#------------------------------------------------------------------------------
#$Date: 2020-08-23 07:26:50 +0300 (Sun, 23 Aug 2020) $
#$Revision: 255589 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/35/2243550.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2243550
loop_
_publ_author_name
'Dodds, Christopher A.'
'Kennedy, Alan R.'
_publ_section_title
;
 Formation of a nonanuclear copper(II) cluster with 3,5-dimethylpyrazolate
 starting from an NHC complex of copper(I) chloride
;
_journal_coeditor_code           HB7934
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1486
_journal_page_last               1490
_journal_paper_doi               10.1107/S2056989020011275
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac
'(C19 H21 N2)2 [Cu9 (C5 H7 N2)8 Cl6 (O H)6], 2C H Cl3'
_chemical_formula_moiety
'2(C19 H21 N2 +), C40 H62 Cl6 Cu9 N16 O6 2-, 2(C H Cl3)'
_chemical_formula_sum            'C80 H106 Cl12 Cu9 N20 O6'
_chemical_formula_weight         2441.10
_chemical_name_systematic
;Bis[1,3-bis(2,6-dimethylphenyl)imidazolium]
di-μ-chlorido-tetrachloridooctakis(μ-3,5-dimethylpyrazolato)hexa-μ₃-hydroxido-nonacopper(II) chloroform disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                106.143(3)
_cell_angle_beta                 93.254(2)
_cell_angle_gamma                99.819(2)
_cell_formula_units_Z            1
_cell_length_a                   12.9974(9)
_cell_length_b                   13.9305(10)
_cell_length_c                   14.7162(10)
_cell_measurement_reflns_used    35050
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.3
_cell_volume                     2506.6(3)
_computing_cell_refinement
;
CrystalClear-SM Expert (Rigaku, 2012)
;
_computing_data_collection
;
CrystalClear-SM Expert (Rigaku, 2012)
;
_computing_data_reduction
;
CrystalClear-SM Expert (Rigaku, 2012)
;
_computing_molecular_graphics
;
Mercury (Macrae et al.,  2020), OLEX2  Dolomanov et
al.,  2003)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku AFC12 Saturn724+ CCD'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37232
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         27.579
_diffrn_reflns_theta_min         3.463
_diffrn_source                   'sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.247
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrystalClear; Rigaku, 2012)
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       Block
_exptl_crystal_F_000             1239
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     598
_refine_ls_number_reflns         11446
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0746P)²+4.3606P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1305
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                10024
_reflns_number_total             11446
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7934sup1.cif
_cod_data_source_block           I
_cod_database_code               2243550
_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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.0000 0.0000 0.0000 0.01912(12) Uani d 1 . .
Cu Cu2 -0.05553(3) -0.08906(3) 0.15325(3) 0.02152(10) Uani d 1 . .
Cu Cu3 -0.21068(3) -0.20781(3) -0.02174(3) 0.02028(10) Uani d 1 . .
Cu Cu4 0.12605(3) 0.09692(3) 0.22732(3) 0.02211(10) Uani d 1 . .
Cu Cu5 0.31920(3) 0.29053(3) 0.24280(3) 0.02350(10) Uani d 1 . .
Cl Cl1 -0.03648(6) -0.25637(6) 0.02371(6) 0.02707(17) Uani d 1 . .
Cl Cl1S 0.58106(12) 0.06358(12) 0.39647(13) 0.0750(4) Uani d 1 . .
Cl Cl2 -0.05437(6) 0.13306(6) 0.19807(6) 0.03094(18) Uani d 1 . .
Cl Cl2S 0.5393(2) 0.2027(2) 0.56923(14) 0.1182(8) Uani d 1 . .
Cl Cl3 0.48127(6) 0.26149(7) 0.27012(7) 0.0354(2) Uani d 1 . .
Cl Cl3S 0.69969(18) 0.26565(18) 0.46028(19) 0.1261(10) Uani d 1 . .
O O1 0.12609(16) 0.06840(17) -0.03527(15) 0.0207(4) Uani d 1 . .
O O2 0.07482(16) -0.01795(17) 0.10925(15) 0.0204(4) Uani d 1 . .
O O3 0.18815(17) 0.20480(17) 0.15822(15) 0.0224(4) Uani d 1 . .
N N1 0.2395(2) -0.2690(2) -0.1084(2) 0.0333(7) Uani d 1 . .
N N2 0.1213(3) -0.3829(2) -0.2101(3) 0.0382(7) Uani d 1 . .
N N3 -0.1984(2) -0.1346(2) 0.18140(19) 0.0233(5) Uani d 1 . .
N N4 -0.2699(2) -0.1792(2) 0.10182(19) 0.0230(5) Uani d 1 . .
N N5 -0.2919(2) -0.3463(2) -0.07161(19) 0.0242(5) Uani d 1 . .
N N6 -0.3505(2) -0.3729(2) -0.1587(2) 0.0275(6) Uani d 1 . .
N N7 0.0389(2) -0.0921(2) 0.25950(18) 0.0245(5) Uani d 1 . .
N N8 0.1245(2) -0.0138(2) 0.28730(19) 0.0261(6) Uani d 1 . .
N N9 0.1711(2) 0.2034(2) 0.34688(19) 0.0276(6) Uani d 1 . .
N N10 0.2632(2) 0.2713(2) 0.35634(19) 0.0286(6) Uani d 1 . .
C C1 0.1374(3) -0.3016(3) -0.1335(3) 0.0325(7) Uani d 1 . .
H H1 0.0839 -0.2717 -0.1019 0.039 Uiso calc 1 . .
C C1S 0.5763(4) 0.1875(4) 0.4541(4) 0.0577(12) Uani d 1 . .
H H1S 0.5235 0.2099 0.4166 0.069 Uiso calc 1 . .
C C2 0.2919(3) -0.3328(3) -0.1725(4) 0.0479(11) Uani d 1 . .
H H2 0.3658 -0.3274 -0.1719 0.058 Uiso calc 1 . .
C C3 0.2187(4) -0.4027(3) -0.2345(4) 0.0482(11) Uani d 1 . .
H H3 0.2310 -0.4564 -0.2862 0.058 Uiso calc 1 . .
C C4 0.2842(3) -0.1802(3) -0.0298(3) 0.0331(8) Uani d 1 . .
C C5 0.2759(3) -0.1873(3) 0.0623(3) 0.0346(8) Uani d 1 . .
C C6 0.3152(3) -0.0996(3) 0.1372(3) 0.0419(9) Uani d 1 . .
H H6 0.3110 -0.1014 0.2010 0.050 Uiso calc 1 . .
C C7 0.3607(3) -0.0095(3) 0.1198(4) 0.0453(10) Uani d 1 . .
H H7 0.3868 0.0498 0.1716 0.054 Uiso calc 1 . .
C C8 0.3681(3) -0.0060(3) 0.0277(4) 0.0431(10) Uani d 1 . .
H H8 0.3999 0.0560 0.0171 0.052 Uiso calc 1 . .
C C9 0.3301(3) -0.0911(3) -0.0504(3) 0.0379(9) Uani d 1 . .
C C10 0.2289(3) -0.2845(3) 0.0825(3) 0.0404(9) Uani d 1 . .
H H10A 0.2328 -0.2733 0.1515 0.061 Uiso calc 1 . .
H H10B 0.2681 -0.3376 0.0543 0.061 Uiso calc 1 . .
H H10C 0.1553 -0.3061 0.0549 0.061 Uiso calc 1 . .
C C11 0.3389(3) -0.0871(3) -0.1505(3) 0.0422(10) Uani d 1 . .
H H11A 0.3619 -0.0162 -0.1502 0.063 Uiso calc 1 . .
H H11B 0.2703 -0.1150 -0.1883 0.063 Uiso calc 1 . .
H H11C 0.3902 -0.1274 -0.1785 0.063 Uiso calc 1 . .
C C12 0.0168(3) -0.4342(3) -0.2573(3) 0.0431(10) Uani d 1 . .
C C13 -0.0492(3) -0.4885(3) -0.2096(4) 0.0451(10) Uani d 1 . .
C C14 -0.1525(4) -0.5298(4) -0.2519(4) 0.0609(14) Uani d 1 . .
H H14 -0.1999 -0.5663 -0.2209 0.073 Uiso calc 1 . .
C C15 -0.1856(5) -0.5181(5) -0.3371(5) 0.0722(17) Uani d 1 . .
H H15 -0.2563 -0.5458 -0.3640 0.087 Uiso calc 1 . .
C C16 -0.1196(5) -0.4675(4) -0.3842(4) 0.0621(14) Uani d 1 . .
H H16 -0.1442 -0.4626 -0.4446 0.075 Uiso calc 1 . .
C C17 -0.0149(5) -0.4219(4) -0.3449(3) 0.0561(12) Uani d 1 . .
C C18 -0.0148(3) -0.5039(3) -0.1173(3) 0.0458(10) Uani d 1 . .
H H18A 0.0605 -0.5051 -0.1136 0.069 Uiso calc 1 . .
H H18B -0.0541 -0.5687 -0.1129 0.069 Uiso calc 1 . .
H H18C -0.0281 -0.4480 -0.0648 0.069 Uiso calc 1 . .
C C19 0.0585(6) -0.3621(4) -0.3931(4) 0.0699(16) Uani d 1 . .
H H19A 0.0828 -0.2926 -0.3508 0.105 Uiso calc 1 . .
H H19B 0.0218 -0.3595 -0.4522 0.105 Uiso calc 1 . .
H H19C 0.1190 -0.3948 -0.4078 0.105 Uiso calc 1 . .
C C20 -0.1967(3) -0.0718(3) 0.3572(3) 0.0380(8) Uani d 1 . .
H H20A -0.1207 -0.0679 0.3562 0.057 Uiso calc 1 . .
H H20B -0.2223 -0.1112 0.3999 0.057 Uiso calc 1 . .
H H20C -0.2112 -0.0029 0.3800 0.057 Uiso calc 1 . .
C C21 -0.2511(3) -0.1228(3) 0.2588(2) 0.0277(7) Uani d 1 . .
C C22 -0.3577(3) -0.1608(3) 0.2292(3) 0.0315(7) Uani d 1 . .
H H22 -0.4131 -0.1630 0.2685 0.038 Uiso calc 1 . .
C C23 -0.3662(3) -0.1947(3) 0.1306(3) 0.0275(7) Uani d 1 . .
C C24 -0.4627(3) -0.2392(3) 0.0604(3) 0.0351(8) Uani d 1 . .
H H24A -0.4782 -0.1884 0.0298 0.053 Uiso calc 1 . .
H H24B -0.5223 -0.2589 0.0937 0.053 Uiso calc 1 . .
H H24C -0.4506 -0.2993 0.0120 0.053 Uiso calc 1 . .
C C25 -0.2711(3) -0.4173(3) 0.0651(3) 0.0337(8) Uani d 1 . .
H H25A -0.1993 -0.3775 0.0773 0.051 Uiso calc 1 . .
H H25B -0.2696 -0.4868 0.0671 0.051 Uiso calc 1 . .
H H25C -0.3132 -0.3856 0.1138 0.051 Uiso calc 1 . .
C C26 -0.3189(3) -0.4206(3) -0.0316(2) 0.0288(7) Uani d 1 . .
C C27 -0.3961(3) -0.4963(3) -0.0922(3) 0.0344(8) Uani d 1 . .
H H27 -0.4296 -0.5579 -0.0818 0.041 Uiso calc 1 . .
C C28 -0.4141(3) -0.4634(3) -0.1711(3) 0.0337(8) Uani d 1 . .
C C29 -0.4879(3) -0.5158(3) -0.2602(3) 0.0438(10) Uani d 1 . .
H H29A -0.5283 -0.4676 -0.2748 0.066 Uiso calc 1 . .
H H29B -0.5360 -0.5736 -0.2507 0.066 Uiso calc 1 . .
H H29C -0.4475 -0.5403 -0.3132 0.066 Uiso calc 1 . .
C C30 -0.0271(3) -0.2591(3) 0.2858(3) 0.0340(8) Uani d 1 . .
H H30A -0.0883 -0.2443 0.3193 0.051 Uiso calc 1 . .
H H30B 0.0039 -0.3083 0.3092 0.051 Uiso calc 1 . .
H H30C -0.0491 -0.2877 0.2174 0.051 Uiso calc 1 . .
C C31 0.0523(3) -0.1631(3) 0.3035(2) 0.0289(7) Uani d 1 . .
C C32 0.1479(3) -0.1288(3) 0.3615(2) 0.0337(8) Uani d 1 . .
H H32 0.1778 -0.1626 0.4012 0.040 Uiso calc 1 . .
C C33 0.1901(3) -0.0362(3) 0.3493(2) 0.0313(7) Uani d 1 . .
C C34 0.2932(3) 0.0341(4) 0.3925(3) 0.0416(9) Uani d 1 . .
H H34A 0.3275 0.0582 0.3431 0.062 Uiso calc 1 . .
H H34B 0.3386 -0.0027 0.4196 0.062 Uiso calc 1 . .
H H34C 0.2806 0.0924 0.4427 0.062 Uiso calc 1 . .
C C35 0.0410(3) 0.1482(3) 0.4489(3) 0.0382(9) Uani d 1 . .
H H35A -0.0100 0.1295 0.3922 0.057 Uiso calc 1 . .
H H35B 0.0109 0.1862 0.5041 0.057 Uiso calc 1 . .
H H35C 0.0579 0.0863 0.4604 0.057 Uiso calc 1 . .
C C36 0.1390(3) 0.2132(3) 0.4339(2) 0.0343(8) Uani d 1 . .
C C37 0.2120(3) 0.2885(3) 0.5009(3) 0.0398(9) Uani d 1 . .
H H37 0.2099 0.3111 0.5678 0.048 Uiso calc 1 . .
C C38 0.2883(3) 0.3232(3) 0.4489(3) 0.0363(8) Uani d 1 . .
C C39 0.3843(3) 0.4062(3) 0.4831(3) 0.0440(10) Uani d 1 . .
H H39A 0.4390 0.3913 0.4410 0.066 Uiso calc 1 . .
H H39B 0.4102 0.4099 0.5481 0.066 Uiso calc 1 . .
H H39C 0.3663 0.4716 0.4825 0.066 Uiso calc 1 . .
H H1H 0.164(3) 0.022(3) -0.056(3) 0.046(13) Uiso d 1 . .
H H2H 0.116(3) -0.062(3) 0.093(3) 0.048(13) Uiso d 1 . .
H H3H 0.138(2) 0.240(3) 0.167(3) 0.037(11) Uiso d 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
O O 0.0106 0.0060 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cu1 O1 2 . 180.0 y
O1 Cu1 O2 2 . 87.68(9) y
O1 Cu1 O2 . . 92.32(9) y
O1 Cu1 O2 2 2 92.32(9) y
O1 Cu1 O2 . 2 87.68(9) y
O2 Cu1 O2 . 2 180.0 y
O1 Cu1 Cu2 2 2 136.36(6) ?
O1 Cu1 Cu2 . 2 43.64(6) ?
O2 Cu1 Cu2 . 2 135.95(6) ?
O2 Cu1 Cu2 2 2 44.05(6) ?
O1 Cu1 Cu2 2 . 43.64(6) ?
O1 Cu1 Cu2 . . 136.36(6) ?
O2 Cu1 Cu2 . . 44.05(6) ?
O2 Cu1 Cu2 2 . 135.95(6) ?
Cu2 Cu1 Cu2 2 . 180.0 ?
N7 Cu2 N3 . . 106.25(11) y
N7 Cu2 O1 . 2 167.65(10) y
N3 Cu2 O1 . 2 85.78(10) y
N7 Cu2 O2 . . 85.87(10) y
N3 Cu2 O2 . . 165.28(10) y
O1 Cu2 O2 2 . 81.83(8) y
N7 Cu2 Cl1 . . 101.13(9) y
N3 Cu2 Cl1 . . 98.45(8) y
O1 Cu2 Cl1 2 . 79.34(7) y
O2 Cu2 Cl1 . . 87.07(7) y
N7 Cu2 Cu1 . . 126.85(8) ?
N3 Cu2 Cu1 . . 126.06(8) ?
O1 Cu2 Cu1 2 . 40.83(6) ?
O2 Cu2 Cu1 . . 41.01(6) ?
Cl1 Cu2 Cu1 . . 81.59(2) ?
N7 Cu2 Cu3 . . 148.15(8) ?
N3 Cu2 Cu3 . . 65.40(8) ?
O1 Cu2 Cu3 2 . 39.93(6) ?
O2 Cu2 Cu3 . . 108.52(6) ?
Cl1 Cu2 Cu3 . . 53.243(19) ?
Cu1 Cu2 Cu3 . . 72.926(12) ?
N5 Cu3 N4 . . 95.03(11) y
N5 Cu3 O1 . 2 177.04(10) y
N4 Cu3 O1 . 2 82.97(10) y
N5 Cu3 O3 . 2 89.83(10) y
N4 Cu3 O3 . 2 158.66(10) y
O1 Cu3 O3 2 2 92.81(9) y
N5 Cu3 Cl1 . . 96.83(8) y
N4 Cu3 Cl1 . . 101.02(8) y
O1 Cu3 Cl1 2 . 81.45(6) y
O3 Cu3 Cl1 2 . 99.01(6) y
N5 Cu3 Cu2 . . 136.06(8) ?
N4 Cu3 Cu2 . . 63.99(8) ?
O1 Cu3 Cu2 2 . 41.03(6) ?
O3 Cu3 Cu2 2 . 124.15(6) ?
Cl1 Cu3 Cu2 . . 54.84(2) ?
N9 Cu4 N8 . . 93.34(12) y
N9 Cu4 O2 . . 176.28(11) y
N8 Cu4 O2 . . 83.51(10) y
N9 Cu4 O3 . . 87.28(10) y
N8 Cu4 O3 . . 157.45(10) y
O2 Cu4 O3 . . 96.39(9) y
N9 Cu4 Cl2 . . 97.75(9) y
N8 Cu4 Cl2 . . 112.62(8) y
O2 Cu4 Cl2 . . 81.71(6) y
O3 Cu4 Cl2 . . 89.57(6) y
N6 Cu5 N10 2 . 150.43(14) y
N6 Cu5 O3 2 . 93.11(10) y
N10 Cu5 O3 . . 92.56(10) y
N6 Cu5 Cl3 2 . 98.22(9) y
N10 Cu5 Cl3 . . 98.93(9) y
O3 Cu5 Cl3 . . 133.07(7) y
Cu3 Cl1 Cu2 . . 71.91(2) ?
Cu1 O1 Cu3 . 2 131.01(12) ?
Cu1 O1 Cu2 . 2 95.53(9) ?
Cu3 O1 Cu2 2 2 99.04(9) ?
Cu1 O1 H1H . . 107(3) ?
Cu3 O1 H1H 2 . 114(3) ?
Cu2 O1 H1H 2 . 106(3) ?
Cu1 O2 Cu4 . . 122.22(11) ?
Cu1 O2 Cu2 . . 94.94(9) ?
Cu4 O2 Cu2 . . 99.60(9) ?
Cu1 O2 H2H . . 112(3) ?
Cu4 O2 H2H . . 116(3) ?
Cu2 O2 H2H . . 107(3) ?
Cu5 O3 Cu3 . 2 106.67(10) ?
Cu5 O3 Cu4 . . 105.71(9) ?
Cu3 O3 Cu4 2 . 137.76(11) ?
Cu5 O3 H3H . . 108(3) ?
Cu3 O3 H3H 2 . 98(3) ?
Cu4 O3 H3H . . 97(3) ?
C1 N1 C2 . . 107.9(3) ?
C1 N1 C4 . . 123.7(3) ?
C2 N1 C4 . . 128.3(3) ?
C1 N2 C3 . . 107.8(3) ?
C1 N2 C12 . . 122.7(3) ?
C3 N2 C12 . . 129.4(4) ?
C21 N3 N4 . . 108.3(3) ?
C21 N3 Cu2 . . 137.0(2) ?
N4 N3 Cu2 . . 114.0(2) ?
C23 N4 N3 . . 108.1(3) ?
C23 N4 Cu3 . . 135.9(2) ?
N3 N4 Cu3 . . 115.96(19) ?
C26 N5 N6 . . 108.1(3) ?
C26 N5 Cu3 . . 132.5(2) ?
N6 N5 Cu3 . . 118.3(2) ?
C28 N6 N5 . . 108.3(3) ?
C28 N6 Cu5 . 2 132.2(2) ?
N5 N6 Cu5 . 2 119.0(2) ?
C31 N7 N8 . . 108.7(3) ?
C31 N7 Cu2 . . 134.7(2) ?
N8 N7 Cu2 . . 115.3(2) ?
C33 N8 N7 . . 107.7(3) ?
C33 N8 Cu4 . . 136.1(2) ?
N7 N8 Cu4 . . 116.14(19) ?
C36 N9 N10 . . 108.3(3) ?
C36 N9 Cu4 . . 130.7(2) ?
N10 N9 Cu4 . . 119.5(2) ?
C38 N10 N9 . . 108.5(3) ?
C38 N10 Cu5 . . 132.3(2) ?
N9 N10 Cu5 . . 118.5(2) ?
N1 C1 N2 . . 109.5(3) ?
N1 C1 H1 . . 125.3 ?
N2 C1 H1 . . 125.3 ?
Cl1S C1S Cl2S . . 112.4(3) ?
Cl1S C1S Cl3S . . 109.8(3) ?
Cl2S C1S Cl3S . . 109.4(3) ?
Cl1S C1S H1S . . 108.4 ?
Cl2S C1S H1S . . 108.4 ?
Cl3S C1S H1S . . 108.4 ?
C3 C2 N1 . . 107.1(4) ?
C3 C2 H2 . . 126.4 ?
N1 C2 H2 . . 126.4 ?
C2 C3 N2 . . 107.8(4) ?
C2 C3 H3 . . 126.1 ?
N2 C3 H3 . . 126.1 ?
C5 C4 C9 . . 123.8(4) ?
C5 C4 N1 . . 117.9(3) ?
C9 C4 N1 . . 118.2(4) ?
C4 C5 C6 . . 117.1(4) ?
C4 C5 C10 . . 122.8(4) ?
C6 C5 C10 . . 120.0(4) ?
C7 C6 C5 . . 120.8(4) ?
C7 C6 H6 . . 119.6 ?
C5 C6 H6 . . 119.6 ?
C8 C7 C6 . . 120.2(4) ?
C8 C7 H7 . . 119.9 ?
C6 C7 H7 . . 119.9 ?
C7 C8 C9 . . 121.8(4) ?
C7 C8 H8 . . 119.1 ?
C9 C8 H8 . . 119.1 ?
C8 C9 C4 . . 116.2(4) ?
C8 C9 C11 . . 121.6(4) ?
C4 C9 C11 . . 122.2(4) ?
C5 C10 H10A . . 109.5 ?
C5 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C5 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C9 C11 H11A . . 109.5 ?
C9 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C9 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 C17 . . 123.0(4) ?
C13 C12 N2 . . 118.0(4) ?
C17 C12 N2 . . 118.9(4) ?
C12 C13 C14 . . 117.4(5) ?
C12 C13 C18 . . 123.1(4) ?
C14 C13 C18 . . 119.5(5) ?
C15 C14 C13 . . 120.7(6) ?
C15 C14 H14 . . 119.6 ?
C13 C14 H14 . . 119.6 ?
C16 C15 C14 . . 121.4(5) ?
C16 C15 H15 . . 119.3 ?
C14 C15 H15 . . 119.3 ?
C15 C16 C17 . . 121.0(5) ?
C15 C16 H16 . . 119.5 ?
C17 C16 H16 . . 119.5 ?
C12 C17 C16 . . 116.5(5) ?
C12 C17 C19 . . 121.1(5) ?
C16 C17 C19 . . 122.4(5) ?
C13 C18 H18A . . 109.5 ?
C13 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C13 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C17 C19 H19A . . 109.5 ?
C17 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C17 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C21 C20 H20A . . 109.5 ?
C21 C20 H20B . . 109.5 ?
H20A C20 H20B . . 109.5 ?
C21 C20 H20C . . 109.5 ?
H20A C20 H20C . . 109.5 ?
H20B C20 H20C . . 109.5 ?
N3 C21 C22 . . 108.7(3) ?
N3 C21 C20 . . 121.8(3) ?
C22 C21 C20 . . 129.4(3) ?
C23 C22 C21 . . 105.8(3) ?
C23 C22 H22 . . 127.1 ?
C21 C22 H22 . . 127.1 ?
N4 C23 C22 . . 109.1(3) ?
N4 C23 C24 . . 121.5(3) ?
C22 C23 C24 . . 129.4(3) ?
C23 C24 H24A . . 109.5 ?
C23 C24 H24B . . 109.5 ?
H24A C24 H24B . . 109.5 ?
C23 C24 H24C . . 109.5 ?
H24A C24 H24C . . 109.5 ?
H24B C24 H24C . . 109.5 ?
C26 C25 H25A . . 109.5 ?
C26 C25 H25B . . 109.5 ?
H25A C25 H25B . . 109.5 ?
C26 C25 H25C . . 109.5 ?
H25A C25 H25C . . 109.5 ?
H25B C25 H25C . . 109.5 ?
N5 C26 C27 . . 109.2(3) ?
N5 C26 C25 . . 123.0(3) ?
C27 C26 C25 . . 127.8(3) ?
C28 C27 C26 . . 105.7(3) ?
C28 C27 H27 . . 127.2 ?
C26 C27 H27 . . 127.2 ?
N6 C28 C27 . . 108.8(3) ?
N6 C28 C29 . . 122.2(3) ?
C27 C28 C29 . . 129.0(3) ?
C28 C29 H29A . . 109.5 ?
C28 C29 H29B . . 109.5 ?
H29A C29 H29B . . 109.5 ?
C28 C29 H29C . . 109.5 ?
H29A C29 H29C . . 109.5 ?
H29B C29 H29C . . 109.5 ?
C31 C30 H30A . . 109.5 ?
C31 C30 H30B . . 109.5 ?
H30A C30 H30B . . 109.5 ?
C31 C30 H30C . . 109.5 ?
H30A C30 H30C . . 109.5 ?
H30B C30 H30C . . 109.5 ?
N7 C31 C32 . . 108.1(3) ?
N7 C31 C30 . . 121.4(3) ?
C32 C31 C30 . . 130.5(3) ?
C33 C32 C31 . . 106.0(3) ?
C33 C32 H32 . . 127.0 ?
C31 C32 H32 . . 127.0 ?
N8 C33 C32 . . 109.5(3) ?
N8 C33 C34 . . 121.2(3) ?
C32 C33 C34 . . 129.3(3) ?
C33 C34 H34A . . 109.5 ?
C33 C34 H34B . . 109.5 ?
H34A C34 H34B . . 109.5 ?
C33 C34 H34C . . 109.5 ?
H34A C34 H34C . . 109.5 ?
H34B C34 H34C . . 109.5 ?
C36 C35 H35A . . 109.5 ?
C36 C35 H35B . . 109.5 ?
H35A C35 H35B . . 109.5 ?
C36 C35 H35C . . 109.5 ?
H35A C35 H35C . . 109.5 ?
H35B C35 H35C . . 109.5 ?
N9 C36 C37 . . 108.8(3) ?
N9 C36 C35 . . 122.0(3) ?
C37 C36 C35 . . 129.2(3) ?
C38 C37 C36 . . 105.3(3) ?
C38 C37 H37 . . 127.3 ?
C36 C37 H37 . . 127.3 ?
N10 C38 C37 . . 109.1(3) ?
N10 C38 C39 . . 121.8(3) ?
C37 C38 C39 . . 129.1(3) ?
C38 C39 H39A . . 109.5 ?
C38 C39 H39B . . 109.5 ?
H39A C39 H39B . . 109.5 ?
C38 C39 H39C . . 109.5 ?
H39A C39 H39C . . 109.5 ?
H39B C39 H39C . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O1 2 1.924(2) y
Cu1 O1 . 1.924(2) y
Cu1 O2 . 1.929(2) y
Cu1 O2 2 1.929(2) y
Cu1 Cu2 2 2.9293(4) ?
Cu1 Cu2 . 2.9293(4) ?
Cu2 N7 . 1.947(3) y
Cu2 N3 . 1.964(3) y
Cu2 O1 2 2.031(2) y
Cu2 O2 . 2.044(2) y
Cu2 Cl1 . 2.6282(9) y
Cu2 Cu3 . 3.0558(5) ?
Cu3 N5 . 1.950(3) y
Cu3 N4 . 1.979(3) y
Cu3 O1 2 1.986(2) y
Cu3 O3 2 2.057(2) y
Cu3 Cl1 . 2.5755(8) y
Cu4 N9 . 1.943(3) y
Cu4 N8 . 1.977(3) y
Cu4 O2 . 1.996(2) y
Cu4 O3 . 2.115(2) y
Cu4 Cl2 . 2.5191(9) y
Cu5 N6 2 1.924(3) y
Cu5 N10 . 1.927(3) y
Cu5 O3 . 2.029(2) y
Cu5 Cl3 . 2.2466(9) y
Cl1S C1S . 1.712(6) ?
Cl2S C1S . 1.753(5) ?
Cl3S C1S . 1.760(6) ?
O1 Cu3 2 1.986(2) ?
O1 Cu2 2 2.031(2) ?
O1 H1H . 0.874(10) ?
O2 H2H . 0.877(10) ?
O3 Cu3 2 2.057(2) ?
O3 H3H . 0.876(10) ?
N1 C1 . 1.322(5) ?
N1 C2 . 1.399(5) ?
N1 C4 . 1.446(5) ?
N2 C1 . 1.334(5) ?
N2 C3 . 1.386(5) ?
N2 C12 . 1.457(5) ?
N3 C21 . 1.347(4) ?
N3 N4 . 1.377(4) ?
N4 C23 . 1.346(4) ?
N5 C26 . 1.335(4) ?
N5 N6 . 1.375(4) ?
N6 C28 . 1.344(4) ?
N6 Cu5 2 1.924(3) ?
N7 C31 . 1.352(4) ?
N7 N8 . 1.371(4) ?
N8 C33 . 1.349(4) ?
N9 C36 . 1.347(4) ?
N9 N10 . 1.368(4) ?
N10 C38 . 1.343(4) ?
C1 H1 . 0.9500 ?
C1S H1S . 1.0000 ?
C2 C3 . 1.334(7) ?
C2 H2 . 0.9500 ?
C3 H3 . 0.9500 ?
C4 C5 . 1.394(6) ?
C4 C9 . 1.402(5) ?
C5 C6 . 1.394(6) ?
C5 C10 . 1.503(5) ?
C6 C7 . 1.390(6) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.378(7) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.396(6) ?
C8 H8 . 0.9500 ?
C9 C11 . 1.500(6) ?
C10 H10A . 0.9800 ?
C10 H10B . 0.9800 ?
C10 H10C . 0.9800 ?
C11 H11A . 0.9800 ?
C11 H11B . 0.9800 ?
C11 H11C . 0.9800 ?
C12 C13 . 1.393(7) ?
C12 C17 . 1.397(7) ?
C13 C14 . 1.401(6) ?
C13 C18 . 1.489(7) ?
C14 C15 . 1.364(9) ?
C14 H14 . 0.9500 ?
C15 C16 . 1.360(9) ?
C15 H15 . 0.9500 ?
C16 C17 . 1.414(8) ?
C16 H16 . 0.9500 ?
C17 C19 . 1.497(8) ?
C18 H18A . 0.9800 ?
C18 H18B . 0.9800 ?
C18 H18C . 0.9800 ?
C19 H19A . 0.9800 ?
C19 H19B . 0.9800 ?
C19 H19C . 0.9800 ?
C20 C21 . 1.498(5) ?
C20 H20A . 0.9800 ?
C20 H20B . 0.9800 ?
C20 H20C . 0.9800 ?
C21 C22 . 1.394(5) ?
C22 C23 . 1.388(5) ?
C22 H22 . 0.9500 ?
C23 C24 . 1.501(5) ?
C24 H24A . 0.9800 ?
C24 H24B . 0.9800 ?
C24 H24C . 0.9800 ?
C25 C26 . 1.505(5) ?
C25 H25A . 0.9800 ?
C25 H25B . 0.9800 ?
C25 H25C . 0.9800 ?
C26 C27 . 1.389(5) ?
C27 C28 . 1.384(5) ?
C27 H27 . 0.9500 ?
C28 C29 . 1.503(5) ?
C29 H29A . 0.9800 ?
C29 H29B . 0.9800 ?
C29 H29C . 0.9800 ?
C30 C31 . 1.493(5) ?
C30 H30A . 0.9800 ?
C30 H30B . 0.9800 ?
C30 H30C . 0.9800 ?
C31 C32 . 1.397(5) ?
C32 C33 . 1.376(5) ?
C32 H32 . 0.9500 ?
C33 C34 . 1.506(5) ?
C34 H34A . 0.9800 ?
C34 H34B . 0.9800 ?
C34 H34C . 0.9800 ?
C35 C36 . 1.498(5) ?
C35 H35A . 0.9800 ?
C35 H35B . 0.9800 ?
C35 H35C . 0.9800 ?
C36 C37 . 1.397(5) ?
C37 C38 . 1.390(5) ?
C37 H37 . 0.9500 ?
C38 C39 . 1.504(5) ?
C39 H39A . 0.9800 ?
C39 H39B . 0.9800 ?
C39 H39C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1 H1H Cl2 2 0.874(10) 2.68(4) 3.098(2) 111(3)
O2 H2H Cl1 . 0.877(10) 2.95(5) 3.246(2) 102(3)
O3 H3H Cl2 . 0.876(10) 2.81(4) 3.277(2) 115(3)
C1 H1 Cl1 . 0.95 2.48 3.336(4) 151
C2 H2 Cl3 2_655 0.95 2.71 3.467(4) 138
C1S H1S Cl3 . 1.00 2.51 3.395(5) 147
C20 H20A N7 . 0.98 2.60 3.477(5) 149
C24 H24C N5 . 0.98 2.55 3.307(5) 134
C25 H25A Cl1 . 0.98 2.77 3.652(4) 150
C29 H29A Cl3 2 0.98 2.81 3.572(5) 135
C35 H35A Cl2 . 0.98 2.90 3.764(4) 148
C39 H39A Cl3 . 0.98 2.80 3.644(4) 144
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C21 N3 N4 C23 . . . . 0.1(4) ?
Cu2 N3 N4 C23 . . . . -172.1(2) ?
C21 N3 N4 Cu3 . . . . -178.5(2) ?
Cu2 N3 N4 Cu3 . . . . 9.3(3) ?
C26 N5 N6 C28 . . . . 0.6(4) ?
Cu3 N5 N6 C28 . . . . -168.8(2) ?
C26 N5 N6 Cu5 . . . 2 -172.4(2) ?
Cu3 N5 N6 Cu5 . . . 2 18.2(3) ?
C31 N7 N8 C33 . . . . -0.7(4) ?
Cu2 N7 N8 C33 . . . . -169.7(2) ?
C31 N7 N8 Cu4 . . . . 177.2(2) ?
Cu2 N7 N8 Cu4 . . . . 8.2(3) ?
C36 N9 N10 C38 . . . . 0.0(4) ?
Cu4 N9 N10 C38 . . . . -167.5(3) ?
C36 N9 N10 Cu5 . . . . -171.0(3) ?
Cu4 N9 N10 Cu5 . . . . 21.4(4) ?
C2 N1 C1 N2 . . . . 0.1(4) ?
C4 N1 C1 N2 . . . . 178.1(3) ?
C3 N2 C1 N1 . . . . 0.0(5) ?
C12 N2 C1 N1 . . . . -177.6(4) ?
C1 N1 C2 C3 . . . . -0.2(5) ?
C4 N1 C2 C3 . . . . -178.1(4) ?
N1 C2 C3 N2 . . . . 0.2(5) ?
C1 N2 C3 C2 . . . . -0.2(5) ?
C12 N2 C3 C2 . . . . 177.2(4) ?
C1 N1 C4 C5 . . . . 73.0(5) ?
C2 N1 C4 C5 . . . . -109.5(4) ?
C1 N1 C4 C9 . . . . -105.0(4) ?
C2 N1 C4 C9 . . . . 72.6(5) ?
C9 C4 C5 C6 . . . . 0.5(5) ?
N1 C4 C5 C6 . . . . -177.3(3) ?
C9 C4 C5 C10 . . . . -178.2(3) ?
N1 C4 C5 C10 . . . . 4.0(5) ?
C4 C5 C6 C7 . . . . 0.0(5) ?
C10 C5 C6 C7 . . . . 178.8(3) ?
C5 C6 C7 C8 . . . . -0.5(6) ?
C6 C7 C8 C9 . . . . 0.5(6) ?
C7 C8 C9 C4 . . . . 0.0(5) ?
C7 C8 C9 C11 . . . . -179.7(4) ?
C5 C4 C9 C8 . . . . -0.5(5) ?
N1 C4 C9 C8 . . . . 177.3(3) ?
C5 C4 C9 C11 . . . . 179.2(3) ?
N1 C4 C9 C11 . . . . -3.1(5) ?
C1 N2 C12 C13 . . . . -69.6(5) ?
C3 N2 C12 C13 . . . . 113.3(5) ?
C1 N2 C12 C17 . . . . 106.5(5) ?
C3 N2 C12 C17 . . . . -70.6(6) ?
C17 C12 C13 C14 . . . . -1.5(6) ?
N2 C12 C13 C14 . . . . 174.4(4) ?
C17 C12 C13 C18 . . . . 178.5(4) ?
N2 C12 C13 C18 . . . . -5.6(6) ?
C12 C13 C14 C15 . . . . 0.9(7) ?
C18 C13 C14 C15 . . . . -179.0(5) ?
C13 C14 C15 C16 . . . . 0.9(8) ?
C14 C15 C16 C17 . . . . -2.3(8) ?
C13 C12 C17 C16 . . . . 0.2(6) ?
N2 C12 C17 C16 . . . . -175.7(4) ?
C13 C12 C17 C19 . . . . 179.4(4) ?
N2 C12 C17 C19 . . . . 3.5(6) ?
C15 C16 C17 C12 . . . . 1.7(7) ?
C15 C16 C17 C19 . . . . -177.5(5) ?
N4 N3 C21 C22 . . . . 0.4(4) ?
Cu2 N3 C21 C22 . . . . 169.8(3) ?
N4 N3 C21 C20 . . . . -177.2(3) ?
Cu2 N3 C21 C20 . . . . -7.7(5) ?
N3 C21 C22 C23 . . . . -0.6(4) ?
C20 C21 C22 C23 . . . . 176.7(4) ?
N3 N4 C23 C22 . . . . -0.5(4) ?
Cu3 N4 C23 C22 . . . . 177.7(3) ?
N3 N4 C23 C24 . . . . 177.8(3) ?
Cu3 N4 C23 C24 . . . . -4.0(5) ?
C21 C22 C23 N4 . . . . 0.7(4) ?
C21 C22 C23 C24 . . . . -177.4(3) ?
N6 N5 C26 C27 . . . . -0.4(4) ?
Cu3 N5 C26 C27 . . . . 167.0(3) ?
N6 N5 C26 C25 . . . . -179.5(3) ?
Cu3 N5 C26 C25 . . . . -12.2(5) ?
N5 C26 C27 C28 . . . . 0.0(4) ?
C25 C26 C27 C28 . . . . 179.1(4) ?
N5 N6 C28 C27 . . . . -0.6(4) ?
Cu5 N6 C28 C27 2 . . . 171.1(3) ?
N5 N6 C28 C29 . . . . -179.0(4) ?
Cu5 N6 C28 C29 2 . . . -7.3(6) ?
C26 C27 C28 N6 . . . . 0.3(5) ?
C26 C27 C28 C29 . . . . 178.6(4) ?
N8 N7 C31 C32 . . . . 0.7(4) ?
Cu2 N7 C31 C32 . . . . 166.7(3) ?
N8 N7 C31 C30 . . . . -178.6(3) ?
Cu2 N7 C31 C30 . . . . -12.7(5) ?
N7 C31 C32 C33 . . . . -0.5(4) ?
C30 C31 C32 C33 . . . . 178.8(4) ?
N7 N8 C33 C32 . . . . 0.4(4) ?
Cu4 N8 C33 C32 . . . . -176.9(3) ?
N7 N8 C33 C34 . . . . 179.0(3) ?
Cu4 N8 C33 C34 . . . . 1.7(6) ?
C31 C32 C33 N8 . . . . 0.0(4) ?
C31 C32 C33 C34 . . . . -178.4(4) ?
N10 N9 C36 C37 . . . . -0.3(5) ?
Cu4 N9 C36 C37 . . . . 165.3(3) ?
N10 N9 C36 C35 . . . . -178.9(4) ?
Cu4 N9 C36 C35 . . . . -13.3(6) ?
N9 C36 C37 C38 . . . . 0.5(5) ?
C35 C36 C37 C38 . . . . 179.0(4) ?
N9 N10 C38 C37 . . . . 0.3(5) ?
Cu5 N10 C38 C37 . . . . 169.7(3) ?
N9 N10 C38 C39 . . . . -178.3(4) ?
Cu5 N10 C38 C39 . . . . -9.0(6) ?
C36 C37 C38 N10 . . . . -0.5(5) ?
C36 C37 C38 C39 . . . . 178.0(4) ?

_cod_database_fobs_code 2243550
