#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/14/4341438.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_4341438
loop_
_publ_author_name
'Bazzicalupi, Carla'
'Bianchi, Antonio'
'Biver, Tarita'
'Giorgi, Claudia'
'Santarelli, Samuele'
'Savastano, Matteo'
_publ_section_title
;
 Formation of Double-Strand Dimetallic Helicates with a Terpyridine-Based
 Macrocycle.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141104130636006
_journal_paper_doi               10.1021/ic502329s
_journal_year                    2014
_chemical_formula_sum            'C58 H60 Cl6.5 Cu3 N15 Na O27.5 S0.5'
_chemical_formula_weight         1867.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 137.782(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   36.131(2)
_cell_length_b                   20.2539(4)
_cell_length_c                   28.6248(18)
_cell_measurement_reflns_used    29953
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.2224
_cell_measurement_theta_min      4.1116
_cell_volume                     14076(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare 1997)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.1241
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            62350
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         72.01
_diffrn_reflns_theta_min         4.10
_diffrn_standards_interval_count infinity
_diffrn_standards_interval_time  infinity
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             7596
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.821
_refine_diff_density_min         -2.565
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         13490
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0874P)²+104.1977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1487
_refine_ls_wR_factor_ref         0.1717
_reflns_number_gt                10688
_reflns_number_total             13490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502329s_si_002.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        14075.8(13)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C58 H60 Cl6.50 Cu3 N15 Na O27.50 S0.50'
_cod_database_code               4341438
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.70790(2) 0.12677(3) 0.33399(3) 0.01718(15) Uani 1 1 d .
Cu2 Cu 0.69566(3) 0.13189(3) 0.19982(3) 0.02120(16) Uani 1 1 d .
Cu3 Cu 0.99566(2) -0.17610(3) 0.68983(3) 0.01774(15) Uani 1 1 d .
Na Na 0.59985(8) -0.07713(11) -0.08535(10) 0.0377(5) Uani 1 1 d .
OW1 O 0.68799(14) -0.10744(19) 0.01429(17) 0.0369(8) Uani 1 1 d .
Cl1 Cl 0.67429(4) 0.05843(6) -0.04989(5) 0.0269(2) Uani 1 1 d .
O11 O 0.63325(17) 0.0371(2) -0.0551(2) 0.0549(11) Uani 1 1 d .
O12 O 0.6587(2) 0.0343(3) -0.1101(2) 0.0674(14) Uani 1 1 d .
O13 O 0.72654(15) 0.03414(19) 0.01269(19) 0.0482(10) Uani 1 1 d .
O14 O 0.67456(17) 0.13054(19) -0.0504(2) 0.0500(10) Uani 1 1 d .
Cl2 Cl 0.57965(4) -0.07224(6) 0.01258(5) 0.0306(3) Uani 1 1 d .
O21 O 0.57025(17) -0.0297(3) -0.0354(2) 0.0799(18) Uani 1 1 d .
O22 O 0.5826(2) -0.1385(3) -0.0016(3) 0.101(2) Uani 1 1 d .
O23 O 0.53596(15) -0.0658(3) 0.0040(2) 0.0543(12) Uani 1 1 d .
O24 O 0.63135(14) -0.05519(17) 0.08258(16) 0.0358(8) Uani 1 1 d .
Cl3 Cl 0.61643(4) -0.26076(6) -0.06711(5) 0.0269(2) Uani 1 1 d .
O31 O 0.58956(15) -0.20035(19) -0.10445(18) 0.0472(10) Uani 1 1 d .
O32 O 0.63574(19) -0.2960(2) -0.0896(2) 0.0565(11) Uani 1 1 d .
O33 O 0.58044(16) -0.3031(2) -0.0755(2) 0.0499(11) Uani 1 1 d .
O34 O 0.66362(15) -0.2459(2) 0.00617(17) 0.0481(10) Uani 1 1 d .
Cl4 Cl 0.51687(13) -0.07990(13) -0.23957(17) 0.0584(13) Uani 0.50 1 d P
O41 O 0.5100(2) -0.0440(3) -0.1999(3) 0.0764(12) Uani 1 1 d .
O43 O 0.5000 -0.1442(4) -0.2500 0.0764(12) Uani 1 2 d S
O42 O 0.5797(5) -0.0870(5) -0.1919(5) 0.0764(12) Uani 0.50 1 d P
Cl5 Cl 0.60388(5) -0.23897(6) 0.16794(6) 0.0329(3) Uani 1 1 d .
O51 O 0.56599(17) -0.18852(18) 0.1477(2) 0.0411(9) Uani 1 1 d .
O52 O 0.57528(19) -0.2835(2) 0.1098(2) 0.0569(12) Uani 1 1 d .
O53 O 0.6508(2) -0.2101(2) 0.1898(3) 0.0599(12) Uani 1 1 d .
O54 O 0.62185(16) -0.27748(19) 0.22485(18) 0.0394(9) Uani 1 1 d .
Cl6 Cl 0.79137(4) -0.18530(5) 0.42037(5) 0.0289(2) Uani 1 1 d .
O61 O 0.79812(17) -0.2081(2) 0.3792(2) 0.0468(10) Uani 1 1 d .
O62 O 0.73764(14) -0.15626(18) 0.37617(19) 0.0386(8) Uani 1 1 d .
O63 O 0.79965(16) -0.23978(19) 0.4602(2) 0.0477(10) Uani 1 1 d .
O64 O 0.83263(15) -0.13546(18) 0.46805(19) 0.0403(9) Uani 1 1 d .
Cl7 Cl 0.82999(5) 0.05090(5) 0.68832(5) 0.0274(2) Uani 1 1 d .
O71 O 0.84091(14) -0.01773(16) 0.68777(18) 0.0338(8) Uani 1 1 d .
O72 O 0.77545(14) 0.05601(18) 0.65823(18) 0.0373(8) Uani 1 1 d .
O73 O 0.87033(15) 0.0746(2) 0.75883(18) 0.0421(9) Uani 1 1 d .
O74 O 0.83181(18) 0.08954(18) 0.6477(2) 0.0448(10) Uani 1 1 d .
N1 N 0.63787(14) 0.16975(18) 0.27627(17) 0.0205(7) Uani 1 1 d .
C1 C 0.63587(18) 0.2290(2) 0.2954(2) 0.0237(9) Uani 1 1 d .
C2 C 0.5863(2) 0.2626(3) 0.2536(3) 0.0343(11) Uani 1 1 d .
H2 H 0.5848 0.3036 0.2667 0.041 Uiso 1 1 calc R
C3 C 0.5389(2) 0.2332(3) 0.1915(3) 0.0419(13) Uani 1 1 d .
H3 H 0.5052 0.2549 0.1625 0.050 Uiso 1 1 calc R
C4 C 0.54171(19) 0.1712(3) 0.1727(3) 0.0351(11) Uani 1 1 d .
H4 H 0.5102 0.1513 0.1313 0.042 Uiso 1 1 calc R
C5 C 0.59228(18) 0.1398(2) 0.2168(2) 0.0243(9) Uani 1 1 d .
N2 N 0.65758(14) 0.06440(17) 0.24407(17) 0.0203(7) Uani 1 1 d .
C6 C 0.60383(18) 0.0748(2) 0.2061(2) 0.0248(9) Uani 1 1 d .
C7 C 0.5639(2) 0.0263(2) 0.1617(2) 0.0303(11) Uani 1 1 d .
H7 H 0.5274 0.0346 0.1357 0.036 Uiso 1 1 calc R
C8 C 0.5784(2) -0.0336(3) 0.1563(2) 0.0327(11) Uani 1 1 d .
H8 H 0.5522 -0.0667 0.1281 0.039 Uiso 1 1 calc R
C9 C 0.6326(2) -0.0440(2) 0.1937(2) 0.0302(10) Uani 1 1 d .
H9 H 0.6434 -0.0843 0.1912 0.036 Uiso 1 1 calc R
C10 C 0.67034(18) 0.0066(2) 0.2349(2) 0.0204(9) Uani 1 1 d .
N3 N 0.74279(15) 0.05206(17) 0.25459(18) 0.0214(7) Uani 1 1 d .
C11 C 0.72679(19) 0.0008(2) 0.2667(2) 0.0238(9) Uani 1 1 d .
C12 C 0.7594(2) -0.0545(2) 0.3037(2) 0.0298(10) Uani 1 1 d .
H12 H 0.7469 -0.0903 0.3095 0.036 Uiso 1 1 calc R
C13 C 0.8114(2) -0.0547(3) 0.3321(2) 0.0377(12) Uani 1 1 d .
H13 H 0.8354 -0.0896 0.3600 0.045 Uiso 1 1 calc R
C14 C 0.8273(2) -0.0029(3) 0.3188(2) 0.0347(12) Uani 1 1 d .
H14 H 0.8619 -0.0030 0.3372 0.042 Uiso 1 1 calc R
C15 C 0.79168(19) 0.0493(2) 0.2780(2) 0.0258(10) Uani 1 1 d .
C16 C 0.8047(2) 0.1070(3) 0.2578(3) 0.0340(11) Uani 1 1 d .
H16C H 0.8286 0.1379 0.2962 0.041 Uiso 1 1 calc R
H16D H 0.8242 0.0908 0.2488 0.041 Uiso 1 1 calc R
N4 N 0.75438(18) 0.1409(2) 0.1960(2) 0.0311(9) Uani 1 1 d .
H4A H 0.7611 0.1840 0.1952 0.047 Uiso 1 1 calc R
C17 C 0.7256(2) 0.1066(3) 0.1301(3) 0.0339(11) Uani 1 1 d .
H17A H 0.7339 0.0598 0.1388 0.041 Uiso 1 1 calc R
H17B H 0.7386 0.1239 0.1126 0.041 Uiso 1 1 calc R
C18 C 0.6644(2) 0.1169(3) 0.0768(3) 0.0349(12) Uani 1 1 d .
H18A H 0.6460 0.0953 0.0337 0.042 Uiso 1 1 calc R
H18B H 0.6562 0.1637 0.0675 0.042 Uiso 1 1 calc R
N5 N 0.64365(16) 0.0890(2) 0.10295(19) 0.0276(8) Uani 1 1 d .
H5A H 0.6473 0.0443 0.1068 0.041 Uiso 1 1 calc R
C19 C 0.5861(2) 0.1081(3) 0.0592(2) 0.0345(11) Uani 1 1 d .
H19A H 0.5693 0.0760 0.0643 0.041 Uiso 1 1 calc R
H19B H 0.5650 0.1093 0.0107 0.041 Uiso 1 1 calc R
N6 N 0.63468(16) 0.19340(19) 0.14567(18) 0.0265(8) Uani 1 1 d .
C20 C 0.5860(2) 0.1757(2) 0.0818(2) 0.0302(10) Uani 1 1 d .
C21 C 0.5410(2) 0.2185(3) 0.0430(3) 0.0371(12) Uani 1 1 d .
H21 H 0.5068 0.2064 -0.0008 0.045 Uiso 1 1 calc R
C22 C 0.5481(2) 0.2791(3) 0.0708(3) 0.0414(13) Uani 1 1 d .
H22 H 0.5186 0.3083 0.0450 0.050 Uiso 1 1 calc R
C23 C 0.5990(2) 0.2973(3) 0.1370(3) 0.0378(12) Uani 1 1 d .
H23 H 0.6037 0.3378 0.1562 0.045 Uiso 1 1 calc R
C24 C 0.6427(2) 0.2523(2) 0.1737(2) 0.0276(10) Uani 1 1 d .
N7 N 0.73009(15) 0.20554(18) 0.27628(18) 0.0233(8) Uani 1 1 d .
C25 C 0.6998(2) 0.2622(2) 0.2435(2) 0.0272(10) Uani 1 1 d .
C26 C 0.7212(2) 0.3246(2) 0.2720(3) 0.0354(12) Uani 1 1 d .
H26 H 0.6989 0.3618 0.2497 0.043 Uiso 1 1 calc R
C27 C 0.7765(2) 0.3300(3) 0.3343(3) 0.0381(13) Uani 1 1 d .
H27 H 0.7925 0.3714 0.3527 0.046 Uiso 1 1 calc R
C28 C 0.8076(2) 0.2740(3) 0.3688(3) 0.0368(13) Uani 1 1 d .
H28 H 0.8447 0.2773 0.4111 0.044 Uiso 1 1 calc R
C29 C 0.7832(2) 0.2119(2) 0.3404(2) 0.0272(10) Uani 1 1 d .
N8 N 0.78491(15) 0.10890(19) 0.38539(17) 0.0227(8) Uani 1 1 d .
C30 C 0.81283(18) 0.1519(3) 0.3841(2) 0.0277(10) Uani 1 1 d .
C31 C 0.8690(2) 0.1428(3) 0.4279(3) 0.0442(15) Uani 1 1 d .
H31 H 0.8882 0.1725 0.4272 0.053 Uiso 1 1 calc R
C32 C 0.8952(2) 0.0899(4) 0.4717(3) 0.0552(19) Uani 1 1 d .
H32 H 0.9324 0.0830 0.5006 0.066 Uiso 1 1 calc R
C33 C 0.8664(2) 0.0464(3) 0.4730(3) 0.0500(17) Uani 1 1 d .
H33 H 0.8842 0.0101 0.5027 0.060 Uiso 1 1 calc R
C34 C 0.8112(2) 0.0572(2) 0.4299(2) 0.0328(11) Uani 1 1 d .
C35 C 0.7770(2) 0.0148(2) 0.4307(2) 0.0370(12) Uani 1 1 d .
H35C H 0.7601 -0.0211 0.3976 0.044 Uiso 1 1 calc R
H35D H 0.8005 -0.0042 0.4765 0.044 Uiso 1 1 calc R
N9 N 0.73409(17) 0.05543(18) 0.41243(19) 0.0264(8) Uani 1 1 d .
H9A H 0.7053 0.0303 0.3954 0.040 Uiso 1 1 calc R
C36 C 0.7559(2) 0.0978(2) 0.4715(2) 0.0293(10) Uani 1 1 d .
H36C H 0.7944 0.1077 0.5020 0.035 Uiso 1 1 calc R
H36D H 0.7529 0.0745 0.4982 0.035 Uiso 1 1 calc R
C37 C 0.7234(2) 0.1610(2) 0.4434(2) 0.0263(10) Uani 1 1 d .
H37A H 0.6849 0.1513 0.4135 0.032 Uiso 1 1 calc R
H37B H 0.7371 0.1884 0.4815 0.032 Uiso 1 1 calc R
N10 N 0.72901(14) 0.19681(18) 0.40293(17) 0.0206(7) Uani 1 1 d .
H10A H 0.7645 0.2101 0.4318 0.031 Uiso 1 1 calc R
C38 C 0.69109(18) 0.2541(2) 0.3635(2) 0.0233(9) Uani 1 1 d .
H38C H 0.7056 0.2858 0.3549 0.028 Uiso 1 1 calc R
H38D H 0.6873 0.2757 0.3899 0.028 Uiso 1 1 calc R
N11 N 0.92495(14) -0.17356(18) 0.69976(17) 0.0197(7) Uani 1 1 d .
C39 C 0.89664(17) -0.2283(2) 0.6868(2) 0.0209(9) Uani 1 1 d .
C40 C 0.83916(19) -0.2307(3) 0.6327(2) 0.0277(10) Uani 1 1 d .
H40 H 0.8208 -0.2689 0.6247 0.033 Uiso 1 1 calc R
C41 C 0.81009(19) -0.1757(3) 0.5914(2) 0.0297(10) Uani 1 1 d .
H41 H 0.7718 -0.1760 0.5559 0.036 Uiso 1 1 calc R
C42 C 0.83833(18) -0.1199(2) 0.6029(2) 0.0278(10) Uani 1 1 d .
H42 H 0.8192 -0.0825 0.5754 0.033 Uiso 1 1 calc R
C43 C 0.89579(17) -0.1207(2) 0.6564(2) 0.0205(9) Uani 1 1 d .
N12 N 0.96796(15) -0.08350(18) 0.67184(16) 0.0205(7) Uani 1 1 d .
C44 C 0.92611(18) -0.0657(2) 0.6619(2) 0.0209(9) Uani 1 1 d .
C45 C 0.9099(2) -0.0002(2) 0.6509(2) 0.0293(10) Uani 1 1 d .
H45 H 0.8813 0.0115 0.6442 0.035 Uiso 1 1 calc R
C46 C 0.9371(2) 0.0478(2) 0.6500(2) 0.0367(12) Uani 1 1 d .
H46 H 0.9279 0.0922 0.6447 0.044 Uiso 1 1 calc R
C47 C 0.9776(2) 0.0290(3) 0.6570(2) 0.0359(12) Uani 1 1 d .
H47 H 0.9950 0.0603 0.6547 0.043 Uiso 1 1 calc R
C48 C 0.99239(18) -0.0374(2) 0.6675(2) 0.0256(9) Uani 1 1 d .
C49 C 1.0338(2) -0.0623(3) 0.6714(2) 0.0315(11) Uani 1 1 d .
H49C H 1.0322 -0.0356 0.6418 0.038 Uiso 1 1 calc R
H49D H 1.0706 -0.0586 0.7187 0.038 Uiso 1 1 calc R
N13 N 1.02216(15) -0.1313(2) 0.64887(19) 0.0265(8) Uani 1 1 d .
H13A H 1.0525 -0.1519 0.6657 0.040 Uiso 1 1 calc R
C50 C 0.9738(2) -0.1405(3) 0.5724(2) 0.0328(11) Uani 1 1 d .
H50A H 0.9852 -0.1371 0.5507 0.039 Uiso 1 1 calc R
H50B H 0.9467 -0.1064 0.5531 0.039 Uiso 1 1 calc R
C51 C 0.94851(19) -0.2083(3) 0.5577(2) 0.0299(11) Uani 1 1 d .
H51E H 0.9171 -0.2146 0.5078 0.036 Uiso 1 1 calc R
H51F H 0.9754 -0.2423 0.5757 0.036 Uiso 1 1 calc R
N14 N 0.93055(15) -0.21478(19) 0.59054(18) 0.0238(8) Uani 1 1 d .
H14A H 0.8991 -0.1915 0.5664 0.036 Uiso 1 1 calc R
C52 C 0.92329(19) -0.2851(2) 0.5973(2) 0.0279(10) Uani 1 1 d .
H52A H 0.9069 -0.3096 0.5563 0.033 Uiso 1 1 calc R
H52B H 0.8991 -0.2883 0.6015 0.033 Uiso 1 1 calc R
N15 N 1.01639(15) -0.26808(18) 0.70823(18) 0.0208(7) Uani 1 1 d .
C53 C 0.9792(2) -0.3137(2) 0.6613(2) 0.0255(9) Uani 1 1 d .
C54 C 0.9931(2) -0.3803(2) 0.6737(3) 0.0340(11) Uani 1 1 d .
H54 H 0.9670 -0.4122 0.6419 0.041 Uiso 1 1 calc R
C55 C 1.0466(2) -0.3980(2) 0.7343(3) 0.0356(12) Uani 1 1 d .
H55 H 1.0565 -0.4423 0.7440 0.043 Uiso 1 1 calc R
C56 C 1.0857(2) -0.3498(2) 0.7810(2) 0.0277(10) Uani 1 1 d .
H56 H 1.1223 -0.3611 0.8206 0.033 Uiso 1 1 calc R
C57 C 1.06868(18) -0.2849(2) 0.7667(2) 0.0222(9) Uani 1 1 d .
C58 C 0.4578(3) 0.4412(4) -0.0572(4) 0.0148(15) Uani 0.50 1 d PU
C59 C 0.5476(4) 0.4742(4) 0.0117(5) 0.029(2) Uani 0.50 1 d P
O1 O 0.4804(3) 0.5381(6) -0.0482(5) 0.108(6) Uani 0.50 1 d P
S1 S 0.50017(18) 0.51363(17) 0.0060(2) 0.0389(8) Uani 0.50 1 d P
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 '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
N1 Cu1 N8 161.00(16) . .
N1 Cu1 N10 80.19(14) . .
N8 Cu1 N10 95.38(14) . .
N1 Cu1 N2 80.15(14) . .
N8 Cu1 N2 104.96(14) . .
N10 Cu1 N2 159.62(14) . .
N1 Cu1 N9 118.04(15) . .
N8 Cu1 N9 79.51(15) . .
N10 Cu1 N9 84.31(14) . .
N2 Cu1 N9 100.31(13) . .
N6 Cu2 N3 161.61(16) . .
N6 Cu2 N5 80.27(16) . .
N3 Cu2 N5 96.45(15) . .
N6 Cu2 N7 79.88(15) . .
N3 Cu2 N7 104.48(14) . .
N5 Cu2 N7 159.07(16) . .
N6 Cu2 N4 118.13(16) . .
N3 Cu2 N4 79.34(15) . .
N5 Cu2 N4 85.42(15) . .
N7 Cu2 N4 98.14(14) . .
N15 Cu3 N12 172.72(15) . .
N15 Cu3 N14 80.03(15) . .
N12 Cu3 N14 99.04(15) . .
N15 Cu3 N13 108.13(15) . .
N12 Cu3 N13 78.92(15) . .
N14 Cu3 N13 85.69(14) . .
N15 Cu3 N11 78.45(14) . 2_756
N12 Cu3 N11 102.71(14) . 2_756
N14 Cu3 N11 158.25(15) . 2_756
N13 Cu3 N11 97.96(13) . 2_756
OW1 Na O41 171.47(19) . .
OW1 Na O11 86.90(16) . .
O41 Na O11 91.87(18) . .
OW1 Na O31 81.36(14) . .
O41 Na O31 98.31(16) . .
O11 Na O31 164.82(16) . .
OW1 Na O21 100.32(15) . .
O41 Na O21 87.51(16) . .
O11 Na O21 75.20(18) . .
O31 Na O21 116.29(19) . .
OW1 Na O42 111.7(3) . .
O41 Na O42 60.1(3) . .
O11 Na O42 97.2(3) . .
O31 Na O42 78.4(3) . .
O21 Na O42 146.8(3) . .
OW1 Na Cl4 142.08(15) . .
O41 Na Cl4 30.46(14) . .
O11 Na Cl4 103.50(14) . .
O31 Na Cl4 80.52(11) . .
O21 Na Cl4 117.56(14) . .
O42 Na Cl4 31.7(3) . .
O13 Cl1 O11 109.4(3) . .
O13 Cl1 O12 111.6(3) . .
O11 Cl1 O12 108.2(3) . .
O13 Cl1 O14 110.3(2) . .
O11 Cl1 O14 108.2(3) . .
O12 Cl1 O14 109.0(3) . .
Cl1 O11 Na 121.2(2) . .
O23 Cl2 O22 110.2(4) . .
O23 Cl2 O21 109.7(3) . .
O22 Cl2 O21 107.9(4) . .
O23 Cl2 O24 110.5(2) . .
O22 Cl2 O24 109.1(2) . .
O21 Cl2 O24 109.4(3) . .
Cl2 O21 Na 114.5(4) . .
O33 Cl3 O31 111.1(2) . .
O33 Cl3 O32 108.2(3) . .
O31 Cl3 O32 112.0(3) . .
O33 Cl3 O34 108.5(3) . .
O31 Cl3 O34 108.9(2) . .
O32 Cl3 O34 108.1(3) . .
Cl3 O31 Na 140.8(2) . .
Cl4 Cl4 O43 71.45(19) 2_654 .
Cl4 Cl4 O41 79.5(5) 2_654 2_654
O43 Cl4 O41 115.5(3) . 2_654
Cl4 Cl4 O41 66.0(5) 2_654 .
O43 Cl4 O41 109.0(4) . .
O41 Cl4 O41 109.2(5) 2_654 .
Cl4 Cl4 O42 169.8(7) 2_654 .
O43 Cl4 O42 103.1(5) . .
O41 Cl4 O42 110.7(6) 2_654 .
O41 Cl4 O42 109.1(4) . .
Cl4 Cl4 Na 112.1(6) 2_654 .
O43 Cl4 Na 97.90(17) . .
O41 Cl4 Na 146.6(3) 2_654 .
O41 Cl4 Na 54.8(2) . .
O42 Cl4 Na 59.4(4) . .
Cl4 O41 Cl4 34.6(3) 2_654 .
Cl4 O41 Na 122.0(3) 2_654 .
Cl4 O41 Na 94.7(3) . .
Cl4 O43 Cl4 37.1(4) . 2_654
Cl4 O42 Na 88.9(5) . .
O53 Cl5 O51 110.6(3) . .
O53 Cl5 O52 111.3(3) . .
O51 Cl5 O52 108.8(2) . .
O53 Cl5 O54 109.1(3) . .
O51 Cl5 O54 109.5(2) . .
O52 Cl5 O54 107.4(2) . .
O62 Cl6 O61 110.2(2) . .
O62 Cl6 O64 108.7(2) . .
O61 Cl6 O64 108.3(2) . .
O62 Cl6 O63 111.1(2) . .
O61 Cl6 O63 109.7(3) . .
O64 Cl6 O63 108.7(2) . .
O73 Cl7 O74 110.2(3) . .
O73 Cl7 O71 109.5(2) . .
O74 Cl7 O71 109.7(2) . .
O73 Cl7 O72 109.1(2) . .
O74 Cl7 O72 109.5(2) . .
O71 Cl7 O72 108.8(2) . .
C1 N1 C5 122.1(4) . .
C1 N1 Cu1 119.2(3) . .
C5 N1 Cu1 118.7(3) . .
N1 C1 C2 120.7(4) . .
N1 C1 C38 114.1(4) . .
C2 C1 C38 125.2(4) . .
C1 C2 C3 118.3(5) . .
C2 C3 C4 120.2(5) . .
C5 C4 C3 118.9(5) . .
N1 C5 C4 119.8(4) . .
N1 C5 C6 113.1(4) . .
C4 C5 C6 127.0(4) . .
C10 N2 C6 117.8(4) . .
C10 N2 Cu1 129.4(3) . .
C6 N2 Cu1 107.8(3) . .
N2 C6 C7 121.3(4) . .
N2 C6 C5 115.1(4) . .
C7 C6 C5 123.6(4) . .
C8 C7 C6 120.0(5) . .
C7 C8 C9 119.0(5) . .
C10 C9 C8 118.8(5) . .
N2 C10 C9 122.9(4) . .
N2 C10 C11 117.0(4) . .
C9 C10 C11 119.8(4) . .
C15 N3 C11 119.5(4) . .
C15 N3 Cu2 117.6(3) . .
C11 N3 Cu2 122.9(3) . .
N3 C11 C12 122.4(4) . .
N3 C11 C10 115.6(4) . .
C12 C11 C10 121.9(4) . .
C11 C12 C13 117.6(5) . .
C14 C13 C12 119.7(5) . .
C13 C14 C15 119.9(5) . .
N3 C15 C14 120.6(4) . .
N3 C15 C16 116.0(4) . .
C14 C15 C16 123.4(4) . .
N4 C16 C15 111.3(4) . .
C16 N4 C17 112.9(4) . .
C16 N4 Cu2 106.2(3) . .
C17 N4 Cu2 103.3(3) . .
N4 C17 C18 110.0(4) . .
C17 C18 N5 110.1(4) . .
C19 N5 C18 112.7(4) . .
C19 N5 Cu2 109.8(3) . .
C18 N5 Cu2 102.5(3) . .
N5 C19 C20 108.7(4) . .
C20 N6 C24 122.4(4) . .
C20 N6 Cu2 119.0(3) . .
C24 N6 Cu2 118.6(3) . .
N6 C20 C21 119.8(5) . .
N6 C20 C19 114.0(4) . .
C21 C20 C19 126.2(4) . .
C22 C21 C20 118.9(5) . .
C21 C22 C23 120.9(5) . .
C22 C23 C24 117.8(5) . .
N6 C24 C23 120.2(5) . .
N6 C24 C25 113.4(4) . .
C23 C24 C25 126.4(5) . .
C29 N7 C25 117.3(4) . .
C29 N7 Cu2 128.3(3) . .
C25 N7 Cu2 108.7(3) . .
N7 C25 C26 123.0(5) . .
N7 C25 C24 114.8(4) . .
C26 C25 C24 122.1(5) . .
C27 C26 C25 118.4(5) . .
C28 C27 C26 119.6(5) . .
C27 C28 C29 119.8(5) . .
N7 C29 C28 121.4(5) . .
N7 C29 C30 118.4(4) . .
C28 C29 C30 119.7(4) . .
C34 N8 C30 120.4(4) . .
C34 N8 Cu1 117.3(3) . .
C30 N8 Cu1 121.6(3) . .
N8 C30 C31 120.4(5) . .
N8 C30 C29 117.6(4) . .
C31 C30 C29 121.7(5) . .
C32 C31 C30 119.2(6) . .
C31 C32 C33 120.1(5) . .
C34 C33 C32 119.4(6) . .
N8 C34 C33 120.4(6) . .
N8 C34 C35 116.2(4) . .
C33 C34 C35 123.3(5) . .
N9 C35 C34 109.5(4) . .
C35 N9 C36 112.7(4) . .
C35 N9 Cu1 105.9(3) . .
C36 N9 Cu1 104.1(3) . .
N9 C36 C37 109.5(4) . .
N10 C37 C36 109.0(3) . .
C38 N10 C37 112.9(3) . .
C38 N10 Cu1 109.3(2) . .
C37 N10 Cu1 103.9(3) . .
N10 C38 C1 108.2(3) . .
C39 N11 C43 118.2(4) . .
C39 N11 Cu3 107.0(3) . 2_756
C43 N11 Cu3 129.5(3) . 2_756
N11 C39 C40 122.2(4) . .
N11 C39 C57 114.9(4) . 2_756
C40 C39 C57 122.9(4) . 2_756
C41 C40 C39 118.9(4) . .
C40 C41 C42 119.7(4) . .
C41 C42 C43 119.0(4) . .
N11 C43 C42 121.8(4) . .
N11 C43 C44 118.7(4) . .
C42 C43 C44 119.2(4) . .
C48 N12 C44 119.8(4) . .
C48 N12 Cu3 115.7(3) . .
C44 N12 Cu3 124.4(3) . .
N12 C44 C45 121.0(4) . .
N12 C44 C43 116.1(4) . .
C45 C44 C43 122.6(4) . .
C44 C45 C46 119.0(5) . .
C47 C46 C45 119.4(5) . .
C46 C47 C48 119.7(5) . .
N12 C48 C47 120.9(4) . .
N12 C48 C49 116.3(4) . .
C47 C48 C49 122.7(4) . .
N13 C49 C48 109.9(4) . .
C49 N13 C50 114.1(4) . .
C49 N13 Cu3 104.9(3) . .
C50 N13 Cu3 103.5(3) . .
N13 C50 C51 109.3(4) . .
N14 C51 C50 110.8(4) . .
C52 N14 C51 111.5(4) . .
C52 N14 Cu3 108.3(3) . .
C51 N14 Cu3 104.4(3) . .
N14 C52 C53 108.5(3) . .
C53 N15 C57 121.1(4) . .
C53 N15 Cu3 119.6(3) . .
C57 N15 Cu3 119.2(3) . .
N15 C53 C54 120.6(5) . .
N15 C53 C52 113.6(4) . .
C54 C53 C52 125.8(4) . .
C55 C54 C53 118.5(5) . .
C54 C55 C56 120.4(5) . .
C57 C56 C55 118.1(5) . .
N15 C57 C56 121.2(4) . .
N15 C57 C39 113.5(4) . 2_756
C56 C57 C39 125.3(4) . 2_756
S1 C58 S1 14.1(3) 5_665 .
S1 C59 S1 19.1(2) 5_665 .
S1 O1 S1 28.6(3) . 5_665
S1 S1 O1 85.0(11) 5_665 .
S1 S1 O1 66.4(10) 5_665 5_665
O1 S1 O1 151.4(3) . 5_665
S1 S1 C59 114.9(9) 5_665 5_665
O1 S1 C59 93.6(8) . 5_665
O1 S1 C59 98.3(7) 5_665 5_665
S1 S1 C58 133.6(9) 5_665 5_665
O1 S1 C58 102.8(6) . 5_665
O1 S1 C58 97.3(6) 5_665 5_665
C59 S1 C58 110.3(5) 5_665 5_665
S1 S1 C59 46.0(7) 5_665 .
O1 S1 C59 85.3(8) . .
O1 S1 C59 75.0(8) 5_665 .
C59 S1 C59 160.9(2) 5_665 .
C58 S1 C59 88.5(5) 5_665 .
S1 S1 C58 32.3(7) 5_665 .
O1 S1 C58 78.8(6) . .
O1 S1 C58 76.8(6) 5_665 .
C59 S1 C58 83.4(4) 5_665 .
C58 S1 C58 165.9(3) 5_665 .
C59 S1 C58 77.6(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.923(4) .
Cu1 N8 1.994(4) .
Cu1 N10 2.064(3) .
Cu1 N2 2.144(3) .
Cu1 N9 2.208(4) .
Cu2 N6 1.937(4) .
Cu2 N3 2.004(4) .
Cu2 N5 2.063(4) .
Cu2 N7 2.128(4) .
Cu2 N4 2.212(4) .
Cu3 N15 1.930(4) .
Cu3 N12 2.005(4) .
Cu3 N14 2.079(4) .
Cu3 N13 2.185(4) .
Cu3 N11 2.189(3) 2_756
Na OW1 2.280(4) .
Na O41 2.443(6) .
Na O11 2.451(5) .
Na O31 2.523(5) .
Na O21 2.525(6) .
Na O42 2.565(10) .
Na Cl4 2.979(4) .
Cl1 O13 1.416(4) .
Cl1 O11 1.443(4) .
Cl1 O12 1.446(4) .
Cl1 O14 1.461(4) .
Cl2 O23 1.413(4) .
Cl2 O22 1.427(5) .
Cl2 O21 1.433(5) .
Cl2 O24 1.442(3) .
Cl3 O33 1.423(4) .
Cl3 O31 1.430(4) .
Cl3 O32 1.440(4) .
Cl3 O34 1.449(3) .
Cl4 Cl4 0.874(7) 2_654
Cl4 O43 1.374(7) .
Cl4 O41 1.408(6) 2_654
Cl4 O41 1.515(6) .
Cl4 O42 1.565(12) .
O41 Cl4 1.408(6) 2_654
O43 Cl4 1.374(7) 2_654
Cl5 O53 1.427(4) .
Cl5 O51 1.442(4) .
Cl5 O52 1.450(4) .
Cl5 O54 1.455(4) .
Cl6 O62 1.441(4) .
Cl6 O61 1.446(4) .
Cl6 O64 1.446(4) .
Cl6 O63 1.449(4) .
Cl7 O73 1.439(4) .
Cl7 O74 1.443(4) .
Cl7 O71 1.448(3) .
Cl7 O72 1.457(4) .
N1 C1 1.343(6) .
N1 C5 1.351(6) .
C1 C2 1.389(6) .
C1 C38 1.509(6) .
C2 C3 1.392(8) .
C3 C4 1.401(8) .
C4 C5 1.385(7) .
C5 C6 1.481(7) .
N2 C10 1.353(6) .
N2 C6 1.368(6) .
C6 C7 1.395(6) .
C7 C8 1.375(7) .
C8 C9 1.387(7) .
C9 C10 1.385(6) .
C10 C11 1.502(6) .
N3 C15 1.349(6) .
N3 C11 1.351(6) .
C11 C12 1.385(6) .
C12 C13 1.391(8) .
C13 C14 1.378(8) .
C14 C15 1.382(7) .
C15 C16 1.523(7) .
C16 N4 1.465(7) .
N4 C17 1.489(6) .
C17 C18 1.505(8) .
C18 N5 1.509(6) .
N5 C19 1.477(7) .
C19 C20 1.517(7) .
N6 C20 1.342(6) .
N6 C24 1.344(6) .
C20 C21 1.399(7) .
C21 C22 1.379(8) .
C22 C23 1.394(8) .
C23 C24 1.406(7) .
C24 C25 1.476(7) .
N7 C29 1.361(6) .
N7 C25 1.370(6) .
C25 C26 1.387(7) .
C26 C27 1.380(8) .
C27 C28 1.372(8) .
C28 C29 1.399(7) .
C29 C30 1.484(7) .
N8 C34 1.352(6) .
N8 C30 1.354(6) .
C30 C31 1.398(7) .
C31 C32 1.363(10) .
C32 C33 1.386(10) .
C33 C34 1.381(8) .
C34 C35 1.519(8) .
C35 N9 1.467(6) .
N9 C36 1.498(6) .
C36 C37 1.504(7) .
C37 N10 1.504(5) .
N10 C38 1.485(6) .
N11 C39 1.360(6) .
N11 C43 1.364(5) .
N11 Cu3 2.189(3) 2_756
C39 C40 1.396(6) .
C39 C57 1.478(6) 2_756
C40 C41 1.381(7) .
C41 C42 1.389(7) .
C42 C43 1.395(6) .
C43 C44 1.486(6) .
N12 C48 1.352(6) .
N12 C44 1.364(6) .
C44 C45 1.389(6) .
C45 C46 1.398(7) .
C46 C47 1.375(8) .
C47 C48 1.395(7) .
C48 C49 1.504(7) .
C49 N13 1.465(6) .
N13 C50 1.488(6) .
C50 C51 1.525(7) .
C51 N14 1.493(5) .
N14 C52 1.487(6) .
C52 C53 1.513(7) .
N15 C53 1.338(6) .
N15 C57 1.342(6) .
C53 C54 1.392(7) .
C54 C55 1.380(8) .
C55 C56 1.392(7) .
C56 C57 1.380(6) .
C57 C39 1.478(6) 2_756
C58 S1 1.413(8) 5_665
C58 S1 1.915(8) .
C59 S1 1.416(9) 5_665
C59 S1 1.785(9) .
O1 S1 1.232(11) .
O1 S1 1.339(10) 5_665
S1 S1 0.644(4) 5_665
S1 O1 1.339(10) 5_665
S1 C59 1.416(9) 5_665
S1 C58 1.413(8) 5_665
