#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:25:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179480 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/77/4337769.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_4337769
loop_
_publ_author_name
'Gomila, Antoine'
'Duval, Sylvain'
'Besnard, Céline'
'Krämer, Karl W'
'Liu, Shi-Xia'
'Decurtins, Silvio'
'Williams, Alan F.'
_publ_section_title
;
 Tetracarboxylate Ligands as New Chelates Supporting Copper(II)
 Paddlewheel-Like Structures.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2683
_journal_page_last               2691
_journal_paper_doi               10.1021/ic403077q
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C104 H100 Cu4 N8 O20, 4(C3 H7 N O)'
_chemical_formula_sum            'C116 H128 Cu4 N12 O24'
_chemical_formula_weight         2328.46
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-16
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.2196(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.86902(13)
_cell_length_b                   18.90939(14)
_cell_length_c                   23.3517(2)
_cell_measurement_reflns_used    9282
_cell_measurement_temperature    179.9
_cell_measurement_theta_max      73.1767
_cell_measurement_theta_min      3.0141
_cell_volume                     5637.47(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      179.9
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_details
;
  1 omega  -50.00   42.00   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6865   38.0000  120.0000 115

  2 omega -113.00   -5.80   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6865  -57.0000 -150.0000 134

  3 omega    9.00   34.60   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -37.6865   38.0000    0.0000 32

  4 omega   57.00  120.20   0.8000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       37.6865  178.0000  -90.0000 79

  5 omega  149.00  175.40   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000   30.0000 33

  6 omega   31.00  141.40   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -61.0000   30.0000 138

  7 omega   34.00   89.20   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499 -113.0000  -24.0000 69

  8 omega   32.00   76.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000 -180.0000 55

  9 omega   97.00  172.20   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499   45.0000 -180.0000 94

 10 omega   55.00   99.00   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -45.0000  120.0000 55

 11 omega   43.00   90.20   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  -30.0000 -150.0000 59

 12 omega  146.00  172.40   0.8000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      109.7499  111.0000  120.0000 33
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0351102000
_diffrn_orient_matrix_UB_12      0.0019139000
_diffrn_orient_matrix_UB_13      -0.0607072000
_diffrn_orient_matrix_UB_21      -0.1004830000
_diffrn_orient_matrix_UB_22      -0.0396531000
_diffrn_orient_matrix_UB_23      -0.0243923000
_diffrn_orient_matrix_UB_31      -0.0568678000
_diffrn_orient_matrix_UB_32      0.0711049000
_diffrn_orient_matrix_UB_33      -0.0119824000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20713
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         73.33
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.796
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.2707
_exptl_crystal_size_mid          0.0996
_exptl_crystal_size_min          0.0395
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         10996
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0383
_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)+(0.0560P)²+1.7309P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                9082
_reflns_number_total             10996
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic403077q_si_002.cif
_cod_data_source_block           cu4DMF
_cod_database_code               4337769
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         'Cu4 C116 N12 O24 H128'
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 '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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.11780(2) 0.860801(14) 0.396440(12) 0.02549(8) Uani 1 1 d . . .
Cu2 Cu 0.27069(2) 0.786928(15) 0.362574(12) 0.02896(8) Uani 1 1 d . . .
O1 O 0.16379(11) 0.71308(7) 0.34268(6) 0.0304(3) Uani 1 1 d . A .
O2 O 0.03127(11) 0.77804(7) 0.36925(6) 0.0301(3) Uani 1 1 d . . .
O3 O 0.28852(11) 0.74875(8) 0.44154(6) 0.0342(3) Uani 1 1 d . A .
O4 O 0.15898(11) 0.81421(7) 0.47067(6) 0.0310(3) Uani 1 1 d . . .
O5 O -0.09458(12) 1.10315(8) 0.68349(6) 0.0332(3) Uani 1 1 d . . .
O6 O -0.22503(12) 1.16760(8) 0.71219(6) 0.0357(3) Uani 1 1 d . . .
O7 O -0.22490(12) 1.06548(8) 0.58559(6) 0.0351(3) Uani 1 1 d . . .
O8 O -0.35600(12) 1.12810(8) 0.61580(7) 0.0389(3) Uani 1 1 d . . .
O9 O -0.00911(12) 0.92166(8) 0.42325(6) 0.0347(3) Uani 1 1 d . . .
O10A O 0.4020(4) 0.7442(3) 0.3273(3) 0.0413(13) Uani 0.502(9) 1 d PU A 2
O10B O 0.3901(5) 0.7171(3) 0.3382(3) 0.0400(14) Uani 0.498(9) 1 d PU A 1
O11 O 0.6842(5) 0.5610(2) 0.4537(2) 0.168(2) Uani 1 1 d . . .
O12 O 0.7703(3) 0.91081(18) 0.28105(13) 0.1069(11) Uani 1 1 d . . .
N1 N 0.10259(13) 0.62187(8) 0.44825(7) 0.0250(3) Uani 1 1 d . A .
N2 N -0.32138(14) 1.01372(9) 0.73013(7) 0.0300(3) Uani 1 1 d . . .
N3 N -0.11859(16) 1.01453(11) 0.40214(9) 0.0432(5) Uani 1 1 d . . .
N4A N 0.4970(5) 0.6572(5) 0.2935(3) 0.0477(15) Uani 0.502(9) 1 d PU A 2
N4B N 0.5163(5) 0.6986(5) 0.2807(2) 0.0467(16) Uani 0.498(9) 1 d PU A 1
N5 N 0.6077(2) 0.65384(14) 0.49050(12) 0.0616(6) Uani 1 1 d . . .
N6 N 0.7276(2) 0.84606(18) 0.35730(12) 0.0743(8) Uani 1 1 d . . .
C1 C 0.06956(16) 0.72314(10) 0.34920(8) 0.0272(4) Uani 1 1 d . A .
C2 C -0.00725(16) 0.66538(10) 0.32907(8) 0.0284(4) Uani 1 1 d . . .
C3 C -0.08932(18) 0.68064(12) 0.28654(10) 0.0389(5) Uani 1 1 d . A .
H3 H -0.0973 0.7272 0.2714 0.047 Uiso 1 1 calc R . .
C4 C -0.15989(19) 0.62839(13) 0.26589(11) 0.0431(5) Uani 1 1 d . . .
H4 H -0.2149 0.6391 0.2361 0.052 Uiso 1 1 calc R A .
C5 C -0.15037(18) 0.56074(12) 0.28856(10) 0.0402(5) Uani 1 1 d . A .
H5 H -0.1991 0.5250 0.2749 0.048 Uiso 1 1 calc R . .
C6 C -0.06895(17) 0.54583(11) 0.33147(9) 0.0334(4) Uani 1 1 d . . .
H6 H -0.0632 0.4996 0.3475 0.040 Uiso 1 1 calc R A .
C7 C 0.00451(15) 0.59677(10) 0.35169(8) 0.0267(4) Uani 1 1 d . A .
C8 C 0.09670(15) 0.57870(9) 0.39560(8) 0.0267(4) Uani 1 1 d . . .
H8A H 0.0922 0.5282 0.4063 0.032 Uiso 1 1 calc R A .
H8B H 0.1620 0.5852 0.3779 0.032 Uiso 1 1 calc R . .
C9 C 0.22679(16) 0.76614(11) 0.47731(9) 0.0307(4) Uani 1 1 d . A .
C10 C 0.23604(16) 0.72653(11) 0.53361(9) 0.0308(4) Uani 1 1 d . . .
C11 C 0.25130(19) 0.76472(13) 0.58459(10) 0.0406(5) Uani 1 1 d . A .
H11 H 0.2568 0.8148 0.5833 0.049 Uiso 1 1 calc R . .
C12 C 0.2586(2) 0.73074(15) 0.63753(10) 0.0489(6) Uani 1 1 d . . .
H12 H 0.2706 0.7575 0.6722 0.059 Uiso 1 1 calc R A .
C13 C 0.2487(2) 0.65821(15) 0.64009(10) 0.0459(6) Uani 1 1 d . A .
H13 H 0.2528 0.6348 0.6763 0.055 Uiso 1 1 calc R . .
C14 C 0.23261(18) 0.61975(13) 0.58905(9) 0.0382(5) Uani 1 1 d . . .
H14 H 0.2255 0.5698 0.5907 0.046 Uiso 1 1 calc R A .
C15 C 0.22667(16) 0.65281(11) 0.53554(9) 0.0306(4) Uani 1 1 d . A .
C16 C 0.20637(16) 0.60893(10) 0.48133(9) 0.0308(4) Uani 1 1 d . . .
H16A H 0.2612 0.6193 0.4564 0.037 Uiso 1 1 calc R A .
H16B H 0.2120 0.5583 0.4919 0.037 Uiso 1 1 calc R . .
C17 C 0.01718(17) 0.60164(10) 0.48130(9) 0.0317(4) Uani 1 1 d . . .
H17A H 0.0393 0.5590 0.5043 0.038 Uiso 1 1 calc R A .
H17B H -0.0444 0.5884 0.4536 0.038 Uiso 1 1 calc R . .
C18 C -0.01676(15) 0.65727(10) 0.52179(8) 0.0279(4) Uani 1 1 d . A .
C19 C -0.03699(18) 0.63792(11) 0.57668(9) 0.0351(4) Uani 1 1 d . . .
H19 H -0.0219 0.5910 0.5898 0.042 Uiso 1 1 calc R A .
C20 C -0.07862(19) 0.68542(12) 0.61266(9) 0.0368(5) Uani 1 1 d . A .
H20 H -0.0916 0.6706 0.6500 0.044 Uiso 1 1 calc R . .
C21 C -0.10190(16) 0.75488(10) 0.59504(8) 0.0288(4) Uani 1 1 d . . .
C22 C -0.07787(16) 0.77469(10) 0.54030(9) 0.0301(4) Uani 1 1 d . A .
H22 H -0.0901 0.8220 0.5276 0.036 Uiso 1 1 calc R . .
C23 C -0.03658(16) 0.72661(11) 0.50422(8) 0.0300(4) Uani 1 1 d . . .
H23 H -0.0218 0.7413 0.4672 0.036 Uiso 1 1 calc R A .
C24 C -0.15264(16) 0.80383(10) 0.63276(8) 0.0294(4) Uani 1 1 d . A .
C25 C -0.22272(18) 0.77795(11) 0.66864(9) 0.0341(4) Uani 1 1 d . . .
H25 H -0.2377 0.7288 0.6687 0.041 Uiso 1 1 calc R A .
C26 C -0.27084(17) 0.82255(11) 0.70420(9) 0.0336(4) Uani 1 1 d . A .
H26 H -0.3188 0.8036 0.7279 0.040 Uiso 1 1 calc R . .
C27 C -0.25012(16) 0.89460(11) 0.70577(8) 0.0303(4) Uani 1 1 d . . .
C28 C -0.18011(18) 0.92089(11) 0.67029(9) 0.0352(4) Uani 1 1 d . A .
H28 H -0.1643 0.9700 0.6710 0.042 Uiso 1 1 calc R . .
C29 C -0.13307(18) 0.87644(11) 0.63392(9) 0.0350(4) Uani 1 1 d . . .
H29 H -0.0867 0.8957 0.6094 0.042 Uiso 1 1 calc R A .
C30 C -0.29765(18) 0.94031(11) 0.74876(9) 0.0350(4) Uani 1 1 d . A .
H30A H -0.3633 0.9177 0.7574 0.042 Uiso 1 1 calc R . .
H30B H -0.2489 0.9415 0.7851 0.042 Uiso 1 1 calc R . .
C31 C -0.42565(16) 1.01973(12) 0.69703(10) 0.0362(5) Uani 1 1 d . . .
H31A H -0.4423 1.0704 0.6905 0.043 Uiso 1 1 calc R . .
H31B H -0.4780 0.9998 0.7202 0.043 Uiso 1 1 calc R . .
C32 C -0.43559(16) 0.98245(12) 0.63941(10) 0.0348(4) Uani 1 1 d . . .
C33 C -0.49504(18) 0.92106(13) 0.63097(11) 0.0434(5) Uani 1 1 d . . .
H33 H -0.5304 0.9039 0.6615 0.052 Uiso 1 1 calc R . .
C34 C -0.5041(2) 0.88441(14) 0.57951(12) 0.0486(6) Uani 1 1 d . . .
H34 H -0.5458 0.8429 0.5748 0.058 Uiso 1 1 calc R . .
C35 C -0.4522(2) 0.90824(14) 0.53485(12) 0.0504(6) Uani 1 1 d . . .
H35 H -0.4583 0.8833 0.4993 0.060 Uiso 1 1 calc R . .
C36 C -0.3913(2) 0.96852(14) 0.54232(11) 0.0449(5) Uani 1 1 d . . .
H36 H -0.3545 0.9844 0.5119 0.054 Uiso 1 1 calc R . .
C37 C -0.38305(17) 1.00624(12) 0.59376(9) 0.0350(4) Uani 1 1 d . . .
C38 C -0.31622(17) 1.07198(12) 0.59912(9) 0.0337(4) Uani 1 1 d . . .
C39 C -0.31767(17) 1.06040(11) 0.78094(9) 0.0329(4) Uani 1 1 d . . .
H39A H -0.3624 1.0405 0.8085 0.040 Uiso 1 1 calc R . .
H39B H -0.3458 1.1075 0.7687 0.040 Uiso 1 1 calc R . .
C40 C -0.20740(18) 1.06832(11) 0.81045(9) 0.0343(4) Uani 1 1 d . . .
C41 C -0.1813(2) 1.04592(13) 0.86710(10) 0.0443(5) Uani 1 1 d . . .
H41 H -0.2347 1.0285 0.8880 0.053 Uiso 1 1 calc R . .
C42 C -0.0794(3) 1.04842(19) 0.89353(11) 0.0632(8) Uani 1 1 d . . .
H42 H -0.0632 1.0336 0.9325 0.076 Uiso 1 1 calc R . .
C43 C -0.0007(3) 1.0724(2) 0.86337(13) 0.0754(11) Uani 1 1 d . . .
H43 H 0.0697 1.0734 0.8813 0.090 Uiso 1 1 calc R . .
C44 C -0.0249(2) 1.09520(18) 0.80671(12) 0.0587(8) Uani 1 1 d . . .
H44 H 0.0292 1.1115 0.7858 0.070 Uiso 1 1 calc R . .
C45 C -0.12791(18) 1.09413(12) 0.78051(9) 0.0370(5) Uani 1 1 d . . .
C46 C -0.15201(17) 1.12345(11) 0.72047(9) 0.0320(4) Uani 1 1 d . . .
C47 C -0.05120(19) 0.96618(12) 0.38936(10) 0.0396(5) Uani 1 1 d . A .
H47 H -0.0338 0.9656 0.3510 0.047 Uiso 1 1 calc R . .
C48 C -0.1475(3) 1.0213(2) 0.45944(12) 0.0704(10) Uani 1 1 d . A .
H48A H -0.1265 0.9785 0.4817 0.106 Uiso 1 1 calc R . .
H48B H -0.2235 1.0275 0.4572 0.106 Uiso 1 1 calc R . .
H48C H -0.1120 1.0624 0.4785 0.106 Uiso 1 1 calc R . .
C49 C -0.1662(3) 1.0635(2) 0.35804(15) 0.0782(11) Uani 1 1 d . A .
H49A H -0.1516 1.0475 0.3199 0.117 Uiso 1 1 calc R . .
H49B H -0.1368 1.1109 0.3657 0.117 Uiso 1 1 calc R . .
H49C H -0.2421 1.0650 0.3589 0.117 Uiso 1 1 calc R . .
C53 C 0.5028(3) 0.6344(3) 0.4671(2) 0.1110(18) Uani 1 1 d . . .
H53A H 0.5055 0.5982 0.4372 0.167 Uiso 1 1 calc R . .
H53B H 0.4658 0.6761 0.4501 0.167 Uiso 1 1 calc R . .
H53C H 0.4657 0.6156 0.4979 0.167 Uiso 1 1 calc R . .
C54 C 0.6227(6) 0.7132(3) 0.5295(3) 0.138(2) Uani 1 1 d . . .
H54A H 0.5887 0.7034 0.5639 0.207 Uiso 1 1 calc R . .
H54B H 0.5917 0.7557 0.5103 0.207 Uiso 1 1 calc R . .
H54C H 0.6978 0.7208 0.5408 0.207 Uiso 1 1 calc R . .
C55 C 0.6880(3) 0.6154(3) 0.4818(2) 0.0878(12) Uani 1 1 d . . .
H55 H 0.7550 0.6311 0.4987 0.105 Uiso 1 1 calc R . .
C56 C 0.6387(4) 0.8864(3) 0.3653(3) 0.148(3) Uani 1 1 d . . .
H56A H 0.5769 0.8557 0.3620 0.222 Uiso 1 1 calc R . .
H56B H 0.6286 0.9235 0.3358 0.222 Uiso 1 1 calc R . .
H56C H 0.6487 0.9082 0.4037 0.222 Uiso 1 1 calc R . .
C57 C 0.7599(5) 0.7898(4) 0.3960(2) 0.140(3) Uani 1 1 d . . .
H57A H 0.8256 0.7698 0.3863 0.210 Uiso 1 1 calc R . .
H57B H 0.7058 0.7531 0.3928 0.210 Uiso 1 1 calc R . .
H57C H 0.7703 0.8079 0.4356 0.210 Uiso 1 1 calc R . .
C58 C 0.7877(4) 0.8643(2) 0.31594(16) 0.0821(11) Uani 1 1 d . . .
H58 H 0.8499 0.8376 0.3144 0.098 Uiso 1 1 calc R . .
C59A C 0.4208(4) 0.6820(3) 0.3213(2) 0.0388(14) Uani 0.502(9) 1 d PU A 2
H59A H 0.3780 0.6486 0.3377 0.047 Uiso 0.502(9) 1 calc PR A 2
C59B C 0.4430(4) 0.7376(3) 0.3014(3) 0.0381(14) Uani 0.498(9) 1 d PU A 1
H59B H 0.4311 0.7841 0.2866 0.046 Uiso 0.498(9) 1 calc PR A 1
C60A C 0.5560(7) 0.7054(5) 0.2627(4) 0.067(2) Uani 0.502(9) 1 d PU A 2
H60A H 0.5314 0.7538 0.2677 0.100 Uiso 0.502(9) 1 calc PR A 2
H60B H 0.5466 0.6933 0.2216 0.100 Uiso 0.502(9) 1 calc PR A 2
H60C H 0.6304 0.7021 0.2778 0.100 Uiso 0.502(9) 1 calc PR A 2
C60B C 0.5779(6) 0.7290(5) 0.2381(3) 0.064(2) Uani 0.498(9) 1 d PU A 1
H60D H 0.5752 0.6974 0.2047 0.097 Uiso 0.498(9) 1 calc PR A 1
H60E H 0.6508 0.7347 0.2555 0.097 Uiso 0.498(9) 1 calc PR A 1
H60F H 0.5490 0.7752 0.2257 0.097 Uiso 0.498(9) 1 calc PR A 1
C61A C 0.5175(6) 0.5822(5) 0.2917(4) 0.075(2) Uani 0.502(9) 1 d PU A 2
H61A H 0.5883 0.5725 0.3108 0.112 Uiso 0.502(9) 1 calc PR A 2
H61B H 0.5116 0.5664 0.2515 0.112 Uiso 0.502(9) 1 calc PR A 2
H61C H 0.4664 0.5567 0.3118 0.112 Uiso 0.502(9) 1 calc PR A 2
C61B C 0.5347(8) 0.6269(6) 0.2986(4) 0.073(3) Uani 0.498(9) 1 d PU A 1
H61D H 0.5963 0.6246 0.3278 0.110 Uiso 0.498(9) 1 calc PR A 1
H61E H 0.5469 0.5980 0.2652 0.110 Uiso 0.498(9) 1 calc PR A 1
H61F H 0.4734 0.6087 0.3149 0.110 Uiso 0.498(9) 1 calc PR A 1
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'
Cu Cu -1.9646 0.5888 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -1 0 0.0446 -0.0000 -1.0000 0.0000 -0.0019 0.0397 -0.0711
0 0 -1 0.0197 0.0000 -0.0000 -1.0000 0.0607 0.0244 0.0120
0 0 1 0.0197 -0.0000 0.0000 1.0000 -0.0607 -0.0244 -0.0120
0 1 1 0.0301 0.0000 1.0000 1.0000 -0.0588 -0.0640 0.0591
0 -1 -1 0.0301 -0.0000 -1.0000 -1.0000 0.0588 0.0640 -0.0591
-1 0 -1 0.0627 -1.0000 0.0000 -1.0000 0.0256 0.1249 0.0689
1 0 1 0.1387 1.0000 -0.0000 1.0000 -0.0256 -0.1249 -0.0689
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
O2 Cu1 Cu2 83.97(4) . .
O2 Cu1 O9 95.69(6) . .
O4 Cu1 Cu2 84.10(4) . .
O4 Cu1 O2 90.40(6) . .
O4 Cu1 O5 169.96(6) . 3_576
O4 Cu1 O7 91.47(6) . 3_576
O4 Cu1 O9 96.54(6) . .
O5 Cu1 Cu2 85.92(4) 3_576 .
O5 Cu1 O2 87.56(6) 3_576 .
O5 Cu1 O9 93.44(6) 3_576 .
O7 Cu1 Cu2 84.81(5) 3_576 .
O7 Cu1 O2 168.37(6) 3_576 .
O7 Cu1 O5 88.61(6) 3_576 3_576
O7 Cu1 O9 95.50(6) 3_576 .
O9 Cu1 Cu2 179.29(4) . .
O1 Cu2 Cu1 85.44(4) . .
O1 Cu2 O8 169.69(6) . 3_576
O1 Cu2 O10A 101.76(15) . .
O1 Cu2 O10B 90.20(17) . .
O3 Cu2 Cu1 85.18(4) . .
O3 Cu2 O1 87.52(6) . .
O3 Cu2 O6 168.12(6) . 3_576
O3 Cu2 O8 93.63(7) . 3_576
O3 Cu2 O10A 102.62(17) . .
O3 Cu2 O10B 91.13(15) . .
O6 Cu2 Cu1 83.27(4) 3_576 .
O6 Cu2 O1 88.78(6) 3_576 .
O6 Cu2 O8 88.04(7) 3_576 3_576
O6 Cu2 O10A 89.19(17) 3_576 .
O6 Cu2 O10B 100.17(15) 3_576 .
O8 Cu2 Cu1 84.45(5) 3_576 .
O8 Cu2 O10A 88.00(16) 3_576 .
O8 Cu2 O10B 100.01(17) 3_576 .
O10A Cu2 Cu1 169.49(16) . .
O10A Cu2 O10B 16.08(11) . .
O10B Cu2 Cu1 174.40(14) . .
C1 O1 Cu2 121.29(12) . .
C1 O2 Cu1 122.59(13) . .
C9 O3 Cu2 120.95(13) . .
C9 O4 Cu1 122.79(13) . .
C46 O5 Cu1 120.58(14) . 3_576
C46 O6 Cu2 124.21(13) . 3_576
C38 O7 Cu1 121.83(14) . 3_576
C38 O8 Cu2 121.96(14) . 3_576
C47 O9 Cu1 117.78(14) . .
C59A O10A Cu2 126.3(5) . .
C59B O10B Cu2 118.0(4) . .
C8 N1 C16 107.08(15) . .
C8 N1 C17 109.34(15) . .
C17 N1 C16 111.64(16) . .
C31 N2 C30 111.73(17) . .
C31 N2 C39 108.22(16) . .
C39 N2 C30 109.96(16) . .
C47 N3 C48 121.7(2) . .
C47 N3 C49 120.6(2) . .
C48 N3 C49 117.7(2) . .
C59A N4A C60A 119.4(8) . .
C59A N4A C61A 120.6(7) . .
C60A N4A C61A 119.9(6) . .
C59B N4B C60B 119.7(7) . .
C59B N4B C61B 121.2(8) . .
C61B N4B C60B 119.1(6) . .
C53 N5 C54 118.9(4) . .
C55 N5 C53 121.6(4) . .
C55 N5 C54 119.2(4) . .
C56 N6 C57 119.9(5) . .
C58 N6 C56 120.2(4) . .
C58 N6 C57 119.7(4) . .
O1 C1 O2 126.64(18) . .
O1 C1 C2 117.23(17) . .
O2 C1 C2 116.08(17) . .
C3 C2 C1 118.89(18) . .
C3 C2 C7 119.94(19) . .
C7 C2 C1 121.15(17) . .
C2 C3 C4 120.5(2) . .
C5 C4 C3 120.2(2) . .
C4 C5 C6 119.2(2) . .
C5 C6 C7 121.7(2) . .
C2 C7 C8 120.32(17) . .
C6 C7 C2 118.46(18) . .
C6 C7 C8 121.19(18) . .
N1 C8 C7 113.38(15) . .
O3 C9 C10 117.37(18) . .
O4 C9 O3 126.17(19) . .
O4 C9 C10 116.45(18) . .
C11 C10 C9 118.6(2) . .
C11 C10 C15 119.7(2) . .
C15 C10 C9 121.74(18) . .
C10 C11 C12 120.7(2) . .
C13 C12 C11 120.2(2) . .
C12 C13 C14 119.2(2) . .
C13 C14 C15 121.4(2) . .
C10 C15 C16 121.80(18) . .
C14 C15 C10 118.8(2) . .
C14 C15 C16 119.39(19) . .
N1 C16 C15 113.43(16) . .
N1 C17 C18 116.10(16) . .
C19 C18 C17 119.68(18) . .
C23 C18 C17 121.89(17) . .
C23 C18 C19 118.23(18) . .
C20 C19 C18 121.42(19) . .
C19 C20 C21 121.11(18) . .
C20 C21 C22 117.09(18) . .
C20 C21 C24 120.36(17) . .
C22 C21 C24 122.53(18) . .
C23 C22 C21 121.50(18) . .
C18 C23 C22 120.59(18) . .
C25 C24 C21 120.23(18) . .
C25 C24 C29 117.54(18) . .
C29 C24 C21 122.22(18) . .
C26 C25 C24 121.25(19) . .
C25 C26 C27 121.02(18) . .
C26 C27 C28 118.16(18) . .
C26 C27 C30 119.12(18) . .
C28 C27 C30 122.56(19) . .
C29 C28 C27 120.91(19) . .
C28 C29 C24 121.10(19) . .
N2 C30 C27 115.36(16) . .
N2 C31 C32 113.76(17) . .
C33 C32 C31 120.0(2) . .
C33 C32 C37 117.9(2) . .
C37 C32 C31 122.09(19) . .
C34 C33 C32 121.8(2) . .
C33 C34 C35 119.8(2) . .
C36 C35 C34 119.6(2) . .
C35 C36 C37 120.8(2) . .
C32 C37 C38 121.63(19) . .
C36 C37 C32 120.0(2) . .
C36 C37 C38 118.39(19) . .
O7 C38 O8 125.9(2) . .
O7 C38 C37 116.02(19) . .
O8 C38 C37 118.03(19) . .
N2 C39 C40 111.18(17) . .
C41 C40 C39 120.4(2) . .
C41 C40 C45 118.6(2) . .
C45 C40 C39 120.86(19) . .
C42 C41 C40 121.2(2) . .
C41 C42 C43 120.0(2) . .
C42 C43 C44 119.8(3) . .
C45 C44 C43 120.1(3) . .
C40 C45 C46 121.1(2) . .
C44 C45 C40 120.2(2) . .
C44 C45 C46 118.6(2) . .
O5 C46 C45 117.1(2) . .
O6 C46 O5 126.0(2) . .
O6 C46 C45 116.90(18) . .
O9 C47 N3 125.2(2) . .
O11 C55 N5 125.3(5) . .
O12 C58 N6 126.5(4) . .
O10A C59A N4A 124.6(6) . .
O10B C59B N4B 124.0(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 Cu2 2.6152(4) .
Cu1 O2 1.9785(14) .
Cu1 O4 1.9572(14) .
Cu1 O5 1.9741(14) 3_576
Cu1 O7 1.9682(15) 3_576
Cu1 O9 2.1542(14) .
Cu2 O1 1.9743(14) .
Cu2 O3 1.9666(15) .
Cu2 O6 1.9684(15) 3_576
Cu2 O8 1.9756(15) 3_576
Cu2 O10A 2.131(6) .
Cu2 O10B 2.155(6) .
O1 C1 1.256(3) .
O2 C1 1.264(2) .
O3 C9 1.266(3) .
O4 C9 1.256(3) .
O5 Cu1 1.9741(14) 3_576
O5 C46 1.265(2) .
O6 Cu2 1.9685(15) 3_576
O6 C46 1.254(3) .
O7 Cu1 1.9682(14) 3_576
O7 C38 1.261(3) .
O8 Cu2 1.9756(15) 3_576
O8 C38 1.261(3) .
O9 C47 1.233(3) .
O10A C59A 1.212(10) .
O10B C59B 1.225(9) .
O11 C55 1.218(6) .
O12 C58 1.201(5) .
N1 C8 1.470(2) .
N1 C16 1.477(3) .
N1 C17 1.471(2) .
N2 C30 1.475(3) .
N2 C31 1.466(3) .
N2 C39 1.475(2) .
N3 C47 1.320(3) .
N3 C48 1.439(3) .
N3 C49 1.461(4) .
N4A C59A 1.328(9) .
N4A C60A 1.436(10) .
N4A C61A 1.445(9) .
N4B C59B 1.335(9) .
N4B C60B 1.466(9) .
N4B C61B 1.430(10) .
N5 C53 1.439(5) .
N5 C54 1.443(5) .
N5 C55 1.300(5) .
N6 C56 1.407(5) .
N6 C57 1.423(6) .
N6 C58 1.356(6) .
C1 C2 1.508(3) .
C2 C3 1.386(3) .
C2 C7 1.402(3) .
C3 C4 1.387(3) .
C4 C5 1.384(3) .
C5 C6 1.385(3) .
C6 C7 1.390(3) .
C7 C8 1.507(3) .
C9 C10 1.505(3) .
C10 C11 1.385(3) .
C10 C15 1.400(3) .
C11 C12 1.386(4) .
C12 C13 1.379(4) .
C13 C14 1.389(3) .
C14 C15 1.391(3) .
C15 C16 1.509(3) .
C17 C18 1.515(3) .
C18 C19 1.389(3) .
C18 C23 1.388(3) .
C19 C20 1.383(3) .
C20 C21 1.397(3) .
C21 C22 1.403(3) .
C21 C24 1.485(3) .
C22 C23 1.390(3) .
C24 C25 1.394(3) .
C24 C29 1.396(3) .
C25 C26 1.383(3) .
C26 C27 1.388(3) .
C27 C28 1.390(3) .
C27 C30 1.511(3) .
C28 C29 1.387(3) .
C31 C32 1.510(3) .
C32 C33 1.391(3) .
C32 C37 1.406(3) .
C33 C34 1.379(4) .
C34 C35 1.383(4) .
C35 C36 1.382(4) .
C36 C37 1.390(3) .
C37 C38 1.508(3) .
C39 C40 1.505(3) .
C40 C41 1.389(3) .
C40 C45 1.398(3) .
C41 C42 1.379(4) .
C42 C43 1.380(4) .
C43 C44 1.389(4) .
C44 C45 1.389(4) .
C45 C46 1.503(3) .
