# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CPX2
_database_code_depnum_ccdc_archive 'CCDC 1898197'
loop_
_audit_author_name
_audit_author_address
'Wen-Hua Zhang'
;Soochow University
China
;

_audit_update_record             
;
2019-02-19 deposited with the CCDC.	2019-05-06 downloaded from the CCDC.
;
_publcif_datablock.id            {39544c4d-e7cd-4718-afa5-b928b6c71c9d}

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H24 B Cu3 N9 S3 W'
_chemical_formula_weight         859.93

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'
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_H-M_alt        'C m c a'
_space_group_name_Hall           '-C 2bc 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   14.223(2)
_cell_length_b                   19.574(3)
_cell_length_c                   19.197(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5344.6(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    5726
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.48

_exptl_crystal_description       prism
_exptl_crystal_colour            black
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.137
_exptl_crystal_F_000             3320
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.120
_exptl_absorpt_coefficient_mu    6.908
_shelx_estimated_absorpt_T_min   0.339
_shelx_estimated_absorpt_T_max   0.491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3387
_exptl_absorpt_correction_T_max  0.4911
_exptl_absorpt_process_details   'SADABS, (Sheldrick 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker ApexII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            12665
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.064
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3167
_reflns_number_gt                2767
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+124.0792P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3167
_refine_ls_number_parameters     183
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1614
_refine_ls_wR_factor_gt          0.1551
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.000000 0.22317(2) 0.19182(2) 0.01360(17) Uani 1 2 d S T P . .
Cu1 Cu 0.10179(7) 0.30864(5) 0.11780(5) 0.0190(3) Uani 1 1 d . . . . .
Cu2 Cu 0.25917(11) 0.500000 0.000000 0.0304(4) Uani 1 2 d S T P . .
S1 S 0.000000 0.23632(14) 0.07093(14) 0.0160(5) Uani 1 2 d S T P . .
S2 S 0.12122(16) 0.28630(11) 0.22940(11) 0.0210(4) Uani 1 1 d . . . . .
B1 B 0.000000 0.0555(7) 0.2394(7) 0.023(3) Uani 1 2 d DS T P . .
H1B H 0.000000 -0.0005(12) 0.2577(9) 0.035 Uiso 1 2 d DS U P . .
N1 N 0.2061(5) 0.4201(4) 0.0397(4) 0.0274(17) Uani 1 1 d . . . . .
N2 N 0.4015(7) 0.500000 0.000000 0.023(2) Uani 1 2 d S T P . .
N3 N 0.0867(6) 0.0699(4) 0.1950(3) 0.0226(16) Uani 1 1 d D . . . .
N4 N 0.1059(5) 0.1355(3) 0.1724(4) 0.0176(14) Uani 1 1 d . . . . .
N5 N 0.000000 0.1029(6) 0.3034(5) 0.018(2) Uani 1 2 d DS T P . .
N6 N 0.000000 0.1723(5) 0.2963(5) 0.0158(19) Uani 1 2 d S T P . .
C1 C 0.1682(6) 0.3762(4) 0.0687(4) 0.0213(17) Uani 1 1 d . . . . .
C2 C 0.4513(6) 0.4426(4) -0.0094(5) 0.0236(18) Uani 1 1 d . . . . .
H2 H 0.418846 0.400730 -0.016309 0.028 Uiso 1 1 calc R U . . .
C3 C 0.1548(12) -0.0477(6) 0.1942(7) 0.058(4) Uani 1 1 d . . . . .
H3A H 0.209336 -0.071044 0.174071 0.088 Uiso 1 1 calc R U . . .
H3B H 0.097014 -0.066279 0.173825 0.088 Uiso 1 1 calc R U . . .
H3C H 0.154019 -0.054641 0.244711 0.088 Uiso 1 1 calc R U . . .
C4 C 0.1609(8) 0.0278(5) 0.1786(5) 0.033(2) Uani 1 1 d . . . . .
C5 C 0.2263(8) 0.0655(6) 0.1460(5) 0.037(3) Uani 1 1 d . . . . .
H5 H 0.284643 0.049602 0.128236 0.044 Uiso 1 1 calc R U . . .
C6 C 0.1929(6) 0.1320(5) 0.1431(4) 0.0203(17) Uani 1 1 d . . . . .
C7 C 0.2434(7) 0.1914(6) 0.1103(5) 0.031(2) Uani 1 1 d . . . . .
H7A H 0.206298 0.208901 0.071169 0.047 Uiso 1 1 calc R U . . .
H7B H 0.305041 0.176376 0.093468 0.047 Uiso 1 1 calc R U . . .
H7C H 0.251758 0.227688 0.144981 0.047 Uiso 1 1 calc R U . . .
C8 C 0.000000 0.0137(7) 0.3977(8) 0.033(3) Uani 1 2 d S T P . .
H8A H 0.000000 0.013709 0.448722 0.050 Uiso 0.5 2 calc R U P . .
H8B H -0.056257 -0.009961 0.380680 0.050 Uiso 0.25 1 calc R U P . .
H8C H 0.056257 -0.009961 0.380680 0.050 Uiso 0.25 1 calc R U P . .
H8D H 0.000000 -0.017851 0.357999 0.050 Uiso 0.5 2 calc R U P . .
H8E H 0.056257 0.005819 0.426042 0.050 Uiso 0.25 1 calc R U P . .
H8F H -0.056257 0.005819 0.426042 0.050 Uiso 0.25 1 calc R U P . .
C9 C 0.000000 0.0856(7) 0.3716(6) 0.020(2) Uani 1 2 d S T P . .
C10 C 0.000000 0.1455(8) 0.4093(6) 0.025(3) Uani 1 2 d S T P . .
H10 H 0.000000 0.149598 0.458628 0.030 Uiso 1 2 calc R U P . .
C11 C 0.000000 0.1995(7) 0.3611(6) 0.022(2) Uani 1 2 d S T P . .
C12 C 0.000000 0.2734(7) 0.3783(7) 0.033(3) Uani 1 2 d S T P . .
H12A H 0.000000 0.279166 0.428996 0.049 Uiso 0.5 2 calc R U P . .
H12B H 0.056257 0.294880 0.358601 0.049 Uiso 0.25 1 calc R U P . .
H12C H -0.056257 0.294880 0.358601 0.049 Uiso 0.25 1 calc R U P . .
H12D H 0.000000 0.300118 0.335135 0.049 Uiso 0.5 2 calc R U P . .
H12E H -0.056257 0.284404 0.405531 0.049 Uiso 0.25 1 calc R U P . .
H12F H 0.056257 0.284404 0.405531 0.049 Uiso 0.25 1 calc R U P . .


_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
W1 N6 2.239(9) . ?
W1 S2 2.241(2) 12 ?
W1 S2 2.241(2) . ?
W1 N4 2.314(7) 12 ?
W1 N4 2.314(7) . ?
W1 S1 2.335(3) . ?
W1 Cu1 2.6294(11) 12 ?
W1 Cu1 2.6294(11) . ?
Cu1 C1 1.879(9) . ?
Cu1 S2 2.204(2) . ?
Cu1 S1 2.216(2) . ?
Cu1 Cu1 2.896(2) 12 ?
Cu2 N1 1.896(8) . ?
Cu2 N1 1.896(8) 4_565 ?
Cu2 N2 2.025(11) . ?
B1 N3 1.525(11) 12 ?
B1 N3 1.525(11) . ?
B1 N5 1.539(17) . ?
B1 H1B 1.15(2) . ?
N1 C1 1.158(12) . ?
N2 C2 1.340(10) 4_565 ?
N2 C2 1.340(10) . ?
N3 C4 1.376(12) . ?
N3 N4 1.384(10) . ?
N4 C6 1.360(10) . ?
N5 C9 1.353(14) . ?
N5 N6 1.366(15) . ?
N6 C11 1.354(15) . ?
C2 C2 1.386(17) 12_655 ?
C2 H2 0.9500 . ?
C3 C4 1.509(15) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.342(17) . ?
C5 C6 1.388(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.505(14) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.494(18) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 H8D 0.9800 . ?
C8 H8E 0.9800 . ?
C8 H8F 0.9800 . ?
C9 C10 1.378(19) . ?
C10 C11 1.403(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.484(19) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C12 H12D 0.9800 . ?
C12 H12E 0.9800 . ?
C12 H12F 0.9800 . ?

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
N6 W1 S2 87.52(17) . 12 ?
N6 W1 S2 87.52(17) . . ?
S2 W1 S2 100.63(12) 12 . ?
N6 W1 N4 79.3(3) . 12 ?
S2 W1 N4 87.68(19) 12 12 ?
S2 W1 N4 164.16(19) . 12 ?
N6 W1 N4 79.3(3) . . ?
S2 W1 N4 164.16(19) 12 . ?
S2 W1 N4 87.68(19) . . ?
N4 W1 N4 81.3(4) 12 . ?
N6 W1 S1 159.9(3) . . ?
S2 W1 S1 105.03(7) 12 . ?
S2 W1 S1 105.03(7) . . ?
N4 W1 S1 85.50(18) 12 . ?
N4 W1 S1 85.50(18) . . ?
N6 W1 Cu1 140.08(13) . 12 ?
S2 W1 Cu1 53.09(6) 12 12 ?
S2 W1 Cu1 104.29(6) . 12 ?
N4 W1 Cu1 91.49(18) 12 12 ?
N4 W1 Cu1 138.02(17) . 12 ?
S1 W1 Cu1 52.61(6) . 12 ?
N6 W1 Cu1 140.08(13) . . ?
S2 W1 Cu1 104.29(6) 12 . ?
S2 W1 Cu1 53.09(6) . . ?
N4 W1 Cu1 138.02(17) 12 . ?
N4 W1 Cu1 91.49(18) . . ?
S1 W1 Cu1 52.61(6) . . ?
Cu1 W1 Cu1 66.82(5) 12 . ?
C1 Cu1 S2 124.3(3) . . ?
C1 Cu1 S1 125.1(3) . . ?
S2 Cu1 S1 110.48(10) . . ?
C1 Cu1 W1 174.7(3) . . ?
S2 Cu1 W1 54.37(6) . . ?
S1 Cu1 W1 56.85(7) . . ?
C1 Cu1 Cu1 120.2(3) . 12 ?
S2 Cu1 Cu1 97.20(6) . 12 ?
S1 Cu1 Cu1 49.20(5) . 12 ?
W1 Cu1 Cu1 56.59(2) . 12 ?
N1 Cu2 N1 133.1(5) . 4_565 ?
N1 Cu2 N2 113.5(2) . . ?
N1 Cu2 N2 113.5(2) 4_565 . ?
Cu1 S1 Cu1 81.60(11) . 12 ?
Cu1 S1 W1 70.54(8) . . ?
Cu1 S1 W1 70.54(8) 12 . ?
Cu1 S2 W1 72.54(7) . . ?
N3 B1 N3 107.9(10) 12 . ?
N3 B1 N5 109.6(7) 12 . ?
N3 B1 N5 109.6(7) . . ?
N3 B1 H1B 110.2(8) 12 . ?
N3 B1 H1B 110.2(8) . . ?
N5 B1 H1B 109.3(12) . . ?
C1 N1 Cu2 172.4(7) . . ?
C2 N2 C2 116.2(11) 4_565 . ?
C2 N2 Cu2 121.9(5) 4_565 . ?
C2 N2 Cu2 121.9(5) . . ?
C4 N3 N4 109.4(8) . . ?
C4 N3 B1 129.7(9) . . ?
N4 N3 B1 120.4(8) . . ?
C6 N4 N3 105.2(7) . . ?
C6 N4 W1 134.1(6) . . ?
N3 N4 W1 120.6(5) . . ?
C9 N5 N6 110.2(10) . . ?
C9 N5 B1 128.5(11) . . ?
N6 N5 B1 121.3(9) . . ?
C11 N6 N5 107.4(10) . . ?
C11 N6 W1 130.5(9) . . ?
N5 N6 W1 122.1(7) . . ?
N1 C1 Cu1 176.7(8) . . ?
N2 C2 C2 121.9(5) . 12_655 ?
N2 C2 H2 119.1 . . ?
C2 C2 H2 119.1 12_655 . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 N3 108.0(9) . . ?
C5 C4 C3 132.1(10) . . ?
N3 C4 C3 119.8(10) . . ?
C4 C5 C6 107.3(9) . . ?
C4 C5 H5 126.3 . . ?
C6 C5 H5 126.3 . . ?
N4 C6 C5 110.0(8) . . ?
N4 C6 C7 124.6(8) . . ?
C5 C6 C7 125.3(8) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C9 C8 H8D 109.5 . . ?
H8A C8 H8D 141.1 . . ?
H8B C8 H8D 56.3 . . ?
H8C C8 H8D 56.3 . . ?
C9 C8 H8E 109.5 . . ?
H8A C8 H8E 56.3 . . ?
H8B C8 H8E 141.1 . . ?
H8C C8 H8E 56.3 . . ?
H8D C8 H8E 109.5 . . ?
C9 C8 H8F 109.5 . . ?
H8A C8 H8F 56.3 . . ?
H8B C8 H8F 56.3 . . ?
H8C C8 H8F 141.1 . . ?
H8D C8 H8F 109.5 . . ?
H8E C8 H8F 109.5 . . ?
N5 C9 C10 107.2(11) . . ?
N5 C9 C8 124.0(12) . . ?
C10 C9 C8 128.8(11) . . ?
C9 C10 C11 107.1(10) . . ?
C9 C10 H10 126.4 . . ?
C11 C10 H10 126.4 . . ?
N6 C11 C10 108.1(11) . . ?
N6 C11 C12 125.9(12) . . ?
C10 C11 C12 126.0(12) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C12 H12D 109.5 . . ?
H12A C12 H12D 141.1 . . ?
H12B C12 H12D 56.3 . . ?
H12C C12 H12D 56.3 . . ?
C11 C12 H12E 109.5 . . ?
H12A C12 H12E 56.3 . . ?
H12B C12 H12E 141.1 . . ?
H12C C12 H12E 56.3 . . ?
H12D C12 H12E 109.5 . . ?
C11 C12 H12F 109.5 . . ?
H12A C12 H12F 56.3 . . ?
H12B C12 H12F 56.3 . . ?
H12C C12 H12F 141.1 . . ?
H12D C12 H12F 109.5 . . ?
H12E C12 H12F 109.5 . . ?

_refine_diff_density_max         1.574
_refine_diff_density_min         -2.926
_refine_diff_density_rms         0.206

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CPX3
_database_code_depnum_ccdc_archive 'CCDC 1898198'
loop_
_audit_author_name
_audit_author_address
'Wen-Hua Zhang'
;Soochow University
China
;

_audit_update_record             
;
2019-02-19 deposited with the CCDC.	2019-05-06 downloaded from the CCDC.
;
_publcif_datablock.id            {4e28baff-dbb4-4407-a54b-9b4036f79da8}

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C22 H26 B Cu3 N9 S3 W), C3 H7 N O'
_chemical_formula_sum            'C47 H59 B2 Cu6 N19 O S6 W2'
_chemical_formula_weight         1869.05

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'
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'
W W -0.8490 6.8722 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.2754(19)
_cell_length_b                   18.5717(18)
_cell_length_c                   19.6406(19)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7030.9(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9800
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      27.54

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_F_000             3640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    5.261
_shelx_estimated_absorpt_T_min   0.419
_shelx_estimated_absorpt_T_max   0.779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.363
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'

_exptl_special_details           ?

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            77834
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.096
_diffrn_reflns_theta_max         27.627
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8158
_reflns_number_gt                6664
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker D8 Quest'
_computing_cell_refinement       'Bruker D8 Quest'
_computing_data_reduction        'Bruker D8 Quest'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'publCIF (Westrip, 2010)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0414P)²+27.4088P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8158
_refine_ls_number_parameters     411
_refine_ls_number_restraints     33
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0286
_refine_ls_wR_factor_ref         0.0946
_refine_ls_wR_factor_gt          0.0826
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.003
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.19472(2) 0.69020(2) 0.02264(2) 0.01278(6) Uani 1 1 d . . . . .
Cu1 Cu 0.12067(3) 0.61220(3) -0.06189(3) 0.01749(12) Uani 1 1 d . . . . .
Cu2 Cu 0.12229(3) 0.76714(3) -0.06385(3) 0.01986(13) Uani 1 1 d . . . . .
Cu3 Cu 0.0000 0.48958(4) -0.2500 0.01986(17) Uani 1 2 d S T P . .
Cu4 Cu 0.0000 0.89009(4) -0.2500 0.0255(2) Uani 1 2 d S T P . .
S1 S 0.23151(6) 0.59703(7) -0.03952(5) 0.0187(2) Uani 1 1 d . . . . .
S2 S 0.07443(5) 0.69107(6) 0.00937(5) 0.0163(2) Uani 1 1 d . . . . .
S3 S 0.23271(6) 0.78311(7) -0.04063(6) 0.0203(2) Uani 1 1 d . . . . .
B1 B 0.2454(3) 0.6937(3) 0.1887(3) 0.0181(10) Uani 1 1 d D . . . .
H1B1 H 0.270(3) 0.696(3) 0.2411(15) 0.022 Uiso 1 1 d D U . . .
N1 N 0.0419(2) 0.5324(2) -0.1717(2) 0.0230(8) Uani 1 1 d . . . . .
N2 N 0.0462(3) 0.8496(2) -0.1743(2) 0.0346(11) Uani 1 1 d . . . . .
N3 N 0.0000 0.3811(3) -0.2500 0.0186(11) Uani 1 2 d S T P . .
N4 N 0.0000 -0.0008(3) -0.2500 0.0230(12) Uani 1 2 d S T P . .
N5 N 0.19935(18) 0.6278(2) 0.17592(18) 0.0169(8) Uani 1 1 d . . . . .
N6 N 0.17666(18) 0.6123(2) 0.11113(18) 0.0156(7) Uani 1 1 d . . . . .
N7 N 0.30815(18) 0.6904(2) 0.14078(19) 0.0159(7) Uani 1 1 d . . . . .
N8 N 0.29955(18) 0.6906(2) 0.07059(19) 0.0174(8) Uani 1 1 d . . . . .
N9 N 0.20355(18) 0.7620(2) 0.17308(19) 0.0177(8) Uani 1 1 d . . . . .
N10 N 0.17618(18) 0.7728(2) 0.10916(17) 0.0148(7) Uani 1 1 d . . . . .
C1 C 0.0712(2) 0.5604(2) -0.1284(2) 0.0149(8) Uani 1 1 d . . . . .
C2 C 0.0748(3) 0.8199(2) -0.1309(2) 0.0225(10) Uani 1 1 d . . . . .
C3 C -0.0104(2) 0.3433(2) -0.1922(2) 0.0192(9) Uani 1 1 d . . . . .
H3 H -0.0175 0.3690 -0.1509 0.023 Uiso 1 1 calc R U . . .
C4 C -0.0113(2) 0.2682(2) -0.1903(2) 0.0187(9) Uani 1 1 d . . . . .
H4 H -0.0194 0.2435 -0.1487 0.022 Uiso 1 1 calc R U . . .
C5 C 0.0000 0.2302(3) -0.2500 0.0159(12) Uani 1 2 d S T P . .
C6 C 0.0000 0.1493(3) -0.2500 0.0151(12) Uani 1 2 d S T P . .
C7 C 0.0254(2) 0.1112(2) -0.1943(2) 0.0187(9) Uani 1 1 d . . . . .
H7 H 0.0431 0.1358 -0.1556 0.022 Uiso 1 1 calc R U . . .
C8 C 0.0243(2) 0.0371(2) -0.1964(2) 0.0208(9) Uani 1 1 d . . . . .
H8 H 0.0416 0.0114 -0.1583 0.025 Uiso 1 1 calc R U . . .
C9 C 0.1971(3) 0.5786(3) 0.2942(3) 0.0336(13) Uani 1 1 d . . . . .
H9A H 0.2474 0.5802 0.3012 0.050 Uiso 1 1 calc R U . . .
H9B H 0.1780 0.5359 0.3168 0.050 Uiso 1 1 calc R U . . .
H9C H 0.1758 0.6220 0.3134 0.050 Uiso 1 1 calc R U . . .
C10 C 0.1818(2) 0.5749(3) 0.2192(2) 0.0210(9) Uani 1 1 d . . . . .
C11 C 0.1470(2) 0.5229(3) 0.1829(2) 0.0214(10) Uani 1 1 d . . . . .
H11 H 0.1284 0.4791 0.2000 0.026 Uiso 1 1 calc R U . . .
C12 C 0.1446(2) 0.5473(3) 0.1157(2) 0.0186(9) Uani 1 1 d . . . . .
C13 C 0.1112(3) 0.5071(3) 0.0582(2) 0.0236(10) Uani 1 1 d . . . . .
H13A H 0.0753 0.5373 0.0373 0.035 Uiso 1 1 calc R U . . .
H13B H 0.0900 0.4628 0.0757 0.035 Uiso 1 1 calc R U . . .
H13C H 0.1463 0.4948 0.0241 0.035 Uiso 1 1 calc R U . . .
C14 C 0.4033(3) 0.6897(3) 0.2268(3) 0.0328(13) Uani 1 1 d . . . . .
H14A H 0.3934 0.7364 0.2479 0.049 Uiso 1 1 calc R U . . .
H14B H 0.4536 0.6817 0.2261 0.049 Uiso 1 1 calc R U . . .
H14C H 0.3809 0.6514 0.2530 0.049 Uiso 1 1 calc R U . . .
C15 C 0.3761(2) 0.6893(3) 0.1555(2) 0.0214(10) Uani 1 1 d . . . . .
C16 C 0.4125(2) 0.6891(3) 0.0957(3) 0.0249(10) Uani 1 1 d . . . . .
H16 H 0.4615 0.6890 0.0909 0.030 Uiso 1 1 calc R U . . .
C17 C 0.3642(2) 0.6893(3) 0.0433(2) 0.0217(10) Uani 1 1 d . . . . .
C18 C 0.3797(3) 0.6882(3) -0.0314(3) 0.0330(13) Uani 1 1 d . . . . .
H18A H 0.4300 0.6911 -0.0384 0.049 Uiso 1 1 calc R U . . .
H18B H 0.3572 0.7294 -0.0534 0.049 Uiso 1 1 calc R U . . .
H18C H 0.3621 0.6434 -0.0513 0.049 Uiso 1 1 calc R U . . .
C19 C 0.2106(3) 0.8213(3) 0.2871(3) 0.0351(13) Uani 1 1 d . . . . .
H19A H 0.1918 0.7792 0.3108 0.053 Uiso 1 1 calc R U . . .
H19B H 0.1924 0.8653 0.3080 0.053 Uiso 1 1 calc R U . . .
H19C H 0.2614 0.8211 0.2905 0.053 Uiso 1 1 calc R U . . .
C20 C 0.1897(2) 0.8188(3) 0.2134(2) 0.0217(10) Uani 1 1 d . . . . .
C21 C 0.1529(2) 0.8681(3) 0.1756(2) 0.0223(10) Uani 1 1 d . . . . .
H21 H 0.1362 0.9136 0.1906 0.027 Uiso 1 1 calc R U . . .
C22 C 0.1450(2) 0.8383(3) 0.1114(2) 0.0176(9) Uani 1 1 d . . . . .
C23 C 0.1056(3) 0.8734(3) 0.0542(2) 0.0244(10) Uani 1 1 d . . . . .
H23A H 0.1363 0.8792 0.0148 0.037 Uiso 1 1 calc R U . . .
H23B H 0.0889 0.9207 0.0689 0.037 Uiso 1 1 calc R U . . .
H23C H 0.0660 0.8431 0.0416 0.037 Uiso 1 1 calc R U . . .
O1 O 0.0948(6) 1.0854(7) -0.0414(5) 0.069(3) Uani 0.5 1 d . U P . .
N11 N 0.1375(5) 1.0927(6) 0.0594(6) 0.043(2) Uani 0.5 1 d . U P . .
C24 C 0.1451(7) 1.1220(6) 0.1142(9) 0.056(3) Uani 0.5 1 d . U P . .
H24A H 0.1893 1.1481 0.1146 0.084 Uiso 0.5 1 calc R U P . .
H24B H 0.1451 1.0857 0.1504 0.084 Uiso 0.5 1 calc R U P . .
H24C H 0.1070 1.1560 0.1218 0.084 Uiso 0.5 1 calc R U P . .
C25 C 0.1970(7) 1.0448(8) 0.0479(8) 0.053(3) Uani 0.5 1 d . U P . .
H25A H 0.1958 1.0268 0.0010 0.080 Uiso 0.5 1 calc R U P . .
H25B H 0.1947 1.0042 0.0796 0.080 Uiso 0.5 1 calc R U P . .
H25C H 0.2401 1.0716 0.0553 0.080 Uiso 0.5 1 calc R U P . .
C26 C 0.1046(8) 1.1043(7) 0.0179(7) 0.046(3) Uani 0.5 1 d . U P . .
H26 H 0.0725 1.1408 0.0301 0.055 Uiso 0.5 1 calc R U P . .


_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
W1 N8 2.229(4) . ?
W1 S1 2.2333(12) . ?
W1 S3 2.2489(12) . ?
W1 N6 2.288(4) . ?
W1 N10 2.317(4) . ?
W1 S2 2.3334(11) . ?
W1 Cu2 2.6224(6) . ?
W1 Cu1 2.6254(6) . ?
Cu1 C1 1.880(4) . ?
Cu1 S1 2.1993(12) . ?
Cu1 S2 2.2132(12) . ?
Cu1 Cu2 2.8779(9) . ?
Cu2 C2 1.879(5) . ?
Cu2 S3 2.1968(13) . ?
Cu2 S2 2.2169(12) . ?
Cu3 N1 1.910(4) . ?
Cu3 N1 1.910(4) 3_554 ?
Cu3 N3 2.015(5) . ?
Cu4 N2 1.889(4) . ?
Cu4 N2 1.889(4) 3_554 ?
Cu4 N4 2.026(6) 1_565 ?
B1 N5 1.533(6) . ?
B1 N7 1.533(6) . ?
B1 N9 1.534(6) . ?
B1 H1B1 1.134(19) . ?
N1 C1 1.148(6) . ?
N2 C2 1.156(6) . ?
N3 C3 1.350(5) 3_554 ?
N3 C3 1.350(5) . ?
N4 C8 1.350(5) 3_554 ?
N4 C8 1.350(5) . ?
N4 Cu4 2.026(6) 1_545 ?
N5 C10 1.343(6) . ?
N5 N6 1.376(5) . ?
N6 C12 1.360(6) . ?
N7 C15 1.342(5) . ?
N7 N8 1.389(5) . ?
N8 C17 1.357(6) . ?
N9 C20 1.346(6) . ?
N9 N10 1.377(5) . ?
N10 C22 1.358(6) . ?
C3 C4 1.396(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(5) . ?
C4 H4 0.9500 . ?
C5 C4 1.386(5) 3_554 ?
C5 C6 1.503(8) . ?
C6 C7 1.392(5) 3_554 ?
C6 C7 1.392(5) . ?
C7 C8 1.376(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C10 1.504(6) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.374(7) . ?
C11 C12 1.396(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.498(6) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.495(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.369(7) . ?
C16 C17 1.387(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.497(7) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.502(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C21 1.376(7) . ?
C21 C22 1.386(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.504(6) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
O1 C26 1.231(16) . ?
N11 C26 1.055(17) . ?
N11 C24 1.215(18) . ?
N11 C25 1.469(18) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 0.9500 . ?

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
N8 W1 S1 86.87(10) . . ?
N8 W1 S3 86.33(10) . . ?
S1 W1 S3 100.90(4) . . ?
N8 W1 N6 79.57(13) . . ?
S1 W1 N6 88.50(10) . . ?
S3 W1 N6 162.63(10) . . ?
N8 W1 N10 80.10(13) . . ?
S1 W1 N10 164.35(9) . . ?
S3 W1 N10 86.98(9) . . ?
N6 W1 N10 80.68(13) . . ?
N8 W1 S2 161.42(10) . . ?
S1 W1 S2 105.05(4) . . ?
S3 W1 S2 104.86(4) . . ?
N6 W1 S2 86.45(9) . . ?
N10 W1 S2 85.65(9) . . ?
N8 W1 Cu2 138.99(10) . . ?
S1 W1 Cu2 103.72(3) . . ?
S3 W1 Cu2 52.94(3) . . ?
N6 W1 Cu2 139.08(9) . . ?
N10 W1 Cu2 91.84(9) . . ?
S2 W1 Cu2 52.76(3) . . ?
N8 W1 Cu1 139.60(10) . . ?
S1 W1 Cu1 53.08(3) . . ?
S3 W1 Cu1 104.53(3) . . ?
N6 W1 Cu1 92.80(9) . . ?
N10 W1 Cu1 138.18(9) . . ?
S2 W1 Cu1 52.62(3) . . ?
Cu2 W1 Cu1 66.516(19) . . ?
C1 Cu1 S1 124.43(13) . . ?
C1 Cu1 S2 124.98(13) . . ?
S1 Cu1 S2 110.46(5) . . ?
C1 Cu1 W1 175.26(13) . . ?
S1 Cu1 W1 54.28(3) . . ?
S2 Cu1 W1 56.90(3) . . ?
C1 Cu1 Cu2 120.49(13) . . ?
S1 Cu1 Cu2 96.91(4) . . ?
S2 Cu1 Cu2 49.54(3) . . ?
W1 Cu1 Cu2 56.691(16) . . ?
C2 Cu2 S3 123.17(16) . . ?
C2 Cu2 S2 125.73(16) . . ?
S3 Cu2 S2 110.77(5) . . ?
C2 Cu2 W1 175.80(16) . . ?
S3 Cu2 W1 54.78(3) . . ?
S2 Cu2 W1 56.92(3) . . ?
C2 Cu2 Cu1 121.70(14) . . ?
S3 Cu2 Cu1 98.21(4) . . ?
S2 Cu2 Cu1 49.43(3) . . ?
W1 Cu2 Cu1 56.793(16) . . ?
N1 Cu3 N1 130.8(2) . 3_554 ?
N1 Cu3 N3 114.58(12) . . ?
N1 Cu3 N3 114.58(12) 3_554 . ?
N2 Cu4 N2 133.1(3) . 3_554 ?
N2 Cu4 N4 113.43(14) . 1_565 ?
N2 Cu4 N4 113.43(14) 3_554 1_565 ?
Cu1 S1 W1 72.64(4) . . ?
Cu1 S2 Cu2 81.03(4) . . ?
Cu1 S2 W1 70.49(3) . . ?
Cu2 S2 W1 70.33(3) . . ?
Cu2 S3 W1 72.28(4) . . ?
N5 B1 N7 108.9(4) . . ?
N5 B1 N9 108.8(4) . . ?
N7 B1 N9 109.0(4) . . ?
N5 B1 H1B1 115(3) . . ?
N7 B1 H1B1 103(3) . . ?
N9 B1 H1B1 112(3) . . ?
C1 N1 Cu3 174.1(4) . . ?
C2 N2 Cu4 174.6(4) . . ?
C3 N3 C3 117.4(5) 3_554 . ?
C3 N3 Cu3 121.3(3) 3_554 . ?
C3 N3 Cu3 121.3(3) . . ?
C8 N4 C8 117.1(6) 3_554 . ?
C8 N4 Cu4 121.5(3) 3_554 1_545 ?
C8 N4 Cu4 121.5(3) . 1_545 ?
C10 N5 N6 110.6(4) . . ?
C10 N5 B1 128.9(4) . . ?
N6 N5 B1 120.2(4) . . ?
C12 N6 N5 105.6(3) . . ?
C12 N6 W1 132.9(3) . . ?
N5 N6 W1 121.5(3) . . ?
C15 N7 N8 109.3(4) . . ?
C15 N7 B1 129.6(4) . . ?
N8 N7 B1 121.0(3) . . ?
C17 N8 N7 106.4(3) . . ?
C17 N8 W1 131.7(3) . . ?
N7 N8 W1 121.8(3) . . ?
C20 N9 N10 110.3(4) . . ?
C20 N9 B1 129.4(4) . . ?
N10 N9 B1 120.3(4) . . ?
C22 N10 N9 105.8(3) . . ?
C22 N10 W1 133.2(3) . . ?
N9 N10 W1 120.9(3) . . ?
N1 C1 Cu1 175.7(4) . . ?
N2 C2 Cu2 176.6(4) . . ?
N3 C3 C4 122.9(4) . . ?
N3 C3 H3 118.5 . . ?
C4 C3 H3 118.5 . . ?
C5 C4 C3 119.0(4) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C4 118.8(6) 3_554 . ?
C4 C5 C6 120.6(3) 3_554 . ?
C4 C5 C6 120.6(3) . . ?
C7 C6 C7 118.9(6) 3_554 . ?
C7 C6 C5 120.6(3) 3_554 . ?
C7 C6 C5 120.6(3) . . ?
C8 C7 C6 118.6(4) . . ?
C8 C7 H7 120.7 . . ?
C6 C7 H7 120.7 . . ?
N4 C8 C7 123.4(4) . . ?
N4 C8 H8 118.3 . . ?
C7 C8 H8 118.3 . . ?
C10 C9 H9A 109.5 . . ?
C10 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C10 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N5 C10 C11 108.0(4) . . ?
N5 C10 C9 122.4(5) . . ?
C11 C10 C9 129.5(4) . . ?
C10 C11 C12 106.2(4) . . ?
C10 C11 H11 126.9 . . ?
C12 C11 H11 126.9 . . ?
N6 C12 C11 109.6(4) . . ?
N6 C12 C13 126.0(4) . . ?
C11 C12 C13 124.4(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 H14A 109.5 . . ?
C15 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C15 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N7 C15 C16 108.4(4) . . ?
N7 C15 C14 123.0(4) . . ?
C16 C15 C14 128.6(4) . . ?
C15 C16 C17 107.0(4) . . ?
C15 C16 H16 126.5 . . ?
C17 C16 H16 126.5 . . ?
N8 C17 C16 108.9(4) . . ?
N8 C17 C18 124.8(4) . . ?
C16 C17 C18 126.3(4) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N9 C20 C21 107.8(4) . . ?
N9 C20 C19 122.5(4) . . ?
C21 C20 C19 129.6(5) . . ?
C20 C21 C22 106.5(4) . . ?
C20 C21 H21 126.8 . . ?
C22 C21 H21 126.8 . . ?
N10 C22 C21 109.7(4) . . ?
N10 C22 C23 126.0(4) . . ?
C21 C22 C23 124.3(4) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C26 N11 C24 131.8(15) . . ?
C26 N11 C25 118.2(15) . . ?
C24 N11 C25 108.3(13) . . ?
N11 C24 H24A 109.5 . . ?
N11 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N11 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N11 C25 H25A 109.5 . . ?
N11 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N11 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N11 C26 O1 140.0(17) . . ?
N11 C26 H26 110.0 . . ?
O1 C26 H26 110.0 . . ?

_refine_diff_density_max         2.002
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.173

_shelxl_version_number           2013-2


####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CPX4
_database_code_depnum_ccdc_archive 'CCDC 1898199'
loop_
_audit_author_name
_audit_author_address
'Wen-Hua Zhang'
;Soochow University
China
;

_audit_update_record             
;
2019-02-19 deposited with the CCDC.	2019-05-06 downloaded from the CCDC.
;
_publcif_datablock.id            {91ec3bf9-bef2-473a-98ac-e38e7b06959c}

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C25 H28 B Cu3 N9 S3 W, 1.5(C1.50 H3.50 N0.50 O0.50)'
_chemical_formula_sum            'C28 H35 B Cu3 N10 O S3 W'
_chemical_formula_weight         1009.12

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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           54
_space_group_name_H-M_alt        'P c c a'
_space_group_name_Hall           '-P 2a 2ac'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   19.161(3)
_cell_length_b                   22.823(4)
_cell_length_c                   19.486(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     8521(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    3370
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      27.11

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             3960
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    4.348
_shelx_estimated_absorpt_T_min   0.477
_shelx_estimated_absorpt_T_max   0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.599
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_process_details   'SADABS, Sheldrick, 2008'

_exptl_special_details           ?

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            40376
_diffrn_reflns_av_unetI/netI     0.1041
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.737
_diffrn_reflns_theta_max         27.501
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9749
_reflns_number_gt                5972
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker D8 Quest'
_computing_cell_refinement       'Bruker D8 Quest'
_computing_data_reduction        'Bruker D8 Quest'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXL-2013 (Sheldrick, 2013)'
_computing_publication_material  'publCIF (Westrip, 2010)'

_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1370P)²+83.7051P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9749
_refine_ls_number_parameters     370
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1388
_refine_ls_R_factor_gt           0.0877
_refine_ls_wR_factor_ref         0.2557
_refine_ls_wR_factor_gt          0.2194
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.002
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 1.19557(2) 0.65580(2) -0.02499(2) 0.00915(16) Uani 1 1 d . . . . .
Cu1 Cu 1.12109(8) 0.59278(7) 0.06074(7) 0.0136(3) Uani 1 1 d . . . . .
Cu2 Cu 1.12439(8) 0.71935(8) 0.06233(8) 0.0166(4) Uani 1 1 d . . . . .
Cu3 Cu 1.0000 0.49210(10) 0.2500 0.0158(5) Uani 1 2 d S T P . .
Cu4 Cu 1.0000 0.81726(11) 0.2500 0.0278(6) Uani 1 2 d S T P . .
S1 S 1.23214(16) 0.57971(15) 0.03750(15) 0.0150(7) Uani 1 1 d . . . . .
S2 S 1.07469(15) 0.65766(15) -0.01067(14) 0.0121(6) Uani 1 1 d . . . . .
S3 S 1.23546(17) 0.73128(16) 0.03809(15) 0.0169(7) Uani 1 1 d . . . . .
B1 B 1.2448(7) 0.6597(7) -0.1931(7) 0.014(3) Uani 1 1 d D . . . .
H1B1 H 1.2607 0.6607 -0.2419 0.017 Uiso 1 1 calc DR U . . .
N1 N 1.0413(6) 0.5277(5) 0.1711(5) 0.020(3) Uani 1 1 d . . . . .
N2 N 1.0466(7) 0.7853(5) 0.1713(6) 0.025(2) Uani 1 1 d . . . . .
N3 N 1.0000 0.4046(7) 0.2500 0.0253(17) Uani 1 2 d S T P . .
N4 N 1.0000 -0.0953(7) 0.2500 0.0253(17) Uani 1 2 d S T P . .
N5 N 1.1988(5) 0.6053(5) -0.1797(5) 0.0114(9) Uani 1 1 d . . . . .
N6 N 1.1762(5) 0.5931(5) -0.1140(5) 0.0114(9) Uani 1 1 d . . . . .
N7 N 1.3087(5) 0.6552(5) -0.1434(5) 0.0114(9) Uani 1 1 d . . . . .
N8 N 1.3001(5) 0.6541(5) -0.0746(5) 0.0114(9) Uani 1 1 d . . . . .
N9 N 1.2047(5) 0.7143(5) -0.1758(5) 0.0114(9) Uani 1 1 d . . . . .
N10 N 1.1780(5) 0.7233(5) -0.1117(5) 0.0114(9) Uani 1 1 d . . . . .
C1 C 1.0714(6) 0.5500(5) 0.1276(6) 0.009(2) Uani 1 1 d . . . . .
C2 C 1.0762(8) 0.7628(6) 0.1281(7) 0.025(2) Uani 1 1 d . . . . .
C3 C 0.9890(7) 0.3731(6) 0.1917(7) 0.020(3) Uani 1 1 d . . . . .
H3 H 0.9813 0.3938 0.1500 0.024 Uiso 1 1 calc R U . . .
C4 C 0.9886(7) 0.3124(6) 0.1900(7) 0.017(3) Uani 1 1 d . . . . .
H4 H 0.9807 0.2919 0.1483 0.020 Uiso 1 1 calc R U . . .
C5 C 1.0000 0.2827(9) 0.2500 0.0253(17) Uani 1 2 d S T P . .
C6 C 1.0000 0.2177(9) 0.2500 0.0253(17) Uani 1 2 d S T P . .
C7 C 1.0285(8) 0.1859(6) 0.1947(10) 0.034(4) Uani 1 1 d . . . . .
H7 H 1.0503 0.2064 0.1582 0.041 Uiso 1 1 calc R U . . .
C8 C 1.0253(9) 0.1253(7) 0.1925(9) 0.035(4) Uani 1 1 d . . . . .
H8 H 1.0401 0.1046 0.1528 0.042 Uiso 1 1 calc R U . . .
C9 C 1.0000 0.0947(9) 0.2500 0.0253(17) Uani 1 2 d S T P . .
C10 C 1.0000 0.0291(9) 0.2500 0.0253(17) Uani 1 2 d S T P . .
C11 C 1.0014(13) -0.0034(8) 0.1891(12) 0.064(7) Uani 1 1 d . . . . .
H11 H 1.0015 0.0159 0.1460 0.077 Uiso 1 1 calc R U . . .
C12 C 1.0028(13) -0.0645(8) 0.1924(12) 0.066(7) Uani 1 1 d . . . . .
H12 H 1.0060 -0.0854 0.1504 0.080 Uiso 1 1 calc R U . . .
C13 C 1.1974(8) 0.5638(7) -0.2960(7) 0.027(3) Uani 1 1 d . . . . .
H13A H 1.1728 0.5321 -0.3196 0.040 Uiso 1 1 calc R U . . .
H13B H 1.2478 0.5593 -0.3027 0.040 Uiso 1 1 calc R U . . .
H13C H 1.1824 0.6016 -0.3148 0.040 Uiso 1 1 calc R U . . .
C14 C 1.1820(7) 0.5618(6) -0.2250(7) 0.019(3) Uani 1 1 d . . . . .
C15 C 1.1474(6) 0.5201(6) -0.1862(7) 0.017(3) Uani 1 1 d . . . . .
H15 H 1.1289 0.4841 -0.2025 0.021 Uiso 1 1 calc R U . . .
C16 C 1.1445(6) 0.5407(5) -0.1179(6) 0.011(2) Uani 1 1 d . . . . .
C17 C 1.1119(7) 0.5073(6) -0.0608(7) 0.019(3) Uani 1 1 d . . . . .
H17A H 1.1484 0.4930 -0.0298 0.029 Uiso 1 1 calc R U . . .
H17B H 1.0859 0.4740 -0.0795 0.029 Uiso 1 1 calc R U . . .
H17C H 1.0800 0.5329 -0.0355 0.029 Uiso 1 1 calc R U . . .
C18 C 1.4043(8) 0.6548(8) -0.2329(7) 0.035(4) Uani 1 1 d . . . . .
H18A H 1.3646 0.6553 -0.2645 0.053 Uiso 1 1 calc R U . . .
H18B H 1.4330 0.6201 -0.2418 0.053 Uiso 1 1 calc R U . . .
H18C H 1.4325 0.6902 -0.2397 0.053 Uiso 1 1 calc R U . . .
C19 C 1.3781(6) 0.6531(6) -0.1601(6) 0.014(2) Uani 1 1 d . . . . .
C20 C 1.4155(7) 0.6517(6) -0.1000(7) 0.023(3) Uani 1 1 d . . . . .
H20 H 1.4649 0.6510 -0.0955 0.028 Uiso 1 1 calc R U . . .
C21 C 1.3661(6) 0.6514(6) -0.0464(7) 0.018(2) Uani 1 1 d . . . . .
C22 C 1.3804(6) 0.6477(6) 0.0271(6) 0.018(2) Uani 1 1 d . . . . .
H22A H 1.4202 0.6728 0.0385 0.026 Uiso 1 1 calc R U . . .
H22B H 1.3912 0.6070 0.0394 0.026 Uiso 1 1 calc R U . . .
H22C H 1.3392 0.6607 0.0528 0.026 Uiso 1 1 calc R U . . .
C23 C 1.2123(9) 0.7641(8) -0.2910(7) 0.034(4) Uani 1 1 d . . . . .
H23A H 1.2632 0.7614 -0.2948 0.051 Uiso 1 1 calc R U . . .
H23B H 1.1965 0.8013 -0.3108 0.051 Uiso 1 1 calc R U . . .
H23C H 1.1908 0.7315 -0.3159 0.051 Uiso 1 1 calc R U . . .
C24 C 1.1916(7) 0.7614(6) -0.2168(6) 0.018(3) Uani 1 1 d . . . . .
C25 C 1.1550(7) 0.8011(6) -0.1781(7) 0.019(3) Uani 1 1 d . . . . .
H25 H 1.1387 0.8383 -0.1929 0.023 Uiso 1 1 calc R U . . .
C26 C 1.1461(6) 0.7773(6) -0.1139(6) 0.013(2) Uani 1 1 d . . . . .
C27 C 1.1106(7) 0.8066(6) -0.0561(7) 0.022(3) Uani 1 1 d . . . . .
H27A H 1.0691 0.7841 -0.0431 0.033 Uiso 1 1 calc R U . . .
H27B H 1.0966 0.8462 -0.0700 0.033 Uiso 1 1 calc R U . . .
H27C H 1.1425 0.8090 -0.0169 0.033 Uiso 1 1 calc R U . . .
O1 O 1.1709(19) 0.0526(13) 0.1198(19) 0.100(8) Uani 0.5 1 d D . P . .
N11 N 1.267(2) 0.0809(16) 0.1743(18) 0.100(8) Uani 0.5 1 d D . P . .
C28 C 1.306(3) 0.089(2) 0.112(2) 0.100(8) Uani 0.5 1 d D . P . .
H28A H 1.3544 0.0997 0.1233 0.149 Uiso 0.5 1 calc R U P . .
H28B H 1.2848 0.1202 0.0846 0.149 Uiso 0.5 1 calc R U P . .
H28C H 1.3061 0.0524 0.0856 0.149 Uiso 0.5 1 calc R U P . .
C29 C 1.306(2) 0.086(2) 0.237(2) 0.100(8) Uani 0.5 1 d D . P . .
H29A H 1.3540 0.0973 0.2272 0.149 Uiso 0.5 1 calc R U P . .
H29B H 1.3054 0.0483 0.2614 0.149 Uiso 0.5 1 calc R U P . .
H29C H 1.2841 0.1160 0.2665 0.149 Uiso 0.5 1 calc R U P . .
C30 C 1.2009(19) 0.066(2) 0.175(2) 0.100(8) Uani 0.5 1 d D . P . .
H30 H 1.1759 0.0655 0.2173 0.119 Uiso 0.5 1 calc R U P . .
O2 O 1.1529(13) 0.0694(9) -0.1169(11) 0.042(4) Uani 0.5 1 d D . P . .
N12 N 1.1286(15) 0.1563(9) -0.0629(13) 0.042(4) Uani 0.5 1 d D . P . .
C31 C 1.0819(19) 0.1827(14) -0.0144(16) 0.042(4) Uani 0.5 1 d D . P . .
H31A H 1.0677 0.1534 0.0197 0.064 Uiso 0.5 1 calc R U P . .
H31B H 1.0405 0.1974 -0.0384 0.064 Uiso 0.5 1 calc R U P . .
H31C H 1.1055 0.2153 0.0088 0.064 Uiso 0.5 1 calc R U P . .
C32 C 1.155(2) 0.1945(12) -0.1155(16) 0.042(4) Uani 0.5 1 d D . P . .
H32A H 1.1895 0.1737 -0.1431 0.064 Uiso 0.5 1 calc R U P . .
H32B H 1.1762 0.2290 -0.0943 0.064 Uiso 0.5 1 calc R U P . .
H32C H 1.1160 0.2070 -0.1450 0.064 Uiso 0.5 1 calc R U P . .
C33 C 1.1402(19) 0.1002(10) -0.0647(14) 0.042(4) Uani 0.5 1 d D . P . .
H33 H 1.1390 0.0802 -0.0220 0.051 Uiso 0.5 1 calc R U P . .


_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
W1 N8 2.224(9) . ?
W1 S1 2.234(3) . ?
W1 S3 2.250(3) . ?
W1 N6 2.279(10) . ?
W1 N10 2.311(10) . ?
W1 S2 2.333(3) . ?
W1 Cu2 2.6190(16) . ?
W1 Cu1 2.6260(16) . ?
Cu1 C1 1.887(12) . ?
Cu1 S1 2.196(3) . ?
Cu1 S2 2.218(3) . ?
Cu1 Cu2 2.890(2) . ?
Cu2 C2 1.865(14) . ?
Cu2 S3 2.197(4) . ?
Cu2 S2 2.217(3) . ?
Cu3 N1 1.911(12) 3_755 ?
Cu3 N1 1.911(12) . ?
Cu3 N3 1.996(17) . ?
Cu4 N2 1.919(11) . ?
Cu4 N2 1.919(11) 3_755 ?
Cu4 N4 1.995(17) 1_565 ?
B1 N9 1.503(18) . ?
B1 N5 1.546(18) . ?
B1 N7 1.565(16) . ?
B1 H1B1 1.0000 . ?
N1 C1 1.143(16) . ?
N2 C2 1.138(17) . ?
N3 C3 1.361(15) 3_755 ?
N3 C3 1.361(15) . ?
N4 C12 1.33(2) . ?
N4 C12 1.33(2) 3_755 ?
N4 Cu4 1.995(17) 1_545 ?
N5 C14 1.367(16) . ?
N5 N6 1.380(13) . ?
N6 C16 1.343(16) . ?
N7 N8 1.350(13) . ?
N7 C19 1.371(15) . ?
N8 C21 1.381(15) . ?
N9 C24 1.361(17) . ?
N9 N10 1.365(13) . ?
N10 C26 1.375(16) . ?
C3 C4 1.386(18) . ?
C3 H3 0.9500 . ?
C4 C5 1.368(16) . ?
C4 H4 0.9500 . ?
C5 C4 1.368(16) 3_755 ?
C5 C6 1.48(3) . ?
C6 C7 1.409(19) . ?
C6 C7 1.409(19) 3_755 ?
C7 C8 1.39(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.406(19) . ?
C8 H8 0.9500 . ?
C9 C8 1.406(19) 3_755 ?
C9 C10 1.50(3) . ?
C10 C11 1.40(2) 3_755 ?
C10 C11 1.40(2) . ?
C11 C12 1.39(2) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.415(18) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.385(19) . ?
C15 C16 1.412(16) . ?
C15 H15 0.9500 . ?
C16 C17 1.486(17) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.505(18) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.372(18) . ?
C20 C21 1.410(18) . ?
C20 H20 0.9500 . ?
C21 C22 1.461(17) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C24 1.501(17) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.373(18) . ?
C25 C26 1.374(17) . ?
C25 H25 0.9500 . ?
C26 C27 1.476(16) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O1 C30 1.264(19) . ?
N11 C30 1.312(18) . ?
N11 C28 1.438(19) . ?
N11 C29 1.441(19) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30 0.9500 . ?
O2 C33 1.260(17) . ?
N12 C33 1.301(17) . ?
N12 C31 1.435(17) . ?
N12 C32 1.435(18) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33 0.9500 . ?

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
N8 W1 S1 86.6(3) . . ?
N8 W1 S3 86.8(3) . . ?
S1 W1 S3 101.00(12) . . ?
N8 W1 N6 78.8(4) . . ?
S1 W1 N6 88.7(3) . . ?
S3 W1 N6 162.2(3) . . ?
N8 W1 N10 79.9(3) . . ?
S1 W1 N10 164.3(3) . . ?
S3 W1 N10 86.5(3) . . ?
N6 W1 N10 80.7(4) . . ?
N8 W1 S2 161.1(3) . . ?
S1 W1 S2 105.09(11) . . ?
S3 W1 S2 104.95(12) . . ?
N6 W1 S2 86.6(3) . . ?
N10 W1 S2 86.0(2) . . ?
N8 W1 Cu2 139.5(3) . . ?
S1 W1 Cu2 103.87(9) . . ?
S3 W1 Cu2 52.98(9) . . ?
N6 W1 Cu2 139.2(2) . . ?
N10 W1 Cu2 91.7(2) . . ?
S2 W1 Cu2 52.79(8) . . ?
N8 W1 Cu1 139.2(3) . . ?
S1 W1 Cu1 52.98(9) . . ?
S3 W1 Cu1 104.86(9) . . ?
N6 W1 Cu1 93.0(3) . . ?
N10 W1 Cu1 138.7(2) . . ?
S2 W1 Cu1 52.73(8) . . ?
Cu2 W1 Cu1 66.86(5) . . ?
C1 Cu1 S1 124.2(4) . . ?
C1 Cu1 S2 125.2(4) . . ?
S1 Cu1 S2 110.47(13) . . ?
C1 Cu1 W1 175.8(4) . . ?
S1 Cu1 W1 54.31(9) . . ?
S2 Cu1 W1 56.84(8) . . ?
C1 Cu1 Cu2 121.4(4) . . ?
S1 Cu1 Cu2 96.70(11) . . ?
S2 Cu1 Cu2 49.31(9) . . ?
W1 Cu1 Cu2 56.45(5) . . ?
C2 Cu2 S3 124.2(5) . . ?
C2 Cu2 S2 124.5(5) . . ?
S3 Cu2 S2 110.91(13) . . ?
C2 Cu2 W1 177.1(5) . . ?
S3 Cu2 W1 54.87(9) . . ?
S2 Cu2 W1 56.97(8) . . ?
C2 Cu2 Cu1 121.9(4) . . ?
S3 Cu2 Cu1 98.21(11) . . ?
S2 Cu2 Cu1 49.36(9) . . ?
W1 Cu2 Cu1 56.69(5) . . ?
N1 Cu3 N1 129.7(7) 3_755 . ?
N1 Cu3 N3 115.2(3) 3_755 . ?
N1 Cu3 N3 115.2(3) . . ?
N2 Cu4 N2 135.2(7) . 3_755 ?
N2 Cu4 N4 112.4(4) . 1_565 ?
N2 Cu4 N4 112.4(4) 3_755 1_565 ?
Cu1 S1 W1 72.71(10) . . ?
Cu2 S2 Cu1 81.33(11) . . ?
Cu2 S2 W1 70.23(9) . . ?
Cu1 S2 W1 70.43(9) . . ?
Cu2 S3 W1 72.15(11) . . ?
N9 B1 N5 109.7(10) . . ?
N9 B1 N7 108.4(10) . . ?
N5 B1 N7 106.8(10) . . ?
N9 B1 H1B1 110.6 . . ?
N5 B1 H1B1 110.6 . . ?
N7 B1 H1B1 110.6 . . ?
C1 N1 Cu3 173.6(11) . . ?
C2 N2 Cu4 174.5(13) . . ?
C3 N3 C3 116.3(16) 3_755 . ?
C3 N3 Cu3 121.9(8) 3_755 . ?
C3 N3 Cu3 121.9(8) . . ?
C12 N4 C12 116(2) . 3_755 ?
C12 N4 Cu4 122.1(11) . 1_545 ?
C12 N4 Cu4 122.1(11) 3_755 1_545 ?
C14 N5 N6 112.3(10) . . ?
C14 N5 B1 127.5(10) . . ?
N6 N5 B1 119.8(10) . . ?
C16 N6 N5 105.6(9) . . ?
C16 N6 W1 132.5(8) . . ?
N5 N6 W1 121.9(8) . . ?
N8 N7 C19 110.8(9) . . ?
N8 N7 B1 121.3(9) . . ?
C19 N7 B1 127.9(10) . . ?
N7 N8 C21 106.4(9) . . ?
N7 N8 W1 122.8(7) . . ?
C21 N8 W1 130.8(8) . . ?
C24 N9 N10 110.5(10) . . ?
C24 N9 B1 128.1(10) . . ?
N10 N9 B1 121.4(10) . . ?
N9 N10 C26 105.8(10) . . ?
N9 N10 W1 120.9(8) . . ?
C26 N10 W1 133.2(8) . . ?
N1 C1 Cu1 175.0(11) . . ?
N2 C2 Cu2 174.4(13) . . ?
N3 C3 C4 123.2(14) . . ?
N3 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C5 C4 C3 118.3(14) . . ?
C5 C4 H4 120.8 . . ?
C3 C4 H4 120.8 . . ?
C4 C5 C4 120.6(18) 3_755 . ?
C4 C5 C6 119.7(9) 3_755 . ?
C4 C5 C6 119.7(9) . . ?
C7 C6 C7 117.9(19) . 3_755 ?
C7 C6 C5 121.0(10) . . ?
C7 C6 C5 121.0(10) 3_755 . ?
C8 C7 C6 121.4(17) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C7 C8 C9 119.1(17) . . ?
C7 C8 H8 120.5 . . ?
C9 C8 H8 120.5 . . ?
C8 C9 C8 120.5(19) . 3_755 ?
C8 C9 C10 119.8(9) . . ?
C8 C9 C10 119.8(9) 3_755 . ?
C11 C10 C11 116(2) 3_755 . ?
C11 C10 C9 122.0(11) 3_755 . ?
C11 C10 C9 122.0(11) . . ?
C12 C11 C10 119(2) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
N4 C12 C11 125(2) . . ?
N4 C12 H12 117.7 . . ?
C11 C12 H12 117.7 . . ?
C14 C13 H13A 109.5 . . ?
C14 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C14 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N5 C14 C15 105.0(11) . . ?
N5 C14 C13 123.9(13) . . ?
C15 C14 C13 131.1(13) . . ?
C14 C15 C16 107.8(11) . . ?
C14 C15 H15 126.1 . . ?
C16 C15 H15 126.1 . . ?
N6 C16 C15 109.4(11) . . ?
N6 C16 C17 127.2(11) . . ?
C15 C16 C17 123.4(11) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 H18A 109.5 . . ?
C19 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C19 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N7 C19 C20 107.7(11) . . ?
N7 C19 C18 123.2(11) . . ?
C20 C19 C18 129.1(12) . . ?
C19 C20 C21 106.4(12) . . ?
C19 C20 H20 126.8 . . ?
C21 C20 H20 126.8 . . ?
N8 C21 C20 108.7(11) . . ?
N8 C21 C22 124.3(11) . . ?
C20 C21 C22 127.0(11) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 H23A 109.5 . . ?
C24 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C24 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N9 C24 C25 107.0(11) . . ?
N9 C24 C23 123.4(12) . . ?
C25 C24 C23 129.6(13) . . ?
C24 C25 C26 107.6(12) . . ?
C24 C25 H25 126.2 . . ?
C26 C25 H25 126.2 . . ?
C25 C26 N10 109.2(11) . . ?
C25 C26 C27 124.9(12) . . ?
N10 C26 C27 125.9(11) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C30 N11 C28 123(3) . . ?
C30 N11 C29 120(3) . . ?
C28 N11 C29 116(4) . . ?
N11 C28 H28A 109.5 . . ?
N11 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
N11 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N11 C29 H29A 109.5 . . ?
N11 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N11 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O1 C30 N11 119(3) . . ?
O1 C30 H30 120.3 . . ?
N11 C30 H30 120.3 . . ?
C33 N12 C31 123(2) . . ?
C33 N12 C32 121(2) . . ?
C31 N12 C32 116(2) . . ?
N12 C31 H31A 109.5 . . ?
N12 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
N12 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N12 C32 H32A 109.5 . . ?
N12 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
N12 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O2 C33 N12 127(2) . . ?
O2 C33 H33 116.4 . . ?
N12 C33 H33 116.4 . . ?

_refine_diff_density_max         10.477
_refine_diff_density_min         -4.344
_refine_diff_density_rms         0.476

_shelxl_version_number           2013-2


