?
N16 C19 N13 117.8(3) . . ?
N14 C19 N13 124.3(3) . . ?
N14 C20 N17 118.2(3) . . ?
N14 C20 N15 124.7(3) . . ?
N17 C20 N15 117.0(3) . . ?
N18 C21 N15 117.9(3) . . ?
N18 C21 N13 118.2(3) . . ?
N15 C21 N13 123.9(3) . . ?
C2 N1 N2 105.7(3) . . ?
C2 N1 W1 133.8(2) . . ?
N2 N1 W1 120.34(18) . . ?
N4 B1 N6 110.0(3) . . ?
N4 B1 N2 108.9(3) . . ?
N6 B1 N2 108.7(3) . . ?
N4 B1 H1 109.8 . . ?
N6 B1 H1 109.8 . . ?
N2 B1 H1 109.8 . . ?
C4 N2 N1 110.4(3) . . ?
C4 N2 B1 128.7(3) . . ?
N1 N2 B1 120.8(3) . . ?
N13 Cu2 S2 123.74(9) . . ?
N13 Cu2 S1 115.77(9) . . ?
S2 Cu2 S1 108.08(4) . . ?
N13 Cu2 Br2 95.35(9) . . ?
S2 Cu2 Br2 106.09(3) . . ?
S1 Cu2 Br2 104.67(3) . . ?
N13 Cu2 W1 157.01(8) . . ?
S2 Cu2 W1 54.80(3) . . ?
S1 Cu2 W1 54.47(2) . . ?
Br2 Cu2 W1 107.14(3) . . ?
N13 Cu2 Cu3 136.20(9) . . ?
S2 Cu2 Cu3 98.69(3) . . ?
S1 Cu2 Cu3 50.60(3) . . ?
Br2 Cu2 Cu3 59.40(2) . . ?
W1 Cu2 Cu3 57.493(14) . . ?
N13 Cu2 Cu1 142.96(8) . . ?
S2 Cu2 Cu1 50.30(2) . . ?
S1 Cu2 Cu1 98.43(3) . . ?
Br2 Cu2 Cu1 60.78(2) . . ?
W1 Cu2 Cu1 57.241(14) . . ?
Cu3 Cu2 Cu1 58.07(3) . . ?
Cu2 S2 Cu1 80.07(4) . . ?
Cu2 S2 W1 72.82(3) . . ?
Cu1 S2 W1 71.96(3) . . ?
Cu2 Br2 Cu3 63.284(19) . . ?
Cu2 Br2 Cu1 63.10(3) . . ?
Cu3 Br2 Cu1 59.95(2) . . ?
C7 N3 N4 106.3(3) . . ?
C7 N3 W1 133.4(2) . . ?
N4 N3 W1 120.3(2) . . ?
N7 Cu3 S3 115.05(8) . . ?
N7 Cu3 S1 127.42(8) . . ?
S3 Cu3 S1 107.25(4) . . ?
N7 Cu3 W1 161.92(9) . . ?
S3 Cu3 W1 54.30(3) . . ?
S1 Cu3 W1 54.84(3) . . ?
N7 Cu3 Br2 91.16(9) . . ?
S3 Cu3 Br2 109.83(3) . . ?
S1 Cu3 Br2 102.76(3) . . ?
W1 Cu3 Br2 106.06(2) . . ?
N7 Cu3 Cu1 129.02(8) . . ?
S3 Cu3 Cu1 51.36(3) . . ?
S1 Cu3 Cu1 101.42(3) . . ?
W1 Cu3 Cu1 58.76(2) . . ?
Br2 Cu3 Cu1 61.402(18) . . ?
N7 Cu3 Cu2 139.04(8) . . ?
S3 Cu3 Cu2 101.05(4) . . ?
S1 Cu3 Cu2 50.60(3) . . ?
W1 Cu3 Cu2 58.276(17) . . ?
Br2 Cu3 Cu2 57.320(17) . . ?
Cu1 Cu3 Cu2 61.60(3) . . ?
Cu1 S3 Cu3 76.98(4) . . ?
Cu1 S3 W1 72.92(3) . . ?
Cu3 S3 W1 72.49(3) . . ?
C9 N4 N3 109.2(3) . . ?
C9 N4 B1 129.6(3) . . ?
N3 N4 B1 121.0(3) . . ?
C12 N5 N6 106.3(3) . . ?
C12 N5 W1 132.9(2) . . ?
N6 N5 W1 120.9(2) . . ?
C14 N6 N5 109.9(3) . . ?
C14 N6 B1 129.1(3) . . ?
N5 N6 B1 121.0(3) . . ?
C18 N7 C16 115.4(3) . . ?
C18 N7 Cu3 121.5(2) . . ?
C16 N7 Cu3 122.9(2) . . ?
C16 N8 C17 114.2(3) . . ?
C17 N9 C18 114.7(3) . . ?
C16 N10 H10D 120.0 . . ?
C16 N10 H10E 120.0 . . ?
H10D N10 H10E 120.0 . . ?
C17 N11 H11D 120.0 . . ?
C17 N11 H11E 120.0 . . ?
H11D N11 H11E 120.0 . . ?
C18 N12 H12A 120.0 . . ?
C18 N12 H12B 120.0 . . ?
H12A N12 H12B 120.0 . . ?
C19 N13 C21 114.7(3) . . ?
C19 N13 Cu2 123.4(2) . . ?
C21 N13 Cu2 120.8(2) . . ?
C19 N14 C20 116.3(3) . . ?
C21 N15 C20 115.6(3) . . ?
C19 N16 H16A 120.0 . . ?
C19 N16 H16B 120.0 . . ?
H16A N16 H16B 120.0 . . ?
C20 N17 H17A 120.0 . . ?
C20 N17 H17B 120.0 . . ?
H17A N17 H17B 120.0 . . ?
C21 N18 H18A 120.0 . . ?
C21 N18 H18B 120.0 . . ?
H18A N18 H18B 120.0 . . ?
C27 C26 H26A 109.5 . . ?
C27 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C27 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N19 C27 C26 143.3(11) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N20 C28 C29 173.3(19) . . ?
C25 O1 C23 120.4(11) . . ?
C22 C23 O1 110.2(12) . . ?
C22 C23 H23A 109.6 . . ?
O1 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
O1 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
O1 C25 C24 119.9(12) . . ?
O1 C25 H25A 107.3 . . ?
C24 C25 H25A 107.3 . . ?
O1 C25 H25B 107.3 . . ?
C24 C25 H25B 107.3 . . ?
H25A C25 H25B 106.9 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 N3 2.275(3) . ?
W1 S3 2.2820(11) . ?
W1 N5 2.289(3) . ?
W1 N1 2.290(3) . ?
W1 S1 2.3033(9) . ?
W1 S2 2.3117(10) . ?
W1 Cu3 2.6798(6) . ?
W1 Cu1 2.6878(7) . ?
W1 Cu2 2.7029(7) . ?
Br1 Cu1 2.3489(8) . ?
Cu1 S3 2.2408(11) . ?
Cu1 S2 2.2627(10) . ?
Cu1 Cu3 2.7950(9) . ?
Cu1 Br2 2.8350(7) . ?
Cu1 Cu2 2.8970(12) . ?
S1 Cu2 2.2541(10) . ?
S1 Cu3 2.2541(11) . ?
C1 C2 1.489(6) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 H1C 0.9700 . ?
C2 N1 1.325(4) . ?
C2 C3 1.409(5) . ?
C3 C4 1.360(5) . ?
C3 H3 0.9400 . ?
C4 N2 1.348(4) . ?
C4 C5 1.508(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 H5C 0.9700 . ?
C6 C7 1.493(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6C 0.9700 . ?
C7 N3 1.356(5) . ?
C7 C8 1.381(6) . ?
C8 C9 1.361(6) . ?
C8 H8 0.9400 . ?
C9 N4 1.356(5) . ?
C9 C10 1.512(6) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 H10C 0.9700 . ?
C11 C12 1.496(6) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 H11C 0.9700 . ?
C12 N5 1.358(5) . ?
C12 C13 1.378(6) . ?
C13 C14 1.359(6) . ?
C13 H13 0.9400 . ?
C14 N6 1.359(5) . ?
C14 C15 1.485(6) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C15 H15C 0.9700 . ?
C16 N10 1.329(4) . ?
C16 N8 1.352(4) . ?
C16 N7 1.355(4) . ?
C17 N9 1.335(4) . ?
C17 N11 1.343(4) . ?
C17 N8 1.355(4) . ?
C18 N12 1.335(4) . ?
C18 N9 1.346(4) . ?
C18 N7 1.349(4) . ?
C19 N16 1.316(5) . ?
C19 N14 1.323(4) . ?
C19 N13 1.367(4) . ?
C20 N14 1.334(5) . ?
C20 N17 1.344(4) . ?
C20 N15 1.356(4) . ?
C21 N18 1.329(4) . ?
C21 N15 1.334(4) . ?
C21 N13 1.374(4) . ?
N1 N2 1.382(4) . ?
B1 N4 1.505(5) . ?
B1 N6 1.526(5) . ?
B1 N2 1.527(5) . ?
B1 H1 0.9900 . ?
Cu2 N13 1.994(3) . ?
Cu2 S2 2.2409(10) . ?
Cu2 Br2 2.6966(8) . ?
Cu2 Cu3 2.8617(8) . ?
Br2 Cu3 2.7575(8) . ?
N3 N4 1.398(4) . ?
Cu3 N7 1.976(3) . ?
Cu3 S3 2.2501(10) . ?
N5 N6 1.367(4) . ?
N10 H10D 0.8700 . ?
N10 H10E 0.8700 . ?
N11 H11D 0.8700 . ?
N11 H11E 0.8700 . ?
N12 H12A 0.8700 . ?
N12 H12B 0.8700 . ?
N16 H16A 0.8700 . ?
N16 H16B 0.8700 . ?
N17 H17A 0.8700 . ?
N17 H17B 0.8700 . ?
N18 H18A 0.8700 . ?
N18 H18B 0.8700 . ?
N19 C27 1.121(15) . ?
C26 C27 1.565(12) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C26 H26C 0.9700 . ?
C29 C28 1.446(12) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C29 H29C 0.9700 . ?
N20 C28 1.215(12) . ?
O1 C25 1.333(18) . ?
O1 C23 1.384(19) . ?
C23 C22 1.288(19) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C25 C24 1.43(2) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C24 H24C 0.9700 . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22C 0.9700 . ?
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
N11 H11D Br1 0.87 2.81 3.495(3) 137.2 2
N12 H12A N9 0.87 2.10 2.965(4) 173.7 2
N11 H11E N15 0.87 2.13 2.997(4) 173.7 7_566
N18 H18A N8 0.87 2.16 3.014(4) 168.1 7_566
C26 H26A Br2 0.97 2.80 3.637(12) 144.7 7_566
N16 H16A Br1 0.87 2.56 3.394(3) 160.9 2_655
N17 H17A N14 0.87 2.40 3.096(4) 137.4 7_666
N17 H17B Br1 0.87 2.80 3.494(3) 137.5 8_566
N10 H10E S1 0.87 2.71 3.530(3) 157.7 .
N10 H10D N19 0.87 2.14 2.927(9) 150.5 .
N12 H12B S3 0.87 2.73 3.370(3) 131.4 .
N16 H16B S2 0.87 2.64 3.442(3) 154.4 .
N18 H18B Br2 0.87 2.79 3.449(3) 134.2 .
C1 H1A S1 0.97 2.74 3.434(4) 128.7 .
C6 H6A S2 0.97 2.71 3.360(4) 124.9 .
C11 H11A S3 0.97 2.83 3.493(5) 126.0 .
C11 H11C S1 0.97 2.80 3.484(4) 127.8 .
