#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/66/2206630.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_2206630
loop_
_publ_author_name
'Reinoso, Santiago'
'Vitoria, Pablo'
'San Felices, Leire'
'Lezama, Luis'
'Gutiérrez-Zorrilla, Juan M.'
_publ_section_title
;μ-Oxalato-κ⁴O¹,O²:O^1'^,O^2'^-bis[aqua(2,2'-bipyridyl-κ²N,N')copper(II)]
 bis(hydrogen squarate)
;
_journal_coeditor_code           BT6702
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1677
_journal_page_last               m1679
_journal_paper_doi               10.1107/S1600536805024165
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'[Cu2 (C2 O4) (C10 H8 N2)2 (H2 O)2] (C4 H O4)2'
_chemical_formula_moiety         'C22 H20 Cu2 N4 O6 2+, 2C4 H O4 -'
_chemical_formula_sum            'C30 H22 Cu2 N4 O14'
_chemical_formula_weight         789.62
_chemical_name_systematic
;
μ-Oxalato-κ⁴O¹,O²:O^1'^,O^2'^-bis[aqua(2,2'-bipyridyl-
κ²N,N')copper(II)] bis(hydrogen squarate)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                92.049(10)
_cell_angle_beta                 94.860(11)
_cell_angle_gamma                109.283(12)
_cell_formula_units_Z            2
_cell_length_a                   8.0147(12)
_cell_length_b                   9.2276(12)
_cell_length_c                   21.728(2)
_cell_measurement_reflns_used    6000
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3.5
_cell_volume                     1507.8(4)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2003)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2003)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF99.2 (Beurskens et al., 1999)'
_diffrn_detector_area_resol_mean '1024 \\times 1024 with blocks 2 \\times 2'
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14798
_diffrn_reflns_theta_full        30
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.84306
_exptl_absorpt_correction_T_min  0.71925
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.138
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.764
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     469
_refine_ls_number_reflns         8613
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.764
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.028P)²] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.074
_refine_ls_wR_factor_ref         0.0808
_reflns_number_gt                3850
_reflns_number_total             8613
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6702.cif
_cod_data_source_block           I
_cod_original_cell_volume        1507.9(4)
_cod_database_code               2206630
_cod_database_fobs_code          2206630
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
C29 0.5897(5) 0.3157(4) -0.02162(14) 0.0549(9) Uani d . 1 C
H29 0.5969 0.2849 -0.0622 0.066 Uiso calc R 1 H
C28 0.7120(4) 0.4495(4) 0.00618(14) 0.0475(8) Uani d . 1 C
H28 0.8025 0.5098 -0.0154 0.057 Uiso calc R 1 H
C26 0.8202(4) 0.6312(3) 0.10226(13) 0.0345(7) Uani d . 1 C
C5 0.0670(4) 0.3497(4) 0.54139(13) 0.0409(8) Uani d . 1 C
H5 -0.0186 0.2845 0.5634 0.049 Uiso calc R 1 H
C4 0.1848(4) 0.4848(4) 0.56987(14) 0.0448(8) Uani d . 1 C
H4 0.18 0.511 0.6112 0.054 Uiso calc R 1 H
C33 0.3812(4) 0.0445(3) 0.36858(13) 0.0354(7) Uani d . 1 C
C40 0.9414(4) 0.2927(3) 0.12524(14) 0.0383(7) Uani d . 1 C
C23 1.0332(4) 0.8774(4) 0.17753(17) 0.0592(10) Uani d . 1 C
H23 1.1056 0.9599 0.2039 0.071 Uiso calc R 1 H
C24 1.0614(4) 0.8649(4) 0.11632(17) 0.0603(10) Uani d . 1 C
H24 1.1529 0.9407 0.1006 0.072 Uiso calc R 1 H
C25 0.9564(4) 0.7425(4) 0.07861(15) 0.0530(9) Uani d . 1 C
H25 0.9761 0.7339 0.0373 0.064 Uiso calc R 1 H
C11 -0.0940(4) 0.0297(3) 0.35031(14) 0.0414(7) Uani d . 1 C
H11 -0.0678 0.0208 0.3097 0.05 Uiso calc R 1 H
C31 0.4503(4) 0.2772(3) 0.06985(13) 0.0453(8) Uani d . 1 C
H31 0.3592 0.2186 0.0916 0.054 Uiso calc R 1 H
C6 0.0764(3) 0.3112(3) 0.47965(12) 0.0311(7) Uani d . 1 C
C37 0.8206(4) 0.2322(3) 0.17338(13) 0.0342(7) Uani d . 1 C
C10 -0.2258(4) -0.0891(3) 0.37155(16) 0.0493(8) Uani d . 1 C
H10 -0.2872 -0.1772 0.3462 0.059 Uiso calc R 1 H
C36 0.5005(4) 0.0884(3) 0.32163(12) 0.0316(7) Uani d . 1 C
C7 -0.0384(3) 0.1688(3) 0.44412(12) 0.0321(7) Uani d . 1 C
C14 0.3445(4) 0.3206(3) 0.25724(12) 0.0283(6) Uani d . 1 C
C39 0.8500(4) 0.1442(4) 0.08631(15) 0.0468(8) Uani d . 1 C
C34 0.2992(4) -0.1092(3) 0.33369(13) 0.0385(7) Uani d . 1 C
C35 0.4280(4) -0.0541(3) 0.28675(13) 0.0349(7) Uani d . 1 C
C38 0.7390(4) 0.0933(3) 0.13617(13) 0.0422(8) Uani d . 1 C
C30 0.4582(5) 0.2287(4) 0.01062(14) 0.0540(9) Uani d . 1 C
H30 0.3752 0.1378 -0.0075 0.065 Uiso calc R 1 H
C8 -0.1715(4) 0.0559(4) 0.46737(15) 0.0444(8) Uani d . 1 C
H8 -0.1984 0.0679 0.5076 0.053 Uiso calc R 1 H
C22 0.8944(4) 0.7641(3) 0.19846(14) 0.0488(8) Uani d . 1 C
H22 0.8728 0.7719 0.2396 0.059 Uiso calc R 1 H
C13 0.4691(4) 0.4637(3) 0.29661(12) 0.0280(6) Uani d . 1 C
Cu1 0.19785(4) 0.33052(4) 0.362303(15) 0.03439(11) Uani d . 1 Cu
Cu2 0.57777(5) 0.48169(4) 0.183733(15) 0.03888(12) Uani d . 1 Cu
N32 0.5689(3) 0.4062(2) 0.09794(10) 0.0334(6) Uani d . 1 N
N21 0.7892(3) 0.6429(3) 0.16202(10) 0.0353(6) Uani d . 1 N
N12 -0.0019(3) 0.1571(2) 0.38534(10) 0.0310(5) Uani d . 1 N
N1 0.2001(3) 0.4058(3) 0.44787(10) 0.0307(5) Uani d . 1 N
O4 0.3831(2) 0.2986(2) 0.20403(8) 0.0371(5) Uani d . 1 O
O3 0.6024(2) 0.5465(2) 0.27259(8) 0.0370(5) Uani d . 1 O
O1 0.4287(2) 0.4853(2) 0.34947(8) 0.0347(5) Uani d . 1 O
O36 0.6260(3) 0.2179(2) 0.31685(9) 0.0405(5) Uani d . 1 O
O35 0.4564(3) -0.1119(2) 0.23731(9) 0.0486(6) Uani d . 1 O
O2 0.2147(2) 0.2350(2) 0.28185(8) 0.0338(5) Uani d . 1 O
O34 0.1749(3) -0.2251(2) 0.34014(10) 0.0651(7) Uani d . 1 O
O37 0.7976(3) 0.2882(2) 0.22423(9) 0.0497(6) Uani d . 1 O
O38 0.6095(3) -0.0340(3) 0.13978(10) 0.0721(9) Uani d . 1 O
O39 0.8640(3) 0.0934(3) 0.03546(11) 0.0786(8) Uani d . 1 O
O33 0.3555(3) 0.1049(2) 0.41626(9) 0.0514(6) Uani d . 1 O
O40 1.0599(3) 0.4112(2) 0.11841(10) 0.0544(6) Uani d . 1 O
O51 0.3770(3) 0.6075(3) 0.17219(13) 0.0548(6) Uani d D 1 O
O50 0.0523(3) 0.4664(2) 0.31318(11) 0.0549(6) Uani d D 1 O
C27 0.6983(4) 0.4927(3) 0.06667(12) 0.0338(7) Uani d . 1 C
C2 0.3118(4) 0.5365(3) 0.47539(13) 0.0389(7) Uani d . 1 C
H2 0.3951 0.6012 0.4525 0.047 Uiso calc R 1 H
C3 0.3094(4) 0.5804(4) 0.53658(13) 0.0451(8) Uani d . 1 C
H3 0.3902 0.6723 0.5548 0.054 Uiso calc R 1 H
C9 -0.2642(4) -0.0740(4) 0.43114(17) 0.0538(9) Uani d . 1 C
H9 -0.3534 -0.1522 0.4468 0.065 Uiso calc R 1 H
H36 0.674(5) 0.223(4) 0.2865(15) 0.081 Uiso d . 1 H
H38 0.564(5) -0.043(4) 0.1711(16) 0.081 Uiso d . 1 H
H51A 0.374(5) 0.676(3) 0.1883(16) 0.081 Uiso d D 1 H
H51B 0.286(3) 0.561(4) 0.1635(17) 0.081 Uiso d D 1 H
H50A 0.095(5) 0.548(2) 0.3122(18) 0.081 Uiso d D 1 H
H50B -0.004(4) 0.434(4) 0.2851(11) 0.081 Uiso d D 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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_publ_flag
N1 Cu1 N12 82.36(9) y
N1 Cu1 O2 171.31(8) y
N1 Cu1 O50 99.90(9) y
N12 Cu1 O1 168.28(8) y
N12 Cu1 O50 100.62(9) y
O1 Cu1 O2 85.40(7) y
O1 Cu1 O50 91.04(9) y
O2 Cu1 O50 88.79(9) y
N21 Cu2 N32 82.50(9) y
N21 Cu2 O4 171.87(9) y
N21 Cu2 O51 99.52(9) y
N32 Cu2 O3 174.38(9) y
N32 Cu2 O51 99.76(9) y
O3 Cu2 O4 85.50(7) y
O3 Cu2 O51 85.84(9) y
O4 Cu2 O51 88.33(8) y
C30 C29 C28 119.7(3) ?
C30 C29 H29 120.1 ?
C28 C29 H29 120.1 ?
C29 C28 C27 119.0(3) ?
C29 C28 H28 120.5 ?
C27 C28 H28 120.5 ?
N21 C26 C25 121.0(3) ?
N21 C26 C27 114.3(2) ?
C25 C26 C27 124.7(3) ?
C4 C5 C6 119.8(3) ?
C4 C5 H5 120.1 ?
C6 C5 H5 120.1 ?
C3 C4 C5 119.4(3) ?
C3 C4 H4 120.3 ?
C5 C4 H4 120.3 ?
O33 C33 C36 136.5(3) ?
O33 C33 C34 135.4(3) ?
C36 C33 C34 88.1(2) ?
O40 C40 C37 136.4(3) ?
O40 C40 C39 134.8(3) ?
C37 C40 C39 88.8(2) ?
C22 C23 C24 117.8(3) ?
C22 C23 H23 121.1 ?
C24 C23 H23 121.1 ?
C25 C24 C23 120.5(3) ?
C25 C24 H24 119.8 ?
C23 C24 H24 119.8 ?
C24 C25 C26 119.3(3) ?
C24 C25 H25 120.4 ?
C26 C25 H25 120.4 ?
N12 C11 C10 122.8(3) ?
N12 C11 H11 118.6 ?
C10 C11 H11 118.6 ?
N32 C31 C30 122.4(3) ?
N32 C31 H31 118.8 ?
C30 C31 H31 118.8 ?
N1 C6 C5 120.0(3) ?
N1 C6 C7 114.7(2) ?
C5 C6 C7 125.3(3) ?
O37 C37 C38 136.3(3) ?
O37 C37 C40 133.7(3) ?
C38 C37 C40 89.9(2) ?
C11 C10 C9 118.1(3) ?
C11 C10 H10 121 ?
C9 C10 H10 121 ?
O36 C36 C35 136.3(3) ?
O36 C36 C33 129.4(3) ?
C35 C36 C33 94.3(2) ?
N12 C7 C8 121.3(3) ?
N12 C7 C6 114.1(2) ?
C8 C7 C6 124.5(3) ?
O4 C14 O2 125.7(3) ?
O4 C14 C13 117.2(2) ?
O2 C14 C13 117.1(2) ?
O39 C39 C38 137.1(3) ?
O39 C39 C40 135.4(3) ?
C38 C39 C40 87.5(2) ?
O34 C34 C35 136.6(3) ?
O34 C34 C33 134.9(3) ?
C35 C34 C33 88.5(2) ?
O35 C35 C36 136.2(3) ?
O35 C35 C34 134.7(3) ?
C36 C35 C34 89.1(2) ?
O38 C38 C37 136.5(3) ?
O38 C38 C39 129.7(3) ?
C37 C38 C39 93.7(2) ?
C31 C30 C29 118.8(3) ?
C31 C30 H30 120.6 ?
C29 C30 H30 120.6 ?
C9 C8 C7 119.5(3) ?
C9 C8 H8 120.2 ?
C7 C8 H8 120.2 ?
N21 C22 C23 122.7(3) ?
N21 C22 H22 118.7 ?
C23 C22 H22 118.7 ?
O1 C13 O3 126.3(3) ?
O1 C13 C14 116.7(2) ?
O3 C13 C14 117.0(2) ?
O2 Cu1 N12 95.98(8) ?
N1 Cu1 O1 94.52(8) ?
N21 Cu2 O3 97.13(8) ?
N32 Cu2 O4 94.12(8) ?
C27 N32 C31 119.3(2) ?
C27 N32 Cu2 114.65(18) ?
C31 N32 Cu2 126.04(19) ?
C22 N21 C26 118.8(2) ?
C22 N21 Cu2 127.02(19) ?
C26 N21 Cu2 114.01(19) ?
C11 N12 C7 118.5(2) ?
C11 N12 Cu1 126.94(19) ?
C7 N12 Cu1 114.46(18) ?
C2 N1 C6 119.9(2) ?
C2 N1 Cu1 125.74(19) ?
C6 N1 Cu1 114.40(18) ?
C14 O4 Cu2 109.20(17) ?
C13 O3 Cu2 109.00(16) ?
C13 O1 Cu1 110.15(17) ?
C36 O36 H36 115(3) ?
C14 O2 Cu1 109.92(16) ?
C38 O38 H38 116(3) ?
Cu2 O51 H51A 131(3) ?
Cu2 O51 H51B 117(3) ?
H51A O51 H51B 106(4) ?
Cu1 O50 H50A 119(3) ?
Cu1 O50 H50B 120(3) ?
H50A O50 H50B 111(4) ?
N32 C27 C28 120.7(3) ?
N32 C27 C26 114.3(2) ?
C28 C27 C26 124.9(3) ?
N1 C2 C3 122.7(3) ?
N1 C2 H2 118.6 ?
C3 C2 H2 118.6 ?
C4 C3 C2 118.3(3) ?
C4 C3 H3 120.9 ?
C2 C3 H3 120.9 ?
C8 C9 C10 119.7(3) ?
C8 C9 H9 120.1 ?
C10 C9 H9 120.1 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N1 1.958(2) y
Cu1 N12 1.969(2) y
Cu1 O1 1.9775(17) y
Cu1 O2 1.9644(17) y
Cu1 O50 2.219(3) y
Cu2 N21 1.957(2) y
Cu2 N32 1.954(2) y
Cu2 O3 1.9746(17) y
Cu2 O4 1.9778(17) y
Cu2 O51 2.277(3) y
C33 O33 1.223(3) y
C33 C34 1.497(4) y
C34 O34 1.219(3) y
C34 C35 1.494(4) y
C35 O35 1.253(3) y
C35 C36 1.411(4) y
C36 O36 1.297(3) y
C36 C33 1.435(4) y
C37 O37 1.256(3) y
C37 C38 1.417(4) y
C38 O38 1.295(3) y
C38 C39 1.453(4) y
C39 O39 1.213(3) y
C39 C40 1.510(4) y
C40 O40 1.212(3) y
C40 C37 1.483(4) y
C29 C30 1.361(4) ?
C29 C28 1.377(4) ?
C29 H29 0.93 ?
C28 C27 1.384(4) ?
C28 H28 0.93 ?
C26 N21 1.350(3) ?
C26 C25 1.379(4) ?
C26 C27 1.470(4) ?
C5 C4 1.377(4) ?
C5 C6 1.390(3) ?
C5 H5 0.93 ?
C4 C3 1.373(4) ?
C4 H4 0.93 ?
C23 C22 1.374(4) ?
C23 C24 1.375(4) ?
C23 H23 0.93 ?
C24 C25 1.358(4) ?
C24 H24 0.93 ?
C25 H25 0.93 ?
C11 N12 1.332(3) ?
C11 C10 1.373(4) ?
C11 H11 0.93 ?
C31 N32 1.340(3) ?
C31 C30 1.361(4) ?
C31 H31 0.93 ?
C6 N1 1.345(3) ?
C6 C7 1.475(4) ?
C10 C9 1.369(4) ?
C10 H10 0.93 ?
C7 N12 1.343(3) ?
C7 C8 1.369(3) ?
C14 O4 1.249(3) ?
C14 O2 1.254(3) ?
C14 C13 1.542(3) ?
C30 H30 0.93 ?
C8 C9 1.362(4) ?
C8 H8 0.93 ?
C22 N21 1.337(3) ?
C22 H22 0.93 ?
C13 O1 1.246(3) ?
C13 O3 1.258(3) ?
N32 C27 1.337(3) ?
N1 C2 1.326(3) ?
O36 H36 0.79(3) ?
O38 H38 0.79(3) ?
O51 H51A 0.722(16) ?
O51 H51B 0.720(16) ?
O50 H50A 0.723(16) ?
O50 H50B 0.719(16) ?
C2 C3 1.380(3) ?
C2 H2 0.93 ?
C3 H3 0.93 ?
C9 H9 0.93 ?
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
_geom_hbond_publ_flag
O36 H36 O37 . 0.79(4) 1.75(4) 2.517(3) 164(4) yes
O38 H38 O35 . 0.79(4) 1.77(4) 2.546(3) 166(4) yes
O50 H50A O34 1_565 0.719(19) 2.03(2) 2.711(3) 158(4) yes
O50 H50B O37 1_455 0.72(3) 2.05(3) 2.737(3) 161(4) yes
O51 H51A O35 1_565 0.72(3) 2.07(3) 2.758(3) 161(4) yes
O51 H51B O40 1_455 0.72(3) 2.03(3) 2.722(3) 164(4) yes
C2 H2 O1 . 0.93 2.52 3.037(3) 115 yes
C3 H3 O33 2_666 0.93 2.39 3.296(4) 166 yes
C5 H5 O34 2_556 0.93 2.52 3.360(4) 151 yes
C8 H8 O33 2_556 0.93 2.47 3.198(4) 136 yes
C25 H25 O39 2_765 0.93 2.42 3.153(4) 136 yes
C30 H30 O39 2_655 0.93 2.37 3.284(4) 169 yes
C31 H31 O4 . 0.93 2.50 3.021(3) 116 yes
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
C30 C29 C28 C27 0.0(5)
C6 C5 C4 C3 0.5(4)
C22 C23 C24 C25 -1.1(5)
C23 C24 C25 C26 0.4(5)
N21 C26 C25 C24 0.5(5)
C27 C26 C25 C24 -179.4(3)
C4 C5 C6 N1 -0.1(4)
C4 C5 C6 C7 178.4(3)
O40 C40 C37 O37 2.5(6)
C39 C40 C37 O37 -175.8(3)
O40 C40 C37 C38 179.0(4)
C39 C40 C37 C38 0.7(2)
N12 C11 C10 C9 0.6(5)
O33 C33 C36 O36 -0.1(6)
C34 C33 C36 O36 179.6(3)
O33 C33 C36 C35 -179.6(4)
C34 C33 C36 C35 0.2(2)
N1 C6 C7 N12 -0.6(3)
C5 C6 C7 N12 -179.2(2)
N1 C6 C7 C8 179.3(3)
C5 C6 C7 C8 0.8(4)
O40 C40 C39 O39 0.1(7)
C37 C40 C39 O39 178.4(4)
O40 C40 C39 C38 -179.1(4)
C37 C40 C39 C38 -0.7(2)
O33 C33 C34 O34 2.8(6)
C36 C33 C34 O34 -177.0(4)
O33 C33 C34 C35 179.6(3)
C36 C33 C34 C35 -0.2(2)
O36 C36 C35 O35 0.0(6)
C33 C36 C35 O35 179.3(3)
O36 C36 C35 C34 -179.5(3)
C33 C36 C35 C34 -0.2(2)
O34 C34 C35 O35 -2.7(6)
C33 C34 C35 O35 -179.4(3)
O34 C34 C35 C36 176.9(4)
C33 C34 C35 C36 0.2(2)
O37 C37 C38 O38 -1.7(7)
C40 C37 C38 O38 -178.1(4)
O37 C37 C38 C39 175.6(4)
C40 C37 C38 C39 -0.8(2)
O39 C39 C38 O38 -0.8(7)
C40 C39 C38 O38 178.4(4)
O39 C39 C38 C37 -178.4(4)
C40 C39 C38 C37 0.7(2)
N32 C31 C30 C29 -1.1(5)
C28 C29 C30 C31 0.4(5)
N12 C7 C8 C9 2.8(4)
C6 C7 C8 C9 -177.2(3)
C24 C23 C22 N21 0.9(5)
O4 C14 C13 O1 179.5(2)
O2 C14 C13 O1 -1.6(4)
O4 C14 C13 O3 -1.2(4)
O2 C14 C13 O3 177.7(2)
C30 C31 N32 C27 1.3(4)
C30 C31 N32 Cu2 -176.8(2)
N21 Cu2 N32 C27 -0.73(19)
O4 Cu2 N32 C27 -173.30(19)
O51 Cu2 N32 C27 97.70(19)
N21 Cu2 N32 C31 177.4(3)
O4 Cu2 N32 C31 4.9(2)
O51 Cu2 N32 C31 -84.1(2)
C23 C22 N21 C26 0.0(4)
C23 C22 N21 Cu2 -175.2(2)
C25 C26 N21 C22 -0.7(4)
C27 C26 N21 C22 179.2(3)
C25 C26 N21 Cu2 175.1(2)
C27 C26 N21 Cu2 -5.0(3)
N32 Cu2 N21 C22 178.6(3)
O3 Cu2 N21 C22 -7.0(3)
O51 Cu2 N21 C22 79.9(3)
N32 Cu2 N21 C26 3.26(19)
O3 Cu2 N21 C26 177.60(19)
O51 Cu2 N21 C26 -95.4(2)
C10 C11 N12 C7 0.8(4)
C10 C11 N12 Cu1 176.5(2)
C8 C7 N12 C11 -2.6(4)
C6 C7 N12 C11 177.4(2)
C8 C7 N12 Cu1 -178.8(2)
C6 C7 N12 Cu1 1.2(3)
N1 Cu1 N12 C11 -176.9(2)
O2 Cu1 N12 C11 -5.5(2)
O1 Cu1 N12 C11 -101.7(4)
O50 Cu1 N12 C11 84.4(2)
N1 Cu1 N12 C7 -1.03(18)
O2 Cu1 N12 C7 170.38(18)
O1 Cu1 N12 C7 74.2(4)
O50 Cu1 N12 C7 -99.73(19)
C5 C6 N1 C2 -0.7(4)
C7 C6 N1 C2 -179.4(2)
C5 C6 N1 Cu1 178.43(19)
C7 C6 N1 Cu1 -0.2(3)
N12 Cu1 N1 C2 179.7(2)
O1 Cu1 N1 C2 11.1(2)
O50 Cu1 N1 C2 -80.7(2)
N12 Cu1 N1 C6 0.66(18)
O1 Cu1 N1 C6 -167.97(18)
O50 Cu1 N1 C6 100.18(18)
O2 C14 O4 Cu2 171.8(2)
C13 C14 O4 Cu2 -9.4(3)
N32 Cu2 O4 C14 -173.49(17)
O3 Cu2 O4 C14 12.13(17)
O51 Cu2 O4 C14 -73.82(18)
O1 C13 O3 Cu2 -169.7(2)
C14 C13 O3 Cu2 11.1(3)
N21 Cu2 O3 C13 174.98(17)
O4 Cu2 O3 C13 -12.75(18)
O51 Cu2 O3 C13 75.89(18)
O3 C13 O1 Cu1 176.0(2)
C14 C13 O1 Cu1 -4.8(3)
N1 Cu1 O1 C13 178.07(18)
O2 Cu1 O1 C13 6.79(17)
N12 Cu1 O1 C13 104.1(4)
O50 Cu1 O1 C13 -81.92(18)
O4 C14 O2 Cu1 -174.1(2)
C13 C14 O2 Cu1 7.1(3)
N12 Cu1 O2 C14 -175.93(18)
O1 Cu1 O2 C14 -7.62(17)
O50 Cu1 O2 C14 83.52(18)
C31 N32 C27 C28 -0.8(4)
Cu2 N32 C27 C28 177.5(2)
C31 N32 C27 C26 180.0(3)
Cu2 N32 C27 C26 -1.7(3)
C29 C28 C27 N32 0.2(4)
C29 C28 C27 C26 179.3(3)
N21 C26 C27 N32 4.5(3)
C25 C26 C27 N32 -175.7(3)
N21 C26 C27 C28 -174.7(3)
C25 C26 C27 C28 5.1(5)
C6 N1 C2 C3 1.1(4)
Cu1 N1 C2 C3 -177.9(2)
C5 C4 C3 C2 -0.2(4)
N1 C2 C3 C4 -0.6(4)
C7 C8 C9 C10 -1.3(5)
C11 C10 C9 C8 -0.4(5)
