#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/56/7035651.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_7035651
loop_
_publ_author_name
'Visinescu, Diana'
'Alexandru, Maria-Gabriela'
'Madalan, Augustin M.'
'Pichon, Céline'
'Duhayon, Carine'
'Sutter, Jean-Pascal'
'Andruh, Marius'
_publ_section_title
;
 Magneto-structural variety of new 3d-4f-4(5)d heterotrimetallic
 complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16713
_journal_page_last               16727
_journal_paper_doi               10.1039/c5dt01738f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C47.3 H44.65 Cu2 Ho Mo N12.65 O9.35'
_chemical_formula_weight         1327.85
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Photo-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-06-15 deposited with the CCDC.
2015-07-06 downloaded from the CCDC.
;
_cell_angle_alpha                105.814(7)
_cell_angle_beta                 92.659(7)
_cell_angle_gamma                116.095(7)
_cell_formula_units_Z            2
_cell_length_a                   11.3617(11)
_cell_length_b                   12.4459(11)
_cell_length_c                   21.2819(17)
_cell_measurement_reflns_used    14140
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      1.85
_cell_volume                     2551.8(5)
_computing_cell_refinement       X-Area
_computing_data_collection       X-Area
_computing_data_reduction        X-Area
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            16234
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.664
_exptl_absorpt_correction_T_max  0.5864
_exptl_absorpt_correction_T_min  0.5352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_description       prism
_exptl_crystal_F_000             1318
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.674
_refine_diff_density_min         -2.010
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     704
_refine_ls_number_reflns         8420
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0466P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1086
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5367
_reflns_number_total             8420
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt01738f2.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
'Adding full bibliography for 7035647--7035658.cif.'
_cod_original_cell_volume        2551.8(4)
_cod_original_formula_sum        'C47.30 H44.65 Cu2 Ho Mo N12.65 O9.35'
_cod_database_code               7035651
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelxl_version_number           2014-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5386(12) 0.4681(11) 0.9103(6) 0.078(4) Uani 1 1 d . . . . .
H1A H 0.4491 0.4003 0.9012 0.117 Uiso 1 1 calc R U . . .
H1B H 0.5931 0.4614 0.9433 0.117 Uiso 1 1 calc R U . . .
H1C H 0.5380 0.5477 0.9264 0.117 Uiso 1 1 calc R U . . .
C2 C 0.7203(9) 0.5502(8) 0.8534(5) 0.043(2) Uani 1 1 d . . . . .
C3 C 0.8143(11) 0.6129(10) 0.9096(6) 0.067(3) Uani 1 1 d . . . . .
H3 H 0.7945 0.5974 0.9492 0.080 Uiso 1 1 calc R U . . .
C4 C 0.9428(12) 0.7023(13) 0.9072(7) 0.090(4) Uani 1 1 d . . . . .
H4 H 1.0082 0.7474 0.9457 0.108 Uiso 1 1 calc R U . . .
C5 C 0.9725(11) 0.7233(12) 0.8485(7) 0.079(4) Uani 1 1 d . . . . .
H5 H 1.0582 0.7811 0.8471 0.094 Uiso 1 1 calc R U . . .
C6 C 0.8736(9) 0.6578(8) 0.7905(5) 0.051(2) Uani 1 1 d . . . . .
C7 C 0.7461(9) 0.5675(7) 0.7927(5) 0.042(2) Uani 1 1 d . . . . .
C8 C 0.9090(10) 0.6884(9) 0.7306(7) 0.064(3) Uani 1 1 d . . . . .
H8 H 0.9954 0.7519 0.7352 0.076 Uiso 1 1 calc R U . . .
C9 C 0.9035(15) 0.7031(16) 0.6248(9) 0.118(6) Uani 0.335 1 d . . P A 1
H9A H 0.9696 0.7900 0.6483 0.142 Uiso 0.335 1 calc R U P A 1
H9B H 0.9481 0.6593 0.6001 0.142 Uiso 0.335 1 calc R U P A 1
C10 C 0.801(3) 0.700(3) 0.579(2) 0.076(11) Uani 0.335 1 d . . P A 1
H10A H 0.8437 0.7625 0.5575 0.092 Uiso 0.335 1 calc R U P A 1
H10B H 0.7421 0.7227 0.6046 0.092 Uiso 0.335 1 calc R U P A 1
C11 C 0.7196(13) 0.5709(13) 0.5268(7) 0.079(4) Uani 0.335 1 d . . P A 1
H11A H 0.6571 0.5767 0.4969 0.095 Uiso 0.335 1 calc R U P A 1
H11B H 0.7794 0.5506 0.5008 0.095 Uiso 0.335 1 calc R U P A 1
C9A C 0.9035(15) 0.7031(16) 0.6248(9) 0.118(6) Uani 0.665 1 d . . P A 2
H9A1 H 0.8869 0.7747 0.6295 0.142 Uiso 0.665 1 calc R U P A 2
H9A2 H 0.9991 0.7365 0.6377 0.142 Uiso 0.665 1 calc R U P A 2
C10A C 0.866(2) 0.629(2) 0.5562(12) 0.094(7) Uani 0.665 1 d . . P A 2
H10C H 0.8898 0.5622 0.5503 0.112 Uiso 0.665 1 calc R U P A 2
H10D H 0.9168 0.6827 0.5313 0.112 Uiso 0.665 1 calc R U P A 2
C11A C 0.7196(13) 0.5709(13) 0.5268(7) 0.079(4) Uani 0.665 1 d . . P A 2
H11C H 0.6889 0.6338 0.5393 0.095 Uiso 0.665 1 calc R U P A 2
H11D H 0.7059 0.5399 0.4786 0.095 Uiso 0.665 1 calc R U P A 2
C12 C 0.5734(11) 0.3561(11) 0.5086(6) 0.061(3) Uani 1 1 d . . . . .
H12 H 0.5763 0.3521 0.4645 0.074 Uiso 1 1 calc R U . . .
C13 C 0.4919(10) 0.2403(10) 0.5195(5) 0.056(3) Uani 1 1 d . . . . .
C14 C 0.4387(13) 0.1281(13) 0.4632(7) 0.085(4) Uani 1 1 d . . . . .
H14 H 0.4581 0.1341 0.4219 0.102 Uiso 1 1 calc R U . . .
C15 C 0.3599(15) 0.0117(13) 0.4685(7) 0.095(4) Uani 1 1 d . . . . .
H15 H 0.3232 -0.0599 0.4308 0.114 Uiso 1 1 calc R U . . .
C16 C 0.3345(12) 0.0002(10) 0.5302(7) 0.073(3) Uani 1 1 d . . . . .
H16 H 0.2831 -0.0792 0.5341 0.088 Uiso 1 1 calc R U . . .
C17 C 0.3864(9) 0.1080(9) 0.5861(5) 0.049(2) Uani 1 1 d . . . . .
C18 C 0.4649(9) 0.2301(8) 0.5825(5) 0.044(2) Uani 1 1 d . . . . .
C19 C 0.2894(12) -0.0154(8) 0.6560(6) 0.079(4) Uani 1 1 d . . . . .
H19A H 0.2868 -0.0063 0.7021 0.119 Uiso 1 1 calc R U . . .
H19B H 0.2007 -0.0490 0.6316 0.119 Uiso 1 1 calc R U . . .
H19C H 0.3251 -0.0720 0.6384 0.119 Uiso 1 1 calc R U . . .
C20 C 0.7482(10) 0.2858(10) 0.6970(6) 0.066(3) Uani 1 1 d . . . . .
H20A H 0.7171 0.3029 0.6601 0.099 Uiso 1 1 calc R U . . .
H20B H 0.8340 0.3551 0.7202 0.099 Uiso 1 1 calc R U . . .
H20C H 0.7556 0.2095 0.6811 0.099 Uiso 1 1 calc R U . . .
C21 C 0.6879(9) 0.2452(8) 0.7983(5) 0.048(2) Uani 1 1 d . . . . .
C22 C 0.8120(11) 0.2508(11) 0.8158(6) 0.067(3) Uani 1 1 d . . . . .
H22 H 0.8780 0.2748 0.7907 0.080 Uiso 1 1 calc R U . . .
C23 C 0.8332(14) 0.2193(13) 0.8721(8) 0.089(4) Uani 1 1 d . . . . .
H23 H 0.9144 0.2227 0.8851 0.106 Uiso 1 1 calc R U . . .
C24 C 0.7334(13) 0.1832(11) 0.9080(7) 0.081(4) Uani 1 1 d . . . . .
H24 H 0.7486 0.1617 0.9450 0.097 Uiso 1 1 calc R U . . .
C25 C 0.6081(10) 0.1776(8) 0.8909(6) 0.055(3) Uani 1 1 d . . . . .
C26 C 0.5897(9) 0.2096(7) 0.8343(5) 0.046(2) Uani 1 1 d . . . . .
C27 C 0.5169(12) 0.1500(11) 0.9341(6) 0.079(4) Uani 1 1 d . . . . .
H27 H 0.5450 0.1365 0.9716 0.094 Uiso 1 1 calc R U . . .
C28 C 0.337(3) 0.139(3) 0.9893(13) 0.063(6) Uani 0.6 1 d . . P B 1
H28A H 0.3889 0.1285 1.0223 0.076 Uiso 0.6 1 calc R U P B 1
H28B H 0.3349 0.2184 1.0086 0.076 Uiso 0.6 1 calc R U P B 1
C29 C 0.198(2) 0.031(2) 0.9683(11) 0.071(6) Uani 0.6 1 d . . P B 1
H29A H 0.1668 0.0096 1.0071 0.085 Uiso 0.6 1 calc R U P B 1
H29B H 0.1988 -0.0425 0.9379 0.085 Uiso 0.6 1 calc R U P B 1
C30 C 0.1012(12) 0.0621(12) 0.9345(7) 0.080(4) Uani 0.6 1 d . . P B 1
H30A H 0.0111 -0.0061 0.9272 0.096 Uiso 0.6 1 calc R U P B 1
H30B H 0.1046 0.1385 0.9641 0.096 Uiso 0.6 1 calc R U P B 1
C28A C 0.315(6) 0.068(5) 0.968(2) 0.096(12) Uani 0.4 1 d . U P B 2
H28C H 0.2583 -0.0196 0.9413 0.115 Uiso 0.4 1 calc R U P B 2
H28D H 0.3688 0.0723 1.0061 0.115 Uiso 0.4 1 calc R U P B 2
C29A C 0.240(6) 0.132(5) 0.9873(19) 0.099(11) Uani 0.4 1 d . U P B 2
H29C H 0.2899 0.2192 0.9889 0.119 Uiso 0.4 1 calc R U P B 2
H29D H 0.2221 0.1313 1.0314 0.119 Uiso 0.4 1 calc R U P B 2
C30A C 0.1012(12) 0.0621(12) 0.9345(7) 0.080(4) Uani 0.4 1 d . . P B 2
H30C H 0.0565 -0.0276 0.9287 0.096 Uiso 0.4 1 calc R U P B 2
H30D H 0.0429 0.0971 0.9508 0.096 Uiso 0.4 1 calc R U P B 2
C31 C 0.0270(12) 0.0467(9) 0.8257(6) 0.062(3) Uani 1 1 d . . . . .
H31 H -0.0551 0.0039 0.8370 0.075 Uiso 1 1 calc R U . . .
C32 C 0.0225(9) 0.0657(9) 0.7621(6) 0.058(3) Uani 1 1 d . . . . .
C33 C -0.1027(11) 0.0154(12) 0.7234(8) 0.086(4) Uani 1 1 d . . . . .
H33 H -0.1782 -0.0321 0.7382 0.103 Uiso 1 1 calc R U . . .
C34 C -0.1172(12) 0.0344(12) 0.6637(8) 0.088(4) Uani 1 1 d . . . . .
H34 H -0.2010 -0.0063 0.6363 0.106 Uiso 1 1 calc R U . . .
C35 C -0.0068(11) 0.1144(11) 0.6442(6) 0.075(3) Uani 1 1 d . . . . .
H35 H -0.0179 0.1320 0.6053 0.090 Uiso 1 1 calc R U . . .
C36 C 0.1198(9) 0.1684(8) 0.6817(5) 0.050(2) Uani 1 1 d . . . . .
C37 C 0.1374(8) 0.1453(8) 0.7416(5) 0.044(2) Uani 1 1 d . . . . .
C38 C 0.2225(12) 0.3098(12) 0.6196(6) 0.082(4) Uani 1 1 d . . . . .
H38A H 0.3095 0.3648 0.6139 0.124 Uiso 1 1 calc R U . . .
H38B H 0.1721 0.2456 0.5778 0.124 Uiso 1 1 calc R U . . .
H38C H 0.1770 0.3582 0.6355 0.124 Uiso 1 1 calc R U . . .
C39 C 0.3023(9) -0.1453(8) 0.7783(5) 0.047(2) Uani 1 1 d . . . . .
C40 C 0.5097(9) -0.1120(9) 0.7242(5) 0.046(2) Uani 1 1 d . . . . .
C41 C 0.4916(10) -0.3430(8) 0.6845(5) 0.049(2) Uani 1 1 d . . . . .
C42 C 0.3882(9) -0.4376(9) 0.7715(5) 0.051(2) Uani 1 1 d . . . . .
C43 C 0.2769(10) -0.3190(9) 0.6569(6) 0.055(3) Uani 1 1 d . . . . .
C44 C 0.1838(10) -0.4056(9) 0.7474(6) 0.057(3) Uani 1 1 d . . . . .
C45 C 0.3706(10) -0.2326(11) 0.8581(7) 0.062(3) Uani 1 1 d . . . . .
C46 C 0.5871(10) -0.1873(9) 0.8134(6) 0.052(3) Uani 1 1 d . . . . .
Cu1 Cu 0.65651(11) 0.49868(10) 0.64909(6) 0.0445(3) Uani 1 1 d . . . . .
Cu2 Cu 0.30841(11) 0.13839(10) 0.84607(6) 0.0454(3) Uani 1 1 d . . . . .
Ho1 Ho 0.45766(4) 0.31085(4) 0.73988(2) 0.03416(13) Uani 1 1 d . . . . .
Mo1 Mo 0.38834(7) -0.27159(6) 0.75505(4) 0.0365(2) Uani 1 1 d . . . . .
N1 N 0.8376(8) 0.6399(8) 0.6730(5) 0.060(2) Uani 1 1 d . . . . .
N2 N 0.6428(9) 0.4642(9) 0.5520(5) 0.056(2) Uani 1 1 d . . . . .
N3 N 0.3995(10) 0.1412(9) 0.9280(5) 0.070(3) Uani 1 1 d . . . . .
N4 N 0.1301(8) 0.0814(7) 0.8685(5) 0.055(2) Uani 1 1 d . . . . .
N5 N 0.2574(8) -0.0780(7) 0.7912(4) 0.054(2) Uani 1 1 d . . . . .
N6 N 0.5691(7) -0.0329(7) 0.7037(4) 0.055(2) Uani 1 1 d . . . . .
N7 N 0.5405(9) -0.3858(8) 0.6490(5) 0.063(3) Uani 1 1 d . . . . .
N8 N 0.3904(8) -0.5255(7) 0.7758(4) 0.053(2) Uani 1 1 d . . . . .
N9 N 0.2191(10) -0.3432(11) 0.6047(5) 0.088(3) Uani 1 1 d . . . . .
N10 N 0.0760(9) -0.4788(9) 0.7424(6) 0.089(4) Uani 1 1 d . . . . .
N11 N 0.3564(12) -0.2110(13) 0.9129(6) 0.103(4) Uani 1 1 d . . . . .
N12 N 0.6930(10) -0.1432(10) 0.8439(6) 0.080(3) Uani 1 1 d . . . . .
O1 O 0.5912(6) 0.4604(5) 0.8509(3) 0.0481(16) Uani 1 1 d . . . . .
O2 O 0.6471(5) 0.4983(5) 0.7401(3) 0.0390(14) Uani 1 1 d . . . . .
O1W O 1.083(3) 0.648(3) 0.447(2) 0.44(2) Uani 1 1 d . . . . .
O3 O 0.5077(6) 0.3272(5) 0.6369(3) 0.0421(14) Uani 1 1 d . . . . .
O4 O 0.3732(6) 0.1066(5) 0.6496(3) 0.0513(16) Uani 1 1 d . . . . .
O5 O 0.6541(6) 0.2706(5) 0.7420(3) 0.0467(15) Uani 1 1 d . . . . .
O6 O 0.4710(5) 0.2018(5) 0.8123(3) 0.0446(16) Uani 1 1 d . . . . .
O7 O 0.2615(5) 0.1928(5) 0.7736(3) 0.0432(15) Uani 1 1 d . . . . .
O8 O 0.2361(6) 0.2507(6) 0.6677(4) 0.0559(18) Uani 1 1 d . . . . .
N21 N 0.219(3) 0.385(2) 0.9274(12) 0.109(7) Uani 0.65 1 d D . P C 1
C51 C 0.169(4) 0.442(3) 0.9211(17) 0.109(16) Uani 0.65 1 d D . P C 1
C52 C 0.109(2) 0.529(2) 0.9172(15) 0.120(9) Uani 0.65 1 d D . P C 1
H52A H 0.0139 0.4805 0.9054 0.180 Uiso 0.65 1 calc R U P C 1
H52B H 0.1427 0.5677 0.8841 0.180 Uiso 0.65 1 calc R U P C 1
H52C H 0.1343 0.5934 0.9597 0.180 Uiso 0.65 1 calc R U P C 1
O2W O 0.199(9) 0.468(7) 0.920(5) 0.26(6) Uani 0.35 1 d . . P D 2
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -1.6832 0.6857 '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 0.0060 '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 C1 H1A 109.5 . .
O1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
O1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 O1 122.8(9) . .
C3 C2 C7 122.7(9) . .
O1 C2 C7 114.5(8) . .
C2 C3 C4 118.7(11) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C5 C4 C3 120.5(11) . .
C5 C4 H4 119.7 . .
C3 C4 H4 119.7 . .
C4 C5 C6 120.1(11) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C7 C6 C5 119.3(10) . .
C7 C6 C8 123.1(9) . .
C5 C6 C8 117.6(9) . .
O2 C7 C2 117.7(8) . .
O2 C7 C6 123.7(8) . .
C2 C7 C6 118.6(9) . .
N1 C8 C6 128.4(9) . .
N1 C8 H8 115.8 . .
C6 C8 H8 115.8 . .
C10 C9 N1 108.3(17) . .
C10 C9 H9A 110.0 . .
N1 C9 H9A 110.0 . .
C10 C9 H9B 110.0 . .
N1 C9 H9B 110.0 . .
H9A C9 H9B 108.4 . .
C9 C10 C11 113(3) . .
C9 C10 H10A 109.1 . .
C11 C10 H10A 109.1 . .
C9 C10 H10B 109.1 . .
C11 C10 H10B 109.1 . .
H10A C10 H10B 107.8 . .
N2 C11 C10 116.0(15) . .
N2 C11 H11A 108.3 . .
C10 C11 H11A 108.3 . .
N2 C11 H11B 108.3 . .
C10 C11 H11B 108.3 . .
H11A C11 H11B 107.4 . .
H10C C10A H10D 107.5 . .
N2 C12 C13 127.6(11) . .
N2 C12 H12 116.2 . .
C13 C12 H12 116.2 . .
C18 C13 C12 124.1(10) . .
C18 C13 C14 119.0(10) . .
C12 C13 C14 116.9(11) . .
C15 C14 C13 121.4(12) . .
C15 C14 H14 119.3 . .
C13 C14 H14 119.3 . .
C14 C15 C16 120.1(12) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C15 C16 C17 119.6(11) . .
C15 C16 H16 120.2 . .
C17 C16 H16 120.2 . .
O4 C17 C16 124.2(9) . .
O4 C17 C18 113.6(8) . .
C16 C17 C18 122.1(10) . .
O3 C18 C17 118.5(8) . .
O3 C18 C13 123.7(8) . .
C17 C18 C13 117.8(9) . .
O4 C19 H19A 109.5 . .
O4 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
O4 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O5 C20 H20A 109.5 . .
O5 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
O5 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C26 C21 O5 115.1(7) . .
C26 C21 C22 121.7(9) . .
O5 C21 C22 123.2(9) . .
C23 C22 C21 118.2(11) . .
C23 C22 H22 120.9 . .
C21 C22 H22 120.9 . .
C24 C23 C22 119.6(11) . .
C24 C23 H23 120.2 . .
C22 C23 H23 120.2 . .
C23 C24 C25 122.7(11) . .
C23 C24 H24 118.7 . .
C25 C24 H24 118.7 . .
C26 C25 C27 125.2(9) . .
C26 C25 C24 116.4(10) . .
C27 C25 C24 118.2(10) . .
O6 C26 C21 117.7(8) . .
O6 C26 C25 120.8(9) . .
C21 C26 C25 121.4(8) . .
N3 C27 C25 127.9(10) . .
N3 C27 H27 116.0 . .
C25 C27 H27 116.0 . .
C29 C28 N3 108(2) . .
C29 C28 H28A 110.2 . .
N3 C28 H28A 110.2 . .
C29 C28 H28B 110.2 . .
N3 C28 H28B 110.2 . .
H28A C28 H28B 108.5 . .
C28 C29 C30 112(2) . .
C28 C29 H29A 109.2 . .
C30 C29 H29A 109.2 . .
C28 C29 H29B 109.2 . .
C30 C29 H29B 109.2 . .
H29A C29 H29B 107.9 . .
N4 C30 C29 113.9(11) . .
N4 C30 H30A 108.8 . .
C29 C30 H30A 108.8 . .
N4 C30 H30B 108.8 . .
C29 C30 H30B 108.8 . .
H30A C30 H30B 107.7 . .
C29A C28A N3 101(4) . .
C29A C28A H28C 111.5 . .
N3 C28A H28C 111.5 . .
C29A C28A H28D 111.5 . .
N3 C28A H28D 111.5 . .
H28C C28A H28D 109.3 . .
C28A C29A H29C 109.8 . .
C28A C29A H29D 109.8 . .
H29C C29A H29D 108.3 . .
N4 C31 C32 127.9(9) . .
N4 C31 H31 116.1 . .
C32 C31 H31 116.1 . .
C33 C32 C37 119.5(10) . .
C33 C32 C31 116.9(10) . .
C37 C32 C31 123.1(9) . .
C34 C33 C32 121.1(11) . .
C34 C33 H33 119.4 . .
C32 C33 H33 119.4 . .
C33 C34 C35 119.7(12) . .
C33 C34 H34 120.1 . .
C35 C34 H34 120.1 . .
C36 C35 C34 121.0(11) . .
C36 C35 H35 119.5 . .
C34 C35 H35 119.5 . .
O8 C36 C35 125.9(9) . .
O8 C36 C37 114.0(8) . .
C35 C36 C37 120.0(9) . .
O7 C37 C36 117.7(8) . .
O7 C37 C32 123.8(9) . .
C36 C37 C32 118.4(9) . .
O8 C38 H38A 109.5 . .
O8 C38 H38B 109.5 . .
H38A C38 H38B 109.5 . .
O8 C38 H38C 109.5 . .
H38A C38 H38C 109.5 . .
H38B C38 H38C 109.5 . .
N5 C39 Mo1 179.4(11) . .
N6 C40 Mo1 175.4(9) . .
N7 C41 Mo1 176.1(8) . .
N8 C42 Mo1 175.2(9) . .
N9 C43 Mo1 179.2(11) . .
N10 C44 Mo1 178.3(10) . .
N11 C45 Mo1 177.1(10) . .
N12 C46 Mo1 179.3(11) . .
O2 Cu1 N1 94.0(3) . .
O2 Cu1 N2 169.1(3) . .
N1 Cu1 N2 95.4(4) . .
O2 Cu1 O3 77.1(2) . .
N1 Cu1 O3 159.3(3) . .
N2 Cu1 O3 92.2(3) . .
O2 Cu1 N7 95.6(3) . 1_565
N1 Cu1 N7 98.0(3) . 1_565
N2 Cu1 N7 88.4(3) . 1_565
O3 Cu1 N7 101.4(3) . 1_565
O6 Cu2 N4 170.0(3) . .
O6 Cu2 N3 92.8(3) . .
N4 Cu2 N3 96.9(4) . .
O6 Cu2 O7 76.8(2) . .
N4 Cu2 O7 93.3(3) . .
N3 Cu2 O7 161.6(3) . .
O6 Cu2 N5 92.0(3) . .
N4 Cu2 N5 90.3(3) . .
N3 Cu2 N5 91.2(4) . .
O7 Cu2 N5 104.0(3) . .
O6 Cu2 Ho1 38.84(15) . .
N4 Cu2 Ho1 131.4(2) . .
N3 Cu2 Ho1 126.6(3) . .
O7 Cu2 Ho1 39.06(16) . .
N5 Cu2 Ho1 107.21(19) . .
O3 Ho1 O7 133.2(2) . .
O3 Ho1 O6 139.4(2) . .
O7 Ho1 O6 62.26(18) . .
O3 Ho1 O2 62.9(2) . .
O7 Ho1 O2 155.6(2) . .
O6 Ho1 O2 120.46(19) . .
O3 Ho1 N8 100.8(2) . 1_565
O7 Ho1 N8 82.2(2) . 1_565
O6 Ho1 N8 119.6(2) . 1_565
O2 Ho1 N8 75.9(2) . 1_565
O3 Ho1 O4 65.2(2) . .
O7 Ho1 O4 80.6(2) . .
O6 Ho1 O4 86.2(2) . .
O2 Ho1 O4 123.0(2) . .
N8 Ho1 O4 136.5(2) 1_565 .
O3 Ho1 O1 126.9(2) . .
O7 Ho1 O1 98.3(2) . .
O6 Ho1 O1 68.95(19) . .
O2 Ho1 O1 64.2(2) . .
N8 Ho1 O1 70.2(2) 1_565 .
O4 Ho1 O1 151.84(19) . .
O3 Ho1 O5 80.9(2) . .
O7 Ho1 O5 123.33(18) . .
O6 Ho1 O5 64.55(19) . .
O2 Ho1 O5 72.47(18) . .
N8 Ho1 O5 143.3(2) 1_565 .
O4 Ho1 O5 77.8(2) . .
O1 Ho1 O5 79.5(2) . .
O3 Ho1 O8 74.3(2) . .
O7 Ho1 O8 63.31(19) . .
O6 Ho1 O8 122.46(19) . .
O2 Ho1 O8 116.71(18) . .
N8 Ho1 O8 68.7(3) 1_565 .
O4 Ho1 O8 67.9(2) . .
O1 Ho1 O8 136.7(2) . .
O5 Ho1 O8 143.7(2) . .
O3 Ho1 Cu2 153.01(15) . .
O7 Ho1 Cu2 32.27(13) . .
O6 Ho1 Cu2 30.85(14) . .
O2 Ho1 Cu2 141.35(15) . .
N8 Ho1 Cu2 98.22(19) 1_565 .
O4 Ho1 Cu2 87.80(14) . .
O1 Ho1 Cu2 77.71(13) . .
O5 Ho1 Cu2 95.02(13) . .
O8 Ho1 Cu2 95.23(14) . .
C44 Mo1 C45 78.7(4) . .
C44 Mo1 C39 80.0(3) . .
C45 Mo1 C39 71.2(4) . .
C44 Mo1 C40 141.7(3) . .
C45 Mo1 C40 117.1(4) . .
C39 Mo1 C40 73.8(3) . .
C44 Mo1 C46 142.9(4) . .
C45 Mo1 C46 72.8(4) . .
C39 Mo1 C46 111.7(4) . .
C40 Mo1 C46 74.1(3) . .
C44 Mo1 C43 71.0(4) . .
C45 Mo1 C43 141.3(4) . .
C39 Mo1 C43 80.1(4) . .
C40 Mo1 C43 77.2(4) . .
C46 Mo1 C43 144.0(4) . .
C44 Mo1 C41 114.2(4) . .
C45 Mo1 C41 141.8(4) . .
C39 Mo1 C41 144.1(3) . .
C40 Mo1 C41 76.0(3) . .
C46 Mo1 C41 77.6(4) . .
C43 Mo1 C41 74.6(4) . .
C44 Mo1 C42 72.9(3) . .
C45 Mo1 C42 80.5(4) . .
C39 Mo1 C42 144.0(3) . .
C40 Mo1 C42 140.9(3) . .
C46 Mo1 C42 79.3(3) . .
C43 Mo1 C42 111.7(4) . .
C41 Mo1 C42 70.5(3) . .
C8 N1 C9 113.6(10) . .
C8 N1 Cu1 123.7(7) . .
C9 N1 Cu1 122.7(9) . .
C12 N2 C11 116.6(10) . .
C12 N2 Cu1 124.5(7) . .
C11 N2 Cu1 118.9(8) . .
C27 N3 C28A 112(2) . .
C27 N3 C28 115.7(14) . .
C27 N3 Cu2 122.9(8) . .
C28A N3 Cu2 117(2) . .
C28 N3 Cu2 121.4(13) . .
C31 N4 C30 114.7(9) . .
C31 N4 Cu2 121.6(8) . .
C30 N4 Cu2 123.4(7) . .
C39 N5 Cu2 144.1(8) . .
C41 N7 Cu1 136.9(8) . 1_545
C42 N8 Ho1 150.3(8) . 1_545
C2 O1 C1 118.6(8) . .
C2 O1 Ho1 117.2(5) . .
C1 O1 Ho1 123.8(6) . .
C7 O2 Cu1 126.5(5) . .
C7 O2 Ho1 121.3(5) . .
Cu1 O2 Ho1 109.5(3) . .
C18 O3 Cu1 124.9(5) . .
C18 O3 Ho1 123.7(5) . .
Cu1 O3 Ho1 109.8(3) . .
C17 O4 C19 115.9(7) . .
C17 O4 Ho1 118.4(5) . .
C19 O4 Ho1 124.7(6) . .
C21 O5 C20 115.2(7) . .
C21 O5 Ho1 115.7(5) . .
C20 O5 Ho1 128.6(5) . .
C26 O6 Cu2 127.9(5) . .
C26 O6 Ho1 120.6(5) . .
Cu2 O6 Ho1 110.3(2) . .
C37 O7 Cu2 123.2(5) . .
C37 O7 Ho1 126.6(5) . .
Cu2 O7 Ho1 108.7(2) . .
C36 O8 C38 116.8(7) . .
C36 O8 Ho1 117.6(5) . .
C38 O8 Ho1 125.0(6) . .
N21 C51 C52 175(4) . .
C51 C52 H52A 109.5 . .
C51 C52 H52B 109.5 . .
H52A C52 H52B 109.5 . .
C51 C52 H52C 109.5 . .
H52A C52 H52C 109.5 . .
H52B C52 H52C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.420(12) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.349(14) .
C2 O1 1.386(10) .
C2 C7 1.389(13) .
C3 C4 1.407(15) .
C3 H3 0.9300 .
C4 C5 1.373(17) .
C4 H4 0.9300 .
C5 C6 1.403(15) .
C5 H5 0.9300 .
C6 C7 1.403(12) .
C6 C8 1.452(15) .
C7 O2 1.329(10) .
C8 N1 1.265(14) .
C8 H8 0.9300 .
C9 C10 1.46(4) .
C9 N1 1.492(15) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 C11 1.52(4) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C11 N2 1.492(12) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C10A H10C 0.9700 .
C10A H10D 0.9700 .
C12 N2 1.268(13) .
C12 C13 1.420(14) .
C12 H12 0.9300 .
C13 C18 1.415(14) .
C13 C14 1.425(17) .
C14 C15 1.368(17) .
C14 H14 0.9300 .
C15 C16 1.389(18) .
C15 H15 0.9300 .
C16 C17 1.391(14) .
C16 H16 0.9300 .
C17 O4 1.371(11) .
C17 C18 1.410(12) .
C18 O3 1.307(11) .
C19 O4 1.443(10) .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C20 O5 1.453(11) .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C21 C26 1.364(13) .
C21 O5 1.396(11) .
C21 C22 1.408(12) .
C22 C23 1.400(16) .
C22 H22 0.9300 .
C23 C24 1.375(18) .
C23 H23 0.9300 .
C24 C25 1.419(14) .
C24 H24 0.9300 .
C25 C26 1.401(13) .
C25 C27 1.408(15) .
C26 O6 1.360(10) .
C27 N3 1.287(14) .
C27 H27 0.9300 .
C28 C29 1.50(4) .
C28 N3 1.51(3) .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C29 C30 1.53(3) .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C30 N4 1.513(14) .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
C28A C29A 1.40(7) .
C28A N3 1.48(5) .
C28A H28C 0.9700 .
C28A H28D 0.9700 .
C29A H29C 0.9700 .
C29A H29D 0.9700 .
C31 N4 1.278(13) .
C31 C32 1.439(15) .
C31 H31 0.9300 .
C32 C33 1.386(15) .
C32 C37 1.423(12) .
C33 C34 1.370(18) .
C33 H33 0.9300 .
C34 C35 1.382(15) .
C34 H34 0.9300 .
C35 C36 1.381(13) .
C35 H35 0.9300 .
C36 O8 1.377(10) .
C36 C37 1.405(13) .
C37 O7 1.326(10) .
C38 O8 1.451(11) .
C38 H38A 0.9600 .
C38 H38B 0.9600 .
C38 H38C 0.9600 .
C39 N5 1.141(10) .
C39 Mo1 2.155(9) .
C40 N6 1.137(11) .
C40 Mo1 2.160(9) .
C41 N7 1.114(11) .
C41 Mo1 2.185(11) .
C42 N8 1.133(10) .
C42 Mo1 2.187(9) .
C43 N9 1.155(13) .
C43 Mo1 2.177(12) .
C44 N10 1.138(11) .
C44 Mo1 2.149(10) .
C45 N11 1.159(14) .
C45 Mo1 2.153(13) .
C46 N12 1.151(12) .
C46 Mo1 2.164(11) .
Cu1 O2 1.946(6) .
Cu1 N1 1.954(9) .
Cu1 N2 1.977(9) .
Cu1 O3 1.991(6) .
Cu1 N7 2.340(8) 1_565
Cu2 O6 1.924(6) .
Cu2 N4 1.961(8) .
Cu2 N3 1.969(9) .
Cu2 O7 1.983(6) .
Cu2 N5 2.409(8) .
Cu2 Ho1 3.5196(11) .
Ho1 O3 2.328(6) .
Ho1 O7 2.341(5) .
Ho1 O6 2.354(5) .
Ho1 O2 2.377(5) .
Ho1 N8 2.427(7) 1_565
Ho1 O4 2.468(6) .
Ho1 O1 2.478(6) .
Ho1 O5 2.494(5) .
Ho1 O8 2.572(6) .
N7 Cu1 2.340(8) 1_545
N8 Ho1 2.427(7) 1_545
N21 C51 1.120(4) .
C51 C52 1.521(4) .
C52 H52A 0.9600 .
C52 H52B 0.9600 .
C52 H52C 0.9600 .
