#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:36:54 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179669 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/22/4512272.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_4512272
loop_
_publ_author_name
'Clegg, William'
'Holcroft, James M.'
_publ_section_title
;
 Structural Variation in Mellitate Complexes of First-Row Transition
 Metals: What Chance for Design?
;
_journal_issue                   12
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              6282
_journal_paper_doi               10.1021/cg5009736
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C24 H34 Cu5 O40,7 H2 O'
_chemical_formula_sum            'C24 H48 Cu5 O47'
_chemical_formula_weight         1406.32
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 113.005(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.350(2)
_cell_length_b                   9.5383(6)
_cell_length_c                   18.5428(16)
_cell_measurement_reflns_used    4218
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.97
_cell_volume                     4452.6(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12708
_diffrn_reflns_point_group_measured_fraction_full 0.776
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.067
_diffrn_source                   'sealed tube with Enhance optics'
_exptl_absorpt_coefficient_mu    2.491
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.098
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2852
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Flack x determined using 1685 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         6109
_refine_ls_number_restraints     1330
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0332P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.553
_reflns_Friedel_fraction_full    0.553
_reflns_Friedel_fraction_max     0.553
_reflns_number_gt                5275
_reflns_number_total             6109
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg5009736_si_001.cif
_cod_data_source_block           jmh29n
_cod_depositor_comments
'Adding full bibliography for 4512266--4512273.cif.'
_cod_database_code               4512272
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.886
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.48013(4) 0.10498(11) 0.76049(6) 0.0108(2) Uani 1 1 d . .
Cu2 Cu 0.65687(4) 0.10482(12) 1.00421(6) 0.0083(3) Uani 1 1 d . .
Cu3 Cu 0.64738(4) 0.61970(11) 0.93768(6) 0.0092(3) Uani 1 1 d . .
Cu4 Cu 0.31218(4) 0.61972(11) 0.73580(6) 0.0102(3) Uani 1 1 d . .
Cu5 Cu 0.30868(4) 0.12372(11) 0.79907(6) 0.0089(3) Uani 1 1 d . .
C1 C 0.6064(4) 0.2007(9) 0.7662(6) 0.0087(10) Uani 1 1 d . U
C2 C 0.6065(3) 0.3452(9) 0.7570(6) 0.0083(10) Uani 1 1 d . U
C3 C 0.6119(3) 0.4011(9) 0.6903(5) 0.0077(10) Uani 1 1 d . U
C4 C 0.6150(4) 0.3107(9) 0.6326(6) 0.0083(10) Uani 1 1 d . U
C5 C 0.6131(3) 0.1671(9) 0.6424(6) 0.0082(10) Uani 1 1 d . U
C6 C 0.6088(3) 0.1112(9) 0.7080(5) 0.0080(10) Uani 1 1 d . U
C7 C 0.6044(3) 0.1422(9) 0.8403(6) 0.0087(10) Uani 1 1 d . U
C8 C 0.6044(4) 0.4427(9) 0.8198(6) 0.0097(11) Uani 1 1 d . U
C9 C 0.6152(4) 0.5588(9) 0.6795(5) 0.0078(11) Uani 1 1 d . U
C10 C 0.6180(4) 0.3695(9) 0.5594(6) 0.0095(11) Uani 1 1 d . U
C11 C 0.6171(4) 0.0738(9) 0.5773(6) 0.0082(11) Uani 1 1 d . U
C12 C 0.6054(4) -0.0464(9) 0.7186(6) 0.0081(12) Uani 1 1 d . U
O1 O 0.5644(2) 0.0857(6) 0.8419(4) 0.0097(11) Uani 1 1 d . U
O2 O 0.6486(2) 0.1529(6) 0.8995(4) 0.0113(12) Uani 1 1 d . U
O3 O 0.5757(3) 0.4105(7) 0.8546(4) 0.0135(13) Uani 1 1 d . U
O4 O 0.6346(2) 0.5470(6) 0.8347(4) 0.0105(12) Uani 1 1 d . U
O5 O 0.5733(2) 0.6273(6) 0.6665(4) 0.0088(12) Uani 1 1 d . U
O6 O 0.6586(2) 0.6045(6) 0.6834(4) 0.0088(12) Uani 1 1 d . U
O7 O 0.5850(3) 0.4536(7) 0.5196(4) 0.0167(14) Uani 1 1 d . U
O8 O 0.6567(2) 0.3207(6) 0.5427(4) 0.0104(11) Uani 1 1 d . U
O9 O 0.5813(2) 0.0827(6) 0.5114(4) 0.0113(13) Uani 1 1 d . U
O10 O 0.6582(2) -0.0027(6) 0.5966(4) 0.0099(11) Uani 1 1 d . U
O11 O 0.6261(2) -0.1002(6) 0.7826(4) 0.0121(13) Uani 1 1 d . U
O12 O 0.5788(2) -0.1100(6) 0.6534(4) 0.0095(12) Uani 1 1 d D U
H12 H 0.572(4) -0.196(3) 0.654(5) 0.014 Uiso 1 1 d D U
C13 C 0.3504(3) 0.3335(10) 0.5977(5) 0.0081(10) Uani 1 1 d . U
C14 C 0.3483(3) 0.1876(9) 0.6074(6) 0.0076(10) Uani 1 1 d . U
C15 C 0.3521(3) 0.0972(9) 0.5505(5) 0.0070(10) Uani 1 1 d . U
C16 C 0.3557(3) 0.1501(9) 0.4840(6) 0.0074(10) Uani 1 1 d . U
C17 C 0.3569(4) 0.2945(9) 0.4726(6) 0.0079(10) Uani 1 1 d . U
C18 C 0.3544(3) 0.3875(9) 0.5300(5) 0.0085(10) Uani 1 1 d . U
C19 C 0.3486(3) 0.4255(9) 0.6613(6) 0.0082(11) Uani 1 1 d . U
C20 C 0.3427(4) 0.1299(9) 0.6791(6) 0.0084(11) Uani 1 1 d . U
C21 C 0.3494(4) -0.0604(9) 0.5601(6) 0.0085(11) Uani 1 1 d . U
C22 C 0.3572(4) 0.0554(9) 0.4205(6) 0.0085(11) Uani 1 1 d . U
C23 C 0.3574(4) 0.3511(9) 0.3964(6) 0.0086(11) Uani 1 1 d . U
C24 C 0.3548(4) 0.5413(9) 0.5175(6) 0.0088(12) Uani 1 1 d . U
O13 O 0.3097(2) 0.5105(6) 0.6442(4) 0.0095(11) Uani 1 1 d . U
O14 O 0.3838(2) 0.4178(6) 0.7287(4) 0.0097(13) Uani 1 1 d . U
O15 O 0.3077(2) 0.1865(7) 0.6980(4) 0.0093(11) Uani 1 1 d . U
O16 O 0.3723(3) 0.0335(6) 0.7158(4) 0.0138(13) Uani 1 1 d . U
O17 O 0.3072(3) -0.1138(6) 0.5577(4) 0.0144(14) Uani 1 1 d . U
O18 O 0.3909(2) -0.1287(6) 0.5675(4) 0.0115(13) Uani 1 1 d . U
O19 O 0.3206(2) -0.0376(6) 0.3986(4) 0.0102(12) Uani 1 1 d . U
O20 O 0.3919(3) 0.0711(6) 0.3940(4) 0.0136(13) Uani 1 1 d . U
O21 O 0.3187(2) 0.3087(6) 0.3357(4) 0.0106(12) Uani 1 1 d . U
O22 O 0.3923(3) 0.4318(6) 0.3962(4) 0.0145(13) Uani 1 1 d . U
O23 O 0.3232(2) 0.5926(7) 0.4556(4) 0.0136(13) Uani 1 1 d . U
O24 O 0.3883(2) 0.6112(6) 0.5743(4) 0.0121(13) Uani 1 1 d D U
H24 H 0.388(4) 0.694(4) 0.559(5) 0.018 Uiso 1 1 d D U
O25 O 0.4781(2) 0.2022(6) 0.6663(4) 0.0145(14) Uani 1 1 d D U
H25A H 0.486(4) 0.181(8) 0.628(4) 0.022 Uiso 1 1 d D U
H25B H 0.488(4) 0.284(4) 0.682(5) 0.022 Uiso 1 1 d D U
O26 O 0.4786(2) 0.2887(6) 0.8066(4) 0.0136(14) Uani 1 1 d D U
H26A H 0.5049(18) 0.336(7) 0.809(5) 0.020 Uiso 1 1 d D U
H26B H 0.4506(16) 0.334(7) 0.783(5) 0.020 Uiso 1 1 d D U
O27 O 0.4697(3) 0.0159(7) 0.8484(4) 0.0168(14) Uani 1 1 d D U
H27A H 0.488(3) 0.065(9) 0.888(3) 0.025 Uiso 1 1 d D U
H27B H 0.4408(19) -0.006(9) 0.851(5) 0.025 Uiso 1 1 d D U
O28 O 0.4787(3) -0.0740(6) 0.7086(4) 0.0163(15) Uani 1 1 d D U
H28A H 0.452(2) -0.099(8) 0.670(4) 0.024 Uiso 1 1 d D U
H28B H 0.493(3) -0.144(5) 0.736(4) 0.024 Uiso 1 1 d D U
O29 O 0.6016(3) 0.2355(7) 1.0037(4) 0.0151(15) Uani 1 1 d D U
H29A H 0.5714(15) 0.211(10) 1.000(5) 0.023 Uiso 1 1 d D U
H29B H 0.599(3) 0.292(8) 0.968(4) 0.023 Uiso 1 1 d D U
O30 O 0.7070(3) 0.2729(7) 1.0908(4) 0.0126(15) Uani 1 1 d D U
H30A H 0.7394(8) 0.274(10) 1.120(4) 0.019 Uiso 1 1 d D U
H30B H 0.689(2) 0.298(10) 1.116(4) 0.019 Uiso 1 1 d D U
O31 O 0.7211(3) 0.0019(7) 1.0114(4) 0.0178(16) Uani 1 1 d D U
H31A H 0.746(3) -0.016(8) 1.055(3) 0.027 Uiso 1 1 d D U
H31B H 0.714(4) -0.072(5) 0.984(4) 0.027 Uiso 1 1 d D U
O32 O 0.6971(3) 0.4654(7) 0.9789(4) 0.0179(16) Uani 1 1 d D U
H32A H 0.716(3) 0.451(10) 1.0263(13) 0.027 Uiso 1 1 d D U
H32B H 0.710(3) 0.424(9) 0.951(4) 0.027 Uiso 1 1 d D U
O33 O 0.5937(3) 0.7707(6) 0.8904(4) 0.0123(15) Uani 1 1 d D U
H33A H 0.595(4) 0.825(6) 0.927(3) 0.018 Uiso 1 1 d D U
H33B H 0.599(4) 0.817(7) 0.856(4) 0.018 Uiso 1 1 d D U
O34 O 0.7203(3) 0.7517(7) 0.9404(4) 0.0150(16) Uani 1 1 d D U
H34A H 0.747(3) 0.701(8) 0.966(4) 0.022 Uiso 1 1 d D U
H34B H 0.715(3) 0.744(9) 0.8926(14) 0.022 Uiso 1 1 d D U
O35 O 0.3731(3) 0.7318(7) 0.7367(4) 0.0153(16) Uani 1 1 d D U
H35A H 0.374(3) 0.816(4) 0.751(5) 0.023 Uiso 1 1 d D U
H35B H 0.4042(13) 0.700(8) 0.753(5) 0.023 Uiso 1 1 d D U
O36 O 0.2596(3) 0.7849(7) 0.6493(4) 0.0145(15) Uani 1 1 d D U
H36A H 0.233(2) 0.781(9) 0.606(3) 0.022 Uiso 1 1 d D U
H36B H 0.282(2) 0.841(8) 0.646(5) 0.022 Uiso 1 1 d D U
O37 O 0.2469(3) 0.5200(7) 0.7319(4) 0.0156(15) Uani 1 1 d D U
H37A H 0.235(3) 0.522(10) 0.767(3) 0.023 Uiso 1 1 d D U
H37B H 0.223(2) 0.546(10) 0.689(2) 0.023 Uiso 1 1 d D U
O38 O 0.3585(3) 0.2738(6) 0.8515(4) 0.0130(15) Uani 1 1 d D U
H38A H 0.376(3) 0.331(7) 0.839(5) 0.019 Uiso 1 1 d D U
H38B H 0.350(4) 0.303(8) 0.887(4) 0.019 Uiso 1 1 d D U
O39 O 0.2544(3) -0.0206(7) 0.7495(4) 0.0131(15) Uani 1 1 d D U
H39A H 0.262(3) -0.086(7) 0.725(4) 0.020 Uiso 1 1 d D U
H39B H 0.2219(11) -0.001(8) 0.727(5) 0.020 Uiso 1 1 d D U
O40 O 0.2360(3) 0.2527(7) 0.7995(4) 0.0164(16) Uani 1 1 d D U
H40A H 0.208(2) 0.221(8) 0.764(4) 0.025 Uiso 1 1 d D U
H40B H 0.243(3) 0.331(5) 0.785(5) 0.025 Uiso 1 1 d D U
O41 O 0.4850(3) 0.1188(8) 0.5326(4) 0.0261(17) Uani 1 1 d D U
H41A H 0.513(2) 0.140(11) 0.526(5) 0.039 Uiso 1 1 d D U
H41B H 0.461(2) 0.100(11) 0.489(3) 0.039 Uiso 1 1 d D U
O42 O 0.2331(4) 0.4391(8) 0.3610(6) 0.041(2) Uani 1 1 d . U
O43 O 0.4819(3) 0.6781(7) 0.7845(4) 0.0227(17) Uani 1 1 d D U
H43A H 0.5119(19) 0.678(10) 0.822(4) 0.034 Uiso 1 1 d D U
H43B H 0.486(4) 0.610(10) 0.751(5) 0.034 Uiso 1 1 d D U
O44 O 0.7302(4) 0.3515(8) 0.8790(6) 0.046(2) Uani 1 1 d . U
O45 O 0.4850(2) 0.4897(6) 0.6709(4) 0.0174(15) Uani 1 1 d D U
H45A H 0.4573(17) 0.525(9) 0.638(4) 0.026 Uiso 1 1 d D U
H45B H 0.5118(18) 0.525(9) 0.667(5) 0.026 Uiso 1 1 d D U
O46 O 0.5017(3) 0.1705(7) 0.9836(4) 0.0172(15) Uani 1 1 d D U
H46A H 0.495(4) 0.138(8) 1.021(4) 0.026 Uiso 1 1 d D U
H46B H 0.495(4) 0.256(3) 0.977(5) 0.026 Uiso 1 1 d D U
O47 O 0.4824(3) 0.5608(7) 0.5041(4) 0.0252(18) Uani 1 1 d D U
H47A H 0.459(2) 0.504(8) 0.477(6) 0.038 Uiso 1 1 d D U
H47B H 0.5126(15) 0.525(9) 0.515(6) 0.038 Uiso 1 1 d D U
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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
O1 Cu1 O25 107.9(2) . .
O1 Cu1 O26 88.3(2) . .
O1 Cu1 O27 81.2(3) . .
O1 Cu1 O28 94.5(3) . .
O25 Cu1 O26 88.2(3) . .
O25 Cu1 O27 170.5(3) . .
O25 Cu1 O28 89.2(3) . .
O26 Cu1 O27 89.4(3) . .
O26 Cu1 O28 176.6(3) . .
O27 Cu1 O28 92.8(3) . .
O2 Cu2 O10 163.3(3) . 2
O2 Cu2 O29 93.3(3) . .
O2 Cu2 O30 110.0(3) . .
O2 Cu2 O31 86.4(3) . .
O10 Cu2 O29 94.1(3) 2 .
O10 Cu2 O30 86.2(3) 2 .
O10 Cu2 O31 89.0(3) 2 .
O29 Cu2 O30 79.0(3) . .
O29 Cu2 O31 169.8(3) . .
O30 Cu2 O31 91.6(3) . .
O4 Cu3 O8 175.0(3) . 2_565
O4 Cu3 O32 86.9(3) . .
O4 Cu3 O33 90.4(3) . .
O4 Cu3 O34 92.1(3) . .
O8 Cu3 O32 91.7(3) 2_565 .
O8 Cu3 O33 90.9(3) 2_565 .
O8 Cu3 O34 92.6(3) 2_565 .
O32 Cu3 O33 176.7(3) . .
O32 Cu3 O34 86.5(3) . .
O33 Cu3 O34 95.5(2) . .
O13 Cu4 O21 168.6(3) . 2_565
O13 Cu4 O35 92.2(3) . .
O13 Cu4 O36 87.7(3) . .
O13 Cu4 O37 89.3(3) . .
O21 Cu4 O35 92.3(3) 2_565 .
O21 Cu4 O36 103.0(3) 2_565 .
O21 Cu4 O37 87.0(3) 2_565 .
O35 Cu4 O36 86.1(3) . .
O35 Cu4 O37 175.4(3) . .
O36 Cu4 O37 89.7(3) . .
O15 Cu5 O19 168.7(3) . 2
O15 Cu5 O38 89.9(3) . .
O15 Cu5 O39 92.3(3) . .
O15 Cu5 O40 98.5(3) . .
O19 Cu5 O38 90.7(3) 2 .
O19 Cu5 O39 87.9(3) 2 .
O19 Cu5 O40 92.7(3) 2 .
O38 Cu5 O39 175.3(3) . .
O38 Cu5 O40 92.4(3) . .
O39 Cu5 O40 83.3(3) . .
C2 C1 C6 120.6(9) . .
C2 C1 C7 118.8(8) . .
C6 C1 C7 120.5(8) . .
C1 C2 C3 119.3(9) . .
C1 C2 C8 121.0(8) . .
C3 C2 C8 119.6(8) . .
C2 C3 C4 119.7(8) . .
C2 C3 C9 121.5(8) . .
C4 C3 C9 118.8(8) . .
C3 C4 C5 119.5(9) . .
C3 C4 C10 120.1(8) . .
C5 C4 C10 120.3(8) . .
C4 C5 C6 121.3(9) . .
C4 C5 C11 116.9(8) . .
C6 C5 C11 121.8(8) . .
C1 C6 C5 119.5(8) . .
C1 C6 C12 118.7(8) . .
C5 C6 C12 121.9(8) . .
C1 C7 O1 122.3(8) . .
C1 C7 O2 113.1(8) . .
O1 C7 O2 124.5(9) . .
C2 C8 O3 118.3(8) . .
C2 C8 O4 116.1(8) . .
O3 C8 O4 125.5(9) . .
C3 C9 O5 116.2(7) . .
C3 C9 O6 116.4(7) . .
O5 C9 O6 127.4(8) . .
C4 C10 O7 120.4(8) . .
C4 C10 O8 114.8(8) . .
O7 C10 O8 124.7(9) . .
C5 C11 O9 117.7(8) . .
C5 C11 O10 116.0(8) . .
O9 C11 O10 126.3(9) . .
C6 C12 O11 121.0(8) . .
C6 C12 O12 112.5(8) . .
O11 C12 O12 126.5(8) . .
Cu1 O1 C7 130.3(6) . .
Cu2 O2 C7 123.1(6) . .
Cu3 O4 C8 110.6(6) . .
Cu3 O8 C10 109.5(6) 2_564 .
Cu2 O10 C11 109.1(6) 2_554 .
C12 O12 H12 119(6) . .
C14 C13 C18 120.1(8) . .
C14 C13 C19 117.8(8) . .
C18 C13 C19 122.1(8) . .
C13 C14 C15 119.6(9) . .
C13 C14 C20 120.1(8) . .
C15 C14 C20 120.3(8) . .
C14 C15 C16 120.3(8) . .
C14 C15 C21 120.0(8) . .
C16 C15 C21 119.6(8) . .
C15 C16 C17 120.9(9) . .
C15 C16 C22 121.3(8) . .
C17 C16 C22 117.8(8) . .
C16 C17 C18 119.7(9) . .
C16 C17 C23 120.1(8) . .
C18 C17 C23 120.1(8) . .
C13 C18 C17 119.3(8) . .
C13 C18 C24 120.8(8) . .
C17 C18 C24 119.9(8) . .
C13 C19 O13 117.5(8) . .
C13 C19 O14 120.6(8) . .
O13 C19 O14 122.0(8) . .
C14 C20 O15 116.1(8) . .
C14 C20 O16 119.4(8) . .
O15 C20 O16 124.5(9) . .
C15 C21 O17 119.2(8) . .
C15 C21 O18 115.9(8) . .
O17 C21 O18 124.9(8) . .
C16 C22 O19 114.2(8) . .
C16 C22 O20 120.0(8) . .
O19 C22 O20 125.8(9) . .
C17 C23 O21 113.7(8) . .
C17 C23 O22 121.1(8) . .
O21 C23 O22 125.3(9) . .
C18 C24 O23 119.3(8) . .
C18 C24 O24 115.6(8) . .
O23 C24 O24 125.0(8) . .
Cu4 O13 C19 112.2(6) . .
Cu5 O15 C20 114.0(6) . .
Cu5 O19 C22 114.7(6) 2_554 .
Cu4 O21 C23 118.1(6) 2_564 .
C24 O24 H24 108(7) . .
Cu1 O25 H25A 135(6) . .
Cu1 O25 H25B 104(6) . .
H25A O25 H25B 110(4) . .
Cu1 O26 H26A 110(6) . .
Cu1 O26 H26B 114(6) . .
H26A O26 H26B 110(3) . .
Cu1 O27 H27A 105(6) . .
Cu1 O27 H27B 128(6) . .
H27A O27 H27B 109(4) . .
Cu1 O28 H28A 121(6) . .
Cu1 O28 H28B 118(6) . .
H28A O28 H28B 110(4) . .
Cu2 O29 H29A 124(7) . .
Cu2 O29 H29B 104(6) . .
H29A O29 H29B 111(4) . .
Cu2 O30 H30A 131(6) . .
Cu2 O30 H30B 106(6) . .
H30A O30 H30B 110(4) . .
Cu2 O31 H31A 121(7) . .
Cu2 O31 H31B 113(6) . .
H31A O31 H31B 108(3) . .
Cu3 O32 H32A 125(6) . .
Cu3 O32 H32B 121(6) . .
H32A O32 H32B 110(4) . .
Cu3 O33 H33A 108(6) . .
Cu3 O33 H33B 113(6) . .
H33A O33 H33B 110(4) . .
Cu3 O34 H34A 103(7) . .
Cu3 O34 H34B 97(7) . .
H34A O34 H34B 109(4) . .
Cu4 O35 H35A 116(6) . .
Cu4 O35 H35B 122(6) . .
H35A O35 H35B 109(4) . .
Cu4 O36 H36A 134(6) . .
Cu4 O36 H36B 102(6) . .
H36A O36 H36B 110(4) . .
Cu4 O37 H37A 125(7) . .
Cu4 O37 H37B 104(6) . .
H37A O37 H37B 110(4) . .
Cu5 O38 H38A 136(6) . .
Cu5 O38 H38B 107(6) . .
H38A O38 H38B 112(4) . .
Cu5 O39 H39A 118(6) . .
Cu5 O39 H39B 122(6) . .
H39A O39 H39B 109(4) . .
Cu5 O40 H40A 109(7) . .
Cu5 O40 H40B 100(7) . .
H40A O40 H40B 109(4) . .
H41A O41 H41B 110(4) . .
H43A O43 H43B 102(7) . .
H45A O45 H45B 110(4) . .
H46A O46 H46B 111(4) . .
H47A O47 H47B 109(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 2.214(6) .
Cu1 O25 1.959(6) .
Cu1 O26 1.957(6) .
Cu1 O27 1.955(6) .
Cu1 O28 1.953(7) .
Cu2 O2 1.920(6) .
Cu2 O10 1.959(7) 2
Cu2 O29 1.957(7) .
Cu2 O30 2.304(7) .
Cu2 O31 1.971(7) .
Cu3 O4 1.931(7) .
Cu3 O8 1.947(7) 2_565
Cu3 O32 1.946(6) .
Cu3 O33 1.997(6) .
Cu3 O34 2.343(7) .
Cu4 O13 1.972(6) .
Cu4 O21 1.917(6) 2_565
Cu4 O35 1.975(7) .
Cu4 O36 2.307(7) .
Cu4 O37 1.998(7) .
Cu5 O15 1.958(7) .
Cu5 O19 1.928(6) 2
Cu5 O38 1.953(6) .
Cu5 O39 1.969(6) .
Cu5 O40 2.339(7) .
C1 C2 1.389(12) .
C1 C6 1.398(13) .
C1 C7 1.506(13) .
C2 C3 1.406(13) .
C2 C8 1.508(13) .
C3 C4 1.402(13) .
C3 C9 1.524(12) .
C4 C5 1.385(13) .
C4 C10 1.500(13) .
C5 C6 1.375(13) .
C5 C11 1.537(13) .
C6 C12 1.523(12) .
C7 O1 1.230(11) .
C7 O2 1.281(10) .
C8 O3 1.235(11) .
C8 O4 1.253(11) .
C9 O5 1.258(10) .
C9 O6 1.239(10) .
C10 O7 1.217(11) .
C10 O8 1.299(11) .
C11 O9 1.234(11) .
C11 O10 1.268(10) .
C12 O11 1.212(11) .
C12 O12 1.292(11) .
O8 Cu3 1.947(7) 2_564
O10 Cu2 1.959(7) 2_554
O12 H12 0.840(14) .
C13 C14 1.407(13) .
C13 C18 1.399(13) .
C13 C19 1.487(13) .
C14 C15 1.399(13) .
C14 C20 1.500(13) .
C15 C16 1.372(13) .
C15 C21 1.518(12) .
C16 C17 1.396(12) .
C16 C22 1.497(13) .
C17 C18 1.409(13) .
C17 C23 1.518(13) .
C18 C24 1.486(12) .
C19 O13 1.276(10) .
C19 O14 1.247(11) .
C20 O15 1.264(11) .
C20 O16 1.238(11) .
C21 O17 1.246(11) .
C21 O18 1.271(11) .
C22 O19 1.280(10) .
C22 O20 1.236(11) .
C23 O21 1.274(11) .
C23 O22 1.225(11) .
C24 O23 1.237(11) .
C24 O24 1.280(11) .
O19 Cu5 1.927(6) 2_554
O21 Cu4 1.917(6) 2_564
O24 H24 0.841(14) .
O25 H25A 0.837(14) .
O25 H25B 0.837(14) .
O26 H26A 0.838(14) .
O26 H26B 0.839(14) .
O27 H27A 0.840(14) .
O27 H27B 0.841(14) .
O28 H28A 0.839(14) .
O28 H28B 0.839(14) .
O29 H29A 0.834(14) .
O29 H29B 0.836(14) .
O30 H30A 0.838(14) .
O30 H30B 0.837(14) .
O31 H31A 0.844(14) .
O31 H31B 0.843(14) .
O32 H32A 0.837(14) .
O32 H32B 0.838(14) .
O33 H33A 0.839(14) .
O33 H33B 0.839(14) .
O34 H34A 0.842(14) .
O34 H34B 0.841(14) .
O35 H35A 0.841(14) .
O35 H35B 0.841(14) .
O36 H36A 0.838(14) .
O36 H36B 0.835(14) .
O37 H37A 0.838(14) .
O37 H37B 0.839(14) .
O38 H38A 0.831(14) .
O38 H38B 0.833(14) .
O39 H39A 0.841(14) .
O39 H39B 0.842(14) .
O40 H40A 0.843(14) .
O40 H40B 0.839(14) .
O41 H41A 0.839(14) .
O41 H41B 0.840(14) .
O43 H43A 0.839(10) .
O43 H43B 0.93(9) .
O45 H45A 0.839(14) .
O45 H45B 0.839(14) .
O46 H46A 0.838(14) .
O46 H46B 0.835(14) .
O47 H47A 0.840(14) .
O47 H47B 0.841(14) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O12 H12 O5 0.840(14) 1.70(3) 2.527(8) 166(9) 1_545
O24 H24 O18 0.841(14) 1.70(4) 2.487(8) 155(9) 1_565
O25 H25A O41 0.837(14) 1.86(3) 2.680(9) 165(9) .
O25 H25B O45 0.837(14) 1.97(5) 2.749(8) 153(9) .
O26 H26A O3 0.838(14) 1.92(4) 2.711(9) 157(8) .
O26 H26B O14 0.839(14) 1.884(17) 2.719(8) 174(8) .
O27 H27A O46 0.840(14) 1.95(4) 2.740(9) 157(8) .
O27 H27B O20 0.841(14) 1.90(4) 2.710(9) 160(9) 2
O28 H28A O18 0.839(14) 1.99(2) 2.823(9) 169(8) .
O28 H28B O43 0.839(14) 1.99(5) 2.736(9) 147(8) 1_545
O29 H29A O46 0.834(14) 1.85(2) 2.680(9) 174(8) .
O29 H29B O3 0.836(14) 2.25(3) 3.066(10) 165(8) .
O30 H30A O15 0.838(14) 1.90(3) 2.720(9) 166(8) 4
O30 H30B O6 0.837(14) 1.98(3) 2.801(9) 166(9) 2_565
O31 H31A O13 0.844(14) 1.88(3) 2.699(9) 163(10) 4
O31 H31B O34 0.843(14) 1.90(3) 2.723(9) 164(8) 1_545
O32 H32A O30 0.837(14) 2.14(9) 2.704(10) 124(9) .
O32 H32B O44 0.838(14) 1.77(2) 2.597(12) 171(8) .
O33 H33A O9 0.839(14) 1.96(3) 2.776(9) 165(8) 2_565
O33 H33B O11 0.839(14) 1.95(3) 2.771(9) 167(9) 1_565
O34 H34A O17 0.842(14) 2.03(3) 2.840(9) 162(8) 4
O34 H34B O40 0.841(14) 2.03(4) 2.809(8) 154(9) 3
O35 H35A O16 0.841(14) 2.17(6) 2.902(9) 145(9) 1_565
O35 H35B O43 0.841(14) 1.98(3) 2.801(10) 164(8) .
O36 H36A O8 0.838(14) 2.00(5) 2.757(9) 150(9) 3_455
O36 H36B O17 0.835(14) 2.06(6) 2.691(10) 132(8) 1_565
O37 H37A O42 0.838(14) 1.80(4) 2.595(12) 158(9) 2_565
O37 H37B O10 0.839(14) 1.99(5) 2.734(9) 148(9) 3_455
O38 H38A O14 0.831(14) 2.28(6) 2.964(9) 140(8) .
O38 H38A O22 0.831(14) 2.46(7) 2.971(9) 120(6) 2_565
O38 H38B O23 0.833(14) 1.96(3) 2.781(9) 167(9) 2_565
O39 H39A O36 0.841(14) 1.85(3) 2.668(9) 163(8) 1_545
O39 H39B O6 0.842(14) 1.89(3) 2.698(9) 160(8) 3_445
O40 H40A O6 0.843(14) 1.93(3) 2.748(9) 163(10) 3_445
O40 H40B O37 0.839(14) 2.08(2) 2.907(10) 170(7) .
O40 H40B O42 0.839(14) 2.68(9) 3.166(10) 119(8) 2_565
O41 H41A O9 0.839(14) 2.07(6) 2.831(10) 151(10) .
O41 H41B O20 0.840(14) 2.03(2) 2.860(10) 168(9) .
O43 H43A O33 0.839(10) 2.28(5) 3.048(10) 153(10) .
O43 H43B O45 0.93(9) 1.87(8) 2.794(10) 170(9) .
O45 H45A O24 0.839(14) 1.97(2) 2.801(9) 170(9) .
O45 H45B O5 0.839(14) 1.95(2) 2.779(8) 172(10) .
O46 H46A O12 0.838(14) 2.64(9) 3.083(9) 115(8) 2
O46 H46A O41 0.838(14) 2.49(7) 2.996(10) 120(6) 2
O46 H46B O47 0.835(14) 1.88(4) 2.675(10) 158(8) 2_565
O47 H47A O22 0.840(14) 1.98(3) 2.782(10) 160(9) .
O47 H47B O7 0.841(14) 2.07(3) 2.894(10) 167(11) .
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
_geom_torsion_site_symmetry_4
C6 C1 C2 C3 -3.3(13) .
C6 C1 C2 C8 -179.5(8) .
C7 C1 C2 C3 176.0(8) .
C7 C1 C2 C8 -0.2(13) .
C1 C2 C3 C4 2.4(12) .
C1 C2 C3 C9 -176.7(8) .
C8 C2 C3 C4 178.7(8) .
C8 C2 C3 C9 -0.4(13) .
C2 C3 C4 C5 -0.5(13) .
C2 C3 C4 C10 177.0(8) .
C9 C3 C4 C5 178.6(8) .
C9 C3 C4 C10 -3.9(12) .
C3 C4 C5 C6 -0.7(13) .
C3 C4 C5 C11 -179.5(8) .
C10 C4 C5 C6 -178.2(8) .
C10 C4 C5 C11 3.0(12) .
C4 C5 C6 C1 -0.2(13) .
C4 C5 C6 C12 178.4(8) .
C11 C5 C6 C1 178.6(8) .
C11 C5 C6 C12 -2.8(13) .
C2 C1 C6 C5 2.2(13) .
C2 C1 C6 C12 -176.5(8) .
C7 C1 C6 C5 -177.1(8) .
C7 C1 C6 C12 4.3(12) .
C2 C1 C7 O1 107.6(10) .
C2 C1 C7 O2 -74.9(10) .
C6 C1 C7 O1 -73.1(12) .
C6 C1 C7 O2 104.4(9) .
C1 C2 C8 O3 -39.0(13) .
C1 C2 C8 O4 137.5(9) .
C3 C2 C8 O3 144.9(9) .
C3 C2 C8 O4 -38.7(12) .
C2 C3 C9 O5 -69.7(11) .
C2 C3 C9 O6 111.1(10) .
C4 C3 C9 O5 111.1(9) .
C4 C3 C9 O6 -68.0(11) .
C3 C4 C10 O7 -53.1(12) .
C3 C4 C10 O8 128.5(9) .
C5 C4 C10 O7 124.4(10) .
C5 C4 C10 O8 -54.0(11) .
C4 C5 C11 O9 -63.5(11) .
C4 C5 C11 O10 114.7(9) .
C6 C5 C11 O9 117.6(10) .
C6 C5 C11 O10 -64.2(11) .
C1 C6 C12 O11 -37.3(12) .
C1 C6 C12 O12 142.8(8) .
C5 C6 C12 O11 144.2(9) .
C5 C6 C12 O12 -35.8(12) .
C1 C7 O1 Cu1 -21.9(12) .
O2 C7 O1 Cu1 160.9(6) .
C1 C7 O2 Cu2 173.7(5) .
O1 C7 O2 Cu2 -8.8(12) .
C2 C8 O4 Cu3 -158.7(6) .
O3 C8 O4 Cu3 17.5(12) .
C4 C10 O8 Cu3 169.7(6) 2_564
O7 C10 O8 Cu3 -8.6(11) 2_564
C5 C11 O10 Cu2 -177.1(6) 2_554
O9 C11 O10 Cu2 0.9(11) 2_554
C18 C13 C14 C15 2.3(12) .
C18 C13 C14 C20 -178.5(8) .
C19 C13 C14 C15 -177.4(8) .
C19 C13 C14 C20 1.8(12) .
C13 C14 C15 C16 -2.6(13) .
C13 C14 C15 C21 -179.5(8) .
C20 C14 C15 C16 178.3(8) .
C20 C14 C15 C21 1.4(12) .
C14 C15 C16 C17 1.4(13) .
C14 C15 C16 C22 -177.0(8) .
C21 C15 C16 C17 178.4(8) .
C21 C15 C16 C22 -0.1(12) .
C15 C16 C17 C18 0.0(13) .
C15 C16 C17 C23 -176.1(8) .
C22 C16 C17 C18 178.5(8) .
C22 C16 C17 C23 2.4(12) .
C14 C13 C18 C17 -0.9(12) .
C14 C13 C18 C24 177.9(8) .
C19 C13 C18 C17 178.8(8) .
C19 C13 C18 C24 -2.4(13) .
C16 C17 C18 C13 -0.3(13) .
C16 C17 C18 C24 -179.1(8) .
C23 C17 C18 C13 175.9(8) .
C23 C17 C18 C24 -2.9(13) .
C14 C13 C19 O13 -118.3(9) .
C14 C13 C19 O14 61.0(12) .
C18 C13 C19 O13 62.0(12) .
C18 C13 C19 O14 -118.7(10) .
C13 C14 C20 O15 46.8(12) .
C13 C14 C20 O16 -132.4(9) .
C15 C14 C20 O15 -134.1(9) .
C15 C14 C20 O16 46.8(12) .
C14 C15 C21 O17 66.2(12) .
C14 C15 C21 O18 -116.2(10) .
C16 C15 C21 O17 -110.7(10) .
C16 C15 C21 O18 66.8(11) .
C15 C16 C22 O19 49.6(12) .
C15 C16 C22 O20 -130.3(9) .
C17 C16 C22 O19 -128.9(8) .
C17 C16 C22 O20 51.2(12) .
C16 C17 C23 O21 56.1(11) .
C16 C17 C23 O22 -125.1(9) .
C18 C17 C23 O21 -120.0(9) .
C18 C17 C23 O22 58.8(12) .
C13 C18 C24 O23 -127.6(10) .
C13 C18 C24 O24 51.1(12) .
C17 C18 C24 O23 51.2(12) .
C17 C18 C24 O24 -130.1(9) .
C13 C19 O13 Cu4 178.1(6) .
O14 C19 O13 Cu4 -1.2(11) .
C14 C20 O15 Cu5 -172.4(6) .
O16 C20 O15 Cu5 6.7(12) .
C16 C22 O19 Cu5 163.0(6) 2_554
O20 C22 O19 Cu5 -17.1(12) 2_554
C17 C23 O21 Cu4 176.6(5) 2_564
O22 C23 O21 Cu4 -2.2(12) 2_564
