#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:09:40 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179315 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/12/4321263.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_4321263
loop_
_publ_author_name
'Catalina Ruiz-Pérez'
'María Hernández-Molina'
'Pablo Lorenzo-Luis'
'Francesc Lloret'
'Juan Cano'
'Miguel Julve'
_publ_section_title
;
 Magnetic Coupling through the Carbon Skeleton of Malonate in Two
 Polymorphs of {[Cu(bpy)(H2O)][Cu(bpy)(mal)(H2O)]}(ClO4)2 (H2mal = Malonic
 Acid; bpy = 2,2'-Bipyridine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3845
_journal_page_last               3852
_journal_paper_doi               10.1021/ic000314n
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C23 H22 Cl2 Cu2 N4 O14'
_chemical_formula_weight         776.1
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 114.580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.743(3)
_cell_length_b                   9.7522(5)
_cell_length_c                   27.731(2)
_cell_measurement_temperature    293(2)
_cell_volume                     5839.2(10)
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            9148
_diffrn_reflns_theta_max         65.05
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    4.171
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_F_000             1552
_refine_diff_density_max         1.072
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.00146(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.359
_refine_ls_goodness_of_fit_obs   1.081
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     812
_refine_ls_number_reflns         9186
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.360
_refine_ls_restrained_S_obs      1.045
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_obs          0.0597
_refine_ls_shift/esd_max         0.211
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.064P)²+4.4143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2113
_refine_ls_wR_factor_obs         0.1591
_reflns_number_observed          7364
_reflns_number_total             9148
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000314n_1.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.064P)^2^+4.4143P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.064P)^2^+4.4143P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5839.1(9)
_cod_database_code               4321263
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -y-1/2, 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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cu2 Cu 0.63961(4) 0.23495(10) 0.98706(3) 0.0321(2) Uani 1 d . .
N21 N 0.5956(2) 0.3278(6) 1.0251(2) 0.0364(13) Uani 1 d . .
N22 N 0.5595(2) 0.1347(6) 0.9544(2) 0.0329(12) Uani 1 d . .
C21 C 0.6199(3) 0.4282(8) 1.0615(3) 0.047(2) Uani 1 d . .
H21 H 0.6600(3) 0.4588(8) 1.0699(3) 0.057 Uiso 1 calc R .
C22 C 0.5852(4) 0.4863(9) 1.0863(3) 0.056(2) Uani 1 d . .
H22 H 0.6023(4) 0.5545(9) 1.1117(3) 0.067 Uiso 1 calc R .
C23 C 0.5268(4) 0.4427(9) 1.0734(3) 0.056(2) Uani 1 d . .
H23 H 0.5033(4) 0.4824(9) 1.0894(3) 0.067 Uiso 1 calc R .
C24 C 0.5019(3) 0.3410(9) 1.0370(3) 0.052(2) Uani 1 d . .
H24 H 0.4623(3) 0.3079(9) 1.0292(3) 0.062 Uiso 1 calc R .
C25 C 0.5375(3) 0.2868(7) 1.0114(3) 0.038(2) Uani 1 d . .
C26 C 0.5162(3) 0.1778(7) 0.9704(3) 0.0363(15) Uani 1 d . .
C27 C 0.4581(3) 0.1200(9) 0.9506(3) 0.052(2) Uani 1 d . .
H27 H 0.4285(3) 0.1498(9) 0.9621(3) 0.063 Uiso 1 calc R .
C28 C 0.4444(4) 0.0141(10) 0.9126(4) 0.060(2) Uani 1 d . .
H28 H 0.4053(4) -0.0259(10) 0.8980(4) 0.072 Uiso 1 calc R .
C29 C 0.4896(3) -0.0283(9) 0.8975(3) 0.054(2) Uani 1 d . .
H29 H 0.4821(3) -0.0979(9) 0.8727(3) 0.065 Uiso 1 calc R .
C20 C 0.5468(3) 0.0352(8) 0.9203(3) 0.045(2) Uani 1 d . .
H20 H 0.5778(3) 0.0050(8) 0.9107(3) 0.054 Uiso 1 calc R .
Cu1 Cu 0.67304(4) -0.04872(9) 0.86923(3) 0.0254(2) Uani 1 d . .
N11 N 0.6354(2) 0.0869(6) 0.8111(2) 0.0314(11) Uani 1 d . .
N12 N 0.5999(2) -0.1583(6) 0.8209(2) 0.0353(13) Uani 1 d . .
C11 C 0.6551(3) 0.2146(8) 0.8105(3) 0.045(2) Uani 1 d . .
H11 H 0.6905(3) 0.2443(8) 0.8391(3) 0.054 Uiso 1 calc R .
C12 C 0.6251(4) 0.3048(9) 0.7694(3) 0.056(2) Uani 1 d . .
H12 H 0.6392(4) 0.3942(9) 0.7704(3) 0.067 Uiso 1 calc R .
C13 C 0.5727(4) 0.2569(10) 0.7262(3) 0.062(2) Uani 1 d . .
H13 H 0.5527(4) 0.3131(10) 0.6969(3) 0.074 Uiso 1 calc R .
C14 C 0.5515(3) 0.1305(9) 0.7269(3) 0.051(2) Uani 1 d . .
H14 H 0.5152(3) 0.1005(9) 0.6993(3) 0.061 Uiso 1 calc R .
C15 C 0.5841(3) 0.0440(8) 0.7693(2) 0.036(2) Uani 1 d . .
C16 C 0.5658(3) -0.0978(8) 0.7741(2) 0.0369(15) Uani 1 d . .
C17 C 0.5187(3) -0.1703(10) 0.7342(3) 0.061(2) Uani 1 d . .
H17 H 0.4953(3) -0.1283(10) 0.7019(3) 0.073 Uiso 1 calc R .
C18 C 0.5069(4) -0.3029(10) 0.7427(4) 0.067(3) Uani 1 d . .
H18 H 0.4763(4) -0.3530(10) 0.7162(4) 0.080 Uiso 1 calc R .
C19 C 0.5415(4) -0.3614(9) 0.7916(4) 0.070(3) Uani 1 d . .
H19 H 0.5330(4) -0.4498(9) 0.7993(4) 0.084 Uiso 1 calc R .
C20 C 0.5882(4) -0.2874(8) 0.8283(3) 0.055(2) Uani 1 d . .
H20 H 0.6132(4) -0.3295(8) 0.8601(3) 0.065 Uiso 1 calc R .
O1W O 0.7369(2) -0.1522(5) 0.8385(2) 0.0435(11) Uani 1 d . .
Cu3 Cu 0.30791(4) 0.48566(9) 0.63125(3) 0.0262(2) Uani 1 d . .
N31 N 0.3273(2) 0.6273(6) 0.6879(2) 0.0311(11) Uani 1 d . .
N32 N 0.2857(2) 0.3801(6) 0.6824(2) 0.0368(13) Uani 1 d . .
C31 C 0.3466(3) 0.7538(7) 0.6866(3) 0.039(2) Uani 1 d . .
H31 H 0.3522(3) 0.7809(7) 0.6567(3) 0.047 Uiso 1 calc R .
C32 C 0.3588(4) 0.8477(9) 0.7266(3) 0.054(2) Uani 1 d . .
H32 H 0.3730(4) 0.9354(9) 0.7247(3) 0.065 Uiso 1 calc R .
C33 C 0.3484(4) 0.8038(9) 0.7707(3) 0.059(2) Uani 1 d . .
H33 H 0.3548(4) 0.8644(9) 0.7984(3) 0.071 Uiso 1 calc R .
C34 C 0.3296(3) 0.6757(9) 0.7730(3) 0.051(2) Uani 1 d . .
H34 H 0.3240(3) 0.6467(9) 0.8027(3) 0.061 Uiso 1 calc R .
C35 C 0.3184(3) 0.5861(7) 0.7312(2) 0.0341(15) Uani 1 d . .
C36 C 0.2964(3) 0.4450(8) 0.7282(2) 0.039(2) Uani 1 d . .
C37 C 0.2872(4) 0.3771(9) 0.7685(3) 0.054(2) Uani 1 d . .
H37 H 0.2935(4) 0.4231(9) 0.7998(3) 0.065 Uiso 1 calc R .
C38 C 0.2693(4) 0.2461(10) 0.7624(3) 0.061(2) Uani 1 d . .
H38 H 0.2639(4) 0.2011(10) 0.7897(3) 0.074 Uiso 1 calc R .
C39 C 0.2584(4) 0.1744(10) 0.7147(3) 0.063(2) Uani 1 d . .
H39 H 0.2461(4) 0.0830(10) 0.7098(3) 0.076 Uiso 1 calc R .
C30 C 0.2673(4) 0.2497(8) 0.6762(3) 0.053(2) Uani 1 d . .
H30 H 0.2601(4) 0.2069(8) 0.6441(3) 0.064 Uiso 1 calc R .
O3W O 0.4023(2) 0.3874(5) 0.6590(2) 0.0471(12) Uani 1 d . .
Cu4 Cu 0.34478(4) 0.26364(10) 0.48263(3) 0.0315(2) Uani 1 d . .
N41 N 0.4278(2) 0.3458(6) 0.5221(2) 0.0322(12) Uani 1 d . .
N42 N 0.3901(2) 0.1588(6) 0.4483(2) 0.0374(13) Uani 1 d . .
C41 C 0.4414(3) 0.4420(8) 0.5592(3) 0.045(2) Uani 1 d . .
H41 H 0.4098(3) 0.4798(8) 0.5664(3) 0.054 Uiso 1 calc R .
C42 C 0.5015(3) 0.4872(9) 0.5875(3) 0.051(2) Uani 1 d . .
H42 H 0.5102(3) 0.5531(9) 0.6138(3) 0.062 Uiso 1 calc R .
C43 C 0.5481(3) 0.4340(10) 0.5762(3) 0.059(2) Uani 1 d . .
H43 H 0.5886(3) 0.4642(10) 0.5948(3) 0.071 Uiso 1 calc R .
C44 C 0.5346(3) 0.3346(9) 0.5368(3) 0.054(2) Uani 1 d . .
H44 H 0.5657(3) 0.2979(9) 0.5286(3) 0.065 Uiso 1 calc R .
C45 C 0.4731(3) 0.2913(8) 0.5099(3) 0.038(2) Uani 1 d . .
C46 C 0.4509(3) 0.1869(8) 0.4680(3) 0.039(2) Uani 1 d . .
C47 C 0.4892(4) 0.1176(10) 0.4482(3) 0.063(2) Uani 1 d . .
H47 H 0.5312(4) 0.1385(10) 0.4611(3) 0.076 Uiso 1 calc R .
C48 C 0.4639(4) 0.0192(10) 0.4098(4) 0.066(2) Uani 1 d . .
H48 H 0.4886(4) -0.0276(10) 0.3965(4) 0.079 Uiso 1 calc R .
C49 C 0.4012(4) -0.0097(10) 0.3909(3) 0.063(2) Uani 1 d . .
H49 H 0.3829(4) -0.0762(10) 0.3651(3) 0.075 Uiso 1 calc R .
C40 C 0.3666(4) 0.0634(9) 0.4118(3) 0.055(2) Uani 1 d . .
H40 H 0.3246(4) 0.0441(9) 0.3995(3) 0.066 Uiso 1 calc R .
Cl1A Cl 0.3774 0.0214 0.5924 0.042 Uani 1 d D .
O1A O 0.4167 0.1314 0.6188 0.113 Uani 1 d D .
O2A O 0.4081 -0.1048 0.6098 0.062 Uani 1 d D .
O3A O 0.3664 0.0347 0.5380 0.112 Uani 1 d D .
O4A O 0.3206 0.0264 0.5950 0.148 Uani 1 d D .
Cl1B Cl 0.4600 0.2690 0.8034 0.046 Uani 1 d D .
O1B O 0.5257 0.2613 0.8294 0.089 Uani 1 d D .
O2B O 0.4370 0.2856 0.8417 0.107 Uani 1 d D .
O3B O 0.4431 0.3845 0.7687 0.093 Uani 1 d D .
O4B O 0.4383 0.1517 0.7740 0.116 Uani 1 d D .
Cl1C Cl 0.7189 -0.0099 1.0959 0.045 Uani 1 d D .
O1C O 0.7796 0.0016 1.1016 0.125 Uani 1 d D .
O2C O 0.7030 0.1012 1.1220 0.102 Uani 1 d D .
O3C O 0.7054 -0.1370 1.1126 0.074 Uani 1 d D .
O4C O 0.6775 -0.0042 1.0414 0.106 Uani 1 d D .
Cl1D Cl 0.6623 -0.3018 0.7038 0.058 Uani 1 d D .
O1D O 0.6018 -0.3240 0.6707 0.178 Uani 1 d D .
O2D O 0.6988 -0.3137 0.6745 0.102 Uani 1 d D .
O3D O 0.6689 -0.1684 0.7240 0.086 Uani 1 d D .
O4D O 0.6874 -0.3905 0.7475 0.138 Uani 1 d D .
O3 O 0.7175 0.3177 1.0305 0.044 Uani 1 d . .
O2 O 0.6719 0.1430 0.9431 0.036 Uani 1 d . .
O1 O 0.7404 0.0725 0.9149 0.027 Uani 1 d . .
O4 O 0.8192 0.3292 1.0715 0.031 Uani 1 d . .
C3 C 0.7705 0.2855 1.0346 0.026 Uani 1 d . .
C2 C 0.7812 0.1935 0.9953 0.031 Uani 1 d . .
H21 H 0.8061 0.2447 0.9813 0.037 Uiso 1 calc R .
H22 H 0.8063 0.1170 1.0151 0.037 Uiso 1 calc R .
C1 C 0.7274 0.1344 0.9486 0.024 Uani 1 d . .
O8 O 0.1729 0.1038 0.4172 0.028 Uani 1 d . .
O5 O 0.2555 0.3604 0.5741 0.032 Uani 1 d . .
O6 O 0.3128 0.3472 0.5287 0.042 Uani 1 d . .
O7 O 0.2681 0.1742 0.4412 0.035 Uani 1 d . .
C6 C 0.2195 0.1671 0.4491 0.023 Uani 1 d . .
C5 C 0.2145 0.2267 0.4975 0.028 Uani 1 d . .
H51 H 0.1764 0.2792 0.4852 0.034 Uiso 1 calc R .
H52 H 0.2098 0.1506 0.5180 0.034 Uiso 1 calc R .
C4 C 0.2654 0.3168 0.5349 0.027 Uani 1 d . .
O2W O 0.6095 0.4193 0.9169 0.053 Uani 1 d . .
O4W O 0.3062 0.4521 0.4159 0.051 Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
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
O2 Cu2 O3 93.45(4) . . ?
O2 Cu2 N22 92.3(2) . . ?
O3 Cu2 N22 169.4(2) . . ?
O2 Cu2 N21 172.7(2) . . ?
O3 Cu2 N21 93.3(2) . . ?
N22 Cu2 N21 81.4(2) . . ?
C25 N21 C21 120.1(6) . . ?
C25 N21 Cu2 115.0(5) . . ?
C21 N21 Cu2 124.8(4) . . ?
C20 N22 C26 119.7(6) . . ?
C20 N22 Cu2 125.9(5) . . ?
C26 N22 Cu2 114.4(5) . . ?
N21 C21 C22 120.4(7) . . ?
N21 C21 H21 119.8(4) . . ?
C22 C21 H21 119.8(5) . . ?
C23 C22 C21 119.6(8) . . ?
C23 C22 H22 120.2(5) . . ?
C21 C22 H22 120.2(5) . . ?
C22 C23 C24 120.5(7) . . ?
C22 C23 H23 119.7(5) . . ?
C24 C23 H23 119.7(4) . . ?
C23 C24 C25 118.6(7) . . ?
C23 C24 H24 120.7(4) . . ?
C25 C24 H24 120.7(4) . . ?
N21 C25 C24 120.6(7) . . ?
N21 C25 C26 114.6(6) . . ?
C24 C25 C26 124.7(6) . . ?
N22 C26 C27 121.2(7) . . ?
N22 C26 C25 114.5(5) . . ?
C27 C26 C25 124.3(6) . . ?
C26 C27 C28 118.6(7) . . ?
C26 C27 H27 120.7(5) . . ?
C28 C27 H27 120.7(4) . . ?
C29 C28 C27 118.8(7) . . ?
C29 C28 H28 120.6(5) . . ?
C27 C28 H28 120.6(4) . . ?
C20 C29 C28 118.2(8) . . ?
C20 C29 H29 120.9(5) . . ?
C28 C29 H29 120.9(5) . . ?
N22 C20 C29 123.5(7) . . ?
N22 C20 H20 118.2(4) . . ?
C29 C20 H20 118.2(5) . . ?
O1 Cu1 O4 93.29(3) . 2_647 ?
O1 Cu1 N11 95.3(2) . . ?
O4 Cu1 N11 158.64(15) 2_647 . ?
O1 Cu1 N12 175.2(2) . . ?
O4 Cu1 N12 89.4(2) 2_647 . ?
N11 Cu1 N12 80.8(2) . . ?
O1 Cu1 O1W 90.97(12) . . ?
O4 Cu1 O1W 101.51(13) 2_647 . ?
N11 Cu1 O1W 97.8(2) . . ?
N12 Cu1 O1W 92.4(2) . . ?
C11 N11 C15 118.3(6) . . ?
C11 N11 Cu1 126.2(4) . . ?
C15 N11 Cu1 115.4(4) . . ?
C20 N12 C16 119.0(6) . . ?
C20 N12 Cu1 125.7(5) . . ?
C16 N12 Cu1 114.6(5) . . ?
N11 C11 C12 122.9(7) . . ?
N11 C11 H11 118.5(4) . . ?
C12 C11 H11 118.5(5) . . ?
C13 C12 C11 117.6(8) . . ?
C13 C12 H12 121.2(5) . . ?
C11 C12 H12 121.2(5) . . ?
C14 C13 C12 120.1(7) . . ?
C14 C13 H13 120.0(5) . . ?
C12 C13 H13 120.0(5) . . ?
C13 C14 C15 119.5(7) . . ?
C13 C14 H14 120.3(5) . . ?
C15 C14 H14 120.3(5) . . ?
N11 C15 C14 121.5(7) . . ?
N11 C15 C16 114.1(5) . . ?
C14 C15 C16 124.4(6) . . ?
N12 C16 C17 120.3(7) . . ?
N12 C16 C15 114.6(5) . . ?
C17 C16 C15 125.1(6) . . ?
C18 C17 C16 119.8(7) . . ?
C18 C17 H17 120.1(5) . . ?
C16 C17 H17 120.1(5) . . ?
C17 C18 C19 118.7(7) . . ?
C17 C18 H18 120.6(5) . . ?
C19 C18 H18 120.6(5) . . ?
C20 C19 C18 118.7(8) . . ?
C20 C19 H19 120.6(5) . . ?
C18 C19 H19 120.6(5) . . ?
N12 C20 C19 123.3(8) . . ?
N12 C20 H20 118.4(4) . . ?
C19 C20 H20 118.4(5) . . ?
O8 Cu3 O5 93.53(3) 2_556 . ?
O8 Cu3 N31 95.14(15) 2_556 . ?
O5 Cu3 N31 156.96(14) . . ?
O8 Cu3 N32 175.1(2) 2_556 . ?
O5 Cu3 N32 89.2(2) . . ?
N31 Cu3 N32 80.8(2) . . ?
O8 Cu3 O3W 90.10(13) 2_556 . ?
O5 Cu3 O3W 102.42(14) . . ?
N31 Cu3 O3W 98.9(2) . . ?
N32 Cu3 O3W 93.3(2) . . ?
C31 N31 C35 118.8(6) . . ?
C31 N31 Cu3 126.4(4) . . ?
C35 N31 Cu3 114.8(4) . . ?
C30 N32 C36 119.6(6) . . ?
C30 N32 Cu3 124.8(5) . . ?
C36 N32 Cu3 115.3(5) . . ?
N31 C31 C32 124.0(7) . . ?
N31 C31 H31 118.0(4) . . ?
C32 C31 H31 118.0(5) . . ?
C33 C32 C31 116.4(8) . . ?
C33 C32 H32 121.8(5) . . ?
C31 C32 H32 121.8(5) . . ?
C34 C33 C32 120.4(7) . . ?
C34 C33 H33 119.8(4) . . ?
C32 C33 H33 119.8(5) . . ?
C33 C34 C35 120.1(7) . . ?
C33 C34 H34 120.0(4) . . ?
C35 C34 H34 120.0(4) . . ?
N31 C35 C34 120.3(7) . . ?
N31 C35 C36 114.2(5) . . ?
C34 C35 C36 125.5(6) . . ?
N32 C36 C37 120.2(7) . . ?
N32 C36 C35 114.8(5) . . ?
C37 C36 C35 125.0(6) . . ?
C38 C37 C36 120.0(7) . . ?
C38 C37 H37 120.0(5) . . ?
C36 C37 H37 120.0(5) . . ?
C37 C38 C39 121.0(7) . . ?
C37 C38 H38 119.5(4) . . ?
C39 C38 H38 119.5(5) . . ?
C30 C39 C38 115.5(8) . . ?
C30 C39 H39 122.3(5) . . ?
C38 C39 H39 122.3(5) . . ?
N32 C30 C39 123.6(8) . . ?
N32 C30 H30 118.2(4) . . ?
C39 C30 H30 118.2(5) . . ?
O7 Cu4 O6 93.03(4) . . ?
O7 Cu4 N41 174.7(2) . . ?
O6 Cu4 N41 92.21(15) . . ?
O7 Cu4 N42 92.7(2) . . ?
O6 Cu4 N42 168.3(2) . . ?
N41 Cu4 N42 82.0(2) . . ?
C41 N41 C45 120.3(6) . . ?
C41 N41 Cu4 125.4(4) . . ?
C45 N41 Cu4 114.3(4) . . ?
C40 N42 C46 119.8(6) . . ?
C40 N42 Cu4 126.3(5) . . ?
C46 N42 Cu4 113.8(5) . . ?
N41 C41 C42 121.7(7) . . ?
N41 C41 H41 119.0(4) . . ?
C42 C41 H41 119.4(5) . . ?
C43 C42 C41 119.4(8) . . ?
C43 C42 H42 120.3(5) . . ?
C41 C42 H42 120.4(5) . . ?
C42 C43 C44 119.8(7) . . ?
C42 C43 H43 120.6(5) . . ?
C44 C43 H43 119.6(4) . . ?
C43 C44 C45 118.5(7) . . ?
C43 C44 H44 121.0(4) . . ?
C45 C44 H44 120.6(5) . . ?
N41 C45 C44 120.4(7) . . ?
N41 C45 C46 113.9(6) . . ?
C44 C45 C46 125.7(6) . . ?
N42 C46 C47 120.1(7) . . ?
N42 C46 C45 115.8(6) . . ?
C47 C46 C45 124.1(6) . . ?
C48 C47 C46 119.4(7) . . ?
C48 C47 H47 120.1(5) . . ?
C46 C47 H47 120.6(5) . . ?
C49 C48 C47 119.2(7) . . ?
C49 C48 H48 120.2(5) . . ?
C47 C48 H48 120.5(5) . . ?
C48 C49 C40 117.9(8) . . ?
C48 C49 H49 120.8(5) . . ?
C40 C49 H49 121.3(5) . . ?
N42 C40 C49 123.5(7) . . ?
N42 C40 H40 118.5(4) . . ?
C49 C40 H40 118.0(5) . . ?
O4A Cl1A O2A 113.0 . . ?
O4A Cl1A O1A 113.3 . . ?
O2A Cl1A O1A 110.5 . . ?
O4A Cl1A O3A 107.4 . . ?
O2A Cl1A O3A 106.4 . . ?
O1A Cl1A O3A 105.6 . . ?
O4B Cl1B O2B 112.4 . . ?
O4B Cl1B O1B 108.6 . . ?
O2B Cl1B O1B 108.4 . . ?
O4B Cl1B O3B 109.0 . . ?
O2B Cl1B O3B 109.5 . . ?
O1B Cl1B O3B 108.9 . . ?
O1C Cl1C O3C 113.7 . . ?
O1C Cl1C O4C 110.3 . . ?
O3C Cl1C O4C 103.5 . . ?
O1C Cl1C O2C 111.1 . . ?
O3C Cl1C O2C 110.7 . . ?
O4C Cl1C O2C 107.2 . . ?
O1D Cl1D O3D 109.2 . . ?
O1D Cl1D O4D 115.7 . . ?
O3D Cl1D O4D 106.9 . . ?
O1D Cl1D O2D 109.0 . . ?
O3D Cl1D O2D 108.2 . . ?
O4D Cl1D O2D 107.6 . . ?
C3 O3 Cu2 128.41(3) . . ?
C1 O2 Cu2 128.86(3) . . ?
C1 O1 Cu1 112.45(2) . . ?
C3 O4 Cu1 128.12(2) . 2_657 ?
O3 C3 O4 122.5 . . ?
O3 C3 C2 123.0 . . ?
O4 C3 C2 114.5 . . ?
C1 C2 C3 120.6 . . ?
C1 C2 H21 107.2 . . ?
C3 C2 H21 107.2 . . ?
C1 C2 H22 107.2 . . ?
C3 C2 H22 107.2 . . ?
H21 C2 H22 106.8 . . ?
O1 C1 O2 120.6 . . ?
O1 C1 C2 116.1 . . ?
O2 C1 C2 123.3 . . ?
C6 O8 Cu3 112.52(3) . 2_546 ?
C4 O5 Cu3 127.70(2) . . ?
C4 O6 Cu4 128.46(3) . . ?
C6 O7 Cu4 129.05(3) . . ?
O8 C6 O7 120.4 . . ?
O8 C6 C5 116.3 . . ?
O7 C6 C5 123.3 . . ?
C4 C5 C6 120.0 . . ?
C4 C5 H51 107.3 . . ?
C6 C5 H51 107.3 . . ?
C4 C5 H52 107.3 . . ?
C6 C5 H52 107.3 . . ?
H51 C5 H52 106.9 . . ?
O6 C4 O5 122.3 . . ?
O6 C4 C5 123.9 . . ?
O5 C4 C5 113.8 . . ?
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
Cu2 O2 1.912(5) . ?
Cu2 O3 1.914(4) . ?
Cu2 N22 1.991(5) . ?
Cu2 N21 1.987(6) . ?
N21 C25 1.331(8) . ?
N21 C21 1.350(9) . ?
N22 C20 1.300(9) . ?
N22 C26 1.343(8) . ?
C21 C22 1.397(10) . ?
C21 H21 0.93 . ?
C22 C23 1.349(12) . ?
C22 H22 0.93 . ?
C23 C24 1.362(12) . ?
C23 H23 0.93 . ?
C24 C25 1.413(9) . ?
C24 H24 0.93 . ?
C25 C26 1.483(10) . ?
C26 C27 1.376(9) . ?
C27 C28 1.414(12) . ?
C27 H27 0.93 . ?
C28 C29 1.367(12) . ?
C28 H28 0.93 . ?
C29 C20 1.383(10) . ?
C29 H29 0.93 . ?
C20 H20 0.93 . ?
Cu1 O1 1.968(3) . ?
Cu1 O4 1.974(4) 2_647 ?
Cu1 N11 1.987(5) . ?
Cu1 N12 2.008(5) . ?
Cu1 O1W 2.257(5) . ?
N11 C11 1.333(9) . ?
N11 C15 1.352(8) . ?
N12 C20 1.323(9) . ?
N12 C16 1.347(8) . ?
C11 C12 1.380(10) . ?
C11 H11 0.93 . ?
C12 C13 1.402(12) . ?
C12 H12 0.93 . ?
C13 C14 1.335(12) . ?
C13 H13 0.93 . ?
C14 C15 1.392(9) . ?
C14 H14 0.93 . ?
C15 C16 1.471(10) . ?
C16 C17 1.395(9) . ?
C17 C18 1.365(13) . ?
C17 H17 0.93 . ?
C18 C19 1.383(13) . ?
C18 H18 0.93 . ?
C19 C20 1.359(10) . ?
C19 H19 0.93 . ?
C20 H20 0.93 . ?
Cu3 O8 1.963(4) 2_556 ?
Cu3 O5 1.978(4) . ?
Cu3 N31 1.997(5) . ?
Cu3 N32 1.998(6) . ?
Cu3 O3W 2.260(5) . ?
N31 C31 1.322(9) . ?
N31 C35 1.363(7) . ?
N32 C30 1.332(9) . ?
N32 C36 1.345(8) . ?
C31 C32 1.373(10) . ?
C31 H31 0.93 . ?
C32 C33 1.412(12) . ?
C32 H32 0.93 . ?
C33 C34 1.337(12) . ?
C33 H33 0.93 . ?
C34 C35 1.387(9) . ?
C34 H34 0.93 . ?
C35 C36 1.462(10) . ?
C36 C37 1.394(9) . ?
C37 C38 1.334(12) . ?
C37 H37 0.93 . ?
C38 C39 1.420(12) . ?
C38 H38 0.93 . ?
C39 C30 1.384(10) . ?
C39 H39 0.93 . ?
C30 H30 0.93 . ?
Cu4 O7 1.911(4) . ?
Cu4 O6 1.919(5) . ?
Cu4 N41 1.983(4) . ?
Cu4 N42 1.987(6) . ?
N41 C41 1.329(9) . ?
N41 C45 1.363(8) . ?
N42 C40 1.314(9) . ?
N42 C46 1.342(8) . ?
C41 C42 1.383(10) . ?
C41 H41 0.93 . ?
C42 C43 1.370(12) . ?
C42 H42 0.93 . ?
C43 C44 1.394(12) . ?
C43 H43 0.93 . ?
C44 C45 1.399(9) . ?
C44 H44 0.93 . ?
C45 C46 1.469(10) . ?
C46 C47 1.415(10) . ?
C47 C48 1.373(12) . ?
C47 H47 0.93 . ?
C48 C49 1.387(12) . ?
C48 H48 0.93 . ?
C49 C40 1.382(10) . ?
C49 H49 0.93 . ?
C40 H40 0.93 . ?
Cl1A O4A 1.38 . ?
Cl1A O2A 1.41 . ?
Cl1A O1A 1.41 . ?
Cl1A O3A 1.43 . ?
Cl1B O4B 1.37 . ?
Cl1B O2B 1.39 . ?
Cl1B O1B 1.42 . ?
Cl1B O3B 1.43 . ?
Cl1C O1C 1.39 . ?
Cl1C O3C 1.41 . ?
Cl1C O4C 1.42 . ?
Cl1C O2C 1.44 . ?
Cl1D O1D 1.36 . ?
Cl1D O3D 1.40 . ?
Cl1D O4D 1.40 . ?
Cl1D O2D 1.42 . ?
O3 C3 1.26 . ?
O2 C1 1.26 . ?
O1 C1 1.26 . ?
O4 C3 1.26 . ?
O4 Cu1 1.9746(8) 2_657 ?
C3 C2 1.51 . ?
C2 C1 1.50 . ?
C2 H21 0.97 . ?
C2 H22 0.97 . ?
O8 C6 1.26 . ?
O8 Cu3 1.9631(8) 2_546 ?
O5 C4 1.28 . ?
O6 C4 1.24 . ?
O7 C6 1.26 . ?
C6 C5 1.51 . ?
C5 C4 1.50 . ?
C5 H51 0.97 . ?
C5 H52 0.97 . ?
