# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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. 
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data_161026c
_database_code_depnum_ccdc_archive 'CCDC 1515325'
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H46 Cu4 N8 O29 W6'
_chemical_formula_weight         2556.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -z'

_cell_length_a                   10.6500(9)
_cell_length_b                   12.1479(11)
_cell_length_c                   13.1931(12)
_cell_angle_alpha                108.267(3)
_cell_angle_beta                 101.159(2)
_cell_angle_gamma                106.443(3)
_cell_volume                     1478.0(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    1024
_cell_measurement_theta_min      3.3095
_cell_measurement_theta_max      28.193

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.872
_exptl_crystal_F_000             1182
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.170
_exptl_absorpt_coefficient_mu    13.126
_shelx_estimated_absorpt_T_min   0.160
_shelx_estimated_absorpt_T_max   0.214
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1603
_exptl_absorpt_correction_T_max  0.2138
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7550
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.258
_diffrn_reflns_theta_max         25.015
_diffrn_reflns_theta_full        25.015
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             5156
_reflns_number_gt                4232
_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-2018/3 (Sheldrick, 2018)'
_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)+(0.1118P)²+61.0228P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5156
_refine_ls_number_parameters     430
_refine_ls_number_restraints     444
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1953
_refine_ls_wR_factor_gt          0.1874
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_restrained_S_all      1.053
_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 0.35147(8) 0.45153(8) 0.32830(7) 0.0299(3) Uani 1 1 d . U . . .
W2 W 0.36228(7) 0.58847(6) 0.58569(6) 0.0179(2) Uani 1 1 d . U . . .
W3 W 0.62263(8) 0.68911(7) 0.49864(7) 0.0272(2) Uani 1 1 d . U . . .
Cu1 Cu 0.17348(18) 0.09212(17) 0.19855(16) 0.0114(4) Uani 1 1 d . U . . .
Cu2 Cu 0.13457(18) 0.22210(17) 0.05099(15) 0.0101(4) Uani 1 1 d . U . . .
N1 N 0.3091(13) 0.0157(12) 0.2451(11) 0.013(3) Uani 1 1 d . . . . .
N2 N 0.0652(13) -0.0032(12) 0.2754(11) 0.012(3) Uani 1 1 d . . . . .
N3 N 0.2355(13) 0.2918(12) -0.0446(10) 0.011(3) Uani 1 1 d . . . . .
N4 N -0.0116(13) 0.2728(12) -0.0225(10) 0.011(3) Uani 1 1 d . . . . .
O1 O 0.2391(11) 0.4095(11) 0.1999(9) 0.0170(18) Uani 1 1 d . U . . .
O2 O 0.7183(13) 0.7029(12) 0.6424(10) 0.0248(10) Uani 1 1 d . U . . .
O3 O 0.2608(11) 0.5231(10) 0.4280(9) 0.0135(16) Uani 1 1 d . U . . .
O4 O 0.2605(11) 0.6513(11) 0.6500(9) 0.016(2) Uani 1 1 d . U . . .
O5 O 0.5103(11) 0.6154(10) 0.7119(9) 0.0128(16) Uani 1 1 d . U . . .
O6 O 0.500000 0.500000 0.500000 0.0139(19) Uani 1 2 d S U P . .
O7 O 0.2900(11) 0.4155(10) 0.5709(9) 0.0141(16) Uani 1 1 d . U . . .
O8 O 0.4716(13) 0.6105(12) 0.3565(11) 0.0273(9) Uani 1 1 d . U . . .
O9 O 0.4809(11) 0.7225(10) 0.5650(9) 0.0129(16) Uani 1 1 d . U . . .
O10 O 0.7040(11) 0.8271(11) 0.4941(10) 0.018(2) Uani 1 1 d . U . . .
O11 O 0.2683(11) 0.1560(11) 0.1053(9) 0.0153(18) Uani 1 1 d . U . . .
H11B H 0.346890 0.212814 0.143411 0.018 Uiso 1 1 d R U . . .
O12 O 0.0300(11) 0.1417(11) 0.1306(9) 0.0155(19) Uani 1 1 d . U . . .
O13 O 0.4060(14) 0.7922(14) 0.9071(12) 0.036(3) Uani 1 1 d . U . . .
H13C H 0.372165 0.746496 0.837324 0.044 Uiso 1 1 d R U . . .
H13D H 0.374855 0.850636 0.920014 0.044 Uiso 1 1 d R U . . .
O14 O 0.280(2) -0.0232(16) 0.9173(14) 0.063(5) Uani 1 1 d . . . . .
H14C H 0.294402 0.038241 0.977123 0.076 Uiso 1 1 d R U . . .
H14D H 0.194302 -0.066979 0.892473 0.076 Uiso 1 1 d R U . . .
O15 O 0.9787(15) 0.2953(16) 0.3205(16) 0.055(5) Uani 1 1 d . . . . .
H15C H 1.062837 0.314793 0.355458 0.066 Uiso 1 1 d R U . . .
H15D H 0.962107 0.244213 0.253988 0.066 Uiso 1 1 d R U . . .
C1 C 0.4299(17) 0.0279(16) 0.2269(15) 0.020(4) Uani 1 1 d . . . . .
H1 H 0.458275 0.072566 0.184346 0.024 Uiso 1 1 calc R U . . .
C2 C 0.5154(17) -0.0265(18) 0.2717(16) 0.024(4) Uani 1 1 d . . . . .
H2 H 0.598946 -0.017547 0.257072 0.029 Uiso 1 1 calc R U . . .
C3 C 0.4799(18) -0.0909(18) 0.3350(16) 0.028(4) Uani 1 1 d . U . . .
H3 H 0.538987 -0.123907 0.365634 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3477(17) -0.1076(16) 0.3542(14) 0.018(3) Uani 1 1 d . . . . .
C5 C 0.2694(15) -0.0502(14) 0.3066(12) 0.011(3) Uani 1 1 d . . . . .
C6 C 0.1346(15) -0.0627(14) 0.3206(13) 0.011(3) Uani 1 1 d . . . . .
C7 C 0.0835(16) -0.1335(14) 0.3816(13) 0.013(3) Uani 1 1 d . U . . .
C8 C 0.1709(19) -0.1865(17) 0.4314(15) 0.024(4) Uani 1 1 d . . . . .
H8 H 0.141266 -0.228776 0.475315 0.028 Uiso 1 1 calc R U . . .
C9 C 0.2972(19) -0.1760(17) 0.4154(15) 0.024(4) Uani 1 1 d . . . . .
H9 H 0.349420 -0.214638 0.445479 0.029 Uiso 1 1 calc R U . . .
C10 C -0.0492(17) -0.1427(16) 0.3916(13) 0.020(4) Uani 1 1 d . . . . .
H10 H -0.088603 -0.189218 0.429214 0.023 Uiso 1 1 calc R U . . .
C11 C -0.1189(17) -0.0816(16) 0.3447(14) 0.019(3) Uani 1 1 d . . . . .
H11 H -0.204985 -0.085810 0.352104 0.022 Uiso 1 1 calc R U . . .
C12 C -0.0606(17) -0.0127(16) 0.2855(14) 0.019(3) Uani 1 1 d . . . . .
H12 H -0.109649 0.026635 0.253123 0.022 Uiso 1 1 calc R U . . .
C13 C 0.3592(17) 0.2986(18) -0.0564(14) 0.021(4) Uani 1 1 d . . . . .
H13 H 0.409747 0.263457 -0.019809 0.026 Uiso 1 1 calc R U . . .
C14 C 0.4148(17) 0.3576(17) -0.1227(15) 0.021(4) Uani 1 1 d . U . . .
H14 H 0.500126 0.358741 -0.130077 0.025 Uiso 1 1 calc R U . . .
C15 C 0.3467(17) 0.4132(17) -0.1762(14) 0.020(4) Uani 1 1 d . . . . .
H15 H 0.385117 0.453953 -0.218215 0.024 Uiso 1 1 calc R U . . .
C16 C 0.2138(15) 0.4064(14) -0.1653(12) 0.010(3) Uani 1 1 d . . . . .
C17 C 0.1638(15) 0.3439(14) -0.1002(12) 0.010(3) Uani 1 1 d . . . . .
C18 C 0.0280(14) 0.3327(14) -0.0886(11) 0.008(3) Uani 1 1 d . . . . .
C19 C -0.0506(16) 0.3869(14) -0.1418(13) 0.012(3) Uani 1 1 d . . . . .
C20 C 0.0023(17) 0.4493(15) -0.2088(13) 0.016(3) Uani 1 1 d . . . . .
H20 H -0.050058 0.483613 -0.244813 0.019 Uiso 1 1 calc R U . . .
C21 C 0.1289(16) 0.4587(15) -0.2202(13) 0.017(3) Uani 1 1 d . U . . .
H21 H 0.161607 0.499612 -0.264126 0.020 Uiso 1 1 calc R U . . .
C22 C -0.1815(16) 0.3723(16) -0.1259(14) 0.019(4) Uani 1 1 d . U . . .
H22 H -0.239866 0.402764 -0.161052 0.023 Uiso 1 1 calc R U . . .
C23 C -0.2216(16) 0.3117(17) -0.0569(14) 0.018(3) Uani 1 1 d . . . . .
H23 H -0.306163 0.303254 -0.044382 0.022 Uiso 1 1 calc R U . . .
C24 C -0.1339(15) 0.2636(15) -0.0063(13) 0.013(3) Uani 1 1 d . . . . .
H24 H -0.161665 0.224081 0.040008 0.015 Uiso 1 1 calc R U . . .


_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 O1 1.700(11) . ?
W1 O8 1.863(13) . ?
W1 O3 1.915(10) . ?
W1 O5 1.955(10) 2_666 ?
W1 O2 2.000(13) 2_666 ?
W1 O6 2.2870(8) . ?
W1 W3 3.2285(12) . ?
W2 O4 1.701(10) . ?
W2 O9 1.890(11) . ?
W2 O5 1.928(11) . ?
W2 O3 1.932(11) . ?
W2 O7 1.953(11) . ?
W2 O6 2.3145(7) . ?
W3 O10 1.680(11) . ?
W3 O7 1.895(11) 2_666 ?
W3 O2 1.903(13) . ?
W3 O9 1.961(10) . ?
W3 O8 1.964(13) . ?
W3 O6 2.3065(8) . ?
Cu1 O11 1.942(11) . ?
Cu1 O12 1.958(10) . ?
Cu1 N1 2.025(13) . ?
Cu1 N2 2.033(13) . ?
Cu2 O12 1.943(11) . ?
Cu2 O11 1.949(11) . ?
Cu2 N4 2.019(13) . ?
Cu2 N3 2.035(13) . ?
Cu2 O1 2.280(12) . ?
N1 C1 1.33(2) . ?
N1 C5 1.35(2) . ?
N2 C12 1.35(2) . ?
N2 C6 1.35(2) . ?
N3 C13 1.34(2) . ?
N3 C17 1.368(19) . ?
N4 C24 1.34(2) . ?
N4 C18 1.356(19) . ?
O11 H11B 0.8499 . ?
O13 H13C 0.8501 . ?
O13 H13D 0.8500 . ?
O14 H14C 0.8500 . ?
O14 H14D 0.8500 . ?
O15 H15C 0.8500 . ?
O15 H15D 0.8500 . ?
C1 C2 1.41(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.35(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.45(2) . ?
C3 H3 0.9300 . ?
C4 C9 1.40(2) . ?
C4 C5 1.41(2) . ?
C5 C6 1.45(2) . ?
C6 C7 1.42(2) . ?
C7 C10 1.42(2) . ?
C7 C8 1.44(2) . ?
C8 C9 1.38(3) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.38(2) . ?
C10 H10 0.9300 . ?
C11 C12 1.41(2) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.41(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.36(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.43(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.40(2) . ?
C16 C21 1.45(2) . ?
C17 C18 1.46(2) . ?
C18 C19 1.41(2) . ?
C19 C22 1.42(2) . ?
C19 C20 1.43(2) . ?
C20 C21 1.36(2) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.39(2) . ?
C22 H22 0.9300 . ?
C23 C24 1.40(2) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O8 103.1(5) . . ?
O1 W1 O3 102.4(5) . . ?
O8 W1 O3 90.1(5) . . ?
O1 W1 O5 101.6(5) . 2_666 ?
O8 W1 O5 89.3(5) . 2_666 ?
O3 W1 O5 155.4(4) . 2_666 ?
O1 W1 O2 100.8(5) . 2_666 ?
O8 W1 O2 155.9(5) . 2_666 ?
O3 W1 O2 87.1(5) . 2_666 ?
O5 W1 O2 83.6(5) 2_666 2_666 ?
O1 W1 O6 177.8(4) . . ?
O8 W1 O6 79.0(4) . . ?
O3 W1 O6 78.2(3) . . ?
O5 W1 O6 77.6(3) 2_666 . ?
O2 W1 O6 77.0(4) 2_666 . ?
O1 W1 W3 136.5(4) . . ?
O8 W1 W3 33.4(4) . . ?
O3 W1 W3 84.1(3) . . ?
O5 W1 W3 82.0(3) 2_666 . ?
O2 W1 W3 122.5(4) 2_666 . ?
O6 W1 W3 45.59(2) . . ?
O4 W2 O9 103.7(5) . . ?
O4 W2 O5 102.0(5) . . ?
O9 W2 O5 88.7(5) . . ?
O4 W2 O3 103.4(5) . . ?
O9 W2 O3 87.9(5) . . ?
O5 W2 O3 154.5(4) . . ?
O4 W2 O7 102.6(5) . . ?
O9 W2 O7 153.7(4) . . ?
O5 W2 O7 86.8(4) . . ?
O3 W2 O7 85.1(5) . . ?
O4 W2 O6 178.8(4) . . ?
O9 W2 O6 77.3(3) . . ?
O5 W2 O6 77.4(3) . . ?
O3 W2 O6 77.2(3) . . ?
O7 W2 O6 76.4(3) . . ?
O10 W3 O7 104.1(5) . 2_666 ?
O10 W3 O2 104.0(6) . . ?
O7 W3 O2 90.6(5) 2_666 . ?
O10 W3 O9 101.9(5) . . ?
O7 W3 O9 153.8(5) 2_666 . ?
O2 W3 O9 86.3(5) . . ?
O10 W3 O8 100.8(5) . . ?
O7 W3 O8 87.8(5) 2_666 . ?
O2 W3 O8 154.7(6) . . ?
O9 W3 O8 84.0(5) . . ?
O10 W3 O6 176.9(4) . . ?
O7 W3 O6 77.7(3) 2_666 . ?
O2 W3 O6 78.4(4) . . ?
O9 W3 O6 76.2(3) . . ?
O8 W3 O6 76.6(4) . . ?
O10 W3 W1 132.4(4) . . ?
O7 W3 W1 81.2(3) 2_666 . ?
O2 W3 W1 123.4(4) . . ?
O9 W3 W1 78.8(3) . . ?
O8 W3 W1 31.5(4) . . ?
O6 W3 W1 45.10(2) . . ?
O11 Cu1 O12 83.2(4) . . ?
O11 Cu1 N1 95.1(5) . . ?
O12 Cu1 N1 170.6(5) . . ?
O11 Cu1 N2 170.4(5) . . ?
O12 Cu1 N2 98.2(5) . . ?
N1 Cu1 N2 82.0(5) . . ?
O12 Cu2 O11 83.3(4) . . ?
O12 Cu2 N4 97.5(5) . . ?
O11 Cu2 N4 173.2(5) . . ?
O12 Cu2 N3 174.9(5) . . ?
O11 Cu2 N3 96.6(5) . . ?
N4 Cu2 N3 81.9(5) . . ?
O12 Cu2 O1 94.2(4) . . ?
O11 Cu2 O1 92.7(4) . . ?
N4 Cu2 O1 93.9(4) . . ?
N3 Cu2 O1 90.9(5) . . ?
C1 N1 C5 118.9(14) . . ?
C1 N1 Cu1 128.3(11) . . ?
C5 N1 Cu1 112.8(10) . . ?
C12 N2 C6 119.3(13) . . ?
C12 N2 Cu1 128.7(11) . . ?
C6 N2 Cu1 112.0(9) . . ?
C13 N3 C17 117.4(13) . . ?
C13 N3 Cu2 130.5(11) . . ?
C17 N3 Cu2 112.0(9) . . ?
C24 N4 C18 118.0(13) . . ?
C24 N4 Cu2 128.3(10) . . ?
C18 N4 Cu2 113.5(10) . . ?
W1 O1 Cu2 131.1(6) . . ?
W3 O2 W1 113.7(6) . 2_666 ?
W1 O3 W2 114.8(5) . . ?
W2 O5 W1 114.5(5) . 2_666 ?
W1 O6 W1 180.0 2_666 . ?
W1 O6 W3 90.69(3) 2_666 . ?
W1 O6 W3 89.31(3) . . ?
W1 O6 W3 89.31(3) 2_666 2_666 ?
W1 O6 W3 90.69(3) . 2_666 ?
W3 O6 W3 180.0 . 2_666 ?
W1 O6 W2 90.41(3) 2_666 . ?
W1 O6 W2 89.59(3) . . ?
W3 O6 W2 90.10(3) . . ?
W3 O6 W2 89.90(3) 2_666 . ?
W1 O6 W2 89.59(3) 2_666 2_666 ?
W1 O6 W2 90.41(3) . 2_666 ?
W3 O6 W2 89.90(3) . 2_666 ?
W3 O6 W2 90.10(3) 2_666 2_666 ?
W2 O6 W2 179.999(18) . 2_666 ?
W3 O7 W2 116.1(5) 2_666 . ?
W1 O8 W3 115.0(7) . . ?
W2 O9 W3 116.3(5) . . ?
Cu1 O11 Cu2 96.6(5) . . ?
Cu1 O11 H11B 112.3 . . ?
Cu2 O11 H11B 112.2 . . ?
Cu2 O12 Cu1 96.3(5) . . ?
H13C O13 H13D 108.1 . . ?
H14C O14 H14D 107.9 . . ?
H15C O15 H15D 107.6 . . ?
N1 C1 C2 120.5(15) . . ?
N1 C1 H1 119.7 . . ?
C2 C1 H1 119.7 . . ?
C3 C2 C1 122.1(15) . . ?
C3 C2 H2 118.9 . . ?
C1 C2 H2 118.9 . . ?
C2 C3 C4 118.4(15) . . ?
C2 C3 H3 120.8 . . ?
C4 C3 H3 120.8 . . ?
C9 C4 C5 120.6(15) . . ?
C9 C4 C3 123.8(15) . . ?
C5 C4 C3 115.6(14) . . ?
N1 C5 C4 124.4(14) . . ?
N1 C5 C6 116.0(14) . . ?
C4 C5 C6 119.5(14) . . ?
N2 C6 C7 123.4(13) . . ?
N2 C6 C5 117.0(13) . . ?
C7 C6 C5 119.5(14) . . ?
C10 C7 C6 116.7(14) . . ?
C10 C7 C8 125.2(15) . . ?
C6 C7 C8 118.1(14) . . ?
C9 C8 C7 121.6(15) . . ?
C9 C8 H8 119.2 . . ?
C7 C8 H8 119.2 . . ?
C8 C9 C4 120.5(16) . . ?
C8 C9 H9 119.7 . . ?
C4 C9 H9 119.7 . . ?
C11 C10 C7 119.2(15) . . ?
C11 C10 H10 120.4 . . ?
C7 C10 H10 120.4 . . ?
C10 C11 C12 120.7(15) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
N2 C12 C11 120.7(15) . . ?
N2 C12 H12 119.6 . . ?
C11 C12 H12 119.6 . . ?
N3 C13 C14 121.8(15) . . ?
N3 C13 H13 119.1 . . ?
C14 C13 H13 119.1 . . ?
C15 C14 C13 121.7(15) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C14 C15 C16 117.5(15) . . ?
C14 C15 H15 121.3 . . ?
C16 C15 H15 121.3 . . ?
C17 C16 C15 117.6(14) . . ?
C17 C16 C21 119.2(14) . . ?
C15 C16 C21 123.2(14) . . ?
N3 C17 C16 123.9(14) . . ?
N3 C17 C18 116.6(13) . . ?
C16 C17 C18 119.5(13) . . ?
N4 C18 C19 124.5(13) . . ?
N4 C18 C17 115.8(13) . . ?
C19 C18 C17 119.7(13) . . ?
C18 C19 C22 116.1(14) . . ?
C18 C19 C20 119.7(14) . . ?
C22 C19 C20 124.1(15) . . ?
C21 C20 C19 120.5(15) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C20 C21 C16 121.5(15) . . ?
C20 C21 H21 119.3 . . ?
C16 C21 H21 119.3 . . ?
C23 C22 C19 119.2(15) . . ?
C23 C22 H22 120.4 . . ?
C19 C22 H22 120.4 . . ?
C22 C23 C24 119.8(14) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
N4 C24 C23 122.2(14) . . ?
N4 C24 H24 118.9 . . ?
C23 C24 H24 118.9 . . ?

_refine_diff_density_max         4.175
_refine_diff_density_min         -4.097
_refine_diff_density_rms         0.433

####################################################################### 
# 
# 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_exp_8433
_database_code_depnum_ccdc_archive 'CCDC 2008846'
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H12 N2'
_chemical_formula_weight         220.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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'

_cell_length_a                   9.580(2)
_cell_length_b                   4.8156(10)
_cell_length_c                   12.595(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.16(3)
_cell_angle_gamma                90
_cell_volume                     565.8(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    508
_cell_measurement_theta_min      5.3590
_cell_measurement_theta_max      70.8590

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_F_000             232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.602
_shelx_estimated_absorpt_T_min   0.884
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1600
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_av_R_equivalents  0.0196
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       2
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.604
_diffrn_reflns_theta_max         67.144
_diffrn_reflns_theta_full        67.144
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.626
_diffrn_reflns_point_group_measured_fraction_full 0.626
_reflns_number_total             1269
_reflns_number_gt                898
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.131
_reflns_Friedel_fraction_max     0.167
_reflns_Friedel_fraction_full    0.167

_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-2018/3 (Sheldrick, 2018)'
_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)+(0.1675P)²+0.0044P] 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_abs_structure_details 
;
 Flack x determined using 102 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   1.7(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1269
_refine_ls_number_parameters     155
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0716
_refine_ls_wR_factor_ref         0.2693
_refine_ls_wR_factor_gt          0.2276
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.003

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
N1 N 0.0523(5) 0.7373(10) 0.1951(3) 0.0508(13) Uani 1 1 d . . . . .
N2 N -0.0825(5) 0.5796(13) 0.3627(3) 0.0606(15) Uani 1 1 d . . . . .
C1 C 0.0896(5) 0.8492(13) 0.2930(4) 0.0495(15) Uani 1 1 d . . . . .
C2 C 0.0189(6) 0.7686(15) 0.3766(4) 0.0606(18) Uani 1 1 d . . . . .
H2 H 0.046170 0.854333 0.444298 0.073 Uiso 1 1 calc R U . . .
C3 C -0.1211(6) 0.4613(14) 0.2618(4) 0.0523(15) Uani 1 1 d . . . . .
C4 C -0.2295(6) 0.2545(13) 0.2407(5) 0.0581(17) Uani 1 1 d . . . . .
H4 H -0.273028 0.199415 0.296177 0.070 Uiso 1 1 calc R U . . .
C5 C -0.2706(6) 0.1360(14) 0.1406(5) 0.0580(17) Uani 1 1 d . . . . .
C6 C -0.2029(6) 0.2139(15) 0.0575(5) 0.0605(17) Uani 1 1 d . . . . .
H6 H -0.229803 0.130544 -0.010710 0.073 Uiso 1 1 calc R U . . .
C7 C -0.0972(6) 0.4123(14) 0.0760(4) 0.0576(16) Uani 1 1 d . . . . .
H7 H -0.054058 0.463275 0.019798 0.069 Uiso 1 1 calc R U . . .
C8 C -0.0535(5) 0.5388(13) 0.1781(4) 0.0497(15) Uani 1 1 d . . . . .
C9 C -0.3865(6) -0.0825(16) 0.1166(5) 0.073(2) Uani 1 1 d . . . . .
H9A H -0.419341 -0.121030 0.181703 0.109 Uiso 1 1 calc R U . . .
H9B H -0.348830 -0.249273 0.092121 0.109 Uiso 1 1 calc R U . . .
H9C H -0.465192 -0.016185 0.060923 0.109 Uiso 1 1 calc R U . . .
C10 C 0.2046(6) 1.0621(13) 0.3134(4) 0.0535(15) Uani 1 1 d . . . . .
C11 C 0.2700(6) 1.1373(16) 0.2292(4) 0.0618(17) Uani 1 1 d . . . . .
H11 H 0.240197 1.055542 0.160892 0.074 Uiso 1 1 calc R U . . .
C12 C 0.3791(6) 1.3326(16) 0.2466(5) 0.073(2) Uani 1 1 d . . . . .
H12 H 0.422880 1.377953 0.190206 0.087 Uiso 1 1 calc R U . . .
C13 C 0.4231(6) 1.4596(19) 0.3458(5) 0.074(2) Uani 1 1 d . . . . .
H13 H 0.495192 1.592881 0.356629 0.089 Uiso 1 1 calc R U . . .
C14 C 0.3596(7) 1.3877(16) 0.4290(5) 0.073(2) Uani 1 1 d . . . . .
H14 H 0.389753 1.471888 0.496834 0.088 Uiso 1 1 calc R U . . .
C15 C 0.2503(6) 1.1901(16) 0.4135(5) 0.0655(18) Uani 1 1 d . . . . .
H15 H 0.207983 1.144281 0.470714 0.079 Uiso 1 1 calc R U . . .


_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
N1 C1 1.318(6) . ?
N1 C8 1.374(7) . ?
N2 C2 1.314(8) . ?
N2 C3 1.364(7) . ?
C1 C2 1.428(7) . ?
C1 C10 1.484(7) . ?
C3 C8 1.407(6) . ?
C3 C4 1.420(8) . ?
C4 C5 1.358(8) . ?
C5 C6 1.402(8) . ?
C5 C9 1.510(9) . ?
C6 C7 1.373(9) . ?
C7 C8 1.398(7) . ?
C10 C15 1.382(8) . ?
C10 C11 1.396(7) . ?
C11 C12 1.385(9) . ?
C12 C13 1.368(9) . ?
C13 C14 1.371(9) . ?
C14 C15 1.395(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C8 117.6(4) . . ?
C2 N2 C3 116.7(5) . . ?
N1 C1 C2 120.3(5) . . ?
N1 C1 C10 118.4(4) . . ?
C2 C1 C10 121.2(5) . . ?
N2 C2 C1 123.4(5) . . ?
N2 C3 C8 120.9(5) . . ?
N2 C3 C4 119.9(5) . . ?
C8 C3 C4 119.2(5) . . ?
C5 C4 C3 120.9(5) . . ?
C4 C5 C6 119.7(6) . . ?
C4 C5 C9 121.5(5) . . ?
C6 C5 C9 118.8(6) . . ?
C7 C6 C5 120.6(6) . . ?
C6 C7 C8 120.9(5) . . ?
N1 C8 C7 120.1(4) . . ?
N1 C8 C3 121.1(5) . . ?
C7 C8 C3 118.8(5) . . ?
C15 C10 C11 118.3(6) . . ?
C15 C10 C1 122.2(5) . . ?
C11 C10 C1 119.5(5) . . ?
C12 C11 C10 120.5(6) . . ?
C13 C12 C11 120.8(6) . . ?
C12 C13 C14 119.1(7) . . ?
C13 C14 C15 121.0(6) . . ?
C10 C15 C14 120.2(6) . . ?

_refine_diff_density_max         0.238
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.064

####################################################################### 
# 
# 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_190312d
_database_code_depnum_ccdc_archive 'CCDC 1918834'
_audit_update_record             
;
2020-06-09 deposited with the CCDC.	2020-08-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H37 Cl Cu2 N8 O21 W6'
_chemical_formula_weight         2327.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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, -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'

_cell_length_a                   26.174(2)
_cell_length_b                   16.2204(14)
_cell_length_c                   14.0404(12)
_cell_angle_alpha                90
_cell_angle_beta                 118.393(4)
_cell_angle_gamma                90
_cell_volume                     5243.9(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    2573
_cell_measurement_theta_min      2.512
_cell_measurement_theta_max      24.251

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.948
_exptl_crystal_F_000             4272
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    14.039
_shelx_estimated_absorpt_T_min   0.148
_shelx_estimated_absorpt_T_max   0.187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.208
_exptl_absorpt_correction_T_max  0.256
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      298(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12977
_diffrn_reflns_av_unetI/netI     0.0632
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.511
_diffrn_reflns_theta_max         25.019
_diffrn_reflns_theta_full        25.019
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4636
_reflns_number_gt                2813
_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-2018/3 (Sheldrick, 2018)'
_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)+(0.1001P)²+8.3574P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4636
_refine_ls_number_parameters     390
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0551
_refine_ls_wR_factor_ref         0.1894
_refine_ls_wR_factor_gt          0.1587
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_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 0.24567(3) 0.39203(4) 0.50547(6) 0.0364(3) Uani 1 1 d . . . . .
W2 W 0.22616(4) 0.25601(4) 0.31960(6) 0.0449(3) Uani 1 1 d . . . . .
W3 W 0.34695(4) 0.25691(5) 0.54720(9) 0.0560(3) Uani 1 1 d . . . . .
Cu1 Cu 0.46829(9) 0.25040(11) 0.37713(19) 0.0407(6) Uani 1 1 d . . . . .
Cl1 Cl 0.500000 0.1823(4) 0.250000 0.0407(15) Uani 1 2 d S T P . .
N1 N 0.4986(6) 0.1757(7) 0.5111(11) 0.028(3) Uani 1 1 d . . . . .
N2 N 0.4015(5) 0.1751(8) 0.3249(11) 0.034(3) Uani 1 1 d . . . . .
N3 N 0.4238(6) 0.3612(8) 0.3341(11) 0.038(3) Uani 1 1 d . . . . .
N4 N 0.5365(6) 0.3257(8) 0.4230(11) 0.040(3) Uani 1 1 d . . . . .
O1 O 0.2430(5) 0.4957(7) 0.5112(9) 0.047(3) Uani 1 1 d . . . . .
O2 O 0.2649(5) 0.3613(7) 0.6494(9) 0.039(3) Uani 1 1 d . . . . .
O3 O 0.1675(4) 0.3585(7) 0.4631(9) 0.038(3) Uani 1 1 d . . . . .
O4 O 0.2281(5) 0.3691(7) 0.3599(9) 0.046(3) Uani 1 1 d . . . . .
O5 O 0.3252(5) 0.3711(6) 0.5408(10) 0.039(3) Uani 1 1 d . . . . .
O6 O 0.250000 0.250000 0.500000 0.027(4) Uani 1 2 d S . P . .
O7 O 0.2070(10) 0.2627(8) 0.1867(13) 0.088(6) Uani 1 1 d . . . . .
O8 O 0.3087(6) 0.2609(7) 0.3929(11) 0.047(3) Uani 1 1 d . . . . .
O9 O 0.4177(6) 0.2647(8) 0.5795(16) 0.076(5) Uani 1 1 d . . . . .
H9 H 0.425271 0.230332 0.545212 0.092 Uiso 0.5 1 calc R U P . .
O10 O 0.3484(5) 0.2533(6) 0.6838(10) 0.042(3) Uani 1 1 d . . . . .
O11 O 0.2392(15) 0.3264(16) 0.048(2) 0.231(16) Uani 1 1 d . . . . .
H11C H 0.228341 0.312590 0.093721 0.277 Uiso 1 1 d R U . . .
H11D H 0.238821 0.378740 0.043511 0.277 Uiso 1 1 d R U . . .
C1 C 0.5471(7) 0.1749(9) 0.6071(14) 0.035(4) Uani 1 1 d . . . . .
H1 H 0.572626 0.218969 0.622807 0.042 Uiso 1 1 calc R U . . .
C2 C 0.5620(9) 0.1145(11) 0.6840(15) 0.049(5) Uani 1 1 d . . . . .
H2 H 0.597221 0.116034 0.747518 0.059 Uiso 1 1 calc R U . . .
C3 C 0.5237(9) 0.0524(12) 0.6642(16) 0.050(5) Uani 1 1 d . . . . .
H3 H 0.533252 0.010360 0.714878 0.060 Uiso 1 1 calc R U . . .
C4 C 0.4700(8) 0.0497(9) 0.5694(14) 0.034(4) Uani 1 1 d . . . . .
C5 C 0.4585(7) 0.1133(9) 0.4908(12) 0.026(3) Uani 1 1 d . . . . .
C6 C 0.4068(7) 0.1117(10) 0.3905(14) 0.034(4) Uani 1 1 d . . . . .
C7 C 0.3681(7) 0.0510(11) 0.3697(15) 0.038(4) Uani 1 1 d . . . . .
C8 C 0.3773(9) -0.0120(11) 0.4454(19) 0.051(6) Uani 1 1 d . . . . .
H8 H 0.349380 -0.052523 0.430737 0.061 Uiso 1 1 calc R U . . .
C9 C 0.4235(10) -0.0121(11) 0.532(2) 0.056(6) Uani 1 1 d . . . . .
H9A H 0.429206 -0.056051 0.578882 0.068 Uiso 1 1 calc R U . . .
C10 C 0.3178(9) 0.0549(14) 0.265(2) 0.066(7) Uani 1 1 d . . . . .
H10 H 0.288848 0.015266 0.244262 0.079 Uiso 1 1 calc R U . . .
C11 C 0.3126(9) 0.1166(13) 0.1948(18) 0.058(6) Uani 1 1 d . . . . .
H11 H 0.280996 0.118514 0.125665 0.070 Uiso 1 1 calc R U . . .
C12 C 0.3534(8) 0.1737(12) 0.2274(15) 0.047(5) Uani 1 1 d . . . . .
H12 H 0.348732 0.216127 0.179366 0.056 Uiso 1 1 calc R U . . .
C13 C 0.3690(8) 0.3784(12) 0.2973(13) 0.042(4) Uani 1 1 d . . . . .
H13 H 0.342884 0.336236 0.287203 0.050 Uiso 1 1 calc R U . . .
C14 C 0.3484(10) 0.4621(16) 0.2721(15) 0.070(8) Uani 1 1 d . . . . .
H14 H 0.309024 0.472879 0.244879 0.084 Uiso 1 1 calc R U . . .
C15 C 0.3843(10) 0.5236(14) 0.2869(16) 0.059(6) Uani 1 1 d . . . . .
H15 H 0.369883 0.576636 0.265591 0.071 Uiso 1 1 calc R U . . .
C16 C 0.4447(9) 0.5087(12) 0.3352(14) 0.050(5) Uani 1 1 d . . . . .
C17 C 0.4607(8) 0.4246(9) 0.3551(13) 0.035(4) Uani 1 1 d . . . . .
C18 C 0.5212(7) 0.4052(10) 0.4005(13) 0.035(4) Uani 1 1 d . . . . .
C19 C 0.5649(10) 0.4683(13) 0.4243(14) 0.051(5) Uani 1 1 d . . . . .
C20 C 0.5464(13) 0.5520(15) 0.4030(19) 0.073(7) Uani 1 1 d . . . . .
H20 H 0.573256 0.594242 0.418784 0.088 Uiso 1 1 calc R U . . .
C21 C 0.4895(13) 0.5685(11) 0.3598(17) 0.070(8) Uani 1 1 d . . . . .
H21 H 0.478194 0.623310 0.344494 0.084 Uiso 1 1 calc R U . . .
C22 C 0.6221(10) 0.4445(15) 0.4648(16) 0.065(7) Uani 1 1 d . . . . .
H22 H 0.651496 0.482331 0.478342 0.078 Uiso 1 1 calc R U . . .
C23 C 0.6332(10) 0.3620(16) 0.4839(17) 0.068(6) Uani 1 1 d . . . . .
H23 H 0.671479 0.344158 0.513520 0.081 Uiso 1 1 calc R U . . .
C24 C 0.5920(8) 0.3061(13) 0.4622(16) 0.051(5) Uani 1 1 d . . . . .
H24 H 0.602572 0.250815 0.475129 0.061 Uiso 1 1 calc R U . . .


_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 O1 1.686(12) . ?
W1 O2 1.902(11) . ?
W1 O4 1.906(12) . ?
W1 O3 1.917(10) . ?
W1 O5 1.928(11) . ?
W1 O6 2.3096(7) . ?
W2 O7 1.690(15) . ?
W2 O8 1.902(14) . ?
W2 O4 1.913(12) . ?
W2 O10 1.935(13) 7_556 ?
W2 O2 1.941(12) 7_556 ?
W2 O6 2.3046(8) . ?
W3 O9 1.688(13) . ?
W3 O10 1.901(13) . ?
W3 O3 1.901(11) 7_556 ?
W3 O8 1.907(14) . ?
W3 O5 1.927(11) . ?
W3 O6 2.3004(9) . ?
Cu1 N2 1.967(13) . ?
Cu1 N4 2.000(13) . ?
Cu1 N1 2.053(12) . ?
Cu1 N3 2.069(14) . ?
Cu1 Cl1 2.551(4) . ?
N1 C1 1.34(2) . ?
N1 C5 1.387(18) . ?
N2 C6 1.34(2) . ?
N2 C12 1.35(2) . ?
N3 C13 1.30(2) . ?
N3 C17 1.34(2) . ?
N4 C24 1.33(2) . ?
N4 C18 1.34(2) . ?
O9 H9 0.8200 . ?
O11 H11C 0.8499 . ?
O11 H11D 0.8499 . ?
C1 C2 1.37(2) . ?
C1 H1 0.9300 . ?
C2 C3 1.35(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.40(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.43(2) . ?
C4 C9 1.47(2) . ?
C5 C6 1.42(2) . ?
C6 C7 1.34(2) . ?
C7 C8 1.41(2) . ?
C7 C10 1.44(3) . ?
C8 C9 1.25(3) . ?
C8 H8 0.9300 . ?
C9 H9A 0.9300 . ?
C10 C11 1.36(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.32(3) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.44(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.32(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.41(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.42(2) . ?
C16 C21 1.43(3) . ?
C17 C18 1.43(2) . ?
C18 C19 1.45(2) . ?
C19 C22 1.38(3) . ?
C19 C20 1.42(3) . ?
C20 C21 1.34(3) . ?
C20 H20 0.9300 . ?
C21 H21 0.9300 . ?
C22 C23 1.37(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.33(3) . ?
C23 H23 0.9300 . ?
C24 H24 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 W1 O2 101.9(5) . . ?
O1 W1 O4 104.6(5) . . ?
O2 W1 O4 153.5(5) . . ?
O1 W1 O3 103.6(5) . . ?
O2 W1 O3 87.7(5) . . ?
O4 W1 O3 86.2(5) . . ?
O1 W1 O5 103.1(5) . . ?
O2 W1 O5 88.4(5) . . ?
O4 W1 O5 85.5(5) . . ?
O3 W1 O5 153.2(5) . . ?
O1 W1 O6 179.3(4) . . ?
O2 W1 O6 77.4(3) . . ?
O4 W1 O6 76.1(3) . . ?
O3 W1 O6 76.6(3) . . ?
O5 W1 O6 76.6(3) . . ?
O7 W2 O8 105.1(9) . . ?
O7 W2 O4 102.6(6) . . ?
O8 W2 O4 86.4(5) . . ?
O7 W2 O10 102.2(9) . 7_556 ?
O8 W2 O10 152.7(5) . 7_556 ?
O4 W2 O10 88.1(5) . 7_556 ?
O7 W2 O2 104.6(5) . 7_556 ?
O8 W2 O2 86.2(5) . 7_556 ?
O4 W2 O2 152.9(5) . 7_556 ?
O10 W2 O2 86.7(4) 7_556 7_556 ?
O7 W2 O6 178.1(7) . . ?
O8 W2 O6 76.3(4) . . ?
O4 W2 O6 76.1(3) . . ?
O10 W2 O6 76.5(4) 7_556 . ?
O2 W2 O6 76.8(3) 7_556 . ?
O9 W3 O10 103.8(8) . . ?
O9 W3 O3 104.3(5) . 7_556 ?
O10 W3 O3 87.3(5) . 7_556 ?
O9 W3 O8 102.7(8) . . ?
O10 W3 O8 153.5(5) . . ?
O3 W3 O8 88.2(5) 7_556 . ?
O9 W3 O5 101.7(5) . . ?
O10 W3 O5 86.6(5) . . ?
O3 W3 O5 154.0(5) 7_556 . ?
O8 W3 O5 86.0(5) . . ?
O9 W3 O6 178.2(6) . . ?
O10 W3 O6 77.2(4) . . ?
O3 W3 O6 77.1(3) 7_556 . ?
O8 W3 O6 76.3(4) . . ?
O5 W3 O6 76.9(3) . . ?
N2 Cu1 N4 177.0(6) . . ?
N2 Cu1 N1 82.1(5) . . ?
N4 Cu1 N1 99.7(5) . . ?
N2 Cu1 N3 98.8(6) . . ?
N4 Cu1 N3 81.7(6) . . ?
N1 Cu1 N3 134.3(5) . . ?
N2 Cu1 Cl1 89.9(4) . . ?
N4 Cu1 Cl1 87.3(4) . . ?
N1 Cu1 Cl1 105.8(3) . . ?
N3 Cu1 Cl1 119.8(4) . . ?
Cu1 Cl1 Cu1 128.6(3) . 2_655 ?
C1 N1 C5 117.4(13) . . ?
C1 N1 Cu1 134.0(11) . . ?
C5 N1 Cu1 108.5(10) . . ?
C6 N2 C12 115.2(15) . . ?
C6 N2 Cu1 115.9(11) . . ?
C12 N2 Cu1 128.5(12) . . ?
C13 N3 C17 117.6(15) . . ?
C13 N3 Cu1 131.6(13) . . ?
C17 N3 Cu1 110.7(11) . . ?
C24 N4 C18 118.3(15) . . ?
C24 N4 Cu1 128.4(12) . . ?
C18 N4 Cu1 113.0(11) . . ?
W1 O2 W2 116.0(5) . 7_556 ?
W3 O3 W1 116.6(5) 7_556 . ?
W1 O4 W2 117.6(6) . . ?
W3 O5 W1 116.1(5) . . ?
W3 O6 W3 180.0 . 7_556 ?
W3 O6 W2 89.98(3) . . ?
W3 O6 W2 90.02(3) 7_556 . ?
W3 O6 W2 90.02(3) . 7_556 ?
W3 O6 W2 89.98(3) 7_556 7_556 ?
W2 O6 W2 180.0 . 7_556 ?
W3 O6 W1 89.62(3) . 7_556 ?
W3 O6 W1 90.38(3) 7_556 7_556 ?
W2 O6 W1 89.86(3) . 7_556 ?
W2 O6 W1 90.14(3) 7_556 7_556 ?
W3 O6 W1 90.38(3) . . ?
W3 O6 W1 89.62(3) 7_556 . ?
W2 O6 W1 90.14(3) . . ?
W2 O6 W1 89.86(3) 7_556 . ?
W1 O6 W1 180.0 7_556 . ?
W2 O8 W3 117.5(6) . . ?
W3 O9 H9 109.5 . . ?
W3 O10 W2 116.2(6) . 7_556 ?
H11C O11 H11D 108.7 . . ?
N1 C1 C2 125.2(16) . . ?
N1 C1 H1 117.4 . . ?
C2 C1 H1 117.4 . . ?
C3 C2 C1 117.8(18) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 121.9(16) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C3 C4 C5 117.2(14) . . ?
C3 C4 C9 130.2(17) . . ?
C5 C4 C9 112.5(16) . . ?
N1 C5 C6 119.3(13) . . ?
N1 C5 C4 120.4(14) . . ?
C6 C5 C4 120.3(14) . . ?
C7 C6 N2 126.3(17) . . ?
C7 C6 C5 119.7(16) . . ?
N2 C6 C5 114.0(14) . . ?
C6 C7 C8 121.9(17) . . ?
C6 C7 C10 114.7(18) . . ?
C8 C7 C10 123.4(17) . . ?
C9 C8 C7 118.6(18) . . ?
C9 C8 H8 120.7 . . ?
C7 C8 H8 120.7 . . ?
C8 C9 C4 127.0(19) . . ?
C8 C9 H9A 116.5 . . ?
C4 C9 H9A 116.5 . . ?
C11 C10 C7 120.1(18) . . ?
C11 C10 H10 120.0 . . ?
C7 C10 H10 120.0 . . ?
C12 C11 C10 119(2) . . ?
C12 C11 H11 120.7 . . ?
C10 C11 H11 120.7 . . ?
C11 C12 N2 125.0(19) . . ?
C11 C12 H12 117.5 . . ?
N2 C12 H12 117.5 . . ?
N3 C13 C14 120.9(19) . . ?
N3 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C13 121(2) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 120(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
C15 C16 C17 115(2) . . ?
C15 C16 C21 127(2) . . ?
C17 C16 C21 118.2(19) . . ?
N3 C17 C16 125.4(18) . . ?
N3 C17 C18 117.2(14) . . ?
C16 C17 C18 117.4(16) . . ?
N4 C18 C17 117.2(14) . . ?
N4 C18 C19 120.7(17) . . ?
C17 C18 C19 122.0(16) . . ?
C22 C19 C20 123(2) . . ?
C22 C19 C18 118.6(19) . . ?
C20 C19 C18 118(2) . . ?
C21 C20 C19 119(2) . . ?
C21 C20 H20 120.7 . . ?
C19 C20 H20 120.7 . . ?
C20 C21 C16 125(2) . . ?
C20 C21 H21 117.3 . . ?
C16 C21 H21 117.3 . . ?
C23 C22 C19 116.2(18) . . ?
C23 C22 H22 121.9 . . ?
C19 C22 H22 121.9 . . ?
C24 C23 C22 123(2) . . ?
C24 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
N4 C24 C23 123(2) . . ?
N4 C24 H24 118.6 . . ?
C23 C24 H24 118.6 . . ?

_refine_diff_density_max         1.933
_refine_diff_density_min         -3.936
_refine_diff_density_rms         0.309

