#------------------------------------------------------------------------------
#$Date: 2019-11-17 13:51:29 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230287 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/75/7057573.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7057573
loop_
_publ_author_name
'Das, Manisha'
'Craig, Gavin A.'
'Escudero, Daniel'
'Murrie, Mark'
'Frontera, Antonio'
'Ray, Debashis'
_publ_section_title
;
 A family of [Cu2], [Cu4] and [Cu5] aggregates: alteration of reaction
 conditions, ancillary bridges and capping anions
;
_journal_issue                   17
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14349
_journal_paper_doi               10.1039/C8NJ02131G
_journal_volume                  42
_journal_year                    2018
_chemical_formula_moiety         'C34 H54 Cl2 Cu4 N4 O22, 2(Cl O4), 2(H2 O)'
_chemical_formula_sum            'C34 H60 Cl4 Cu4 N4 O32'
_chemical_formula_weight         1432.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-07 deposited with the CCDC.
2018-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                105.525(6)
_cell_angle_beta                 94.758(6)
_cell_angle_gamma                112.669(6)
_cell_formula_units_Z            2
_cell_length_a                   13.616(3)
_cell_length_b                   14.129(3)
_cell_length_c                   15.755(4)
_cell_measurement_reflns_used    33413
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.296
_cell_measurement_theta_min      1.652
_cell_volume                     2635.1(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Diamond
_computing_publication_material
'SHELXL-2014/7 (Sheldrick, 2014), PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33413
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.296
_diffrn_reflns_theta_min         1.652
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.896
_exptl_absorpt_correction_T_max  0.724
_exptl_absorpt_correction_T_min  0.534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         10379
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0520P)²+4.7614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1009
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9010
_reflns_number_total             10379
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj02131g2.cif
_cod_data_source_block           Complex2
_cod_depositor_comments
'Adding full bibliography for 7057571--7057573.cif.'
_cod_database_code               7057573
_shelx_shelxl_version_number     2014/7
_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'
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
Cu1 Cu 0.43555(3) 0.29267(3) 0.14281(2) 0.01652(10) Uani 1 1 d . .
Cu2 Cu 0.66201(3) 0.44565(3) 0.22451(2) 0.01628(10) Uani 1 1 d . .
Cu3 Cu 0.44330(3) 0.81360(3) 0.12669(2) 0.01510(10) Uani 1 1 d . .
Cu4 Cu 0.67106(3) -0.05793(3) 0.21931(2) 0.01442(9) Uani 1 1 d . .
Cl1 Cl 0.64244(7) 0.16937(6) 0.17304(5) 0.02106(16) Uani 1 1 d . .
Cl3 Cl 0.61568(6) 0.65260(5) 0.13008(5) 0.01561(15) Uani 1 1 d . .
O1 O 0.52912(17) 0.37395(16) 0.25986(13) 0.0155(4) Uani 1 1 d . .
O2 O 0.57029(18) 0.36896(17) 0.10473(14) 0.0164(4) Uani 1 1 d D .
O3 O 0.34111(17) 0.19834(17) 0.02600(14) 0.0177(4) Uani 1 1 d D .
O4 O 0.79614(18) 0.53210(18) 0.19479(15) 0.0215(5) Uani 1 1 d D .
O12 O 0.53234(16) 0.86640(17) 0.24440(13) 0.0157(4) Uani 1 1 d . .
O13 O 0.58321(17) 0.89280(17) 0.09917(13) 0.0147(4) Uani 1 1 d D .
O15 O 0.81672(18) 0.99839(18) 0.19301(14) 0.0202(5) Uani 1 1 d D .
O14 O 0.35676(18) 0.74828(18) 0.00613(14) 0.0199(5) Uani 1 1 d D .
O6 O 0.8300(2) 0.72797(19) 0.45966(16) 0.0249(5) Uani 1 1 d D .
O5 O 0.0612(2) 0.1605(2) 0.04773(17) 0.0317(6) Uani 1 1 d D .
O17 O 1.00771(19) 1.21647(19) 0.39036(16) 0.0271(5) Uani 1 1 d D .
O16 O 0.15973(18) 0.47666(18) -0.03253(15) 0.0204(5) Uani 1 1 d D .
O11 O 0.3827(3) 0.4328(3) 0.1426(3) 0.0738(13) Uani 1 1 d . .
O18 O 0.3814(2) 0.9512(2) 0.15363(19) 0.0298(6) Uani 1 1 d D .
O10 O 0.6479(2) 0.1035(2) 0.08834(16) 0.0365(7) Uani 1 1 d . .
O8 O 0.6695(2) 0.12957(19) 0.24268(15) 0.0297(6) Uani 1 1 d . .
O7 O 0.71701(19) 0.28163(18) 0.19208(16) 0.0253(5) Uani 1 1 d . .
O9 O 0.5338(2) 0.1621(2) 0.1695(2) 0.0477(8) Uani 1 1 d . .
O24 O 0.5967(2) 0.61124(19) 0.20411(15) 0.0291(5) Uani 1 1 d . .
O23 O 0.64280(19) 0.58074(18) 0.06220(14) 0.0221(5) Uani 1 1 d . .
O25 O 0.52038(18) 0.65938(18) 0.09154(16) 0.0257(5) Uani 1 1 d . .
O26 O 0.70549(18) 0.75931(17) 0.16138(15) 0.0234(5) Uani 1 1 d . .
N1 N 0.3163(2) 0.2142(2) 0.19223(16) 0.0152(5) Uani 1 1 d . .
N2 N 0.7456(2) 0.5066(2) 0.34513(16) 0.0159(5) Uani 1 1 d . .
N3 N 0.3160(2) 0.7239(2) 0.16177(16) 0.0145(5) Uani 1 1 d . .
N4 N 0.7442(2) 0.98145(19) 0.34153(16) 0.0137(5) Uani 1 1 d . .
C1 C 0.5120(2) 0.3655(2) 0.34017(19) 0.0135(6) Uani 1 1 d . .
C2 C 0.5974(2) 0.4244(2) 0.41740(19) 0.0151(6) Uani 1 1 d . .
C3 C 0.5746(3) 0.4199(2) 0.50170(19) 0.0166(6) Uani 1 1 d . .
H3A H 0.6307 0.4605 0.5523 0.020 Uiso 1 1 calc R U
C4 C 0.4735(3) 0.3587(2) 0.51352(19) 0.0165(6) Uani 1 1 d . .
C5 C 0.3917(3) 0.2974(2) 0.43696(19) 0.0162(6) Uani 1 1 d . .
H5A H 0.3230 0.2541 0.4431 0.019 Uiso 1 1 calc R U
C6 C 0.4089(2) 0.2984(2) 0.35049(19) 0.0154(6) Uani 1 1 d . .
C7 C 0.4524(3) 0.3584(3) 0.60602(19) 0.0195(6) Uani 1 1 d . .
H7A H 0.4705 0.4311 0.6435 0.029 Uiso 1 1 calc R U
H7B H 0.4964 0.3300 0.6322 0.029 Uiso 1 1 calc R U
H7C H 0.3769 0.3138 0.6012 0.029 Uiso 1 1 calc R U
C8 C 0.3170(2) 0.2275(2) 0.2761(2) 0.0176(6) Uani 1 1 d . .
H8 H 0.2523 0.1878 0.2907 0.021 Uiso 1 1 calc R U
C9 C 0.7085(3) 0.4918(2) 0.4157(2) 0.0164(6) Uani 1 1 d . .
H9 H 0.7578 0.5277 0.4707 0.020 Uiso 1 1 calc R U
C10 C 0.2160(3) 0.1433(2) 0.1213(2) 0.0190(6) Uiso 1 1 d . .
C11 C 0.2542(3) 0.1059(3) 0.0359(2) 0.0207(6) Uiso 1 1 d . .
H11C H 0.2798 0.0516 0.0395 0.025 Uiso 1 1 calc R U
H11D H 0.1943 0.0738 -0.0158 0.025 Uiso 1 1 calc R U
C12 C 0.1401(3) 0.0437(3) 0.1422(2) 0.0287(8) Uani 1 1 d . .
H12A H 0.1146 0.0666 0.1956 0.043 Uiso 1 1 calc R U
H12B H 0.1789 0.0020 0.1516 0.043 Uiso 1 1 calc R U
H12C H 0.0791 -0.0001 0.0925 0.043 Uiso 1 1 calc R U
C13 C 0.1598(3) 0.2172(3) 0.1135(2) 0.0261(7) Uani 1 1 d . .
H13A H 0.1445 0.2461 0.1714 0.031 Uiso 1 1 calc R U
H13B H 0.2085 0.2777 0.0975 0.031 Uiso 1 1 calc R U
C14 C 0.8605(2) 0.5830(2) 0.3543(2) 0.0181(6) Uani 1 1 d . .
C15 C 0.8879(3) 0.5527(3) 0.2613(2) 0.0236(7) Uani 1 1 d . .
H15A H 0.9526 0.6116 0.2576 0.028 Uiso 1 1 calc R U
H15B H 0.9016 0.4885 0.2510 0.028 Uiso 1 1 calc R U
C16 C 0.8653(3) 0.6982(2) 0.3788(2) 0.0222(7) Uani 1 1 d . .
H16A H 0.9396 0.7498 0.3850 0.027 Uiso 1 1 calc R U
H16B H 0.8201 0.7020 0.3301 0.027 Uiso 1 1 calc R U
C17 C 0.9400(3) 0.5737(3) 0.4215(2) 0.0272(7) Uani 1 1 d . .
H17A H 1.0132 0.6147 0.4170 0.041 Uiso 1 1 calc R U
H17B H 0.9266 0.4989 0.4088 0.041 Uiso 1 1 calc R U
H17C H 0.9306 0.6016 0.4814 0.041 Uiso 1 1 calc R U
C54 C 0.5037(2) 0.8560(2) 0.32119(19) 0.0130(6) Uiso 1 1 d . .
C55 C 0.3946(2) 0.7929(2) 0.32300(19) 0.0138(6) Uiso 1 1 d . .
C56 C 0.3673(2) 0.7881(2) 0.4062(2) 0.0159(6) Uani 1 1 d . .
H56 H 0.2953 0.7470 0.4070 0.019 Uiso 1 1 calc R U
C57 C 0.4426(3) 0.8418(2) 0.4871(2) 0.0163(6) Uani 1 1 d . .
C58 C 0.4101(3) 0.8349(3) 0.5756(2) 0.0213(7) Uani 1 1 d . .
H58A H 0.4451 0.7983 0.6008 0.032 Uiso 1 1 calc R U
H58B H 0.3325 0.7953 0.5654 0.032 Uiso 1 1 calc R U
H58C H 0.4319 0.9067 0.6167 0.032 Uiso 1 1 calc R U
C59 C 0.5494(3) 0.8986(2) 0.48367(19) 0.0157(6) Uani 1 1 d . .
H59 H 0.6016 0.9328 0.5371 0.019 Uiso 1 1 calc R U
C60 C 0.5828(2) 0.9070(2) 0.40275(19) 0.0135(6) Uani 1 1 d . .
C61 C 0.6983(2) 0.9643(2) 0.40807(19) 0.0146(6) Uani 1 1 d . .
H61 H 0.7438 0.9914 0.4645 0.018 Uiso 1 1 calc R U
C62 C 0.3076(2) 0.7280(2) 0.2428(2) 0.0162(6) Uani 1 1 d . .
H62 H 0.2399 0.6858 0.2515 0.019 Uiso 1 1 calc R U
C63 C 0.2237(2) 0.6517(2) 0.0830(2) 0.0169(6) Uani 1 1 d . .
C64 C 0.2447(3) 0.7086(3) 0.0111(2) 0.0222(7) Uani 1 1 d . .
H64A H 0.2006 0.6577 -0.0471 0.027 Uiso 1 1 calc R U
H64B H 0.2239 0.7684 0.0260 0.027 Uiso 1 1 calc R U
C65 C 0.2357(3) 0.5446(2) 0.0512(2) 0.0178(6) Uiso 1 1 d . .
H65A H 0.3094 0.5592 0.0431 0.021 Uiso 1 1 calc R U
H65B H 0.2214 0.5083 0.0961 0.021 Uiso 1 1 calc R U
C66 C 0.1130(3) 0.6342(3) 0.1032(2) 0.0256(7) Uani 1 1 d . .
H66A H 0.1131 0.7030 0.1335 0.038 Uiso 1 1 calc R U
H66B H 0.0958 0.5895 0.1411 0.038 Uiso 1 1 calc R U
H66C H 0.0594 0.5991 0.0479 0.038 Uiso 1 1 calc R U
C67 C 0.8643(2) 1.0387(2) 0.3558(2) 0.0172(6) Uani 1 1 d . .
C68 C 0.8911(3) 0.9997(3) 0.2644(2) 0.0223(7) Uani 1 1 d . .
H68A H 0.9649 1.0474 0.2644 0.027 Uiso 1 1 calc R U
H68B H 0.8869 0.9273 0.2538 0.027 Uiso 1 1 calc R U
C69 C 0.9256(3) 1.0132(3) 0.4249(2) 0.0232(7) Uani 1 1 d . .
H69A H 1.0018 1.0438 0.4243 0.035 Uiso 1 1 calc R U
H69B H 0.8988 0.9360 0.4105 0.035 Uiso 1 1 calc R U
H69C H 0.9149 1.0438 0.4837 0.035 Uiso 1 1 calc R U
C70 C 0.8933(3) 1.1603(2) 0.3831(2) 0.0204(6) Uiso 1 1 d . .
H70A H 0.8536 1.1752 0.3382 0.025 Uiso 1 1 calc R U
H70B H 0.8741 1.1841 0.4404 0.025 Uiso 1 1 calc R U
Cl2 Cl 0.15137(6) 0.90637(6) 0.31784(5) 0.02225(17) Uani 1 1 d . .
O20 O 0.1519(2) 0.8485(2) 0.37981(18) 0.0375(6) Uani 1 1 d . .
O22 O 0.0456(3) 0.8538(3) 0.2592(2) 0.0505(8) Uani 1 1 d . .
O21 O 0.2319(3) 0.9045(3) 0.2669(2) 0.0606(10) Uani 1 1 d . .
O19 O 0.1724(3) 1.0153(2) 0.3658(2) 0.0447(7) Uani 1 1 d . .
Cl4 Cl 0.13226(9) 0.44476(8) 0.30656(7) 0.0410(2) Uani 1 1 d . .
O29 O 0.1944(3) 0.3940(3) 0.3299(3) 0.0852(14) Uani 1 1 d . .
O30 O 0.0192(3) 0.3726(3) 0.3020(2) 0.0587(9) Uani 1 1 d . .
O27 O 0.1600(3) 0.5433(3) 0.3759(4) 0.121(2) Uani 1 1 d . .
O28 O 0.1357(6) 0.4537(6) 0.2218(4) 0.143(3) Uani 1 1 d . .
O1W O 0.8953(2) 0.7494(2) 0.08958(18) 0.0298(6) Uani 1 1 d D .
O2W O 0.9058(2) 0.1684(2) 0.1462(2) 0.0388(6) Uani 1 1 d D .
H3 H 0.363(3) 0.171(3) -0.0151(19) 0.025(10) Uiso 1 1 d D .
H13 H 0.591(3) 0.945(2) 0.087(2) 0.020(10) Uiso 1 1 d D .
H2 H 0.560(3) 0.408(3) 0.083(2) 0.022(10) Uiso 1 1 d D .
H6 H 0.876(2) 0.745(3) 0.4997(19) 0.023(11) Uiso 1 1 d D .
H15 H 0.839(3) 1.051(2) 0.178(3) 0.030(11) Uiso 1 1 d D .
H4 H 0.808(3) 0.528(3) 0.1469(16) 0.024(10) Uiso 1 1 d D .
H5 H 0.074(5) 0.184(4) 0.005(3) 0.076(19) Uiso 1 1 d D .
H16 H 0.147(4) 0.4139(18) -0.042(3) 0.049(14) Uiso 1 1 d D .
H17 H 1.021(4) 1.261(3) 0.366(3) 0.045(14) Uiso 1 1 d D .
H14 H 0.371(4) 0.705(3) -0.030(3) 0.060(16) Uiso 1 1 d D .
H1WA H 0.939(4) 0.776(4) 0.136(2) 0.065(17) Uiso 1 1 d D .
H2WA H 0.922(5) 0.227(3) 0.181(3) 0.08(2) Uiso 1 1 d D .
H2WB H 0.940(4) 0.158(4) 0.109(3) 0.062(17) Uiso 1 1 d D .
H1WB H 0.847(4) 0.743(6) 0.117(4) 0.11(3) Uiso 1 1 d D .
H18B H 0.423(4) 1.014(2) 0.165(4) 0.071(18) Uiso 1 1 d D .
H18A H 0.348(3) 0.953(4) 0.193(2) 0.050(14) Uiso 1 1 d D .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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'
Cl Cl 0.1480 0.1590 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3200 1.2650 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 Cu1 N1 92.59(9) . .
O1 Cu1 O3 174.68(9) . .
N1 Cu1 O3 85.20(10) . .
O1 Cu1 O2 81.46(9) . .
N1 Cu1 O2 171.80(10) . .
O3 Cu1 O2 100.23(9) . .
O1 Cu1 O11 92.15(12) . .
N1 Cu1 O11 95.87(12) . .
O3 Cu1 O11 92.89(12) . .
O2 Cu1 O11 90.03(12) . .
O1 Cu1 Cu2 40.25(6) . .
N1 Cu1 Cu2 132.44(7) . .
O3 Cu1 Cu2 141.06(6) . .
O2 Cu1 Cu2 41.23(6) . .
O11 Cu1 Cu2 92.51(8) . .
O1 Cu1 H2 89.1(9) . .
N1 Cu1 H2 168.5(7) . .
O3 Cu1 H2 94.0(9) . .
O2 Cu1 H2 18.6(7) . .
O11 Cu1 H2 72.7(7) . .
Cu2 Cu1 H2 51.4(8) . .
N2 Cu2 O1 93.28(10) . .
N2 Cu2 O2 173.77(10) . .
O1 Cu2 O2 82.46(9) . .
N2 Cu2 O4 84.72(10) . .
O1 Cu2 O4 174.21(9) . .
O2 Cu2 O4 99.95(9) . .
N2 Cu2 O7 91.37(9) . .
O1 Cu2 O7 95.91(8) . .
O2 Cu2 O7 84.59(8) . .
O4 Cu2 O7 89.58(9) . .
N2 Cu2 Cu1 133.39(8) . .
O1 Cu2 Cu1 40.42(6) . .
O2 Cu2 Cu1 42.07(6) . .
O4 Cu2 Cu1 141.89(7) . .
O7 Cu2 Cu1 89.39(5) . .
N2 Cu2 H2 167.5(7) . .
O1 Cu2 H2 88.7(9) . .
O2 Cu2 H2 18.0(7) . .
O4 Cu2 H2 92.1(9) . .
O7 Cu2 H2 100.7(7) . .
Cu1 Cu2 H2 50.9(9) . .
O12 Cu3 O14 174.41(9) . .
O12 Cu3 N3 93.11(10) . .
O14 Cu3 N3 86.26(10) . .
O12 Cu3 O13 81.52(9) . .
O14 Cu3 O13 98.39(9) . .
N3 Cu3 O13 171.10(10) . .
O12 Cu3 O18 95.27(10) . .
O14 Cu3 O18 90.28(10) . .
N3 Cu3 O18 89.07(10) . .
O13 Cu3 O18 98.45(9) . .
O12 Cu3 Cu4 40.23(6) . 1_565
O14 Cu3 Cu4 139.28(7) . 1_565
N3 Cu3 Cu4 132.80(8) . 1_565
O13 Cu3 Cu4 41.30(6) . 1_565
O18 Cu3 Cu4 99.81(7) . 1_565
O12 Cu4 N4 92.14(9) 1_545 1_545
O12 Cu4 O13 81.79(9) 1_545 1_545
N4 Cu4 O13 173.89(10) 1_545 1_545
O12 Cu4 O15 170.66(10) 1_545 1_545
N4 Cu4 O15 86.07(10) 1_545 1_545
O13 Cu4 O15 99.79(9) 1_545 1_545
O12 Cu4 O8 99.83(9) 1_545 .
N4 Cu4 O8 93.43(9) 1_545 .
O13 Cu4 O8 88.36(8) 1_545 .
O15 Cu4 O8 89.44(9) 1_545 .
O12 Cu4 Cu3 40.19(6) 1_545 1_545
N4 Cu4 Cu3 132.30(7) 1_545 1_545
O13 Cu4 Cu3 41.62(6) 1_545 1_545
O15 Cu4 Cu3 140.42(7) 1_545 1_545
O8 Cu4 Cu3 96.27(6) . 1_545
O10 Cl1 O9 109.29(19) . .
O10 Cl1 O8 108.58(14) . .
O9 Cl1 O8 109.67(18) . .
O10 Cl1 O7 110.61(15) . .
O9 Cl1 O7 108.59(15) . .
O8 Cl1 O7 110.09(15) . .
O25 Cl3 O24 110.58(15) . .
O25 Cl3 O23 109.24(14) . .
O24 Cl3 O23 109.00(14) . .
O25 Cl3 O26 109.30(14) . .
O24 Cl3 O26 109.59(14) . .
O23 Cl3 O26 109.10(14) . .
C1 O1 Cu2 129.81(19) . .
C1 O1 Cu1 129.59(18) . .
Cu2 O1 Cu1 99.33(9) . .
Cu2 O2 Cu1 96.70(9) . .
Cu2 O2 H2 111(3) . .
Cu1 O2 H2 107(3) . .
C11 O3 Cu1 110.18(17) . .
C11 O3 H3 103(3) . .
Cu1 O3 H3 123(3) . .
C15 O4 Cu2 109.50(19) . .
C15 O4 H4 114(3) . .
Cu2 O4 H4 127(3) . .
C54 O12 Cu3 129.37(18) . .
C54 O12 Cu4 131.00(18) . 1_565
Cu3 O12 Cu4 99.59(9) . 1_565
Cu4 O13 Cu3 97.08(9) 1_565 .
Cu4 O13 H13 107(3) 1_565 .
Cu3 O13 H13 117(3) . .
C68 O15 Cu4 107.44(18) . 1_565
C68 O15 H15 114(3) . .
Cu4 O15 H15 122(3) 1_565 .
C64 O14 Cu3 108.54(18) . .
C64 O14 H14 113(4) . .
Cu3 O14 H14 118(4) . .
C16 O6 H6 109(3) . .
C13 O5 H5 106(4) . .
C70 O17 H17 112(3) . .
C65 O16 H16 111(3) . .
Cu3 O18 H18B 121(4) . .
Cu3 O18 H18A 115(3) . .
H18B O18 H18A 103(5) . .
Cl1 O8 Cu4 126.32(13) . .
Cl1 O7 Cu2 125.08(14) . .
C8 N1 C10 122.1(3) . .
C8 N1 Cu1 125.9(2) . .
C10 N1 Cu1 111.66(18) . .
C9 N2 C14 120.4(3) . .
C9 N2 Cu2 125.7(2) . .
C14 N2 Cu2 113.83(19) . .
C62 N3 C63 122.5(3) . .
C62 N3 Cu3 125.1(2) . .
C63 N3 Cu3 112.31(18) . .
C61 N4 C67 120.6(2) . .
C61 N4 Cu4 126.3(2) . 1_565
C67 N4 Cu4 113.11(18) . 1_565
O1 C1 C6 121.1(3) . .
O1 C1 C2 120.4(3) . .
C6 C1 C2 118.4(3) . .
C3 C2 C1 118.9(3) . .
C3 C2 C9 116.9(3) . .
C1 C2 C9 124.2(3) . .
C4 C3 C2 123.4(3) . .
C4 C3 H3A 118.3 . .
C2 C3 H3A 118.3 . .
C3 C4 C5 117.2(3) . .
C3 C4 C7 121.4(3) . .
C5 C4 C7 121.4(3) . .
C4 C5 C6 122.4(3) . .
C4 C5 H5A 118.8 . .
C6 C5 H5A 118.8 . .
C5 C6 C1 119.6(3) . .
C5 C6 C8 116.4(3) . .
C1 C6 C8 124.0(3) . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
N1 C8 C6 126.3(3) . .
N1 C8 H8 116.8 . .
C6 C8 H8 116.8 . .
N2 C9 C2 126.3(3) . .
N2 C9 H9 116.8 . .
C2 C9 H9 116.8 . .
N1 C10 C11 105.9(2) . .
N1 C10 C12 113.9(3) . .
C11 C10 C12 108.9(3) . .
N1 C10 C13 104.9(2) . .
C11 C10 C13 111.9(3) . .
C12 C10 C13 111.1(3) . .
O3 C11 C10 108.7(2) . .
O3 C11 H11C 109.9 . .
C10 C11 H11C 109.9 . .
O3 C11 H11D 109.9 . .
C10 C11 H11D 109.9 . .
H11C C11 H11D 108.3 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
O5 C13 C10 111.7(3) . .
O5 C13 H13A 109.3 . .
C10 C13 H13A 109.3 . .
O5 C13 H13B 109.3 . .
C10 C13 H13B 109.3 . .
H13A C13 H13B 107.9 . .
N2 C14 C17 113.0(3) . .
N2 C14 C15 106.3(2) . .
C17 C14 C15 108.2(3) . .
N2 C14 C16 107.2(2) . .
C17 C14 C16 112.5(3) . .
C15 C14 C16 109.4(3) . .
O4 C15 C14 107.8(2) . .
O4 C15 H15A 110.1 . .
C14 C15 H15A 110.1 . .
O4 C15 H15B 110.1 . .
C14 C15 H15B 110.1 . .
H15A C15 H15B 108.5 . .
O6 C16 C14 112.9(3) . .
O6 C16 H16A 109.0 . .
C14 C16 H16A 109.0 . .
O6 C16 H16B 109.0 . .
C14 C16 H16B 109.0 . .
H16A C16 H16B 107.8 . .
C14 C17 H17A 109.5 . .
C14 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C14 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
O12 C54 C55 120.9(2) . .
O12 C54 C60 120.3(3) . .
C55 C54 C60 118.8(3) . .
C56 C55 C54 118.9(3) . .
C56 C55 C62 116.8(3) . .
C54 C55 C62 124.2(3) . .
C57 C56 C55 123.0(3) . .
C57 C56 H56 118.5 . .
C55 C56 H56 118.5 . .
C59 C57 C56 117.4(3) . .
C59 C57 C58 121.1(3) . .
C56 C57 C58 121.5(3) . .
C57 C58 H58A 109.5 . .
C57 C58 H58B 109.5 . .
H58A C58 H58B 109.5 . .
C57 C58 H58C 109.5 . .
H58A C58 H58C 109.5 . .
H58B C58 H58C 109.5 . .
C57 C59 C60 122.8(3) . .
C57 C59 H59 118.6 . .
C60 C59 H59 118.6 . .
C59 C60 C54 119.0(3) . .
C59 C60 C61 117.1(3) . .
C54 C60 C61 123.8(3) . .
N4 C61 C60 126.1(3) . .
N4 C61 H61 117.0 . .
C60 C61 H61 117.0 . .
N3 C62 C55 126.0(3) . .
N3 C62 H62 117.0 . .
C55 C62 H62 117.0 . .
N3 C63 C66 114.2(2) . .
N3 C63 C65 105.5(2) . .
C66 C63 C65 112.0(3) . .
N3 C63 C64 105.0(2) . .
C66 C63 C64 109.9(3) . .
C65 C63 C64 109.9(2) . .
O14 C64 C63 110.6(2) . .
O14 C64 H64A 109.5 . .
C63 C64 H64A 109.5 . .
O14 C64 H64B 109.5 . .
C63 C64 H64B 109.5 . .
H64A C64 H64B 108.1 . .
O16 C65 C63 108.8(2) . .
O16 C65 H65A 109.9 . .
C63 C65 H65A 109.9 . .
O16 C65 H65B 109.9 . .
C63 C65 H65B 109.9 . .
H65A C65 H65B 108.3 . .
C63 C66 H66A 109.5 . .
C63 C66 H66B 109.5 . .
H66A C66 H66B 109.5 . .
C63 C66 H66C 109.5 . .
H66A C66 H66C 109.5 . .
H66B C66 H66C 109.5 . .
N4 C67 C69 113.8(2) . .
N4 C67 C68 105.3(2) . .
C69 C67 C68 108.9(3) . .
N4 C67 C70 107.0(2) . .
C69 C67 C70 111.2(3) . .
C68 C67 C70 110.5(3) . .
O15 C68 C67 111.0(2) . .
O15 C68 H68A 109.4 . .
C67 C68 H68A 109.4 . .
O15 C68 H68B 109.4 . .
C67 C68 H68B 109.4 . .
H68A C68 H68B 108.0 . .
C67 C69 H69A 109.5 . .
C67 C69 H69B 109.5 . .
H69A C69 H69B 109.5 . .
C67 C69 H69C 109.5 . .
H69A C69 H69C 109.5 . .
H69B C69 H69C 109.5 . .
O17 C70 C67 107.9(2) . .
O17 C70 H70A 110.1 . .
C67 C70 H70A 110.1 . .
O17 C70 H70B 110.1 . .
C67 C70 H70B 110.1 . .
H70A C70 H70B 108.4 . .
O21 Cl2 O19 110.2(2) . .
O21 Cl2 O20 109.13(18) . .
O19 Cl2 O20 109.94(17) . .
O21 Cl2 O22 110.0(2) . .
O19 Cl2 O22 109.22(19) . .
O20 Cl2 O22 108.34(18) . .
O28 Cl4 O29 113.0(3) . .
O28 Cl4 O27 114.7(4) . .
O29 Cl4 O27 109.2(3) . .
O28 Cl4 O30 105.6(3) . .
O29 Cl4 O30 105.7(3) . .
O27 Cl4 O30 108.0(2) . .
H1WA O1W H1WB 90(6) . .
H2WA O2W H2WB 122(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.921(2) .
Cu1 N1 1.938(2) .
Cu1 O3 1.947(2) .
Cu1 O2 1.973(2) .
Cu1 O11 2.354(3) .
Cu1 Cu2 2.9243(8) .
Cu1 H2 2.32(3) .
Cu2 N2 1.913(2) .
Cu2 O1 1.915(2) .
Cu2 O2 1.941(2) .
Cu2 O4 1.943(2) .
Cu2 O7 2.638(2) .
Cu2 H2 2.34(3) .
Cu3 O12 1.912(2) .
Cu3 O14 1.923(2) .
Cu3 N3 1.938(3) .
Cu3 O13 1.955(2) .
Cu3 O18 2.357(3) .
Cu3 Cu4 2.9213(8) 1_565
Cu4 O12 1.913(2) 1_545
Cu4 N4 1.921(2) 1_545
Cu4 O13 1.943(2) 1_545
Cu4 O15 1.958(2) 1_545
Cu4 O8 2.584(2) .
Cu4 Cu3 2.9213(8) 1_545
Cl1 O10 1.434(2) .
Cl1 O9 1.438(3) .
Cl1 O8 1.442(2) .
Cl1 O7 1.446(2) .
Cl3 O25 1.435(2) .
Cl3 O24 1.438(2) .
Cl3 O23 1.444(2) .
Cl3 O26 1.447(2) .
O1 C1 1.334(3) .
O2 H2 0.775(18) .
O3 C11 1.442(4) .
O3 H3 0.799(18) .
O4 C15 1.444(4) .
O4 H4 0.778(18) .
O12 C54 1.329(3) .
O12 Cu4 1.913(2) 1_565
O13 Cu4 1.943(2) 1_565
O13 H13 0.785(18) .
O15 C68 1.440(4) .
O15 Cu4 1.958(2) 1_565
O15 H15 0.799(19) .
O14 C64 1.425(4) .
O14 H14 0.814(19) .
O6 C16 1.415(4) .
O6 H6 0.768(19) .
O5 C13 1.419(4) .
O5 H5 0.83(2) .
O17 C70 1.428(4) .
O17 H17 0.790(19) .
O16 C65 1.437(4) .
O16 H16 0.804(19) .
O18 H18B 0.81(2) .
O18 H18A 0.796(19) .
N1 C8 1.283(4) .
N1 C10 1.487(4) .
N2 C9 1.293(4) .
N2 C14 1.487(4) .
N3 C62 1.280(4) .
N3 C63 1.495(4) .
N4 C61 1.294(4) .
N4 C67 1.484(4) .
N4 Cu4 1.921(2) 1_565
C1 C6 1.410(4) .
C1 C2 1.415(4) .
C2 C3 1.401(4) .
C2 C9 1.451(4) .
C3 C4 1.374(4) .
C3 H3A 0.9300 .
C4 C5 1.385(4) .
C4 C7 1.509(4) .
C5 C6 1.404(4) .
C5 H5A 0.9300 .
C6 C8 1.451(4) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C11 1.519(4) .
C10 C12 1.530(4) .
C10 C13 1.536(5) .
C11 H11C 0.9700 .
C11 H11D 0.9700 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C14 C17 1.518(5) .
C14 C15 1.531(4) .
C14 C16 1.543(4) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C54 C55 1.415(4) .
C54 C60 1.417(4) .
C55 C56 1.404(4) .
C55 C62 1.461(4) .
C56 C57 1.385(4) .
C56 H56 0.9300 .
C57 C59 1.378(4) .
C57 C58 1.513(4) .
C58 H58A 0.9600 .
C58 H58B 0.9600 .
C58 H58C 0.9600 .
C59 C60 1.408(4) .
C59 H59 0.9300 .
C60 C61 1.448(4) .
C61 H61 0.9300 .
C62 H62 0.9300 .
C63 C66 1.506(4) .
C63 C65 1.538(4) .
C63 C64 1.542(4) .
C64 H64A 0.9700 .
C64 H64B 0.9700 .
C65 H65A 0.9700 .
C65 H65B 0.9700 .
C66 H66A 0.9600 .
C66 H66B 0.9600 .
C66 H66C 0.9600 .
C67 C69 1.518(4) .
C67 C68 1.526(4) .
C67 C70 1.532(4) .
C68 H68A 0.9700 .
C68 H68B 0.9700 .
C69 H69A 0.9600 .
C69 H69B 0.9600 .
C69 H69C 0.9600 .
C70 H70A 0.9700 .
C70 H70B 0.9700 .
Cl2 O21 1.416(3) .
Cl2 O19 1.423(3) .
Cl2 O20 1.433(3) .
Cl2 O22 1.438(3) .
Cl4 O28 1.378(5) .
Cl4 O29 1.387(4) .
Cl4 O27 1.409(4) .
Cl4 O30 1.466(3) .
O1W H1WA 0.799(19) .
O1W H1WB 0.80(2) .
O2W H2WA 0.80(2) .
O2W H2WB 0.794(19) .
