# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_1
_database_code_depnum_ccdc_archive 'CCDC 1060172'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 Cu2 La Mo N12 O10'
_chemical_formula_weight         1286.86

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'
La La -0.2871 2.4523 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4503(6)
_cell_length_b                   12.4739(7)
_cell_length_c                   20.7387(12)
_cell_angle_alpha                94.775(4)
_cell_angle_beta                 102.112(4)
_cell_angle_gamma                115.971(4)
_cell_volume                     2551.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    28620
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.000

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_F_000             1282
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.950
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4121
_exptl_absorpt_correction_T_max  0.4863
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28620
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.290
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measured_fraction_theta_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             11954
_reflns_number_gt                8903
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0536P)²+2.5135P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11954
_refine_ls_number_parameters     667
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1254
_refine_ls_wR_factor_gt          0.1164
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.8669(8) 0.4417(8) 0.4202(4) 0.088(3) Uani 1 1 d . . . . .
H1A H 0.9496 0.4970 0.4117 0.131 Uiso 1 1 calc R U . . .
H1B H 0.8424 0.4852 0.4506 0.131 Uiso 1 1 calc R U . . .
H1C H 0.8791 0.3791 0.4398 0.131 Uiso 1 1 calc R U . . .
C2 C 0.6337(6) 0.3049(6) 0.3592(3) 0.0486(13) Uani 1 1 d . . . . .
C3 C 0.5866(7) 0.3037(7) 0.4151(4) 0.0667(19) Uani 1 1 d . . . . .
H3 H 0.6411 0.3599 0.4549 0.080 Uiso 1 1 calc R U . . .
C4 C 0.4556(8) 0.2165(9) 0.4110(4) 0.085(3) Uani 1 1 d . . . . .
H4 H 0.4218 0.2142 0.4482 0.103 Uiso 1 1 calc R U . . .
C5 C 0.3789(7) 0.1363(9) 0.3537(4) 0.079(2) Uani 1 1 d . . . . .
H5 H 0.2924 0.0778 0.3522 0.095 Uiso 1 1 calc R U . . .
C6 C 0.4229(6) 0.1365(6) 0.2960(3) 0.0508(14) Uani 1 1 d . . . . .
C7 C 0.5529(5) 0.2248(5) 0.2978(3) 0.0420(12) Uani 1 1 d . . . . .
C8 C 0.3347(6) 0.0432(6) 0.2378(4) 0.0600(17) Uani 1 1 d . . . . .
H8 H 0.2544 -0.0151 0.2436 0.072 Uiso 1 1 calc R U . . .
C9 C 0.2454(11) -0.0859(11) 0.1331(6) 0.132(5) Uani 0.57 1 d . . P A 1
H9A H 0.2772 -0.1461 0.1369 0.159 Uiso 0.57 1 calc R U P A 1
H9B H 0.1651 -0.1143 0.1491 0.159 Uiso 0.57 1 calc R U P A 1
C10 C 0.2075(13) -0.0842(14) 0.0666(8) 0.079(4) Uani 0.57 1 d . . P A 1
H10A H 0.1707 -0.0275 0.0622 0.094 Uiso 0.57 1 calc R U P A 1
H10B H 0.1351 -0.1644 0.0438 0.094 Uiso 0.57 1 calc R U P A 1
C11 C 0.3185(8) -0.0492(7) 0.0296(4) 0.076(2) Uani 0.57 1 d . . P A 1
H11A H 0.3665 -0.0963 0.0387 0.091 Uiso 0.57 1 calc R U P A 1
H11B H 0.2784 -0.0660 -0.0186 0.091 Uiso 0.57 1 calc R U P A 1
C9A C 0.2454(11) -0.0859(11) 0.1331(6) 0.132(5) Uani 0.43 1 d . . P A 2
H9A1 H 0.2221 -0.1510 0.1582 0.159 Uiso 0.43 1 calc R U P A 2
H9A2 H 0.1648 -0.0772 0.1165 0.159 Uiso 0.43 1 calc R U P A 2
C10A C 0.283(2) -0.1197(18) 0.0783(12) 0.095(7) Uani 0.43 1 d . . P A 2
H10C H 0.2088 -0.1981 0.0541 0.114 Uiso 0.43 1 calc R U P A 2
H10D H 0.3589 -0.1339 0.0967 0.114 Uiso 0.43 1 calc R U P A 2
C11A C 0.3185(8) -0.0492(7) 0.0296(4) 0.076(2) Uani 0.43 1 d . . P A 2
H11C H 0.2361 -0.0573 -0.0002 0.091 Uiso 0.43 1 calc R U P A 2
H11D H 0.3583 -0.0836 0.0027 0.091 Uiso 0.43 1 calc R U P A 2
C12 C 0.4312(7) 0.1477(7) 0.0090(3) 0.0617(19) Uani 1 1 d . . . . .
H12 H 0.3800 0.1080 -0.0349 0.074 Uiso 1 1 calc R U . . .
C13 C 0.5207(7) 0.2743(7) 0.0182(3) 0.0578(16) Uani 1 1 d . . . . .
C14 C 0.5085(9) 0.3262(10) -0.0396(4) 0.078(2) Uani 1 1 d . . . . .
H14 H 0.4446 0.2781 -0.0798 0.094 Uiso 1 1 calc R U . . .
C15 C 0.5896(11) 0.4457(10) -0.0364(4) 0.094(3) Uani 1 1 d . . . . .
H15 H 0.5800 0.4788 -0.0745 0.113 Uiso 1 1 calc R U . . .
C16 C 0.6868(9) 0.5196(8) 0.0224(4) 0.072(2) Uani 1 1 d . . . . .
H16 H 0.7432 0.6012 0.0239 0.087 Uiso 1 1 calc R U . . .
C17 C 0.6977(6) 0.4692(6) 0.0788(3) 0.0495(14) Uani 1 1 d . . . . .
C18 C 0.6169(6) 0.3460(6) 0.0775(3) 0.0456(13) Uani 1 1 d . . . . .
C19 C 0.8771(9) 0.6603(6) 0.1435(5) 0.082(2) Uani 1 1 d . . . . .
H19A H 0.9325 0.6975 0.1888 0.123 Uiso 1 1 calc R U . . .
H19B H 0.9333 0.6638 0.1145 0.123 Uiso 1 1 calc R U . . .
H19C H 0.8271 0.7030 0.1290 0.123 Uiso 1 1 calc R U . . .
C20 C 0.4682(6) 0.4181(7) 0.2050(4) 0.0671(19) Uani 1 1 d . . . . .
H20A H 0.4637 0.3638 0.1678 0.101 Uiso 1 1 calc R U . . .
H20B H 0.4063 0.3727 0.2292 0.101 Uiso 1 1 calc R U . . .
H20C H 0.4445 0.4776 0.1884 0.101 Uiso 1 1 calc R U . . .
C21 C 0.6242(6) 0.5616(6) 0.3062(3) 0.0531(15) Uani 1 1 d . . . . .
C22 C 0.5238(8) 0.5722(10) 0.3265(4) 0.084(3) Uani 1 1 d . . . . .
H22 H 0.4340 0.5234 0.3023 0.101 Uiso 1 1 calc R U . . .
C23 C 0.5577(10) 0.6577(12) 0.3844(5) 0.108(4) Uani 1 1 d . . . . .
H23 H 0.4898 0.6649 0.3993 0.129 Uiso 1 1 calc R U . . .
C24 C 0.6889(9) 0.7302(10) 0.4191(5) 0.090(3) Uani 1 1 d . . . . .
H24 H 0.7102 0.7882 0.4568 0.108 Uiso 1 1 calc R U . . .
C25 C 0.7925(7) 0.7185(7) 0.3987(4) 0.0621(17) Uani 1 1 d . . . . .
C26 C 0.7614(6) 0.6341(6) 0.3413(3) 0.0496(14) Uani 1 1 d . . . . .
C27 C 0.9276(8) 0.7929(8) 0.4415(4) 0.074(2) Uani 1 1 d . . . . .
H27 H 0.9364 0.8435 0.4797 0.089 Uiso 1 1 calc R U . . .
C28 C 1.1611(11) 0.8785(14) 0.4881(6) 0.154(7) Uani 0.6 1 d . . P B 1
H28A H 1.1390 0.9302 0.5153 0.185 Uiso 0.6 1 calc R U P B 1
H28B H 1.1822 0.8277 0.5164 0.185 Uiso 0.6 1 calc R U P B 1
C29 C 1.2744(13) 0.9509(13) 0.4716(7) 0.071(3) Uani 0.6 1 d . . P B 1
H29A H 1.3400 1.0082 0.5120 0.085 Uiso 0.6 1 calc R U P B 1
H29B H 1.2526 0.9976 0.4405 0.085 Uiso 0.6 1 calc R U P B 1
C30 C 1.3402(8) 0.8852(9) 0.4400(5) 0.091(3) Uani 0.6 1 d . . P B 1
H30A H 1.4225 0.9452 0.4321 0.109 Uiso 0.6 1 calc R U P B 1
H30B H 1.3651 0.8405 0.4715 0.109 Uiso 0.6 1 calc R U P B 1
C28A C 1.1611(11) 0.8785(14) 0.4881(6) 0.154(7) Uani 0.4 1 d . . P B 2
H28C H 1.1841 0.9617 0.4839 0.185 Uiso 0.4 1 calc R U P B 2
H28D H 1.1372 0.8680 0.5302 0.185 Uiso 0.4 1 calc R U P B 2
C29A C 1.265(2) 0.867(2) 0.4934(9) 0.069(5) Uani 0.4 1 d . . P B 2
H29C H 1.2426 0.7859 0.5014 0.083 Uiso 0.4 1 calc R U P B 2
H29D H 1.3302 0.9230 0.5343 0.083 Uiso 0.4 1 calc R U P B 2
C30A C 1.3402(8) 0.8852(9) 0.4400(5) 0.091(3) Uani 0.4 1 d . . P B 2
H30C H 1.3721 0.9682 0.4330 0.109 Uiso 0.4 1 calc R U P B 2
H30D H 1.4183 0.8722 0.4551 0.109 Uiso 0.4 1 calc R U P B 2
C31 C 1.3157(6) 0.7901(7) 0.3335(4) 0.0630(18) Uani 1 1 d . . . . .
H31 H 1.4077 0.8439 0.3456 0.076 Uiso 1 1 calc R U . . .
C32 C 1.2629(6) 0.7064(6) 0.2701(4) 0.0608(17) Uani 1 1 d . . . . .
C33 C 1.3550(7) 0.7188(9) 0.2323(5) 0.085(3) Uani 1 1 d . . . . .
H33 H 1.4426 0.7826 0.2472 0.102 Uiso 1 1 calc R U . . .
C34 C 1.3182(9) 0.6404(10) 0.1754(6) 0.094(3) Uani 1 1 d . . . . .
H34 H 1.3797 0.6522 0.1503 0.113 Uiso 1 1 calc R U . . .
C35 C 1.1869(8) 0.5387(8) 0.1521(5) 0.078(2) Uani 1 1 d . . . . .
H35 H 1.1628 0.4829 0.1129 0.093 Uiso 1 1 calc R U . . .
C36 C 1.0968(6) 0.5253(6) 0.1892(4) 0.0556(15) Uani 1 1 d . . . . .
C37 C 1.1305(6) 0.6104(6) 0.2472(3) 0.0481(13) Uani 1 1 d . . . . .
C38 C 0.9307(8) 0.3318(8) 0.1193(5) 0.086(3) Uani 1 1 d . . . . .
H38A H 0.8384 0.2724 0.1125 0.129 Uiso 1 1 calc R U . . .
H38B H 0.9415 0.3617 0.0787 0.129 Uiso 1 1 calc R U . . .
H38C H 0.9884 0.2951 0.1311 0.129 Uiso 1 1 calc R U . . .
C39 C 0.9849(5) 0.9171(5) 0.2723(3) 0.0459(13) Uani 1 1 d . . . . .
C40 C 0.7280(6) 0.8343(6) 0.2201(3) 0.0469(13) Uani 1 1 d . . . . .
C41 C 0.7168(6) 1.0341(6) 0.1840(3) 0.0468(13) Uani 1 1 d . . . . .
C42 C 0.9038(6) 1.2033(6) 0.2757(3) 0.0525(15) Uani 1 1 d . . . . .
C43 C 0.8863(6) 0.9659(6) 0.1510(3) 0.0514(14) Uani 1 1 d . . . . .
C44 C 1.0715(6) 1.1472(6) 0.2369(4) 0.0620(18) Uani 1 1 d . . . . .
C45 C 1.0063(7) 1.0876(8) 0.3538(4) 0.0656(19) Uani 1 1 d . . . . .
C46 C 0.7445(6) 0.9975(7) 0.3139(3) 0.0594(17) Uani 1 1 d . . . . .
Cu1 Cu 0.50351(6) 0.14679(6) 0.15173(3) 0.04141(16) Uani 1 1 d . . . . .
Cu2 Cu 1.05150(7) 0.71922(6) 0.35063(4) 0.04457(17) Uani 1 1 d . . . . .
La1 La 0.79996(3) 0.42939(3) 0.24249(2) 0.03493(9) Uani 1 1 d . . . . .
Mo1 Mo 0.88090(4) 1.02261(4) 0.25120(2) 0.03704(11) Uani 1 1 d . . . . .
N1 N 0.3503(5) 0.0289(5) 0.1797(3) 0.0607(14) Uani 1 1 d . . . . .
N2 N 0.4128(5) 0.0821(5) 0.0537(3) 0.0531(13) Uani 1 1 d . . . . .
N3 N 1.0377(7) 0.7975(7) 0.4327(3) 0.081(2) Uani 1 1 d . . . . .
N4 N 1.2508(5) 0.7988(5) 0.3750(3) 0.0579(14) Uani 1 1 d . . . . .
N5 N 1.0413(5) 0.8611(5) 0.2856(3) 0.0538(13) Uani 1 1 d . . . . .
N6 N 0.6496(5) 0.7348(5) 0.2031(3) 0.0646(15) Uani 1 1 d . . . . .
N7 N 0.6316(5) 1.0463(5) 0.1510(3) 0.0589(14) Uani 1 1 d . . . . .
N8 N 0.9127(6) 1.2987(5) 0.2857(3) 0.0641(16) Uani 1 1 d . . . . .
N9 N 0.8879(7) 0.9358(8) 0.0978(3) 0.081(2) Uani 1 1 d . . . . .
N10 N 1.1691(7) 1.2124(7) 0.2267(6) 0.107(3) Uani 1 1 d . . . . .
N11 N 1.0778(8) 1.1215(8) 0.4062(3) 0.094(3) Uani 1 1 d . . . . .
N12 N 0.6711(7) 0.9837(7) 0.3457(4) 0.087(2) Uani 1 1 d . . . . .
O1 O 0.7617(4) 0.3878(4) 0.3581(2) 0.0531(11) Uani 1 1 d . . . . .
O2 O 0.6013(4) 0.2369(3) 0.24474(19) 0.0410(8) Uani 1 1 d . . . . .
O1W O 0.869(2) 0.7960(19) -0.0435(11) 0.317(11) Uani 1 1 d . . . . .
O3 O 0.6343(4) 0.3036(4) 0.13391(19) 0.0438(9) Uani 1 1 d . . . . .
O2W O 0.7795(12) 0.5015(19) 0.5847(6) 0.351(14) Uani 1 1 d . . . . .
O4 O 0.7851(5) 0.5362(4) 0.1408(2) 0.0569(11) Uani 1 1 d . . . . .
O5 O 0.6038(4) 0.4788(4) 0.2493(2) 0.0508(10) Uani 1 1 d . . . . .
O6 O 0.8556(4) 0.6176(3) 0.3180(2) 0.0433(9) Uani 1 1 d . . . . .
O7 O 1.0364(4) 0.5950(4) 0.2789(2) 0.0473(9) Uani 1 1 d . . . . .
O8 O 0.9659(4) 0.4295(4) 0.1719(2) 0.0595(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.435(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.375(9) . ?
C2 O1 1.382(7) . ?
C2 C7 1.401(8) . ?
C3 C4 1.394(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.334(12) . ?
C4 H4 0.9300 . ?
C5 C6 1.392(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.402(8) . ?
C6 C8 1.435(9) . ?
C7 O2 1.323(7) . ?
C8 N1 1.263(9) . ?
C8 H8 0.9300 . ?
C9 C10 1.36(2) . ?
C9 N1 1.484(10) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.541(18) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.479(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C12 N2 1.278(9) . ?
C12 C13 1.425(11) . ?
C12 H12 0.9300 . ?
C13 C18 1.383(8) . ?
C13 C14 1.419(10) . ?
C14 C15 1.354(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.387(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.381(9) . ?
C16 H16 0.9300 . ?
C17 O4 1.378(7) . ?
C17 C18 1.399(9) . ?
C18 O3 1.336(7) . ?
C19 O4 1.429(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O5 1.443(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.357(9) . ?
C21 C26 1.408(9) . ?
C21 O5 1.408(8) . ?
C22 C23 1.401(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.356(13) . ?
C23 H23 0.9300 . ?
C24 C25 1.398(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.393(9) . ?
C25 C27 1.439(10) . ?
C26 O6 1.354(7) . ?
C27 N3 1.289(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.353(18) . ?
C28 N3 1.487(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.526(17) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N4 1.496(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C31 N4 1.276(10) . ?
C31 C32 1.438(10) . ?
C31 H31 0.9300 . ?
C32 C37 1.404(9) . ?
C32 C33 1.405(11) . ?
C33 C34 1.328(13) . ?
C33 H33 0.9300 . ?
C34 C35 1.423(12) . ?
C34 H34 0.9300 . ?
C35 C36 1.375(10) . ?
C35 H35 0.9300 . ?
C36 O8 1.392(8) . ?
C36 C37 1.399(9) . ?
C37 O7 1.329(7) . ?
C38 O8 1.414(9) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N5 1.155(7) . ?
C39 Mo1 2.143(6) . ?
C40 N6 1.135(8) . ?
C40 Mo1 2.161(6) . ?
C41 N7 1.145(7) . ?
C41 Mo1 2.160(6) . ?
C42 N8 1.146(8) . ?
C42 Mo1 2.155(7) . ?
C43 N9 1.142(9) . ?
C43 Mo1 2.161(7) . ?
C44 N10 1.134(9) . ?
C44 Mo1 2.155(7) . ?
C45 N11 1.131(9) . ?
C45 Mo1 2.158(7) . ?
C46 N12 1.140(9) . ?
C46 Mo1 2.172(7) . ?
Cu1 O2 1.967(4) . ?
Cu1 N1 1.971(5) . ?
Cu1 N2 1.992(5) . ?
Cu1 O3 1.998(4) . ?
Cu1 N7 2.311(5) 1_545 ?
Cu1 La1 3.6367(7) . ?
Cu2 O6 1.956(4) . ?
Cu2 N3 1.962(6) . ?
Cu2 N4 1.975(5) . ?
Cu2 O7 1.978(4) . ?
Cu2 N5 2.340(5) . ?
Cu2 La1 3.6353(8) . ?
La1 O6 2.456(4) . ?
La1 O3 2.478(4) . ?
La1 O7 2.480(4) . ?
La1 O2 2.494(4) . ?
La1 O1 2.580(4) . ?
La1 N8 2.593(6) 1_545 ?
La1 O4 2.602(5) . ?
La1 O5 2.603(4) . ?
La1 O8 2.631(4) . ?
N7 Cu1 2.311(5) 1_565 ?
N8 La1 2.593(6) 1_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 123.2(6) . . ?
C3 C2 C7 122.3(6) . . ?
O1 C2 C7 114.5(5) . . ?
C2 C3 C4 118.6(7) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 120.0(7) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 C6 122.7(7) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C7 119.0(6) . . ?
C5 C6 C8 118.4(6) . . ?
C7 C6 C8 122.6(6) . . ?
O2 C7 C2 119.1(5) . . ?
O2 C7 C6 123.6(5) . . ?
C2 C7 C6 117.3(5) . . ?
N1 C8 C6 129.4(6) . . ?
N1 C8 H8 115.3 . . ?
C6 C8 H8 115.3 . . ?
C10 C9 N1 118.5(12) . . ?
C10 C9 H9A 107.7 . . ?
N1 C9 H9A 107.7 . . ?
C10 C9 H9B 107.7 . . ?
N1 C9 H9B 107.7 . . ?
H9A C9 H9B 107.1 . . ?
C9 C10 C11 116.6(12) . . ?
C9 C10 H10A 108.2 . . ?
C11 C10 H10A 108.2 . . ?
C9 C10 H10B 108.2 . . ?
C11 C10 H10B 108.2 . . ?
H10A C10 H10B 107.3 . . ?
N2 C11 C10 108.2(7) . . ?
N2 C11 H11A 110.1 . . ?
C10 C11 H11A 110.1 . . ?
N2 C11 H11B 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
H10C C10A H10D 106.4 . . ?
N2 C12 C13 127.9(6) . . ?
N2 C12 H12 116.1 . . ?
C13 C12 H12 116.1 . . ?
C18 C13 C14 119.7(7) . . ?
C18 C13 C12 124.9(6) . . ?
C14 C13 C12 115.4(6) . . ?
C15 C14 C13 120.1(7) . . ?
C15 C14 H14 119.9 . . ?
C13 C14 H14 119.9 . . ?
C14 C15 C16 121.4(8) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C17 C16 C15 118.4(8) . . ?
C17 C16 H16 120.8 . . ?
C15 C16 H16 120.8 . . ?
O4 C17 C16 123.1(6) . . ?
O4 C17 C18 114.9(5) . . ?
C16 C17 C18 122.0(6) . . ?
O3 C18 C13 123.1(6) . . ?
O3 C18 C17 118.5(5) . . ?
C13 C18 C17 118.4(6) . . ?
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 . . ?
C22 C21 C26 122.2(7) . . ?
C22 C21 O5 124.6(6) . . ?
C26 C21 O5 113.2(5) . . ?
C21 C22 C23 119.0(8) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C22 120.5(8) . . ?
C24 C23 H23 119.8 . . ?
C22 C23 H23 119.8 . . ?
C23 C24 C25 120.7(8) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C26 C25 C24 119.9(7) . . ?
C26 C25 C27 123.4(6) . . ?
C24 C25 C27 116.6(7) . . ?
O6 C26 C25 123.6(6) . . ?
O6 C26 C21 118.7(6) . . ?
C25 C26 C21 117.7(6) . . ?
N3 C27 C25 127.4(7) . . ?
N3 C27 H27 116.3 . . ?
C25 C27 H27 116.3 . . ?
C29 C28 N3 118.2(11) . . ?
C29 C28 H28A 107.8 . . ?
N3 C28 H28A 107.8 . . ?
C29 C28 H28B 107.8 . . ?
N3 C28 H28B 107.8 . . ?
H28A C28 H28B 107.1 . . ?
C28 C29 C30 115.5(13) . . ?
C28 C29 H29A 108.4 . . ?
C30 C29 H29A 108.4 . . ?
C28 C29 H29B 108.4 . . ?
C30 C29 H29B 108.4 . . ?
H29A C29 H29B 107.5 . . ?
N4 C30 C29 113.4(7) . . ?
N4 C30 H30A 108.9 . . ?
C29 C30 H30A 108.9 . . ?
N4 C30 H30B 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
H29C C29A H29D 106.4 . . ?
N4 C31 C32 127.5(6) . . ?
N4 C31 H31 116.3 . . ?
C32 C31 H31 116.3 . . ?
C37 C32 C33 119.5(7) . . ?
C37 C32 C31 124.0(6) . . ?
C33 C32 C31 116.3(7) . . ?
C34 C33 C32 120.7(8) . . ?
C34 C33 H33 119.7 . . ?
C32 C33 H33 119.7 . . ?
C33 C34 C35 121.5(8) . . ?
C33 C34 H34 119.2 . . ?
C35 C34 H34 119.2 . . ?
C36 C35 C34 118.0(8) . . ?
C36 C35 H35 121.0 . . ?
C34 C35 H35 121.0 . . ?
C35 C36 O8 123.5(7) . . ?
C35 C36 C37 121.5(6) . . ?
O8 C36 C37 115.0(5) . . ?
O7 C37 C36 118.4(5) . . ?
O7 C37 C32 123.1(6) . . ?
C36 C37 C32 118.5(6) . . ?
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 178.0(6) . . ?
N6 C40 Mo1 178.4(6) . . ?
N7 C41 Mo1 176.0(5) . . ?
N8 C42 Mo1 176.7(6) . . ?
N9 C43 Mo1 179.3(6) . . ?
N10 C44 Mo1 177.2(8) . . ?
N11 C45 Mo1 176.0(7) . . ?
N12 C46 Mo1 178.7(7) . . ?
O2 Cu1 N1 92.3(2) . . ?
O2 Cu1 N2 170.7(2) . . ?
N1 Cu1 N2 94.2(2) . . ?
O2 Cu1 O3 80.22(16) . . ?
N1 Cu1 O3 160.3(2) . . ?
N2 Cu1 O3 91.4(2) . . ?
O2 Cu1 N7 93.67(18) . 1_545 ?
N1 Cu1 N7 101.2(2) . 1_545 ?
N2 Cu1 N7 91.5(2) . 1_545 ?
O3 Cu1 N7 97.48(19) . 1_545 ?
O2 Cu1 La1 40.54(11) . . ?
N1 Cu1 La1 132.16(17) . . ?
N2 Cu1 La1 131.64(17) . . ?
O3 Cu1 La1 40.35(11) . . ?
N7 Cu1 La1 91.62(14) 1_545 . ?
O6 Cu2 N3 92.2(2) . . ?
O6 Cu2 N4 170.3(2) . . ?
N3 Cu2 N4 96.2(3) . . ?
O6 Cu2 O7 78.52(15) . . ?
N3 Cu2 O7 162.3(3) . . ?
N4 Cu2 O7 92.1(2) . . ?
O6 Cu2 N5 91.11(17) . . ?
N3 Cu2 N5 96.5(3) . . ?
N4 Cu2 N5 92.6(2) . . ?
O7 Cu2 N5 98.7(2) . . ?
O6 Cu2 La1 39.29(11) . . ?
N3 Cu2 La1 126.7(2) . . ?
N4 Cu2 La1 131.07(17) . . ?
O7 Cu2 La1 40.25(11) . . ?
N5 Cu2 La1 103.14(13) . . ?
O6 La1 O3 137.14(13) . . ?
O6 La1 O7 60.58(12) . . ?
O3 La1 O7 136.18(13) . . ?
O6 La1 O2 118.89(12) . . ?
O3 La1 O2 61.83(13) . . ?
O7 La1 O2 157.18(13) . . ?
O6 La1 O1 68.94(14) . . ?
O3 La1 O1 123.42(13) . . ?
O7 La1 O1 99.97(13) . . ?
O2 La1 O1 62.15(12) . . ?
O6 La1 N8 117.90(16) . 1_545 ?
O3 La1 N8 104.40(16) . 1_545 ?
O7 La1 N8 82.84(16) . 1_545 ?
O2 La1 N8 77.91(16) . 1_545 ?
O1 La1 N8 70.76(19) . 1_545 ?
O6 La1 O4 89.16(14) . . ?
O3 La1 O4 62.00(13) . . ?
O7 La1 O4 83.08(14) . . ?
O2 La1 O4 119.49(13) . . ?
O1 La1 O4 151.91(15) . . ?
N8 La1 O4 137.03(19) 1_545 . ?
O6 La1 O5 62.15(12) . . ?
O3 La1 O5 80.43(13) . . ?
O7 La1 O5 119.57(13) . . ?
O2 La1 O5 72.03(13) . . ?
O1 La1 O5 75.88(14) . . ?
N8 La1 O5 142.70(18) 1_545 . ?
O4 La1 O5 78.39(14) . . ?
O6 La1 O8 119.47(13) . . ?
O3 La1 O8 80.09(13) . . ?
O7 La1 O8 61.62(13) . . ?
O2 La1 O8 121.25(13) . . ?
O1 La1 O8 138.28(15) . . ?
N8 La1 O8 70.00(19) 1_545 . ?
O4 La1 O8 67.57(16) . . ?
O5 La1 O8 145.70(15) . . ?
O6 La1 Cu2 30.28(8) . . ?
O3 La1 Cu2 152.33(9) . . ?
O7 La1 Cu2 31.03(9) . . ?
O2 La1 Cu2 140.75(9) . . ?
O1 La1 Cu2 79.43(9) . . ?
N8 La1 Cu2 97.73(13) 1_545 . ?
O4 La1 Cu2 90.46(10) . . ?
O5 La1 Cu2 92.01(9) . . ?
O8 La1 Cu2 92.31(10) . . ?
O6 La1 Cu1 138.78(8) . . ?
O3 La1 Cu1 31.47(9) . . ?
O7 La1 Cu1 160.30(9) . . ?
O2 La1 Cu1 30.83(9) . . ?
O1 La1 Cu1 92.97(9) . . ?
N8 La1 Cu1 87.55(13) 1_545 . ?
O4 La1 Cu1 92.48(10) . . ?
O5 La1 Cu1 77.88(9) . . ?
O8 La1 Cu1 98.93(10) . . ?
Cu2 La1 Cu1 168.668(18) . . ?
C39 Mo1 C44 81.8(2) . . ?
C39 Mo1 C42 141.9(2) . . ?
C44 Mo1 C42 72.9(3) . . ?
C39 Mo1 C45 70.8(3) . . ?
C44 Mo1 C45 79.2(3) . . ?
C42 Mo1 C45 76.7(3) . . ?
C39 Mo1 C41 145.9(2) . . ?
C44 Mo1 C41 110.4(3) . . ?
C42 Mo1 C41 71.3(2) . . ?
C45 Mo1 C41 141.4(2) . . ?
C39 Mo1 C40 74.0(2) . . ?
C44 Mo1 C40 141.2(3) . . ?
C42 Mo1 C40 141.4(2) . . ?
C45 Mo1 C40 118.9(3) . . ?
C41 Mo1 C40 77.7(2) . . ?
C39 Mo1 C43 79.9(2) . . ?
C44 Mo1 C43 71.3(3) . . ?
C42 Mo1 C43 116.6(3) . . ?
C45 Mo1 C43 140.9(2) . . ?
C41 Mo1 C43 74.7(2) . . ?
C40 Mo1 C43 74.9(2) . . ?
C39 Mo1 C46 110.7(3) . . ?
C44 Mo1 C46 144.0(3) . . ?
C42 Mo1 C46 77.8(3) . . ?
C45 Mo1 C46 74.0(3) . . ?
C41 Mo1 C46 78.7(3) . . ?
C40 Mo1 C46 74.1(2) . . ?
C43 Mo1 C46 142.6(2) . . ?
C8 N1 C9 115.2(7) . . ?
C8 N1 Cu1 123.5(5) . . ?
C9 N1 Cu1 121.3(6) . . ?
C12 N2 C11 116.5(6) . . ?
C12 N2 Cu1 123.8(5) . . ?
C11 N2 Cu1 119.6(5) . . ?
C27 N3 C28 114.6(7) . . ?
C27 N3 Cu2 124.6(5) . . ?
C28 N3 Cu2 120.5(6) . . ?
C31 N4 C30 113.3(6) . . ?
C31 N4 Cu2 122.3(5) . . ?
C30 N4 Cu2 124.1(5) . . ?
C39 N5 Cu2 142.7(5) . . ?
C41 N7 Cu1 142.7(5) . 1_565 ?
C42 N8 La1 142.6(5) . 1_565 ?
C2 O1 C1 118.7(5) . . ?
C2 O1 La1 117.6(3) . . ?
C1 O1 La1 123.6(4) . . ?
C7 O2 Cu1 127.0(3) . . ?
C7 O2 La1 120.8(3) . . ?
Cu1 O2 La1 108.64(16) . . ?
C18 O3 Cu1 125.5(3) . . ?
C18 O3 La1 124.4(4) . . ?
Cu1 O3 La1 108.18(16) . . ?
C17 O4 C19 116.9(6) . . ?
C17 O4 La1 120.1(4) . . ?
C19 O4 La1 122.5(4) . . ?
C21 O5 C20 115.3(5) . . ?
C21 O5 La1 117.8(3) . . ?
C20 O5 La1 126.5(4) . . ?
C26 O6 Cu2 126.4(4) . . ?
C26 O6 La1 122.2(4) . . ?
Cu2 O6 La1 110.43(16) . . ?
C37 O7 Cu2 124.5(4) . . ?
C37 O7 La1 125.6(4) . . ?
Cu2 O7 La1 108.73(16) . . ?
C36 O8 C38 118.0(5) . . ?
C36 O8 La1 119.3(4) . . ?
C38 O8 La1 122.6(4) . . ?

_refine_diff_density_max         0.815
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.102

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_2
_database_code_depnum_ccdc_archive 'CCDC 1060173'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 Ce Cu2 Mo N12 O10'
_chemical_formula_weight         1288.07

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'
Ce Ce -0.2486 2.6331 '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'
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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4758(10)
_cell_length_b                   12.4508(11)
_cell_length_c                   20.8054(17)
_cell_angle_alpha                94.748(7)
_cell_angle_beta                 102.203(7)
_cell_angle_gamma                116.332(6)
_cell_volume                     2550.7(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    22081
_cell_measurement_theta_min      2.17
_cell_measurement_theta_max      27.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_F_000             1284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    2.005
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7550
_exptl_absorpt_correction_T_max  0.8792
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22081
_diffrn_reflns_av_unetI/netI     0.1304
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.174
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measured_fraction_theta_full 0.912
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_Laue_measured_fraction_full 0.912
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_point_group_measured_fraction_full 0.912
_reflns_number_total             10111
_reflns_number_gt                5839
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0164P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         10111
_refine_ls_number_parameters     667
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.0805
_refine_ls_wR_factor_gt          0.0694
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_restrained_S_all      0.877
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.8693(8) 0.4453(8) 0.4201(3) 0.082(3) Uani 1 1 d . . . . .
H1A H 0.9527 0.4999 0.4118 0.123 Uiso 1 1 calc R U . . .
H1B H 0.8448 0.4903 0.4495 0.123 Uiso 1 1 calc R U . . .
H1C H 0.8803 0.3830 0.4408 0.123 Uiso 1 1 calc R U . . .
C2 C 0.6379(8) 0.3084(7) 0.3596(3) 0.050(2) Uani 1 1 d . . . . .
C3 C 0.5881(9) 0.3061(8) 0.4153(3) 0.067(3) Uani 1 1 d . . . . .
H3 H 0.6430 0.3622 0.4552 0.081 Uiso 1 1 calc R U . . .
C4 C 0.4601(10) 0.2223(10) 0.4115(4) 0.096(4) Uani 1 1 d . . . . .
H4 H 0.4289 0.2209 0.4494 0.116 Uiso 1 1 calc R U . . .
C5 C 0.3753(9) 0.1395(9) 0.3537(4) 0.078(3) Uani 1 1 d . . . . .
H5 H 0.2871 0.0838 0.3521 0.094 Uiso 1 1 calc R U . . .
C6 C 0.4233(8) 0.1396(6) 0.2958(3) 0.052(2) Uani 1 1 d . . . . .
C7 C 0.5530(7) 0.2268(6) 0.2978(3) 0.0402(17) Uani 1 1 d . . . . .
C8 C 0.3302(8) 0.0450(7) 0.2383(4) 0.066(3) Uani 1 1 d . . . . .
H8 H 0.2487 -0.0121 0.2440 0.079 Uiso 1 1 calc R U . . .
C9 C 0.2403(10) -0.0845(9) 0.1339(5) 0.117(5) Uani 0.58 1 d . . P A 1
H9A H 0.2693 -0.1465 0.1378 0.140 Uiso 0.58 1 calc R U P A 1
H9B H 0.1599 -0.1107 0.1496 0.140 Uiso 0.58 1 calc R U P A 1
C10 C 0.2038(16) -0.0807(17) 0.0652(10) 0.087(7) Uani 0.58 1 d . . P A 1
H10A H 0.1732 -0.0199 0.0610 0.105 Uiso 0.58 1 calc R U P A 1
H10B H 0.1281 -0.1594 0.0417 0.105 Uiso 0.58 1 calc R U P A 1
C11 C 0.3154(9) -0.0514(8) 0.0309(4) 0.076(3) Uani 0.58 1 d . . P A 1
H11A H 0.3613 -0.0993 0.0427 0.091 Uiso 0.58 1 calc R U P A 1
H11B H 0.2777 -0.0710 -0.0174 0.091 Uiso 0.58 1 calc R U P A 1
C9A C 0.2403(10) -0.0845(9) 0.1339(5) 0.117(5) Uani 0.42 1 d . . P A 2
H9A1 H 0.2144 -0.1486 0.1597 0.140 Uiso 0.42 1 calc R U P A 2
H9A2 H 0.1616 -0.0738 0.1165 0.140 Uiso 0.42 1 calc R U P A 2
C10A C 0.277(3) -0.1230(18) 0.0795(11) 0.091(9) Uani 0.42 1 d . . P A 2
H10C H 0.2014 -0.2013 0.0554 0.109 Uiso 0.42 1 calc R U P A 2
H10D H 0.3516 -0.1386 0.0984 0.109 Uiso 0.42 1 calc R U P A 2
C11A C 0.3154(9) -0.0514(8) 0.0309(4) 0.076(3) Uani 0.42 1 d . . P A 2
H11C H 0.2336 -0.0594 0.0010 0.091 Uiso 0.42 1 calc R U P A 2
H11D H 0.3541 -0.0874 0.0045 0.091 Uiso 0.42 1 calc R U P A 2
C12 C 0.4304(8) 0.1448(8) 0.0094(3) 0.057(2) Uani 1 1 d . . . . .
H12 H 0.3790 0.1035 -0.0343 0.069 Uiso 1 1 calc R U . . .
C13 C 0.5206(8) 0.2731(7) 0.0179(3) 0.050(2) Uani 1 1 d . . . . .
C14 C 0.5104(10) 0.3267(9) -0.0392(3) 0.072(3) Uani 1 1 d . . . . .
H14 H 0.4467 0.2783 -0.0794 0.087 Uiso 1 1 calc R U . . .
C15 C 0.5905(11) 0.4453(10) -0.0364(4) 0.081(3) Uani 1 1 d . . . . .
H15 H 0.5820 0.4783 -0.0746 0.097 Uiso 1 1 calc R U . . .
C16 C 0.6868(9) 0.5199(8) 0.0233(3) 0.066(2) Uani 1 1 d . . . . .
H16 H 0.7431 0.6022 0.0252 0.079 Uiso 1 1 calc R U . . .
C17 C 0.6974(8) 0.4704(7) 0.0794(3) 0.0479(19) Uani 1 1 d . . . . .
C18 C 0.6164(7) 0.3466(7) 0.0787(3) 0.0417(17) Uani 1 1 d . . . . .
C19 C 0.8767(9) 0.6647(7) 0.1442(4) 0.078(3) Uani 1 1 d . . . . .
H19A H 0.9324 0.7035 0.1894 0.117 Uiso 1 1 calc R U . . .
H19B H 0.9330 0.6686 0.1153 0.117 Uiso 1 1 calc R U . . .
H19C H 0.8257 0.7062 0.1293 0.117 Uiso 1 1 calc R U . . .
C20 C 0.4656(7) 0.4170(7) 0.2037(3) 0.059(2) Uani 1 1 d . . . . .
H20A H 0.4603 0.3633 0.1660 0.089 Uiso 1 1 calc R U . . .
H20B H 0.4035 0.3705 0.2275 0.089 Uiso 1 1 calc R U . . .
H20C H 0.4427 0.4775 0.1881 0.089 Uiso 1 1 calc R U . . .
C21 C 0.6208(8) 0.5574(7) 0.3047(3) 0.051(2) Uani 1 1 d . . . . .
C22 C 0.5195(8) 0.5638(9) 0.3262(4) 0.077(3) Uani 1 1 d . . . . .
H22 H 0.4294 0.5115 0.3030 0.092 Uiso 1 1 calc R U . . .
C23 C 0.5532(11) 0.6514(11) 0.3844(4) 0.100(4) Uani 1 1 d . . . . .
H23 H 0.4849 0.6571 0.3993 0.120 Uiso 1 1 calc R U . . .
C24 C 0.6858(10) 0.7273(9) 0.4187(4) 0.084(3) Uani 1 1 d . . . . .
H24 H 0.7071 0.7866 0.4557 0.101 Uiso 1 1 calc R U . . .
C25 C 0.7889(8) 0.7167(7) 0.3986(3) 0.059(2) Uani 1 1 d . . . . .
C26 C 0.7578(7) 0.6304(6) 0.3397(3) 0.0471(19) Uani 1 1 d . . . . .
C27 C 0.9255(9) 0.7945(8) 0.4399(4) 0.073(3) Uani 1 1 d . . . . .
H27 H 0.9345 0.8452 0.4781 0.087 Uiso 1 1 calc R U . . .
C28 C 1.1579(11) 0.8857(14) 0.4854(6) 0.134(6) Uani 0.49 1 d . . P B 1
H28A H 1.1358 0.9393 0.5110 0.161 Uiso 0.49 1 calc R U P B 1
H28B H 1.1764 0.8356 0.5150 0.161 Uiso 0.49 1 calc R U P B 1
C29 C 1.2680(19) 0.9532(15) 0.4725(8) 0.061(5) Uani 0.49 1 d . . P B 1
H29A H 1.3318 1.0093 0.5138 0.073 Uiso 0.49 1 calc R U P B 1
H29B H 1.2508 1.0019 0.4415 0.073 Uiso 0.49 1 calc R U P B 1
C30 C 1.3379(9) 0.8835(9) 0.4413(4) 0.087(3) Uani 0.49 1 d . . P B 1
H30A H 1.4218 0.9433 0.4345 0.105 Uiso 0.49 1 calc R U P B 1
H30B H 1.3596 0.8375 0.4728 0.105 Uiso 0.49 1 calc R U P B 1
C28A C 1.1579(11) 0.8857(14) 0.4854(6) 0.134(6) Uani 0.51 1 d . . P B 2
H28C H 1.1865 0.9684 0.4778 0.161 Uiso 0.51 1 calc R U P B 2
H28D H 1.1338 0.8830 0.5274 0.161 Uiso 0.51 1 calc R U P B 2
C29A C 1.261(2) 0.866(2) 0.4929(8) 0.082(6) Uani 0.51 1 d . . P B 2
H29C H 1.2297 0.7818 0.4985 0.098 Uiso 0.51 1 calc R U P B 2
H29D H 1.3253 0.9173 0.5351 0.098 Uiso 0.51 1 calc R U P B 2
C30A C 1.3379(9) 0.8835(9) 0.4413(4) 0.087(3) Uani 0.51 1 d . . P B 2
H30C H 1.3731 0.9674 0.4351 0.105 Uiso 0.51 1 calc R U P B 2
H30D H 1.4139 0.8682 0.4568 0.105 Uiso 0.51 1 calc R U P B 2
C31 C 1.3131(8) 0.7906(7) 0.3354(4) 0.057(2) Uani 1 1 d . . . . .
H31 H 1.4055 0.8444 0.3482 0.069 Uiso 1 1 calc R U . . .
C32 C 1.2607(7) 0.7073(7) 0.2710(4) 0.050(2) Uani 1 1 d . . . . .
C33 C 1.3545(9) 0.7195(8) 0.2339(4) 0.076(3) Uani 1 1 d . . . . .
H33 H 1.4426 0.7832 0.2494 0.092 Uiso 1 1 calc R U . . .
C34 C 1.3178(9) 0.6399(9) 0.1763(5) 0.086(3) Uani 1 1 d . . . . .
H34 H 1.3797 0.6501 0.1517 0.103 Uiso 1 1 calc R U . . .
C35 C 1.1857(8) 0.5414(8) 0.1533(4) 0.070(3) Uani 1 1 d . . . . .
H35 H 1.1601 0.4862 0.1136 0.084 Uiso 1 1 calc R U . . .
C36 C 1.0949(7) 0.5269(7) 0.1894(3) 0.050(2) Uani 1 1 d . . . . .
C37 C 1.1283(7) 0.6119(6) 0.2479(3) 0.0439(18) Uani 1 1 d . . . . .
C38 C 0.9270(9) 0.3299(7) 0.1188(4) 0.081(3) Uani 1 1 d . . . . .
H38A H 0.8337 0.2711 0.1111 0.122 Uiso 1 1 calc R U . . .
H38B H 0.9406 0.3588 0.0782 0.122 Uiso 1 1 calc R U . . .
H38C H 0.9829 0.2923 0.1321 0.122 Uiso 1 1 calc R U . . .
C39 C 0.9852(7) 0.9216(6) 0.2737(3) 0.0431(18) Uani 1 1 d . . . . .
C40 C 0.7285(8) 0.8364(7) 0.2203(3) 0.048(2) Uani 1 1 d . . . . .
C41 C 0.7142(7) 1.0338(6) 0.1845(3) 0.0440(18) Uani 1 1 d . . . . .
C42 C 0.9033(7) 1.2084(7) 0.2747(3) 0.052(2) Uani 1 1 d . . . . .
C43 C 0.8858(7) 0.9700(7) 0.1508(3) 0.052(2) Uani 1 1 d . . . . .
C44 C 1.0717(8) 1.1512(7) 0.2381(4) 0.065(2) Uani 1 1 d . . . . .
C45 C 1.0085(8) 1.0952(8) 0.3536(3) 0.061(2) Uani 1 1 d . . . . .
C46 C 0.7458(8) 0.9993(7) 0.3139(4) 0.059(2) Uani 1 1 d . . . . .
Cu1 Cu 0.50280(8) 0.14657(7) 0.15217(4) 0.0413(2) Uani 1 1 d . . . . .
Cu2 Cu 1.04905(8) 0.72133(7) 0.35028(4) 0.0417(2) Uani 1 1 d . . . . .
Ce1 Ce 0.79787(4) 0.43138(4) 0.24219(2) 0.03329(11) Uani 1 1 d . . . . .
Mo1 Mo 0.88113(6) 1.02636(5) 0.25156(3) 0.03657(16) Uani 1 1 d . . . . .
N1 N 0.3483(6) 0.0312(6) 0.1797(3) 0.0605(19) Uani 1 1 d . . . . .
N2 N 0.4128(6) 0.0820(5) 0.0539(3) 0.0509(17) Uani 1 1 d . . . . .
N3 N 1.0341(7) 0.8028(6) 0.4312(3) 0.068(2) Uani 1 1 d . . . . .
N4 N 1.2483(6) 0.7988(5) 0.3763(3) 0.0525(17) Uani 1 1 d . . . . .
N5 N 1.0393(6) 0.8654(5) 0.2865(3) 0.0493(16) Uani 1 1 d . . . . .
N6 N 0.6480(6) 0.7356(6) 0.2037(3) 0.0587(18) Uani 1 1 d . . . . .
N7 N 0.6287(6) 1.0437(6) 0.1522(3) 0.0595(19) Uani 1 1 d . . . . .
N8 N 0.9129(6) 1.3029(6) 0.2841(3) 0.0597(19) Uani 1 1 d . . . . .
N9 N 0.8871(8) 0.9380(8) 0.0978(3) 0.083(3) Uani 1 1 d . . . . .
N10 N 1.1674(9) 1.2158(8) 0.2270(5) 0.112(3) Uani 1 1 d . . . . .
N11 N 1.0801(8) 1.1323(8) 0.4064(3) 0.102(3) Uani 1 1 d . . . . .
N12 N 0.6717(8) 0.9873(7) 0.3459(3) 0.082(3) Uani 1 1 d . . . . .
O1 O 0.7650(5) 0.3896(4) 0.35802(19) 0.0513(14) Uani 1 1 d . . . . .
O2 O 0.6018(4) 0.2373(4) 0.24500(19) 0.0405(12) Uani 1 1 d . . . . .
O1W O 0.8647(19) 0.7920(13) -0.0455(8) 0.288(8) Uani 1 1 d . . . . .
O3 O 0.6344(4) 0.3043(4) 0.13472(19) 0.0449(12) Uani 1 1 d . . . . .
O2W O 0.7842(13) 0.5178(19) 0.5816(5) 0.396(14) Uani 1 1 d . . . . .
O4 O 0.7853(5) 0.5388(4) 0.1421(2) 0.0521(14) Uani 1 1 d . . . . .
O5 O 0.6010(4) 0.4765(4) 0.2477(2) 0.0461(12) Uani 1 1 d . . . . .
O6 O 0.8529(4) 0.6198(4) 0.31699(19) 0.0399(12) Uani 1 1 d . . . . .
O7 O 1.0335(4) 0.5964(4) 0.2786(2) 0.0406(12) Uani 1 1 d . . . . .
O8 O 0.9627(5) 0.4320(5) 0.1714(2) 0.0559(15) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.430(7) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.367(8) . ?
C2 C3 1.394(9) . ?
C2 C7 1.418(8) . ?
C3 C4 1.353(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.366(11) . ?
C4 H4 0.9300 . ?
C5 C6 1.426(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.389(9) . ?
C6 C8 1.438(9) . ?
C7 O2 1.325(7) . ?
C8 N1 1.290(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.41(2) . ?
C9 N1 1.486(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.516(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.494(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C12 N2 1.251(9) . ?
C12 C13 1.437(11) . ?
C12 H12 0.9300 . ?
C13 C18 1.406(8) . ?
C13 C14 1.418(11) . ?
C14 C15 1.338(12) . ?
C14 H14 0.9300 . ?
C15 C16 1.396(11) . ?
C15 H15 0.9300 . ?
C16 C17 1.371(10) . ?
C16 H16 0.9300 . ?
C17 O4 1.394(7) . ?
C17 C18 1.400(10) . ?
C18 O3 1.332(7) . ?
C19 O4 1.439(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O5 1.438(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.361(10) . ?
C21 O5 1.399(7) . ?
C21 C26 1.403(10) . ?
C22 C23 1.419(10) . ?
C22 H22 0.9300 . ?
C23 C24 1.368(12) . ?
C23 H23 0.9300 . ?
C24 C25 1.389(10) . ?
C24 H24 0.9300 . ?
C25 C26 1.429(8) . ?
C25 C27 1.442(11) . ?
C26 O6 1.330(8) . ?
C27 N3 1.258(9) . ?
C27 H27 0.9300 . ?
C28 C29 1.270(19) . ?
C28 N3 1.478(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.60(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N4 1.488(8) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C31 N4 1.269(9) . ?
C31 C32 1.452(9) . ?
C31 H31 0.9300 . ?
C32 C37 1.395(9) . ?
C32 C33 1.416(10) . ?
C33 C34 1.347(10) . ?
C33 H33 0.9300 . ?
C34 C35 1.407(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.367(10) . ?
C35 H35 0.9300 . ?
C36 O8 1.391(8) . ?
C36 C37 1.406(8) . ?
C37 O7 1.326(7) . ?
C38 O8 1.449(7) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N5 1.136(8) . ?
C39 Mo1 2.143(8) . ?
C40 N6 1.146(8) . ?
C40 Mo1 2.162(8) . ?
C41 N7 1.129(8) . ?
C41 Mo1 2.161(7) . ?
C42 N8 1.128(8) . ?
C42 Mo1 2.165(7) . ?
C43 N9 1.148(8) . ?
C43 Mo1 2.174(7) . ?
C44 N10 1.123(10) . ?
C44 Mo1 2.143(9) . ?
C45 N11 1.136(8) . ?
C45 Mo1 2.158(7) . ?
C46 N12 1.154(9) . ?
C46 Mo1 2.160(8) . ?
Cu1 N1 1.960(6) . ?
Cu1 O2 1.967(3) . ?
Cu1 O3 1.997(5) . ?
Cu1 N2 1.999(5) . ?
Cu1 N7 2.318(6) 1_545 ?
Cu2 O6 1.953(4) . ?
Cu2 N3 1.971(6) . ?
Cu2 N4 1.971(6) . ?
Cu2 O7 1.983(4) . ?
Cu2 N5 2.345(7) . ?
Ce1 O6 2.447(4) . ?
Ce1 O3 2.456(4) . ?
Ce1 O7 2.461(4) . ?
Ce1 O2 2.482(4) . ?
Ce1 O1 2.576(4) . ?
Ce1 O4 2.579(5) . ?
Ce1 O5 2.580(4) . ?
Ce1 N8 2.584(7) 1_545 ?
Ce1 O8 2.630(5) . ?
N7 Cu1 2.318(6) 1_565 ?
N8 Ce1 2.584(7) 1_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
O1 C2 C3 124.7(6) . . ?
O1 C2 C7 115.0(6) . . ?
C3 C2 C7 120.3(7) . . ?
C4 C3 C2 120.1(7) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C4 C5 121.9(8) . . ?
C3 C4 H4 119.0 . . ?
C5 C4 H4 119.0 . . ?
C4 C5 C6 119.3(8) . . ?
C4 C5 H5 120.3 . . ?
C6 C5 H5 120.3 . . ?
C7 C6 C5 119.9(6) . . ?
C7 C6 C8 124.4(6) . . ?
C5 C6 C8 115.7(7) . . ?
O2 C7 C6 123.4(5) . . ?
O2 C7 C2 118.3(6) . . ?
C6 C7 C2 118.4(6) . . ?
N1 C8 C6 126.6(7) . . ?
N1 C8 H8 116.7 . . ?
C6 C8 H8 116.7 . . ?
C10 C9 N1 116.8(11) . . ?
C10 C9 H9A 108.1 . . ?
N1 C9 H9A 108.1 . . ?
C10 C9 H9B 108.1 . . ?
N1 C9 H9B 108.1 . . ?
H9A C9 H9B 107.3 . . ?
C9 C10 C11 115.2(14) . . ?
C9 C10 H10A 108.5 . . ?
C11 C10 H10A 108.5 . . ?
C9 C10 H10B 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
N2 C11 C10 107.9(8) . . ?
N2 C11 H11A 110.1 . . ?
C10 C11 H11A 110.1 . . ?
N2 C11 H11B 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
H10C C10A H10D 106.6 . . ?
N2 C12 C13 127.7(6) . . ?
N2 C12 H12 116.2 . . ?
C13 C12 H12 116.2 . . ?
C18 C13 C14 119.2(7) . . ?
C18 C13 C12 123.9(7) . . ?
C14 C13 C12 117.0(7) . . ?
C15 C14 C13 121.4(7) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 120.4(8) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 119.2(8) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
C16 C17 O4 123.3(7) . . ?
C16 C17 C18 122.4(7) . . ?
O4 C17 C18 114.2(6) . . ?
O3 C18 C17 119.1(5) . . ?
O3 C18 C13 123.5(7) . . ?
C17 C18 C13 117.4(6) . . ?
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 . . ?
C22 C21 O5 124.6(7) . . ?
C22 C21 C26 122.4(6) . . ?
O5 C21 C26 112.9(6) . . ?
C21 C22 C23 119.1(8) . . ?
C21 C22 H22 120.5 . . ?
C23 C22 H22 120.5 . . ?
C24 C23 C22 120.3(8) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.6(7) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C25 C26 120.2(7) . . ?
C24 C25 C27 117.3(6) . . ?
C26 C25 C27 122.5(7) . . ?
O6 C26 C21 120.1(5) . . ?
O6 C26 C25 122.6(6) . . ?
C21 C26 C25 117.3(7) . . ?
N3 C27 C25 128.6(6) . . ?
N3 C27 H27 115.7 . . ?
C25 C27 H27 115.7 . . ?
C29 C28 N3 121.3(13) . . ?
C29 C28 H28A 107.0 . . ?
N3 C28 H28A 107.0 . . ?
C29 C28 H28B 107.0 . . ?
N3 C28 H28B 107.0 . . ?
H28A C28 H28B 106.7 . . ?
C28 C29 C30 116.0(16) . . ?
C28 C29 H29A 108.3 . . ?
C30 C29 H29A 108.3 . . ?
C28 C29 H29B 108.3 . . ?
C30 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
N4 C30 C29 111.8(8) . . ?
N4 C30 H30A 109.3 . . ?
C29 C30 H30A 109.3 . . ?
N4 C30 H30B 109.3 . . ?
C29 C30 H30B 109.3 . . ?
H30A C30 H30B 107.9 . . ?
H29C C29A H29D 106.7 . . ?
N4 C31 C32 127.9(7) . . ?
N4 C31 H31 116.1 . . ?
C32 C31 H31 116.1 . . ?
C37 C32 C33 119.8(6) . . ?
C37 C32 C31 123.3(7) . . ?
C33 C32 C31 116.7(6) . . ?
C34 C33 C32 120.9(8) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 119.9(8) . . ?
C33 C34 H34 120.1 . . ?
C35 C34 H34 120.1 . . ?
C36 C35 C34 119.9(7) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 O8 124.2(6) . . ?
C35 C36 C37 121.5(7) . . ?
O8 C36 C37 114.2(6) . . ?
O7 C37 C32 123.5(6) . . ?
O7 C37 C36 118.6(6) . . ?
C32 C37 C36 117.9(7) . . ?
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 178.6(7) . . ?
N6 C40 Mo1 179.7(7) . . ?
N7 C41 Mo1 175.8(6) . . ?
N8 C42 Mo1 177.3(7) . . ?
N9 C43 Mo1 178.7(8) . . ?
N10 C44 Mo1 175.7(10) . . ?
N11 C45 Mo1 177.1(7) . . ?
N12 C46 Mo1 177.4(8) . . ?
N1 Cu1 O2 92.3(2) . . ?
N1 Cu1 O3 159.1(2) . . ?
O2 Cu1 O3 80.08(17) . . ?
N1 Cu1 N2 94.7(2) . . ?
O2 Cu1 N2 170.4(2) . . ?
O3 Cu1 N2 91.1(2) . . ?
N1 Cu1 N7 101.7(3) . 1_545 ?
O2 Cu1 N7 93.38(19) . 1_545 ?
O3 Cu1 N7 98.2(2) . 1_545 ?
N2 Cu1 N7 91.6(2) . 1_545 ?
O6 Cu2 N3 92.0(2) . . ?
O6 Cu2 N4 169.9(2) . . ?
N3 Cu2 N4 96.4(3) . . ?
O6 Cu2 O7 78.58(16) . . ?
N3 Cu2 O7 163.3(3) . . ?
N4 Cu2 O7 91.9(2) . . ?
O6 Cu2 N5 90.7(2) . . ?
N3 Cu2 N5 94.4(3) . . ?
N4 Cu2 N5 94.1(2) . . ?
O7 Cu2 N5 99.43(19) . . ?
O6 Ce1 O3 137.47(16) . . ?
O6 Ce1 O7 61.04(14) . . ?
O3 Ce1 O7 136.07(15) . . ?
O6 Ce1 O2 119.04(14) . . ?
O3 Ce1 O2 62.19(14) . . ?
O7 Ce1 O2 156.19(15) . . ?
O6 Ce1 O1 69.27(15) . . ?
O3 Ce1 O1 124.23(15) . . ?
O7 Ce1 O1 98.98(14) . . ?
O2 Ce1 O1 62.44(13) . . ?
O6 Ce1 O4 88.74(14) . . ?
O3 Ce1 O4 62.73(15) . . ?
O7 Ce1 O4 82.83(15) . . ?
O2 Ce1 O4 120.62(14) . . ?
O1 Ce1 O4 152.95(16) . . ?
O6 Ce1 O5 62.71(13) . . ?
O3 Ce1 O5 80.28(14) . . ?
O7 Ce1 O5 120.69(14) . . ?
O2 Ce1 O5 72.04(15) . . ?
O1 Ce1 O5 77.30(16) . . ?
O4 Ce1 O5 78.66(16) . . ?
O6 Ce1 N8 118.32(16) . 1_545 ?
O3 Ce1 N8 103.77(17) . 1_545 ?
O7 Ce1 N8 81.85(18) . 1_545 ?
O2 Ce1 N8 77.90(18) . 1_545 ?
O1 Ce1 N8 70.48(19) . 1_545 ?
O4 Ce1 N8 136.01(18) . 1_545 ?
O5 Ce1 N8 143.41(19) . 1_545 ?
O6 Ce1 O8 119.71(15) . . ?
O3 Ce1 O8 79.41(14) . . ?
O7 Ce1 O8 61.67(13) . . ?
O2 Ce1 O8 120.83(14) . . ?
O1 Ce1 O8 137.26(17) . . ?
O4 Ce1 O8 67.13(17) . . ?
O5 Ce1 O8 145.36(16) . . ?
N8 Ce1 O8 69.3(2) 1_545 . ?
C39 Mo1 C44 81.7(3) . . ?
C39 Mo1 C45 70.8(3) . . ?
C44 Mo1 C45 78.2(3) . . ?
C39 Mo1 C46 109.7(3) . . ?
C44 Mo1 C46 144.1(3) . . ?
C45 Mo1 C46 74.2(3) . . ?
C39 Mo1 C41 145.7(2) . . ?
C44 Mo1 C41 111.7(3) . . ?
C45 Mo1 C41 141.3(3) . . ?
C46 Mo1 C41 78.5(3) . . ?
C39 Mo1 C40 73.9(3) . . ?
C44 Mo1 C40 140.9(3) . . ?
C45 Mo1 C40 119.8(3) . . ?
C46 Mo1 C40 74.0(3) . . ?
C41 Mo1 C40 76.9(3) . . ?
C39 Mo1 C42 142.2(2) . . ?
C44 Mo1 C42 73.0(3) . . ?
C45 Mo1 C42 76.7(3) . . ?
C46 Mo1 C42 78.6(3) . . ?
C41 Mo1 C42 71.4(2) . . ?
C40 Mo1 C42 141.5(3) . . ?
C39 Mo1 C43 80.9(3) . . ?
C44 Mo1 C43 71.4(3) . . ?
C45 Mo1 C43 141.0(3) . . ?
C46 Mo1 C43 142.5(3) . . ?
C41 Mo1 C43 74.4(3) . . ?
C40 Mo1 C43 74.9(3) . . ?
C42 Mo1 C43 115.6(3) . . ?
C8 N1 C9 113.1(7) . . ?
C8 N1 Cu1 124.8(5) . . ?
C9 N1 Cu1 122.1(5) . . ?
C12 N2 C11 116.7(6) . . ?
C12 N2 Cu1 125.2(5) . . ?
C11 N2 Cu1 118.1(6) . . ?
C27 N3 C28 115.4(7) . . ?
C27 N3 Cu2 124.9(5) . . ?
C28 N3 Cu2 119.6(6) . . ?
C31 N4 C30 113.0(6) . . ?
C31 N4 Cu2 122.1(5) . . ?
C30 N4 Cu2 124.5(5) . . ?
C39 N5 Cu2 143.5(6) . . ?
C41 N7 Cu1 142.6(5) . 1_565 ?
C42 N8 Ce1 142.4(6) . 1_565 ?
C2 O1 C1 118.2(5) . . ?
C2 O1 Ce1 117.0(3) . . ?
C1 O1 Ce1 124.9(4) . . ?
C7 O2 Cu1 127.0(4) . . ?
C7 O2 Ce1 120.3(3) . . ?
Cu1 O2 Ce1 108.41(19) . . ?
C18 O3 Cu1 125.2(4) . . ?
C18 O3 Ce1 124.2(4) . . ?
Cu1 O3 Ce1 108.42(19) . . ?
C17 O4 C19 116.1(6) . . ?
C17 O4 Ce1 119.7(4) . . ?
C19 O4 Ce1 123.7(4) . . ?
C21 O5 C20 114.5(5) . . ?
C21 O5 Ce1 117.0(4) . . ?
C20 O5 Ce1 128.0(4) . . ?
C26 O6 Cu2 128.1(4) . . ?
C26 O6 Ce1 120.3(4) . . ?
Cu2 O6 Ce1 110.07(18) . . ?
C37 O7 Cu2 124.4(4) . . ?
C37 O7 Ce1 126.0(3) . . ?
Cu2 O7 Ce1 108.48(18) . . ?
C36 O8 C38 117.6(5) . . ?
C36 O8 Ce1 119.4(3) . . ?
C38 O8 Ce1 122.5(4) . . ?

_refine_diff_density_max         0.466
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.090

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_3
_database_code_depnum_ccdc_archive 'CCDC 1060174'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 Cu2 Eu Mo N12 O10'
_chemical_formula_weight         1299.91

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'
Eu Eu -0.1578 3.6682 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4089(4)
_cell_length_b                   12.4074(5)
_cell_length_c                   20.6391(9)
_cell_angle_alpha                94.967(3)
_cell_angle_beta                 102.028(3)
_cell_angle_gamma                116.494(3)
_cell_volume                     2502.96(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    31261
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      30.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_F_000             1294
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_absorpt_coefficient_mu    2.387
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5062
_exptl_absorpt_correction_T_max  0.6913
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31261
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_av_R_equivalents  0.0515
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.360
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measured_fraction_theta_full 0.936
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_Laue_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_point_group_measured_fraction_full 0.936
_reflns_number_total             13999
_reflns_number_gt                11072
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0676P)²+3.3783P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         13999
_refine_ls_number_parameters     668
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1383
_refine_ls_wR_factor_gt          0.1301
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.8807(8) 0.4505(8) 0.4180(4) 0.083(3) Uani 1 1 d . . . . .
H1A H 0.9629 0.5065 0.4083 0.125 Uiso 1 1 calc R U . . .
H1B H 0.8592 0.4943 0.4502 0.125 Uiso 1 1 calc R U . . .
H1C H 0.8935 0.3868 0.4364 0.125 Uiso 1 1 calc R U . . .
C2 C 0.6447(6) 0.3138(5) 0.3605(3) 0.0463(12) Uani 1 1 d . . . . .
C3 C 0.5988(9) 0.3146(8) 0.4173(4) 0.072(2) Uani 1 1 d . . . . .
H3 H 0.6553 0.3725 0.4569 0.086 Uiso 1 1 calc R U . . .
C4 C 0.4670(10) 0.2280(10) 0.4146(5) 0.092(3) Uani 1 1 d . . . . .
H4 H 0.4345 0.2277 0.4524 0.110 Uiso 1 1 calc R U . . .
C5 C 0.3862(8) 0.1442(9) 0.3568(4) 0.076(2) Uani 1 1 d . . . . .
H5 H 0.2986 0.0861 0.3557 0.091 Uiso 1 1 calc R U . . .
C6 C 0.4298(6) 0.1420(6) 0.2990(3) 0.0514(13) Uani 1 1 d . . . . .
C7 C 0.5600(5) 0.2310(5) 0.2999(3) 0.0396(10) Uani 1 1 d . . . . .
C8 C 0.3387(7) 0.0444(7) 0.2405(4) 0.0637(17) Uani 1 1 d . . . . .
H8 H 0.2583 -0.0150 0.2468 0.076 Uiso 1 1 calc R U . . .
C9 C 0.2502(11) -0.0876(9) 0.1366(6) 0.124(5) Uani 0.7 1 d . . P A 1
H9A H 0.2863 -0.1452 0.1386 0.149 Uiso 0.7 1 calc R U P A 1
H9B H 0.1704 -0.1209 0.1534 0.149 Uiso 0.7 1 calc R U P A 1
C10 C 0.2068(11) -0.0837(11) 0.0672(7) 0.081(4) Uani 0.7 1 d . . P A 1
H10A H 0.1716 -0.0255 0.0648 0.097 Uiso 0.7 1 calc R U P A 1
H10B H 0.1322 -0.1641 0.0437 0.097 Uiso 0.7 1 calc R U P A 1
C11 C 0.3149(8) -0.0484(7) 0.0305(4) 0.068(2) Uani 0.7 1 d . . P A 1
H11A H 0.3620 -0.0966 0.0387 0.081 Uiso 0.7 1 calc R U P A 1
H11B H 0.2736 -0.0649 -0.0178 0.081 Uiso 0.7 1 calc R U P A 1
C9A C 0.2502(11) -0.0876(9) 0.1366(6) 0.124(5) Uani 0.3 1 d . . P A 2
H9A1 H 0.2327 -0.1533 0.1616 0.149 Uiso 0.3 1 calc R U P A 2
H9A2 H 0.1662 -0.0832 0.1225 0.149 Uiso 0.3 1 calc R U P A 2
C10A C 0.282(3) -0.121(3) 0.0781(19) 0.086(9) Uani 0.3 1 d . . P A 2
H10C H 0.3577 -0.1368 0.0937 0.103 Uiso 0.3 1 calc R U P A 2
H10D H 0.2047 -0.1988 0.0536 0.103 Uiso 0.3 1 calc R U P A 2
C11A C 0.3149(8) -0.0484(7) 0.0305(4) 0.068(2) Uani 0.3 1 d . . P A 2
H11C H 0.2310 -0.0554 0.0027 0.081 Uiso 0.3 1 calc R U P A 2
H11D H 0.3512 -0.0832 0.0013 0.081 Uiso 0.3 1 calc R U P A 2
C12 C 0.4342(7) 0.1494(7) 0.0097(3) 0.0562(15) Uani 1 1 d . . . . .
H12 H 0.3834 0.1083 -0.0345 0.067 Uiso 1 1 calc R U . . .
C13 C 0.5262(7) 0.2771(7) 0.0190(3) 0.0552(14) Uani 1 1 d . . . . .
C14 C 0.5172(10) 0.3325(9) -0.0372(4) 0.081(2) Uani 1 1 d . . . . .
H14 H 0.4533 0.2850 -0.0780 0.097 Uiso 1 1 calc R U . . .
C15 C 0.6002(12) 0.4540(10) -0.0329(4) 0.092(3) Uani 1 1 d . . . . .
H15 H 0.5922 0.4883 -0.0708 0.110 Uiso 1 1 calc R U . . .
C16 C 0.6959(10) 0.5272(8) 0.0267(4) 0.076(2) Uani 1 1 d . . . . .
H16 H 0.7534 0.6099 0.0289 0.091 Uiso 1 1 calc R U . . .
C17 C 0.7056(7) 0.4769(6) 0.0828(3) 0.0495(13) Uani 1 1 d . . . . .
C18 C 0.6226(6) 0.3499(5) 0.0805(3) 0.0421(11) Uani 1 1 d . . . . .
C19 C 0.8855(9) 0.6674(6) 0.1496(4) 0.075(2) Uani 1 1 d . . . . .
H19A H 0.9392 0.7049 0.1957 0.113 Uiso 1 1 calc R U . . .
H19B H 0.9441 0.6703 0.1217 0.113 Uiso 1 1 calc R U . . .
H19C H 0.8375 0.7112 0.1340 0.113 Uiso 1 1 calc R U . . .
C20 C 0.4623(6) 0.4079(7) 0.1981(4) 0.0626(17) Uani 1 1 d . . . . .
H20A H 0.4604 0.3567 0.1598 0.094 Uiso 1 1 calc R U . . .
H20B H 0.3993 0.3578 0.2211 0.094 Uiso 1 1 calc R U . . .
H20C H 0.4370 0.4675 0.1830 0.094 Uiso 1 1 calc R U . . .
C21 C 0.6151(6) 0.5487(6) 0.3025(3) 0.0496(13) Uani 1 1 d . . . . .
C22 C 0.5114(9) 0.5516(10) 0.3247(5) 0.082(3) Uani 1 1 d . . . . .
H22 H 0.4212 0.4968 0.3016 0.098 Uiso 1 1 calc R U . . .
C23 C 0.5426(11) 0.6384(13) 0.3829(6) 0.112(4) Uani 1 1 d . . . . .
H23 H 0.4734 0.6434 0.3979 0.135 Uiso 1 1 calc R U . . .
C24 C 0.6755(11) 0.7146(11) 0.4167(5) 0.095(3) Uani 1 1 d . . . . .
H24 H 0.6962 0.7707 0.4557 0.114 Uiso 1 1 calc R U . . .
C25 C 0.7820(8) 0.7116(7) 0.3948(4) 0.0636(17) Uani 1 1 d . . . . .
C26 C 0.7531(6) 0.6281(5) 0.3372(3) 0.0464(12) Uani 1 1 d . . . . .
C27 C 0.9171(9) 0.7912(8) 0.4375(4) 0.075(2) Uani 1 1 d . . . . .
H27 H 0.9240 0.8422 0.4755 0.090 Uiso 1 1 calc R U . . .
C28 C 1.1547(12) 0.8910(14) 0.4833(7) 0.142(6) Uani 0.55 1 d . . P B 1
H28A H 1.1330 0.9495 0.5051 0.170 Uiso 0.55 1 calc R U P B 1
H28B H 1.1714 0.8459 0.5170 0.170 Uiso 0.55 1 calc R U P B 1
C29 C 1.2691(17) 0.9545(18) 0.4706(10) 0.093(6) Uani 0.55 1 d . . P B 1
H29A H 1.3338 1.0116 0.5119 0.111 Uiso 0.55 1 calc R U P B 1
H29B H 1.2560 1.0029 0.4381 0.111 Uiso 0.55 1 calc R U P B 1
C30 C 1.3324(9) 0.8806(9) 0.4428(5) 0.094(3) Uani 0.55 1 d . . P B 1
H30A H 1.4197 0.9376 0.4372 0.113 Uiso 0.55 1 calc R U P B 1
H30B H 1.3492 0.8345 0.4760 0.113 Uiso 0.55 1 calc R U P B 1
C28A C 1.1547(12) 0.8910(14) 0.4833(7) 0.142(6) Uani 0.45 1 d . . P B 2
H28C H 1.1868 0.9708 0.4708 0.170 Uiso 0.45 1 calc R U P B 2
H28D H 1.1314 0.8985 0.5254 0.170 Uiso 0.45 1 calc R U P B 2
C29A C 1.2592(18) 0.8633(16) 0.4946(7) 0.059(4) Uani 0.45 1 d . . P B 2
H29C H 1.2230 0.7781 0.4992 0.071 Uiso 0.45 1 calc R U P B 2
H29D H 1.3241 0.9137 0.5375 0.071 Uiso 0.45 1 calc R U P B 2
C30A C 1.3324(9) 0.8806(9) 0.4428(5) 0.094(3) Uani 0.45 1 d . . P B 2
H30C H 1.4117 0.8695 0.4589 0.113 Uiso 0.45 1 calc R U P B 2
H30D H 1.3641 0.9641 0.4358 0.113 Uiso 0.45 1 calc R U P B 2
C31 C 1.3116(6) 0.7813(6) 0.3359(4) 0.0616(17) Uani 1 1 d . . . . .
H31 H 1.4052 0.8335 0.3495 0.074 Uiso 1 1 calc R U . . .
C32 C 1.2594(6) 0.6982(6) 0.2716(4) 0.0593(16) Uani 1 1 d . . . . .
C33 C 1.3519(7) 0.7085(8) 0.2336(5) 0.077(2) Uani 1 1 d . . . . .
H33 H 1.4415 0.7714 0.2493 0.092 Uiso 1 1 calc R U . . .
C34 C 1.3134(9) 0.6304(10) 0.1760(6) 0.093(3) Uani 1 1 d . . . . .
H34 H 1.3763 0.6402 0.1518 0.111 Uiso 1 1 calc R U . . .
C35 C 1.1806(9) 0.5336(8) 0.1507(5) 0.077(2) Uani 1 1 d . . . . .
H35 H 1.1549 0.4798 0.1100 0.092 Uiso 1 1 calc R U . . .
C36 C 1.0873(6) 0.5192(6) 0.1878(4) 0.0526(14) Uani 1 1 d . . . . .
C37 C 1.1233(5) 0.6026(5) 0.2470(3) 0.0467(12) Uani 1 1 d . . . . .
C38 C 0.9182(9) 0.3232(8) 0.1160(5) 0.078(2) Uani 1 1 d . . . . .
H38A H 0.8236 0.2648 0.1076 0.117 Uiso 1 1 calc R U . . .
H38B H 0.9339 0.3523 0.0755 0.117 Uiso 1 1 calc R U . . .
H38C H 0.9730 0.2845 0.1298 0.117 Uiso 1 1 calc R U . . .
C39 C 0.9889(5) 0.9240(4) 0.2751(3) 0.0430(12) Uani 1 1 d . . . . .
C40 C 0.7284(5) 0.8355(5) 0.2210(3) 0.0445(11) Uani 1 1 d . . . . .
C41 C 0.7126(5) 1.0307(5) 0.1834(3) 0.0429(11) Uani 1 1 d . . . . .
C42 C 0.8984(5) 1.2085(5) 0.2720(3) 0.0475(13) Uani 1 1 d . . . . .
C43 C 0.8868(6) 0.9697(6) 0.1503(3) 0.0513(13) Uani 1 1 d . . . . .
C44 C 1.0728(6) 1.1531(6) 0.2371(5) 0.071(2) Uani 1 1 d . . . . .
C45 C 1.0100(8) 1.1038(8) 0.3530(4) 0.0671(19) Uani 1 1 d . . . . .
C46 C 0.7447(7) 0.9985(7) 0.3147(3) 0.0584(15) Uani 1 1 d . . . . .
Cu1 Cu 0.50612(6) 0.14892(6) 0.15314(3) 0.03872(14) Uani 1 1 d . . . . .
Cu2 Cu 1.04500(7) 0.71756(6) 0.34910(4) 0.04274(15) Uani 1 1 d . . . . .
Eu1 Eu 0.79655(2) 0.43161(2) 0.24160(2) 0.03215(8) Uani 1 1 d . . . . .
Mo1 Mo 0.88099(4) 1.02683(4) 0.25126(2) 0.03503(10) Uani 1 1 d . . . . .
N1 N 0.3539(5) 0.0298(5) 0.1837(3) 0.0590(14) Uani 1 1 d . . . . .
N2 N 0.4135(5) 0.0849(5) 0.0552(3) 0.0506(12) Uani 1 1 d . . . . .
N3 N 1.0277(7) 0.8006(6) 0.4298(3) 0.0747(18) Uani 1 1 d . . . . .
N4 N 1.2457(5) 0.7925(5) 0.3765(3) 0.0557(13) Uani 1 1 d . . . . .
N5 N 1.0450(5) 0.8687(4) 0.2888(3) 0.0529(13) Uani 1 1 d . . . . .
N6 N 0.6507(6) 0.7336(5) 0.2035(3) 0.0625(15) Uani 1 1 d . . . . .
N7 N 0.6237(6) 1.0374(5) 0.1496(3) 0.0575(14) Uani 1 1 d . . . . .
N8 N 0.9032(5) 1.3018(5) 0.2790(3) 0.0588(14) Uani 1 1 d . . . . .
N9 N 0.8907(8) 0.9386(9) 0.0974(4) 0.085(2) Uani 1 1 d . . . . .
N10 N 1.1727(8) 1.2212(9) 0.2270(7) 0.125(4) Uani 1 1 d . . . . .
N11 N 1.0840(9) 1.1426(10) 0.4059(4) 0.112(3) Uani 1 1 d . . . . .
N12 N 0.6705(8) 0.9829(8) 0.3466(4) 0.085(2) Uani 1 1 d . . . . .
O1 O 0.7718(4) 0.3970(4) 0.3573(2) 0.0471(9) Uani 1 1 d . . . . .
O2 O 0.6079(4) 0.2414(3) 0.24595(19) 0.0387(7) Uani 1 1 d . . . . .
O1W O 0.8669(19) 0.7943(15) -0.0435(8) 0.230(7) Uani 1 1 d . . . . .
O3 O 0.6406(4) 0.3074(3) 0.13619(18) 0.0400(7) Uani 1 1 d . . . . .
O2W O 0.7856(19) 0.528(2) 0.5840(10) 0.341(13) Uani 1 1 d . . . . .
O4 O 0.7895(5) 0.5420(4) 0.1458(2) 0.0519(10) Uani 1 1 d . . . . .
O5 O 0.5982(4) 0.4703(4) 0.2439(2) 0.0467(9) Uani 1 1 d . . . . .
O6 O 0.8483(4) 0.6171(3) 0.3129(2) 0.0411(8) Uani 1 1 d . . . . .
O7 O 1.0279(4) 0.5889(3) 0.2780(2) 0.0439(8) Uani 1 1 d . . . . .
O8 O 0.9542(4) 0.4255(4) 0.1689(3) 0.0567(11) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.424(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.375(7) . ?
C2 C3 1.382(9) . ?
C2 C7 1.393(8) . ?
C3 C4 1.390(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.351(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.386(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.396(7) . ?
C6 C8 1.452(10) . ?
C7 O2 1.331(6) . ?
C8 N1 1.231(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.428(18) . ?
C9 N1 1.484(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.500(16) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.488(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C10A H10C 0.9700 . ?
C10A H10D 0.9700 . ?
C12 N2 1.276(9) . ?
C12 C13 1.425(10) . ?
C12 H12 0.9300 . ?
C13 C18 1.403(8) . ?
C13 C14 1.407(10) . ?
C14 C15 1.358(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.375(12) . ?
C15 H15 0.9300 . ?
C16 C17 1.369(9) . ?
C16 H16 0.9300 . ?
C17 O4 1.368(7) . ?
C17 C18 1.420(8) . ?
C18 O3 1.322(6) . ?
C19 O4 1.432(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O5 1.444(7) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.367(9) . ?
C21 O5 1.406(7) . ?
C21 C26 1.410(9) . ?
C22 C23 1.410(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.359(15) . ?
C23 H23 0.9300 . ?
C24 C25 1.397(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(9) . ?
C25 C27 1.433(11) . ?
C26 O6 1.341(7) . ?
C27 N3 1.259(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.29(2) . ?
C28 N3 1.499(11) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.54(2) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N4 1.503(10) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C31 N4 1.274(10) . ?
C31 C32 1.436(10) . ?
C31 H31 0.9300 . ?
C32 C33 1.409(11) . ?
C32 C37 1.415(8) . ?
C33 C34 1.322(13) . ?
C33 H33 0.9300 . ?
C34 C35 1.396(12) . ?
C34 H34 0.9300 . ?
C35 C36 1.394(10) . ?
C35 H35 0.9300 . ?
C36 O8 1.382(7) . ?
C36 C37 1.388(9) . ?
C37 O7 1.329(7) . ?
C38 O8 1.442(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N5 1.145(6) . ?
C39 Mo1 2.155(5) . ?
C40 N6 1.142(8) . ?
C40 Mo1 2.158(6) . ?
C41 N7 1.147(7) . ?
C41 Mo1 2.150(5) . ?
C42 N8 1.129(7) . ?
C42 Mo1 2.168(5) . ?
C43 N9 1.143(9) . ?
C43 Mo1 2.167(7) . ?
C44 N10 1.152(10) . ?
C44 Mo1 2.148(7) . ?
C45 N11 1.140(9) . ?
C45 Mo1 2.144(7) . ?
C46 N12 1.139(10) . ?
C46 Mo1 2.167(7) . ?
Cu1 O2 1.959(4) . ?
Cu1 N2 1.980(5) . ?
Cu1 N1 1.981(5) . ?
Cu1 O3 1.998(4) . ?
Cu1 N7 2.323(5) 1_545 ?
Cu1 Eu1 3.5518(6) . ?
Cu2 O6 1.948(4) . ?
Cu2 N3 1.974(6) . ?
Cu2 N4 1.974(5) . ?
Cu2 O7 1.983(4) . ?
Cu2 N5 2.339(5) . ?
Cu2 Eu1 3.5479(7) . ?
Eu1 O3 2.374(3) . ?
Eu1 O6 2.377(4) . ?
Eu1 O7 2.380(4) . ?
Eu1 O2 2.407(4) . ?
Eu1 N8 2.499(5) 1_545 ?
Eu1 O4 2.508(4) . ?
Eu1 O1 2.512(4) . ?
Eu1 O5 2.523(4) . ?
Eu1 O8 2.591(5) . ?
N7 Cu1 2.323(5) 1_565 ?
N8 Eu1 2.499(5) 1_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
O1 C2 C3 123.9(6) . . ?
O1 C2 C7 114.6(5) . . ?
C3 C2 C7 121.3(6) . . ?
C2 C3 C4 119.2(7) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 119.7(8) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 122.1(7) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C7 119.1(6) . . ?
C5 C6 C8 118.2(6) . . ?
C7 C6 C8 122.7(6) . . ?
O2 C7 C2 118.0(5) . . ?
O2 C7 C6 123.6(5) . . ?
C2 C7 C6 118.4(5) . . ?
N1 C8 C6 128.5(6) . . ?
N1 C8 H8 115.7 . . ?
C6 C8 H8 115.7 . . ?
C10 C9 N1 117.6(10) . . ?
C10 C9 H9A 107.9 . . ?
N1 C9 H9A 107.9 . . ?
C10 C9 H9B 107.9 . . ?
N1 C9 H9B 107.9 . . ?
H9A C9 H9B 107.2 . . ?
C9 C10 C11 115.2(10) . . ?
C9 C10 H10A 108.5 . . ?
C11 C10 H10A 108.5 . . ?
C9 C10 H10B 108.5 . . ?
C11 C10 H10B 108.5 . . ?
H10A C10 H10B 107.5 . . ?
N2 C11 C10 109.2(7) . . ?
N2 C11 H11A 109.8 . . ?
C10 C11 H11A 109.8 . . ?
N2 C11 H11B 109.8 . . ?
C10 C11 H11B 109.8 . . ?
H11A C11 H11B 108.3 . . ?
H10C C10A H10D 106.4 . . ?
N2 C12 C13 127.4(6) . . ?
N2 C12 H12 116.3 . . ?
C13 C12 H12 116.3 . . ?
C18 C13 C14 118.8(7) . . ?
C18 C13 C12 124.1(6) . . ?
C14 C13 C12 117.2(6) . . ?
C15 C14 C13 121.3(7) . . ?
C15 C14 H14 119.4 . . ?
C13 C14 H14 119.4 . . ?
C14 C15 C16 121.1(7) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 H15 119.5 . . ?
C17 C16 C15 119.3(8) . . ?
C17 C16 H16 120.4 . . ?
C15 C16 H16 120.4 . . ?
O4 C17 C16 124.6(6) . . ?
O4 C17 C18 113.7(5) . . ?
C16 C17 C18 121.7(6) . . ?
O3 C18 C13 123.9(5) . . ?
O3 C18 C17 118.2(5) . . ?
C13 C18 C17 117.9(5) . . ?
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 . . ?
C22 C21 O5 125.2(6) . . ?
C22 C21 C26 121.9(7) . . ?
O5 C21 C26 112.9(5) . . ?
C21 C22 C23 119.4(8) . . ?
C21 C22 H22 120.3 . . ?
C23 C22 H22 120.3 . . ?
C24 C23 C22 118.8(8) . . ?
C24 C23 H23 120.6 . . ?
C22 C23 H23 120.6 . . ?
C23 C24 C25 122.1(8) . . ?
C23 C24 H24 118.9 . . ?
C25 C24 H24 118.9 . . ?
C26 C25 C24 119.7(8) . . ?
C26 C25 C27 123.7(7) . . ?
C24 C25 C27 116.4(7) . . ?
O6 C26 C25 124.0(6) . . ?
O6 C26 C21 118.0(5) . . ?
C25 C26 C21 118.0(6) . . ?
N3 C27 C25 127.8(7) . . ?
N3 C27 H27 116.1 . . ?
C25 C27 H27 116.1 . . ?
C29 C28 N3 123.1(13) . . ?
C29 C28 H28A 106.6 . . ?
N3 C28 H28A 106.6 . . ?
C29 C28 H28B 106.6 . . ?
N3 C28 H28B 106.6 . . ?
H28A C28 H28B 106.5 . . ?
C28 C29 C30 115.9(16) . . ?
C28 C29 H29A 108.3 . . ?
C30 C29 H29A 108.3 . . ?
C28 C29 H29B 108.3 . . ?
C30 C29 H29B 108.3 . . ?
H29A C29 H29B 107.4 . . ?
N4 C30 C29 114.1(8) . . ?
N4 C30 H30A 108.7 . . ?
C29 C30 H30A 108.7 . . ?
N4 C30 H30B 108.7 . . ?
C29 C30 H30B 108.7 . . ?
H30A C30 H30B 107.6 . . ?
H29C C29A H29D 107.4 . . ?
N4 C31 C32 128.1(6) . . ?
N4 C31 H31 115.9 . . ?
C32 C31 H31 115.9 . . ?
C33 C32 C37 118.9(7) . . ?
C33 C32 C31 117.6(6) . . ?
C37 C32 C31 123.4(7) . . ?
C34 C33 C32 121.1(7) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.4 . . ?
C33 C34 C35 121.7(8) . . ?
C33 C34 H34 119.1 . . ?
C35 C34 H34 119.1 . . ?
C36 C35 C34 118.6(8) . . ?
C36 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
O8 C36 C37 114.9(6) . . ?
O8 C36 C35 124.1(7) . . ?
C37 C36 C35 120.9(6) . . ?
O7 C37 C36 118.4(5) . . ?
O7 C37 C32 123.0(6) . . ?
C36 C37 C32 118.6(6) . . ?
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 178.7(6) . . ?
N6 C40 Mo1 177.3(6) . . ?
N7 C41 Mo1 176.6(5) . . ?
N8 C42 Mo1 176.0(6) . . ?
N9 C43 Mo1 179.0(6) . . ?
N10 C44 Mo1 177.2(10) . . ?
N11 C45 Mo1 175.7(7) . . ?
N12 C46 Mo1 178.3(7) . . ?
O2 Cu1 N2 169.72(19) . . ?
O2 Cu1 N1 91.9(2) . . ?
N2 Cu1 N1 95.6(2) . . ?
O2 Cu1 O3 79.03(15) . . ?
N2 Cu1 O3 91.7(2) . . ?
N1 Cu1 O3 160.7(2) . . ?
O2 Cu1 N7 95.32(17) . 1_545 ?
N2 Cu1 N7 90.6(2) . 1_545 ?
N1 Cu1 N7 98.2(2) . 1_545 ?
O3 Cu1 N7 99.58(19) . 1_545 ?
O2 Cu1 Eu1 40.01(11) . . ?
N2 Cu1 Eu1 131.03(17) . . ?
N1 Cu1 Eu1 131.01(17) . . ?
O3 Cu1 Eu1 39.36(10) . . ?
N7 Cu1 Eu1 95.66(14) 1_545 . ?
O6 Cu2 N3 92.5(2) . . ?
O6 Cu2 N4 169.02(19) . . ?
N3 Cu2 N4 97.1(3) . . ?
O6 Cu2 O7 77.45(15) . . ?
N3 Cu2 O7 162.4(3) . . ?
N4 Cu2 O7 91.9(2) . . ?
O6 Cu2 N5 91.55(16) . . ?
N3 Cu2 N5 92.3(3) . . ?
N4 Cu2 N5 93.4(2) . . ?
O7 Cu2 N5 102.3(2) . . ?
O6 Cu2 Eu1 39.06(11) . . ?
N3 Cu2 Eu1 126.8(2) . . ?
N4 Cu2 Eu1 129.97(16) . . ?
O7 Cu2 Eu1 39.51(11) . . ?
N5 Cu2 Eu1 105.92(13) . . ?
O3 Eu1 O6 136.95(12) . . ?
O3 Eu1 O7 135.56(14) . . ?
O6 Eu1 O7 62.26(13) . . ?
O3 Eu1 O2 63.56(13) . . ?
O6 Eu1 O2 119.38(13) . . ?
O7 Eu1 O2 153.80(13) . . ?
O3 Eu1 N8 101.32(16) . 1_545 ?
O6 Eu1 N8 121.43(16) . 1_545 ?
O7 Eu1 N8 81.84(15) . 1_545 ?
O2 Eu1 N8 75.76(16) . 1_545 ?
O3 Eu1 O4 64.22(13) . . ?
O6 Eu1 O4 86.10(14) . . ?
O7 Eu1 O4 82.52(14) . . ?
O2 Eu1 O4 123.20(13) . . ?
N8 Eu1 O4 135.66(19) 1_545 . ?
O3 Eu1 O1 126.76(13) . . ?
O6 Eu1 O1 69.09(14) . . ?
O7 Eu1 O1 96.54(14) . . ?
O2 Eu1 O1 63.57(12) . . ?
N8 Eu1 O1 71.22(19) 1_545 . ?
O4 Eu1 O1 151.93(14) . . ?
O3 Eu1 O5 79.45(13) . . ?
O6 Eu1 O5 63.73(12) . . ?
O7 Eu1 O5 123.40(12) . . ?
O2 Eu1 O5 71.87(12) . . ?
N8 Eu1 O5 143.26(18) 1_545 . ?
O4 Eu1 O5 78.23(15) . . ?
O1 Eu1 O5 79.05(14) . . ?
O3 Eu1 O8 76.83(14) . . ?
O6 Eu1 O8 121.34(13) . . ?
O7 Eu1 O8 63.05(14) . . ?
O2 Eu1 O8 118.94(13) . . ?
N8 Eu1 O8 68.50(19) 1_545 . ?
O4 Eu1 O8 67.40(16) . . ?
O1 Eu1 O8 136.78(15) . . ?
O5 Eu1 O8 144.17(15) . . ?
O3 Eu1 Cu2 152.98(9) . . ?
O6 Eu1 Cu2 31.09(9) . . ?
O7 Eu1 Cu2 32.02(9) . . ?
O2 Eu1 Cu2 139.72(9) . . ?
N8 Eu1 Cu2 99.01(12) 1_545 . ?
O4 Eu1 Cu2 88.78(10) . . ?
O1 Eu1 Cu2 76.82(9) . . ?
O5 Eu1 Cu2 94.61(9) . . ?
O8 Eu1 Cu2 94.49(10) . . ?
O3 Eu1 Cu1 32.27(9) . . ?
O6 Eu1 Cu1 138.65(9) . . ?
O7 Eu1 Cu1 158.96(9) . . ?
O2 Eu1 Cu1 31.55(9) . . ?
N8 Eu1 Cu1 85.43(12) 1_545 . ?
O4 Eu1 Cu1 95.21(10) . . ?
O1 Eu1 Cu1 95.12(9) . . ?
O5 Eu1 Cu1 76.06(9) . . ?
O8 Eu1 Cu1 96.69(10) . . ?
Cu2 Eu1 Cu1 168.820(18) . . ?
C45 Mo1 C44 77.3(4) . . ?
C45 Mo1 C41 140.5(2) . . ?
C44 Mo1 C41 111.7(3) . . ?
C45 Mo1 C39 71.8(2) . . ?
C44 Mo1 C39 81.5(2) . . ?
C41 Mo1 C39 145.8(2) . . ?
C45 Mo1 C40 121.3(3) . . ?
C44 Mo1 C40 141.1(3) . . ?
C41 Mo1 C40 76.7(2) . . ?
C39 Mo1 C40 74.25(19) . . ?
C45 Mo1 C43 140.9(3) . . ?
C44 Mo1 C43 71.1(3) . . ?
C41 Mo1 C43 74.3(2) . . ?
C39 Mo1 C43 81.2(2) . . ?
C40 Mo1 C43 75.5(2) . . ?
C45 Mo1 C46 74.4(3) . . ?
C44 Mo1 C46 144.4(3) . . ?
C41 Mo1 C46 79.0(3) . . ?
C39 Mo1 C46 109.1(3) . . ?
C40 Mo1 C46 73.5(2) . . ?
C43 Mo1 C46 142.8(2) . . ?
C45 Mo1 C42 76.1(3) . . ?
C44 Mo1 C42 73.6(3) . . ?
C41 Mo1 C42 70.5(2) . . ?
C39 Mo1 C42 142.85(19) . . ?
C40 Mo1 C42 140.5(2) . . ?
C43 Mo1 C42 114.7(3) . . ?
C46 Mo1 C42 79.0(3) . . ?
C8 N1 C9 115.9(7) . . ?
C8 N1 Cu1 124.7(5) . . ?
C9 N1 Cu1 119.4(6) . . ?
C12 N2 C11 115.9(6) . . ?
C12 N2 Cu1 124.7(4) . . ?
C11 N2 Cu1 119.3(5) . . ?
C27 N3 C28 116.4(8) . . ?
C27 N3 Cu2 124.6(5) . . ?
C28 N3 Cu2 118.7(7) . . ?
C31 N4 C30 114.9(7) . . ?
C31 N4 Cu2 122.0(5) . . ?
C30 N4 Cu2 122.5(6) . . ?
C39 N5 Cu2 142.6(5) . . ?
C41 N7 Cu1 138.8(5) . 1_565 ?
C42 N8 Eu1 147.4(5) . 1_565 ?
C2 O1 C1 118.4(5) . . ?
C2 O1 Eu1 116.6(3) . . ?
C1 O1 Eu1 124.8(4) . . ?
C7 O2 Cu1 126.7(3) . . ?
C7 O2 Eu1 120.4(3) . . ?
Cu1 O2 Eu1 108.44(16) . . ?
C18 O3 Cu1 124.8(3) . . ?
C18 O3 Eu1 124.1(3) . . ?
Cu1 O3 Eu1 108.37(16) . . ?
C17 O4 C19 115.9(5) . . ?
C17 O4 Eu1 119.7(3) . . ?
C19 O4 Eu1 123.6(4) . . ?
C21 O5 C20 115.3(5) . . ?
C21 O5 Eu1 115.8(3) . . ?
C20 O5 Eu1 128.2(4) . . ?
C26 O6 Cu2 126.5(4) . . ?
C26 O6 Eu1 121.1(3) . . ?
Cu2 O6 Eu1 109.85(16) . . ?
C37 O7 Cu2 124.3(3) . . ?
C37 O7 Eu1 125.9(4) . . ?
Cu2 O7 Eu1 108.48(16) . . ?
C36 O8 C38 117.5(5) . . ?
C36 O8 Eu1 117.7(4) . . ?
C38 O8 Eu1 124.3(4) . . ?

_refine_diff_density_max         1.779
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.127

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_4
_database_code_depnum_ccdc_archive 'CCDC 1060175'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 Cu2 Mo N12 O10 Tb'
_chemical_formula_weight         1306.87

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'
Tb Tb -0.1723 4.1537 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.4193(7)
_cell_length_b                   12.3706(9)
_cell_length_c                   20.6069(15)
_cell_angle_alpha                95.112(6)
_cell_angle_beta                 101.921(5)
_cell_angle_gamma                116.803(5)
_cell_volume                     2486.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    26.817
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      30.00

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_F_000             1298
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    2.564
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5933
_exptl_absorpt_correction_T_max  0.7301
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26817
_diffrn_reflns_av_unetI/netI     0.1009
_diffrn_reflns_av_R_equivalents  0.0723
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.490
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measured_fraction_theta_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 0.900
_reflns_number_total             13551
_reflns_number_gt                8281
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0476P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13551
_refine_ls_number_parameters     659
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0548
_refine_ls_wR_factor_ref         0.1174
_refine_ls_wR_factor_gt          0.1012
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_restrained_S_all      0.926
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.8904(9) 0.4541(9) 0.4189(4) 0.080(3) Uani 1 1 d . . . . .
H1A H 0.9735 0.5086 0.4091 0.121 Uiso 1 1 calc R U . . .
H1B H 0.8712 0.5000 0.4513 0.121 Uiso 1 1 calc R U . . .
H1C H 0.9005 0.3891 0.4372 0.121 Uiso 1 1 calc R U . . .
C2 C 0.6504(7) 0.3190(6) 0.3626(3) 0.0446(15) Uani 1 1 d . . . . .
C3 C 0.6084(9) 0.3250(8) 0.4191(4) 0.062(2) Uani 1 1 d . . . . .
H3 H 0.6668 0.3853 0.4579 0.075 Uiso 1 1 calc R U . . .
C4 C 0.4750(11) 0.2387(11) 0.4179(5) 0.082(3) Uani 1 1 d . . . . .
H4 H 0.4446 0.2391 0.4564 0.099 Uiso 1 1 calc R U . . .
C5 C 0.3907(9) 0.1540(10) 0.3593(4) 0.076(3) Uani 1 1 d . . . . .
H5 H 0.3013 0.0992 0.3581 0.091 Uiso 1 1 calc R U . . .
C6 C 0.4338(7) 0.1469(7) 0.3012(4) 0.0503(17) Uani 1 1 d . . . . .
C7 C 0.5660(6) 0.2341(6) 0.3013(3) 0.0372(13) Uani 1 1 d . . . . .
C8 C 0.3420(7) 0.0495(8) 0.2438(4) 0.060(2) Uani 1 1 d . . . . .
H8 H 0.2601 -0.0073 0.2504 0.072 Uiso 1 1 calc R U . . .
C9 C 0.2493(10) -0.0895(9) 0.1408(6) 0.105(4) Uani 1 1 d . . . . .
H9A H 0.2805 -0.1502 0.1458 0.125 Uiso 1 1 calc R U . . .
H9B H 0.1679 -0.1171 0.1564 0.125 Uiso 1 1 calc R U . . .
C10 C 0.2129(13) -0.0885(12) 0.0711(7) 0.136(6) Uani 1 1 d . . . . .
H10A H 0.1706 -0.0359 0.0667 0.163 Uiso 1 1 calc R U . . .
H10B H 0.1422 -0.1719 0.0484 0.163 Uiso 1 1 calc R U . . .
C11 C 0.3123(8) -0.0504(8) 0.0324(4) 0.066(2) Uani 1 1 d . . . . .
H11A H 0.2657 -0.0657 -0.0151 0.080 Uiso 1 1 calc R U . . .
H11B H 0.3593 -0.0990 0.0368 0.080 Uiso 1 1 calc R U . . .
C12 C 0.4343(7) 0.1467(7) 0.0113(3) 0.0499(18) Uani 1 1 d . . . . .
H12 H 0.3828 0.1046 -0.0329 0.060 Uiso 1 1 calc R U . . .
C13 C 0.5281(8) 0.2767(8) 0.0196(3) 0.0499(17) Uani 1 1 d . . . . .
C14 C 0.5165(10) 0.3293(10) -0.0366(4) 0.068(2) Uani 1 1 d . . . . .
H14 H 0.4518 0.2801 -0.0773 0.082 Uiso 1 1 calc R U . . .
C15 C 0.5989(12) 0.4521(11) -0.0330(4) 0.080(3) Uani 1 1 d . . . . .
H15 H 0.5904 0.4861 -0.0710 0.096 Uiso 1 1 calc R U . . .
C16 C 0.6954(10) 0.5266(9) 0.0275(4) 0.065(2) Uani 1 1 d . . . . .
H16 H 0.7524 0.6101 0.0297 0.078 Uiso 1 1 calc R U . . .
C17 C 0.7067(7) 0.4772(7) 0.0839(3) 0.0441(15) Uani 1 1 d . . . . .
C18 C 0.6239(6) 0.3494(6) 0.0818(3) 0.0384(13) Uani 1 1 d . . . . .
C19 C 0.8908(10) 0.6707(7) 0.1502(5) 0.067(2) Uani 1 1 d . . . . .
H19A H 0.9453 0.7096 0.1962 0.100 Uiso 1 1 calc R U . . .
H19B H 0.9487 0.6716 0.1223 0.100 Uiso 1 1 calc R U . . .
H19C H 0.8438 0.7150 0.1341 0.100 Uiso 1 1 calc R U . . .
C20 C 0.4624(7) 0.4040(8) 0.1956(4) 0.058(2) Uani 1 1 d . . . . .
H20A H 0.4623 0.3545 0.1570 0.086 Uiso 1 1 calc R U . . .
H20B H 0.3983 0.3516 0.2176 0.086 Uiso 1 1 calc R U . . .
H20C H 0.4368 0.4638 0.1812 0.086 Uiso 1 1 calc R U . . .
C21 C 0.6112(7) 0.5420(7) 0.3008(3) 0.0457(16) Uani 1 1 d . . . . .
C22 C 0.5059(9) 0.5385(9) 0.3246(4) 0.064(2) Uani 1 1 d . . . . .
H22 H 0.4159 0.4815 0.3015 0.077 Uiso 1 1 calc R U . . .
C23 C 0.5353(10) 0.6211(11) 0.3836(5) 0.088(3) Uani 1 1 d . . . . .
H23 H 0.4644 0.6202 0.3994 0.105 Uiso 1 1 calc R U . . .
C24 C 0.6679(10) 0.7037(10) 0.4185(5) 0.079(3) Uani 1 1 d . . . . .
H24 H 0.6862 0.7588 0.4578 0.095 Uiso 1 1 calc R U . . .
C25 C 0.7769(8) 0.7059(8) 0.3955(4) 0.059(2) Uani 1 1 d . . . . .
C26 C 0.7489(7) 0.6248(6) 0.3368(3) 0.0436(15) Uani 1 1 d . . . . .
C27 C 0.9121(9) 0.7896(9) 0.4379(4) 0.068(3) Uani 1 1 d . . . . .
H27 H 0.9175 0.8400 0.4759 0.082 Uiso 1 1 calc R U . . .
C28 C 1.1504(12) 0.8964(13) 0.4822(6) 0.126(6) Uani 0.4 1 d . . P A 1
H28A H 1.1294 0.9595 0.4989 0.151 Uiso 0.4 1 calc R U P A 1
H28B H 1.1593 0.8550 0.5193 0.151 Uiso 0.4 1 calc R U P A 1
C29 C 1.265(2) 0.953(2) 0.4758(10) 0.065(6) Uani 0.4 1 d . . P A 1
H29A H 1.3261 1.0003 0.5203 0.078 Uiso 0.4 1 calc R U P A 1
H29B H 1.2653 1.0123 0.4480 0.078 Uiso 0.4 1 calc R U P A 1
C30 C 1.3311(9) 0.8804(9) 0.4446(4) 0.076(3) Uani 0.4 1 d . . P A 1
H30A H 1.4168 0.9402 0.4381 0.092 Uiso 0.4 1 calc R U P A 1
H30B H 1.3521 0.8353 0.4772 0.092 Uiso 0.4 1 calc R U P A 1
C28A C 1.1504(12) 0.8964(13) 0.4822(6) 0.126(6) Uani 0.6 1 d . . P A 2
H28C H 1.1826 0.9751 0.4680 0.151 Uiso 0.6 1 calc R U P A 2
H28D H 1.1272 0.9069 0.5241 0.151 Uiso 0.6 1 calc R U P A 2
C29A C 1.2594(17) 0.8681(16) 0.4957(7) 0.070(4) Uani 0.6 1 d . . P A 2
H29C H 1.2233 0.7836 0.5023 0.084 Uiso 0.6 1 calc R U P A 2
H29D H 1.3248 0.9217 0.5381 0.084 Uiso 0.6 1 calc R U P A 2
C30A C 1.3311(9) 0.8804(9) 0.4446(4) 0.076(3) Uani 0.6 1 d . . P A 2
H30C H 1.4091 0.8681 0.4615 0.092 Uiso 0.6 1 calc R U P A 2
H30D H 1.3655 0.9641 0.4368 0.092 Uiso 0.6 1 calc R U P A 2
C31 C 1.3116(7) 0.7790(7) 0.3389(4) 0.0559(19) Uani 1 1 d . . . . .
H31 H 1.4058 0.8296 0.3534 0.067 Uiso 1 1 calc R U . . .
C32 C 1.2605(7) 0.6974(7) 0.2746(4) 0.0473(16) Uani 1 1 d . . . . .
C33 C 1.3556(7) 0.7072(8) 0.2377(5) 0.067(2) Uani 1 1 d . . . . .
H33 H 1.4462 0.7687 0.2550 0.080 Uiso 1 1 calc R U . . .
C34 C 1.3180(9) 0.6299(9) 0.1785(5) 0.076(3) Uani 1 1 d . . . . .
H34 H 1.3808 0.6404 0.1540 0.091 Uiso 1 1 calc R U . . .
C35 C 1.1818(8) 0.5320(8) 0.1535(4) 0.064(2) Uani 1 1 d . . . . .
H35 H 1.1560 0.4762 0.1132 0.077 Uiso 1 1 calc R U . . .
C36 C 1.0882(7) 0.5195(6) 0.1886(4) 0.0464(16) Uani 1 1 d . . . . .
C37 C 1.1239(6) 0.6023(6) 0.2490(3) 0.0413(14) Uani 1 1 d . . . . .
C38 C 0.9189(9) 0.3239(8) 0.1159(5) 0.071(3) Uani 1 1 d . . . . .
H38A H 0.8235 0.2660 0.1060 0.106 Uiso 1 1 calc R U . . .
H38B H 0.9385 0.3530 0.0757 0.106 Uiso 1 1 calc R U . . .
H38C H 0.9716 0.2840 0.1310 0.106 Uiso 1 1 calc R U . . .
C39 C 0.9921(6) 0.9268(5) 0.2761(3) 0.0381(13) Uani 1 1 d . . . . .
C40 C 0.7348(6) 0.8374(6) 0.2202(4) 0.0425(15) Uani 1 1 d . . . . .
C41 C 0.7107(6) 1.0290(6) 0.1828(3) 0.0432(15) Uani 1 1 d . . . . .
C42 C 0.8990(7) 1.2101(6) 0.2701(4) 0.0455(15) Uani 1 1 d . . . . .
C43 C 0.8901(7) 0.9726(8) 0.1494(3) 0.0484(17) Uani 1 1 d . . . . .
C44 C 1.0747(8) 1.1564(8) 0.2361(5) 0.065(2) Uani 1 1 d . . . . .
C45 C 1.0144(9) 1.1116(8) 0.3522(4) 0.063(2) Uani 1 1 d . . . . .
C46 C 0.7494(7) 0.9986(7) 0.3154(4) 0.0537(19) Uani 1 1 d . . . . .
Cu1 Cu 0.50807(7) 0.14786(7) 0.15477(4) 0.03710(17) Uani 1 1 d . . . . .
Cu2 Cu 1.04342(8) 0.71940(7) 0.34950(4) 0.03975(18) Uani 1 1 d . . . . .
Tb1 Tb 0.79705(3) 0.43318(3) 0.24133(2) 0.03040(7) Uani 1 1 d . . . . .
Mo1 Mo 0.88328(5) 1.02915(5) 0.25059(3) 0.03374(12) Uani 1 1 d . . . . .
N1 N 0.3556(6) 0.0293(5) 0.1856(3) 0.0547(16) Uani 1 1 d . . . . .
N2 N 0.4129(6) 0.0824(5) 0.0564(3) 0.0454(13) Uani 1 1 d . . . . .
N3 N 1.0249(7) 0.8039(7) 0.4302(3) 0.068(2) Uani 1 1 d . . . . .
N4 N 1.2460(6) 0.7923(5) 0.3796(3) 0.0502(14) Uani 1 1 d . . . . .
N5 N 1.0481(6) 0.8729(5) 0.2910(3) 0.0484(14) Uani 1 1 d . . . . .
N6 N 0.6531(6) 0.7330(6) 0.2033(3) 0.0555(15) Uani 1 1 d . . . . .
N7 N 0.6222(6) 1.0344(6) 0.1505(3) 0.0566(17) Uani 1 1 d . . . . .
N8 N 0.9025(6) 1.3047(6) 0.2763(3) 0.0539(16) Uani 1 1 d . . . . .
N9 N 0.8913(8) 0.9401(9) 0.0960(4) 0.079(2) Uani 1 1 d . . . . .
N10 N 1.1734(9) 1.2235(9) 0.2248(7) 0.119(4) Uani 1 1 d . . . . .
N11 N 1.0908(9) 1.1576(9) 0.4053(4) 0.095(3) Uani 1 1 d . . . . .
N12 N 0.6749(8) 0.9812(8) 0.3478(4) 0.082(3) Uani 1 1 d . . . . .
O1 O 0.7796(5) 0.4011(5) 0.3574(2) 0.0485(12) Uani 1 1 d . . . . .
O2 O 0.6122(4) 0.2422(4) 0.2475(2) 0.0390(10) Uani 1 1 d . . . . .
O1W O 0.8566(17) 0.7883(12) -0.0464(8) 0.203(6) Uani 1 1 d . . . . .
O3 O 0.6438(4) 0.3075(4) 0.1372(2) 0.0389(9) Uani 1 1 d . . . . .
O2W O 0.7969(16) 0.5516(14) 0.5807(11) 0.278(11) Uani 1 1 d . . . . .
O4 O 0.7919(5) 0.5438(4) 0.1475(2) 0.0461(11) Uani 1 1 d . . . . .
O5 O 0.5971(4) 0.4670(4) 0.2425(2) 0.0427(10) Uani 1 1 d . . . . .
O6 O 0.8461(4) 0.6182(4) 0.3111(2) 0.0367(9) Uani 1 1 d . . . . .
O7 O 1.0262(4) 0.5876(4) 0.2796(2) 0.0399(10) Uani 1 1 d . . . . .
O8 O 0.9536(5) 0.4267(4) 0.1680(2) 0.0491(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.441(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.356(10) . ?
C2 O1 1.398(8) . ?
C2 C7 1.405(8) . ?
C3 C4 1.405(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.366(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.396(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.404(9) . ?
C6 C8 1.430(10) . ?
C7 O2 1.315(7) . ?
C8 N1 1.258(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.413(18) . ?
C9 N1 1.473(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.451(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.477(9) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.268(10) . ?
C12 C13 1.444(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.390(12) . ?
C13 C18 1.406(9) . ?
C14 C15 1.365(14) . ?
C14 H14 0.9300 . ?
C15 C16 1.388(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.370(10) . ?
C16 H16 0.9300 . ?
C17 O4 1.378(8) . ?
C17 C18 1.421(9) . ?
C18 O3 1.315(8) . ?
C19 O4 1.450(9) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O5 1.441(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.374(9) . ?
C21 O5 1.385(7) . ?
C21 C26 1.414(9) . ?
C22 C23 1.390(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.371(13) . ?
C23 H23 0.9300 . ?
C24 C25 1.410(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(9) . ?
C25 C27 1.434(11) . ?
C26 O6 1.355(7) . ?
C27 N3 1.266(10) . ?
C27 H27 0.9300 . ?
C28 C29 1.22(2) . ?
C28 N3 1.476(11) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.58(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N4 1.474(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C31 N4 1.280(10) . ?
C31 C32 1.423(10) . ?
C31 H31 0.9300 . ?
C32 C37 1.411(8) . ?
C32 C33 1.419(10) . ?
C33 C34 1.338(12) . ?
C33 H33 0.9300 . ?
C34 C35 1.418(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.371(10) . ?
C35 H35 0.9300 . ?
C36 O8 1.382(8) . ?
C36 C37 1.396(9) . ?
C37 O7 1.344(7) . ?
C38 O8 1.433(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N5 1.135(8) . ?
C39 Mo1 2.166(6) . ?
C40 N6 1.165(8) . ?
C40 Mo1 2.137(7) . ?
C41 N7 1.123(8) . ?
C41 Mo1 2.167(6) . ?
C42 N8 1.148(8) . ?
C42 Mo1 2.156(7) . ?
C43 N9 1.142(9) . ?
C43 Mo1 2.167(7) . ?
C44 N10 1.145(10) . ?
C44 Mo1 2.144(8) . ?
C45 N11 1.154(10) . ?
C45 Mo1 2.147(7) . ?
C46 N12 1.144(9) . ?
C46 Mo1 2.163(7) . ?
Cu1 O2 1.960(4) . ?
Cu1 N1 1.976(6) . ?
Cu1 N2 1.987(5) . ?
Cu1 O3 2.008(5) . ?
Cu1 N7 2.312(6) 1_545 ?
Cu1 Tb1 3.5315(8) . ?
Cu2 O6 1.953(4) . ?
Cu2 N3 1.984(6) . ?
Cu2 O7 1.987(4) . ?
Cu2 N4 1.994(6) . ?
Cu2 N5 2.325(6) . ?
Cu2 Tb1 3.5270(8) . ?
Tb1 O3 2.342(4) . ?
Tb1 O7 2.343(4) . ?
Tb1 O6 2.354(4) . ?
Tb1 O2 2.392(5) . ?
Tb1 N8 2.463(6) 1_545 ?
Tb1 O4 2.473(5) . ?
Tb1 O1 2.493(5) . ?
Tb1 O5 2.504(4) . ?
Tb1 O8 2.590(4) . ?
N7 Cu1 2.312(6) 1_565 ?
N8 Tb1 2.463(6) 1_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 123.9(6) . . ?
C3 C2 C7 123.7(7) . . ?
O1 C2 C7 112.3(6) . . ?
C2 C3 C4 118.8(7) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 119.0(8) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 122.4(8) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C5 C6 C7 119.1(7) . . ?
C5 C6 C8 118.6(7) . . ?
C7 C6 C8 122.3(7) . . ?
O2 C7 C6 123.9(6) . . ?
O2 C7 C2 119.2(6) . . ?
C6 C7 C2 116.9(6) . . ?
N1 C8 C6 129.6(7) . . ?
N1 C8 H8 115.2 . . ?
C6 C8 H8 115.2 . . ?
C10 C9 N1 116.1(10) . . ?
C10 C9 H9A 108.3 . . ?
N1 C9 H9A 108.3 . . ?
C10 C9 H9B 108.3 . . ?
N1 C9 H9B 108.3 . . ?
H9A C9 H9B 107.4 . . ?
C9 C10 C11 122.1(12) . . ?
C9 C10 H10A 106.8 . . ?
C11 C10 H10A 106.8 . . ?
C9 C10 H10B 106.8 . . ?
C11 C10 H10B 106.8 . . ?
H10A C10 H10B 106.6 . . ?
C10 C11 N2 111.1(7) . . ?
C10 C11 H11A 109.4 . . ?
N2 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
N2 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N2 C12 C13 128.4(6) . . ?
N2 C12 H12 115.8 . . ?
C13 C12 H12 115.8 . . ?
C14 C13 C18 120.7(8) . . ?
C14 C13 C12 116.8(7) . . ?
C18 C13 C12 122.5(7) . . ?
C15 C14 C13 120.8(8) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 120.2(9) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C17 C16 C15 120.0(9) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 O4 125.0(7) . . ?
C16 C17 C18 121.4(7) . . ?
O4 C17 C18 113.5(6) . . ?
O3 C18 C13 124.9(7) . . ?
O3 C18 C17 118.1(5) . . ?
C13 C18 C17 116.9(6) . . ?
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 . . ?
C22 C21 O5 125.6(7) . . ?
C22 C21 C26 121.1(6) . . ?
O5 C21 C26 113.4(5) . . ?
C21 C22 C23 119.3(8) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
C24 C23 C22 120.6(8) . . ?
C24 C23 H23 119.7 . . ?
C22 C23 H23 119.7 . . ?
C23 C24 C25 120.5(8) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C26 C25 C24 119.4(8) . . ?
C26 C25 C27 124.0(7) . . ?
C24 C25 C27 116.6(7) . . ?
O6 C26 C25 123.9(6) . . ?
O6 C26 C21 117.0(5) . . ?
C25 C26 C21 119.1(6) . . ?
N3 C27 C25 128.5(6) . . ?
N3 C27 H27 115.8 . . ?
C25 C27 H27 115.8 . . ?
C29 C28 N3 127.9(13) . . ?
C29 C28 H28A 105.3 . . ?
N3 C28 H28A 105.3 . . ?
C29 C28 H28B 105.3 . . ?
N3 C28 H28B 105.3 . . ?
H28A C28 H28B 106.0 . . ?
C28 C29 C30 119.9(18) . . ?
C28 C29 H29A 107.3 . . ?
C30 C29 H29A 107.3 . . ?
C28 C29 H29B 107.3 . . ?
C30 C29 H29B 107.3 . . ?
H29A C29 H29B 106.9 . . ?
N4 C30 C29 115.3(10) . . ?
N4 C30 H30A 108.4 . . ?
C29 C30 H30A 108.4 . . ?
N4 C30 H30B 108.4 . . ?
C29 C30 H30B 108.4 . . ?
H30A C30 H30B 107.5 . . ?
H29C C29A H29D 107.4 . . ?
N4 C31 C32 129.0(6) . . ?
N4 C31 H31 115.5 . . ?
C32 C31 H31 115.5 . . ?
C37 C32 C33 119.1(6) . . ?
C37 C32 C31 123.3(6) . . ?
C33 C32 C31 117.4(6) . . ?
C34 C33 C32 121.5(7) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C33 C34 C35 119.6(7) . . ?
C33 C34 H34 120.2 . . ?
C35 C34 H34 120.2 . . ?
C36 C35 C34 120.1(7) . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 O8 123.9(6) . . ?
C35 C36 C37 121.2(6) . . ?
O8 C36 C37 114.9(6) . . ?
O7 C37 C36 118.3(5) . . ?
O7 C37 C32 123.3(6) . . ?
C36 C37 C32 118.5(6) . . ?
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 178.1(6) . . ?
N6 C40 Mo1 179.4(7) . . ?
N7 C41 Mo1 175.9(6) . . ?
N8 C42 Mo1 175.7(7) . . ?
N9 C43 Mo1 178.4(9) . . ?
N10 C44 Mo1 176.4(11) . . ?
N11 C45 Mo1 176.3(9) . . ?
N12 C46 Mo1 177.7(7) . . ?
O2 Cu1 N1 92.2(2) . . ?
O2 Cu1 N2 169.5(2) . . ?
N1 Cu1 N2 95.4(3) . . ?
O2 Cu1 O3 78.86(18) . . ?
N1 Cu1 O3 160.5(2) . . ?
N2 Cu1 O3 91.7(2) . . ?
O2 Cu1 N7 95.53(19) . 1_545 ?
N1 Cu1 N7 98.1(3) . 1_545 ?
N2 Cu1 N7 90.6(2) . 1_545 ?
O3 Cu1 N7 100.0(2) . 1_545 ?
O2 Cu1 Tb1 40.08(14) . . ?
N1 Cu1 Tb1 131.17(18) . . ?
N2 Cu1 Tb1 130.71(19) . . ?
O3 Cu1 Tb1 39.01(11) . . ?
N7 Cu1 Tb1 96.79(16) 1_545 . ?
O6 Cu2 N3 93.1(2) . . ?
O6 Cu2 O7 76.92(16) . . ?
N3 Cu2 O7 161.6(3) . . ?
O6 Cu2 N4 168.1(2) . . ?
N3 Cu2 N4 96.9(3) . . ?
O7 Cu2 N4 91.7(2) . . ?
O6 Cu2 N5 91.72(19) . . ?
N3 Cu2 N5 91.4(3) . . ?
O7 Cu2 N5 104.1(2) . . ?
N4 Cu2 N5 94.4(2) . . ?
O6 Cu2 Tb1 38.97(11) . . ?
N3 Cu2 Tb1 127.1(2) . . ?
O7 Cu2 Tb1 38.97(12) . . ?
N4 Cu2 Tb1 129.22(17) . . ?
N5 Cu2 Tb1 106.80(14) . . ?
O3 Tb1 O7 136.52(15) . . ?
O3 Tb1 O6 136.80(15) . . ?
O7 Tb1 O6 62.88(13) . . ?
O3 Tb1 O2 64.33(14) . . ?
O7 Tb1 O2 151.21(16) . . ?
O6 Tb1 O2 119.12(14) . . ?
O3 Tb1 N8 100.02(18) . 1_545 ?
O7 Tb1 N8 80.78(18) . 1_545 ?
O6 Tb1 N8 122.92(18) . 1_545 ?
O2 Tb1 N8 74.99(18) . 1_545 ?
O3 Tb1 O4 65.17(15) . . ?
O7 Tb1 O4 83.46(17) . . ?
O6 Tb1 O4 85.13(15) . . ?
O2 Tb1 O4 124.86(15) . . ?
N8 Tb1 O4 134.9(2) 1_545 . ?
O3 Tb1 O1 127.90(15) . . ?
O7 Tb1 O1 93.86(16) . . ?
O6 Tb1 O1 69.36(16) . . ?
O2 Tb1 O1 63.82(14) . . ?
N8 Tb1 O1 71.1(2) 1_545 . ?
O4 Tb1 O1 152.29(16) . . ?
O3 Tb1 O5 79.13(14) . . ?
O7 Tb1 O5 124.93(14) . . ?
O6 Tb1 O5 64.05(14) . . ?
O2 Tb1 O5 71.77(15) . . ?
N8 Tb1 O5 143.4(2) 1_545 . ?
O4 Tb1 O5 78.47(16) . . ?
O1 Tb1 O5 80.65(16) . . ?
O3 Tb1 O8 76.20(14) . . ?
O7 Tb1 O8 63.83(14) . . ?
O6 Tb1 O8 121.83(14) . . ?
O2 Tb1 O8 118.69(14) . . ?
N8 Tb1 O8 67.8(2) 1_545 . ?
O4 Tb1 O8 67.32(17) . . ?
O1 Tb1 O8 135.52(17) . . ?
O5 Tb1 O8 143.83(16) . . ?
O3 Tb1 Cu2 153.74(11) . . ?
O7 Tb1 Cu2 32.22(9) . . ?
O6 Tb1 Cu2 31.45(10) . . ?
O2 Tb1 Cu2 138.56(9) . . ?
N8 Tb1 Cu2 99.43(14) 1_545 . ?
O4 Tb1 Cu2 88.58(11) . . ?
O1 Tb1 Cu2 75.42(11) . . ?
O5 Tb1 Cu2 95.39(10) . . ?
O8 Tb1 Cu2 95.19(10) . . ?
O3 Tb1 Cu1 32.66(11) . . ?
O7 Tb1 Cu1 158.98(10) . . ?
O6 Tb1 Cu1 138.12(10) . . ?
O2 Tb1 Cu1 31.85(10) . . ?
N8 Tb1 Cu1 84.66(14) 1_545 . ?
O4 Tb1 Cu1 96.41(11) . . ?
O1 Tb1 Cu1 95.66(11) . . ?
O5 Tb1 Cu1 75.23(10) . . ?
O8 Tb1 Cu1 96.63(10) . . ?
Cu2 Tb1 Cu1 168.174(18) . . ?
C40 Mo1 C44 140.0(3) . . ?
C40 Mo1 C45 122.4(3) . . ?
C44 Mo1 C45 76.6(4) . . ?
C40 Mo1 C42 141.2(2) . . ?
C44 Mo1 C42 73.7(3) . . ?
C45 Mo1 C42 75.7(3) . . ?
C40 Mo1 C46 74.2(3) . . ?
C44 Mo1 C46 144.5(3) . . ?
C45 Mo1 C46 74.0(3) . . ?
C42 Mo1 C46 79.9(3) . . ?
C40 Mo1 C39 73.5(2) . . ?
C44 Mo1 C39 81.8(3) . . ?
C45 Mo1 C39 72.0(3) . . ?
C42 Mo1 C39 143.1(2) . . ?
C46 Mo1 C39 107.3(3) . . ?
C40 Mo1 C41 76.6(3) . . ?
C44 Mo1 C41 112.6(3) . . ?
C45 Mo1 C41 139.9(3) . . ?
C42 Mo1 C41 70.5(2) . . ?
C46 Mo1 C41 79.3(3) . . ?
C39 Mo1 C41 146.0(2) . . ?
C40 Mo1 C43 75.2(3) . . ?
C44 Mo1 C43 70.6(3) . . ?
C45 Mo1 C43 140.5(3) . . ?
C42 Mo1 C43 114.0(3) . . ?
C46 Mo1 C43 143.7(3) . . ?
C39 Mo1 C43 82.0(3) . . ?
C41 Mo1 C43 74.9(2) . . ?
C8 N1 C9 115.7(7) . . ?
C8 N1 Cu1 123.0(5) . . ?
C9 N1 Cu1 121.4(6) . . ?
C12 N2 C11 116.3(6) . . ?
C12 N2 Cu1 124.4(5) . . ?
C11 N2 Cu1 119.2(5) . . ?
C27 N3 C28 117.4(7) . . ?
C27 N3 Cu2 124.0(5) . . ?
C28 N3 Cu2 118.4(6) . . ?
C31 N4 C30 115.4(6) . . ?
C31 N4 Cu2 121.0(5) . . ?
C30 N4 Cu2 122.9(5) . . ?
C39 N5 Cu2 142.8(6) . . ?
C41 N7 Cu1 138.8(5) . 1_565 ?
C42 N8 Tb1 148.9(6) . 1_565 ?
C2 O1 C1 117.1(6) . . ?
C2 O1 Tb1 116.4(4) . . ?
C1 O1 Tb1 126.5(5) . . ?
C7 O2 Cu1 126.8(4) . . ?
C7 O2 Tb1 119.9(4) . . ?
Cu1 O2 Tb1 108.1(2) . . ?
C18 O3 Cu1 124.4(4) . . ?
C18 O3 Tb1 123.9(4) . . ?
Cu1 O3 Tb1 108.34(19) . . ?
C17 O4 C19 115.3(6) . . ?
C17 O4 Tb1 119.1(4) . . ?
C19 O4 Tb1 124.5(5) . . ?
C21 O5 C20 115.4(5) . . ?
C21 O5 Tb1 115.5(4) . . ?
C20 O5 Tb1 128.4(4) . . ?
C26 O6 Cu2 126.3(4) . . ?
C26 O6 Tb1 120.1(4) . . ?
Cu2 O6 Tb1 109.58(17) . . ?
C37 O7 Cu2 123.4(4) . . ?
C37 O7 Tb1 125.9(4) . . ?
Cu2 O7 Tb1 108.81(17) . . ?
C36 O8 C38 117.2(5) . . ?
C36 O8 Tb1 117.0(4) . . ?
C38 O8 Tb1 124.8(4) . . ?

_refine_diff_density_max         1.043
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.123

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_5
_database_code_depnum_ccdc_archive 'CCDC 1060176'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C47.30 H44.65 Cu2 Ho Mo N12.65 O9.35'
_chemical_formula_weight         1327.85

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3617(11)
_cell_length_b                   12.4459(11)
_cell_length_c                   21.2819(17)
_cell_angle_alpha                105.814(7)
_cell_angle_beta                 92.659(7)
_cell_angle_gamma                116.095(7)
_cell_volume                     2551.8(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14140
_cell_measurement_theta_min      1.85
_cell_measurement_theta_max      28.15

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_F_000             1318
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.664
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5352
_exptl_absorpt_correction_T_max  0.5864
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE-IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16234
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.862
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measured_fraction_theta_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_point_group_measured_fraction_full 0.911
_reflns_number_total             8420
_reflns_number_gt                5367
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
3 geometrical restraints were used for the refinement of the acetonitrile molecule and 6 restraints were used to model the fragment C28A-C29A-C30A
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0466P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8420
_refine_ls_number_parameters     704
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1086
_refine_ls_wR_factor_gt          0.0989
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_restrained_S_all      0.894
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?

_refine_diff_density_max         1.674
_refine_diff_density_min         -2.010
_refine_diff_density_rms         0.125

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_6
_database_code_depnum_ccdc_archive 'CCDC 1060177'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H44 Cu2 N12 O10 Tb W'
_chemical_formula_weight         1394.78

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'
Tb Tb -0.1723 4.1537 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.3977(5)
_cell_length_b                   12.3689(6)
_cell_length_c                   20.5363(10)
_cell_angle_alpha                95.088(4)
_cell_angle_beta                 101.795(4)
_cell_angle_gamma                116.645(3)
_cell_volume                     2478.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    34535
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      32.79

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             1362
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    4.638
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1564
_exptl_absorpt_correction_T_max  0.2404
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            51385
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_av_R_equivalents  0.0664
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.360
_diffrn_reflns_theta_max         33.435
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             19188
_reflns_number_gt                11863
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0553P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         19188
_refine_ls_number_parameters     658
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1003
_refine_ls_R_factor_gt           0.0530
_refine_ls_wR_factor_ref         0.1194
_refine_ls_wR_factor_gt          0.1051
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_restrained_S_all      0.955
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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 0.8889(9) 0.4558(9) 0.4190(4) 0.092(3) Uani 1 1 d . . . . .
H1A H 0.9717 0.5102 0.4089 0.138 Uiso 1 1 calc R U . . .
H1B H 0.8691 0.5017 0.4513 0.138 Uiso 1 1 calc R U . . .
H1C H 0.8996 0.3913 0.4377 0.138 Uiso 1 1 calc R U . . .
C2 C 0.6506(7) 0.3209(6) 0.3627(3) 0.0461(13) Uani 1 1 d . . . . .
C3 C 0.6066(9) 0.3244(8) 0.4199(4) 0.066(2) Uani 1 1 d . . . . .
H3 H 0.6647 0.3830 0.4593 0.080 Uiso 1 1 calc R U . . .
C4 C 0.4754(10) 0.2402(10) 0.4184(5) 0.086(3) Uani 1 1 d . . . . .
H4 H 0.4435 0.2434 0.4563 0.103 Uiso 1 1 calc R U . . .
C5 C 0.3917(8) 0.1512(9) 0.3605(4) 0.076(3) Uani 1 1 d . . . . .
H5 H 0.3043 0.0931 0.3603 0.091 Uiso 1 1 calc R U . . .
C6 C 0.4355(6) 0.1464(6) 0.3023(3) 0.0510(14) Uani 1 1 d . . . . .
C7 C 0.5658(5) 0.2339(5) 0.3016(3) 0.0386(11) Uani 1 1 d . . . . .
C8 C 0.3447(7) 0.0475(7) 0.2447(4) 0.065(2) Uani 1 1 d . . . . .
H8 H 0.2648 -0.0119 0.2519 0.078 Uiso 1 1 calc R U . . .
C9 C 0.2541(11) -0.0924(9) 0.1411(5) 0.118(5) Uani 1 1 d . . . . .
H9A H 0.2918 -0.1488 0.1432 0.142 Uiso 1 1 calc R U . . .
H9B H 0.1747 -0.1260 0.1584 0.142 Uiso 1 1 calc R U . . .
C10 C 0.2119(11) -0.0865(11) 0.0718(6) 0.115(4) Uani 1 1 d . . . . .
H10A H 0.1748 -0.0295 0.0707 0.138 Uiso 1 1 calc R U . . .
H10B H 0.1376 -0.1675 0.0482 0.138 Uiso 1 1 calc R U . . .
C11 C 0.3130(8) -0.0492(7) 0.0328(4) 0.069(2) Uani 1 1 d . . . . .
H11A H 0.2669 -0.0648 -0.0150 0.083 Uiso 1 1 calc R U . . .
H11B H 0.3596 -0.0983 0.0377 0.083 Uiso 1 1 calc R U . . .
C12 C 0.4345(7) 0.1484(7) 0.0113(3) 0.0546(16) Uani 1 1 d . . . . .
H12 H 0.3815 0.1074 -0.0329 0.066 Uiso 1 1 calc R U . . .
C13 C 0.5295(7) 0.2779(7) 0.0203(3) 0.0539(16) Uani 1 1 d . . . . .
C14 C 0.5182(10) 0.3326(10) -0.0364(4) 0.075(2) Uani 1 1 d . . . . .
H14 H 0.4535 0.2844 -0.0771 0.090 Uiso 1 1 calc R U . . .
C15 C 0.6008(13) 0.4548(11) -0.0323(5) 0.096(3) Uani 1 1 d . . . . .
H15 H 0.5924 0.4890 -0.0704 0.115 Uiso 1 1 calc R U . . .
C16 C 0.6969(10) 0.5287(8) 0.0276(4) 0.071(2) Uani 1 1 d . . . . .
H16 H 0.7544 0.6120 0.0302 0.085 Uiso 1 1 calc R U . . .
C17 C 0.7058(7) 0.4766(6) 0.0834(3) 0.0482(14) Uani 1 1 d . . . . .
C18 C 0.6260(6) 0.3518(6) 0.0816(3) 0.0410(12) Uani 1 1 d . . . . .
C19 C 0.8926(10) 0.6691(6) 0.1497(4) 0.076(3) Uani 1 1 d . . . . .
H19A H 0.9478 0.7068 0.1957 0.114 Uiso 1 1 calc R U . . .
H19B H 0.9496 0.6696 0.1210 0.114 Uiso 1 1 calc R U . . .
H19C H 0.8464 0.7145 0.1343 0.114 Uiso 1 1 calc R U . . .
C20 C 0.4627(7) 0.4035(8) 0.1963(4) 0.0621(18) Uani 1 1 d . . . . .
H20A H 0.4619 0.3543 0.1572 0.093 Uiso 1 1 calc R U . . .
H20B H 0.4006 0.3509 0.2191 0.093 Uiso 1 1 calc R U . . .
H20C H 0.4351 0.4625 0.1821 0.093 Uiso 1 1 calc R U . . .
C21 C 0.6133(7) 0.5437(6) 0.3016(4) 0.0507(14) Uani 1 1 d . . . . .
C22 C 0.5086(8) 0.5419(9) 0.3245(4) 0.075(2) Uani 1 1 d . . . . .
H22 H 0.4186 0.4869 0.3005 0.090 Uiso 1 1 calc R U . . .
C23 C 0.5371(10) 0.6234(11) 0.3843(5) 0.094(3) Uani 1 1 d . . . . .
H23 H 0.4666 0.6211 0.4012 0.113 Uiso 1 1 calc R U . . .
C24 C 0.6710(10) 0.7072(11) 0.4180(5) 0.093(3) Uani 1 1 d . . . . .
H24 H 0.6903 0.7643 0.4565 0.112 Uiso 1 1 calc R U . . .
C25 C 0.7767(8) 0.7069(7) 0.3950(4) 0.0613(18) Uani 1 1 d . . . . .
C26 C 0.7506(7) 0.6257(6) 0.3365(3) 0.0473(13) Uani 1 1 d . . . . .
C27 C 0.9129(9) 0.7915(8) 0.4373(4) 0.073(2) Uani 1 1 d . . . . .
H27 H 0.9187 0.8428 0.4751 0.087 Uiso 1 1 calc R U . . .
C28 C 1.1514(11) 0.8968(12) 0.4820(6) 0.118(5) Uani 0.5 1 d . . P A 1
H28A H 1.1313 0.9610 0.4983 0.141 Uiso 0.5 1 calc R U P A 1
H28B H 1.1597 0.8559 0.5195 0.141 Uiso 0.5 1 calc R U P A 1
C29 C 1.265(2) 0.950(2) 0.4742(12) 0.104(8) Uani 0.5 1 d . . P A 1
H29A H 1.3263 0.9997 0.5183 0.124 Uiso 0.5 1 calc R U P A 1
H29B H 1.2638 1.0077 0.4452 0.124 Uiso 0.5 1 calc R U P A 1
C30 C 1.3319(9) 0.8789(9) 0.4446(5) 0.085(3) Uani 0.5 1 d . . P A 1
H30A H 1.4180 0.9383 0.4383 0.103 Uiso 0.5 1 calc R U P A 1
H30B H 1.3516 0.8332 0.4773 0.103 Uiso 0.5 1 calc R U P A 1
C28A C 1.1514(11) 0.8968(12) 0.4820(6) 0.118(5) Uani 0.5 1 d . . P A 2
H28C H 1.1851 0.9755 0.4678 0.141 Uiso 0.5 1 calc R U P A 2
H28D H 1.1273 0.9078 0.5239 0.141 Uiso 0.5 1 calc R U P A 2
C29A C 1.2569(16) 0.8659(14) 0.4956(6) 0.054(3) Uani 0.5 1 d . . P A 2
H29C H 1.2184 0.7808 0.5011 0.065 Uiso 0.5 1 calc R U P A 2
H29D H 1.3214 0.9172 0.5386 0.065 Uiso 0.5 1 calc R U P A 2
C30A C 1.3319(9) 0.8789(9) 0.4446(5) 0.085(3) Uani 0.5 1 d . . P A 2
H30C H 1.4085 0.8646 0.4615 0.103 Uiso 0.5 1 calc R U P A 2
H30D H 1.3680 0.9629 0.4372 0.103 Uiso 0.5 1 calc R U P A 2
C31 C 1.3132(7) 0.7780(7) 0.3384(4) 0.0607(18) Uani 1 1 d . . . . .
H31 H 1.4074 0.8278 0.3531 0.073 Uiso 1 1 calc R U . . .
C32 C 1.2599(7) 0.6947(6) 0.2735(4) 0.0577(17) Uani 1 1 d . . . . .
C33 C 1.3553(7) 0.7050(8) 0.2372(5) 0.076(3) Uani 1 1 d . . . . .
H33 H 1.4458 0.7663 0.2544 0.091 Uiso 1 1 calc R U . . .
C34 C 1.3169(9) 0.6271(10) 0.1781(6) 0.090(3) Uani 1 1 d . . . . .
H34 H 1.3805 0.6372 0.1539 0.108 Uiso 1 1 calc R U . . .
C35 C 1.1823(9) 0.5302(9) 0.1518(5) 0.076(2) Uani 1 1 d . . . . .
H35 H 1.1575 0.4753 0.1112 0.092 Uiso 1 1 calc R U . . .
C36 C 1.0871(7) 0.5177(6) 0.1873(4) 0.0529(15) Uani 1 1 d . . . . .
C37 C 1.1231(6) 0.6011(5) 0.2481(3) 0.0446(13) Uani 1 1 d . . . . .
C38 C 0.9175(9) 0.3236(8) 0.1148(5) 0.078(3) Uani 1 1 d . . . . .
H38A H 0.8223 0.2656 0.1057 0.116 Uiso 1 1 calc R U . . .
H38B H 0.9353 0.3534 0.0744 0.116 Uiso 1 1 calc R U . . .
H38C H 0.9710 0.2837 0.1288 0.116 Uiso 1 1 calc R U . . .
C39 C 0.9919(5) 0.9266(5) 0.2750(3) 0.0400(11) Uani 1 1 d . . . . .
C40 C 0.7324(6) 0.8342(6) 0.2204(3) 0.0430(13) Uani 1 1 d . . . . .
C41 C 0.7123(6) 1.0286(5) 0.1829(3) 0.0442(13) Uani 1 1 d . . . . .
C42 C 0.8986(6) 1.2092(6) 0.2696(3) 0.0473(14) Uani 1 1 d . . . . .
C43 C 0.8893(7) 0.9680(7) 0.1499(4) 0.0527(15) Uani 1 1 d . . . . .
C44 C 1.0751(7) 1.1543(7) 0.2358(5) 0.068(2) Uani 1 1 d . . . . .
C45 C 1.0142(8) 1.1114(7) 0.3526(4) 0.0624(19) Uani 1 1 d . . . . .
C46 C 0.7502(7) 0.9991(6) 0.3144(3) 0.0532(16) Uani 1 1 d . . . . .
Cu1 Cu 0.50898(6) 0.14931(6) 0.15481(3) 0.03752(14) Uani 1 1 d . . . . .
Cu2 Cu 1.04397(7) 0.71898(6) 0.34902(4) 0.04372(16) Uani 1 1 d . . . . .
Tb1 Tb 0.79751(2) 0.43326(2) 0.24142(2) 0.03205(6) Uani 1 1 d . . . . .
W1 W 0.88339(2) 1.02852(2) 0.25044(2) 0.03409(6) Uani 1 1 d . . . . .
N1 N 0.3584(5) 0.0303(5) 0.1862(3) 0.0572(15) Uani 1 1 d . . . . .
N2 N 0.4148(5) 0.0843(5) 0.0565(3) 0.0482(12) Uani 1 1 d . . . . .
N3 N 1.0259(7) 0.8043(6) 0.4291(3) 0.0717(19) Uani 1 1 d . . . . .
N4 N 1.2448(5) 0.7911(5) 0.3784(3) 0.0519(13) Uani 1 1 d . . . . .
N5 N 1.0490(5) 0.8726(5) 0.2898(3) 0.0497(12) Uani 1 1 d . . . . .
N6 N 0.6540(6) 0.7330(5) 0.2033(3) 0.0570(14) Uani 1 1 d . . . . .
N7 N 0.6232(6) 1.0349(6) 0.1487(3) 0.0596(15) Uani 1 1 d . . . . .
N8 N 0.9023(6) 1.3042(5) 0.2766(4) 0.0592(15) Uani 1 1 d . . . . .
N9 N 0.8910(8) 0.9387(9) 0.0954(4) 0.082(2) Uani 1 1 d . . . . .
N10 N 1.1737(9) 1.2237(8) 0.2260(7) 0.125(4) Uani 1 1 d . . . . .
N11 N 1.0883(9) 1.1543(10) 0.4059(4) 0.107(3) Uani 1 1 d . . . . .
N12 N 0.6750(8) 0.9813(8) 0.3475(4) 0.087(3) Uani 1 1 d . . . . .
O1 O 0.7794(5) 0.4027(4) 0.3581(2) 0.0520(11) Uani 1 1 d . . . . .
O2 O 0.6134(4) 0.2436(3) 0.24731(19) 0.0377(8) Uani 1 1 d . . . . .
O1W O 0.8613(16) 0.7919(13) -0.0446(7) 0.189(5) Uani 1 1 d . . . . .
O3 O 0.6441(4) 0.3072(3) 0.13727(18) 0.0373(8) Uani 1 1 d . . . . .
O2W O 0.7991(17) 0.5523(16) 0.5817(11) 0.274(10) Uani 1 1 d . . . . .
O4 O 0.7936(5) 0.5436(4) 0.1467(2) 0.0502(10) Uani 1 1 d . . . . .
O5 O 0.5990(4) 0.4681(4) 0.2421(2) 0.0452(9) Uani 1 1 d . . . . .
O6 O 0.8480(4) 0.6204(4) 0.3111(2) 0.0415(8) Uani 1 1 d . . . . .
O7 O 1.0281(4) 0.5878(4) 0.2789(2) 0.0459(10) Uani 1 1 d . . . . .
O8 O 0.9532(4) 0.4252(4) 0.1677(2) 0.0553(12) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.426(8) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.372(9) . ?
C2 O1 1.389(8) . ?
C2 C7 1.414(8) . ?
C3 C4 1.378(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.377(13) . ?
C4 H4 0.9300 . ?
C5 C6 1.393(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.396(8) . ?
C6 C8 1.440(10) . ?
C7 O2 1.327(6) . ?
C8 N1 1.255(10) . ?
C8 H8 0.9300 . ?
C9 C10 1.424(17) . ?
C9 N1 1.502(9) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.466(14) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.489(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C12 N2 1.264(10) . ?
C12 C13 1.443(11) . ?
C12 H12 0.9300 . ?
C13 C18 1.399(8) . ?
C13 C14 1.409(11) . ?
C14 C15 1.359(14) . ?
C14 H14 0.9300 . ?
C15 C16 1.379(13) . ?
C15 H15 0.9300 . ?
C16 C17 1.370(10) . ?
C16 H16 0.9300 . ?
C17 O4 1.383(8) . ?
C17 C18 1.389(9) . ?
C18 O3 1.331(7) . ?
C19 O4 1.439(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O5 1.447(8) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.362(10) . ?
C21 O5 1.405(8) . ?
C21 C26 1.407(9) . ?
C22 C23 1.397(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.380(14) . ?
C23 H23 0.9300 . ?
C24 C25 1.382(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(9) . ?
C25 C27 1.446(11) . ?
C26 O6 1.344(7) . ?
C27 N3 1.273(11) . ?
C27 H27 0.9300 . ?
C28 C29 1.21(2) . ?
C28 N3 1.487(10) . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.56(3) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 N4 1.494(9) . ?
C30 H30A 0.9700 . ?
C30 H30B 0.9700 . ?
C29A H29C 0.9700 . ?
C29A H29D 0.9700 . ?
C31 N4 1.288(10) . ?
C31 C32 1.439(10) . ?
C31 H31 0.9300 . ?
C32 C33 1.407(10) . ?
C32 C37 1.409(8) . ?
C33 C34 1.337(13) . ?
C33 H33 0.9300 . ?
C34 C35 1.407(12) . ?
C34 H34 0.9300 . ?
C35 C36 1.388(10) . ?
C35 H35 0.9300 . ?
C36 O8 1.379(8) . ?
C36 C37 1.404(9) . ?
C37 O7 1.319(7) . ?
C38 O8 1.430(8) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N5 1.144(7) . ?
C39 W1 2.151(6) . ?
C40 N6 1.130(8) . ?
C40 W1 2.171(6) . ?
C41 N7 1.148(8) . ?
C41 W1 2.150(6) . ?
C42 N8 1.151(8) . ?
C42 W1 2.156(6) . ?
C43 N9 1.152(9) . ?
C43 W1 2.159(7) . ?
C44 N10 1.140(10) . ?
C44 W1 2.142(7) . ?
C45 N11 1.144(10) . ?
C45 W1 2.155(7) . ?
C46 N12 1.158(9) . ?
C46 W1 2.137(7) . ?
Cu1 O2 1.955(4) . ?
Cu1 N1 1.970(5) . ?
Cu1 N2 1.981(5) . ?
Cu1 O3 1.992(4) . ?
Cu1 N7 2.324(6) 1_545 ?
Cu1 Tb1 3.5292(7) . ?
Cu2 O6 1.939(4) . ?
Cu2 N3 1.972(6) . ?
Cu2 N4 1.977(5) . ?
Cu2 O7 1.989(4) . ?
Cu2 N5 2.330(6) . ?
Cu2 Tb1 3.5265(7) . ?
Tb1 O3 2.345(3) . ?
Tb1 O7 2.358(4) . ?
Tb1 O6 2.370(4) . ?
Tb1 O2 2.379(4) . ?
Tb1 N8 2.462(6) 1_545 ?
Tb1 O4 2.478(5) . ?
Tb1 O5 2.488(4) . ?
Tb1 O1 2.494(4) . ?
Tb1 O8 2.585(4) . ?
N7 Cu1 2.324(6) 1_565 ?
N8 Tb1 2.462(6) 1_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 124.2(6) . . ?
C3 C2 C7 122.4(6) . . ?
O1 C2 C7 113.4(5) . . ?
C2 C3 C4 119.3(7) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 119.9(7) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
C4 C5 C6 121.3(7) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C5 C6 C7 120.0(6) . . ?
C5 C6 C8 118.2(6) . . ?
C7 C6 C8 121.8(6) . . ?
O2 C7 C6 124.7(5) . . ?
O2 C7 C2 118.2(5) . . ?
C6 C7 C2 117.1(5) . . ?
N1 C8 C6 129.0(6) . . ?
N1 C8 H8 115.5 . . ?
C6 C8 H8 115.5 . . ?
C10 C9 N1 113.9(9) . . ?
C10 C9 H9A 108.8 . . ?
N1 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
N1 C9 H9B 108.8 . . ?
H9A C9 H9B 107.7 . . ?
C9 C10 C11 118.6(10) . . ?
C9 C10 H10A 107.7 . . ?
C11 C10 H10A 107.7 . . ?
C9 C10 H10B 107.7 . . ?
C11 C10 H10B 107.7 . . ?
H10A C10 H10B 107.1 . . ?
C10 C11 N2 111.2(7) . . ?
C10 C11 H11A 109.4 . . ?
N2 C11 H11A 109.4 . . ?
C10 C11 H11B 109.4 . . ?
N2 C11 H11B 109.4 . . ?
H11A C11 H11B 108.0 . . ?
N2 C12 C13 127.6(5) . . ?
N2 C12 H12 116.2 . . ?
C13 C12 H12 116.2 . . ?
C18 C13 C14 119.0(7) . . ?
C18 C13 C12 124.4(6) . . ?
C14 C13 C12 116.6(6) . . ?
C15 C14 C13 120.9(8) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C16 120.8(9) . . ?
C14 C15 H15 119.6 . . ?
C16 C15 H15 119.6 . . ?
C17 C16 C15 118.5(8) . . ?
C17 C16 H16 120.7 . . ?
C15 C16 H16 120.7 . . ?
C16 C17 O4 123.2(6) . . ?
C16 C17 C18 123.0(7) . . ?
O4 C17 C18 113.8(5) . . ?
O3 C18 C17 119.5(5) . . ?
O3 C18 C13 122.7(6) . . ?
C17 C18 C13 117.8(6) . . ?
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 . . ?
C22 C21 O5 125.4(6) . . ?
C22 C21 C26 121.8(7) . . ?
O5 C21 C26 112.8(5) . . ?
C21 C22 C23 119.5(8) . . ?
C21 C22 H22 120.2 . . ?
C23 C22 H22 120.2 . . ?
C24 C23 C22 119.4(8) . . ?
C24 C23 H23 120.3 . . ?
C22 C23 H23 120.3 . . ?
C23 C24 C25 120.6(8) . . ?
C23 C24 H24 119.7 . . ?
C25 C24 H24 119.7 . . ?
C24 C25 C26 120.8(8) . . ?
C24 C25 C27 115.9(7) . . ?
C26 C25 C27 123.2(7) . . ?
O6 C26 C25 124.0(6) . . ?
O6 C26 C21 118.2(5) . . ?
C25 C26 C21 117.8(6) . . ?
N3 C27 C25 127.9(7) . . ?
N3 C27 H27 116.0 . . ?
C25 C27 H27 116.0 . . ?
C29 C28 N3 125.9(14) . . ?
C29 C28 H28A 105.9 . . ?
N3 C28 H28A 105.9 . . ?
C29 C28 H28B 105.8 . . ?
N3 C28 H28B 105.9 . . ?
H28A C28 H28B 106.2 . . ?
C28 C29 C30 122(2) . . ?
C28 C29 H29A 106.9 . . ?
C30 C29 H29A 106.9 . . ?
C28 C29 H29B 106.9 . . ?
C30 C29 H29B 106.9 . . ?
H29A C29 H29B 106.7 . . ?
N4 C30 C29 113.6(10) . . ?
N4 C30 H30A 108.9 . . ?
C29 C30 H30A 108.9 . . ?
N4 C30 H30B 108.9 . . ?
C29 C30 H30B 108.9 . . ?
H30A C30 H30B 107.7 . . ?
H29C C29A H29D 107.4 . . ?
N4 C31 C32 127.2(6) . . ?
N4 C31 H31 116.4 . . ?
C32 C31 H31 116.4 . . ?
C33 C32 C37 120.0(7) . . ?
C33 C32 C31 116.1(6) . . ?
C37 C32 C31 123.7(6) . . ?
C34 C33 C32 120.5(7) . . ?
C34 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C33 C34 C35 121.4(8) . . ?
C33 C34 H34 119.3 . . ?
C35 C34 H34 119.3 . . ?
C36 C35 C34 118.9(8) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
O8 C36 C35 124.5(6) . . ?
O8 C36 C37 114.6(5) . . ?
C35 C36 C37 120.9(6) . . ?
O7 C37 C36 118.7(5) . . ?
O7 C37 C32 123.1(6) . . ?
C36 C37 C32 118.2(6) . . ?
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 W1 178.1(6) . . ?
N6 C40 W1 178.5(6) . . ?
N7 C41 W1 176.3(5) . . ?
N8 C42 W1 176.5(6) . . ?
N9 C43 W1 177.5(7) . . ?
N10 C44 W1 176.5(9) . . ?
N11 C45 W1 176.6(8) . . ?
N12 C46 W1 178.1(6) . . ?
O2 Cu1 N1 92.4(2) . . ?
O2 Cu1 N2 169.4(2) . . ?
N1 Cu1 N2 95.7(2) . . ?
O2 Cu1 O3 78.52(15) . . ?
N1 Cu1 O3 161.3(2) . . ?
N2 Cu1 O3 91.8(2) . . ?
O2 Cu1 N7 96.15(18) . 1_545 ?
N1 Cu1 N7 97.7(3) . 1_545 ?
N2 Cu1 N7 89.6(2) . 1_545 ?
O3 Cu1 N7 99.5(2) . 1_545 ?
O2 Cu1 Tb1 39.71(11) . . ?
N1 Cu1 Tb1 131.11(16) . . ?
N2 Cu1 Tb1 130.78(17) . . ?
O3 Cu1 Tb1 39.02(10) . . ?
N7 Cu1 Tb1 97.01(15) 1_545 . ?
O6 Cu2 N3 92.9(2) . . ?
O6 Cu2 N4 168.6(2) . . ?
N3 Cu2 N4 96.9(3) . . ?
O6 Cu2 O7 77.61(16) . . ?
N3 Cu2 O7 162.4(3) . . ?
N4 Cu2 O7 91.4(2) . . ?
O6 Cu2 N5 91.40(18) . . ?
N3 Cu2 N5 91.1(3) . . ?
N4 Cu2 N5 94.1(2) . . ?
O7 Cu2 N5 103.8(2) . . ?
O6 Cu2 Tb1 39.32(11) . . ?
N3 Cu2 Tb1 127.3(2) . . ?
N4 Cu2 Tb1 129.34(16) . . ?
O7 Cu2 Tb1 39.44(11) . . ?
N5 Cu2 Tb1 106.87(13) . . ?
O3 Tb1 O7 136.23(14) . . ?
O3 Tb1 O6 136.91(14) . . ?
O7 Tb1 O6 62.75(13) . . ?
O3 Tb1 O2 63.84(13) . . ?
O7 Tb1 O2 151.68(15) . . ?
O6 Tb1 O2 119.89(13) . . ?
O3 Tb1 N8 99.81(17) . 1_545 ?
O7 Tb1 N8 80.98(17) . 1_545 ?
O6 Tb1 N8 123.05(18) . 1_545 ?
O2 Tb1 N8 74.87(17) . 1_545 ?
O3 Tb1 O4 65.33(14) . . ?
O7 Tb1 O4 82.98(16) . . ?
O6 Tb1 O4 84.99(14) . . ?
O2 Tb1 O4 124.73(14) . . ?
N8 Tb1 O4 134.6(2) 1_545 . ?
O3 Tb1 O5 79.02(13) . . ?
O7 Tb1 O5 124.97(14) . . ?
O6 Tb1 O5 64.34(13) . . ?
O2 Tb1 O5 72.07(14) . . ?
N8 Tb1 O5 143.55(19) 1_545 . ?
O4 Tb1 O5 78.47(16) . . ?
O3 Tb1 O1 127.86(14) . . ?
O7 Tb1 O1 94.25(15) . . ?
O6 Tb1 O1 69.39(15) . . ?
O2 Tb1 O1 64.30(13) . . ?
N8 Tb1 O1 71.5(2) 1_545 . ?
O4 Tb1 O1 152.16(15) . . ?
O5 Tb1 O1 80.63(16) . . ?
O3 Tb1 O8 76.07(14) . . ?
O7 Tb1 O8 63.68(13) . . ?
O6 Tb1 O8 121.58(14) . . ?
O2 Tb1 O8 118.21(14) . . ?
N8 Tb1 O8 67.8(2) 1_545 . ?
O4 Tb1 O8 67.03(17) . . ?
O5 Tb1 O8 143.48(16) . . ?
O1 Tb1 O8 135.88(17) . . ?
O3 Tb1 Cu2 153.80(9) . . ?
O7 Tb1 Cu2 32.40(10) . . ?
O6 Tb1 Cu2 31.22(10) . . ?
O2 Tb1 Cu2 139.05(9) . . ?
N8 Tb1 Cu2 99.55(13) 1_545 . ?
O4 Tb1 Cu2 88.49(10) . . ?
O5 Tb1 Cu2 95.46(9) . . ?
O1 Tb1 Cu2 75.37(10) . . ?
O8 Tb1 Cu2 95.27(10) . . ?
O3 Tb1 Cu1 32.33(9) . . ?
O7 Tb1 Cu1 158.70(10) . . ?
O6 Tb1 Cu1 138.52(10) . . ?
O2 Tb1 Cu1 31.67(9) . . ?
N8 Tb1 Cu1 84.62(13) 1_545 . ?
O4 Tb1 Cu1 96.29(10) . . ?
O5 Tb1 Cu1 75.26(9) . . ?
O1 Tb1 Cu1 95.97(10) . . ?
O8 Tb1 Cu1 96.32(10) . . ?
Cu2 Tb1 Cu1 168.402(19) . . ?
C46 W1 C44 144.6(3) . . ?
C46 W1 C41 79.1(3) . . ?
C44 W1 C41 112.9(3) . . ?
C46 W1 C39 108.1(3) . . ?
C44 W1 C39 81.1(3) . . ?
C41 W1 C39 145.6(2) . . ?
C46 W1 C45 74.1(3) . . ?
C44 W1 C45 76.6(4) . . ?
C41 W1 C45 139.7(3) . . ?
C39 W1 C45 72.6(3) . . ?
C46 W1 C42 79.8(3) . . ?
C44 W1 C42 74.1(3) . . ?
C41 W1 C42 70.4(2) . . ?
C39 W1 C42 143.3(2) . . ?
C45 W1 C42 75.6(3) . . ?
C46 W1 C43 142.9(2) . . ?
C44 W1 C43 71.3(3) . . ?
C41 W1 C43 75.3(2) . . ?
C39 W1 C43 80.6(2) . . ?
C45 W1 C43 140.8(3) . . ?
C42 W1 C43 115.2(3) . . ?
C46 W1 C40 73.9(2) . . ?
C44 W1 C40 140.1(3) . . ?
C41 W1 C40 76.6(2) . . ?
C39 W1 C40 73.6(2) . . ?
C45 W1 C40 122.3(3) . . ?
C42 W1 C40 140.9(2) . . ?
C43 W1 C40 74.5(2) . . ?
C8 N1 C9 115.2(6) . . ?
C8 N1 Cu1 123.8(4) . . ?
C9 N1 Cu1 121.0(5) . . ?
C12 N2 C11 116.5(6) . . ?
C12 N2 Cu1 124.6(4) . . ?
C11 N2 Cu1 118.9(5) . . ?
C27 N3 C28 116.5(7) . . ?
C27 N3 Cu2 124.4(5) . . ?
C28 N3 Cu2 119.1(6) . . ?
C31 N4 C30 113.8(6) . . ?
C31 N4 Cu2 122.3(4) . . ?
C30 N4 Cu2 123.4(6) . . ?
C39 N5 Cu2 142.2(5) . . ?
C41 N7 Cu1 137.3(5) . 1_565 ?
C42 N8 Tb1 148.5(5) . 1_565 ?
C2 O1 C1 117.8(6) . . ?
C2 O1 Tb1 115.9(3) . . ?
C1 O1 Tb1 126.3(5) . . ?
C7 O2 Cu1 125.9(3) . . ?
C7 O2 Tb1 120.3(3) . . ?
Cu1 O2 Tb1 108.62(17) . . ?
C18 O3 Cu1 125.3(3) . . ?
C18 O3 Tb1 122.6(3) . . ?
Cu1 O3 Tb1 108.65(16) . . ?
C17 O4 C19 116.4(6) . . ?
C17 O4 Tb1 118.7(4) . . ?
C19 O4 Tb1 124.1(4) . . ?
C21 O5 C20 114.9(5) . . ?
C21 O5 Tb1 115.2(4) . . ?
C20 O5 Tb1 128.8(4) . . ?
C26 O6 Cu2 127.2(4) . . ?
C26 O6 Tb1 118.9(3) . . ?
Cu2 O6 Tb1 109.46(17) . . ?
C37 O7 Cu2 124.2(3) . . ?
C37 O7 Tb1 125.8(3) . . ?
Cu2 O7 Tb1 108.16(17) . . ?
C36 O8 C38 117.1(5) . . ?
C36 O8 Tb1 117.2(4) . . ?
C38 O8 Tb1 125.0(4) . . ?

_refine_diff_density_max         2.240
_refine_diff_density_min         -2.669
_refine_diff_density_rms         0.159

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_10
_database_code_depnum_ccdc_archive 'CCDC 1060179'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H35 Cu Dy Mo N11 O10'
_chemical_formula_weight         1019.66

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'
Dy Dy -0.1892 4.4098 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.0527(5)
_cell_length_b                   20.2580(8)
_cell_length_c                   10.3391(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.115(4)
_cell_angle_gamma                90
_cell_volume                     1885.29(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    32240
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      32.51

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_F_000             1006
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    2.915
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3924
_exptl_absorpt_correction_T_max  0.5013
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19278
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.476
_diffrn_reflns_theta_max         26.992
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_point_group_measured_fraction_full 0.961
_reflns_number_total             7897
_reflns_number_gt                7082
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.886
_reflns_Friedel_fraction_max     0.928
_reflns_Friedel_fraction_full    0.932

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3008 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.007(7)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7897
_refine_ls_number_parameters     503
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0666
_refine_ls_wR_factor_gt          0.0652
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_restrained_S_all      0.977
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 0.6901(10) 0.3569(5) 0.8228(9) 0.043(2) Uani 1 1 d . . . . .
H1A H 0.6507 0.3876 0.7543 0.065 Uiso 1 1 calc R U . . .
H1B H 0.7257 0.3819 0.9012 0.065 Uiso 1 1 calc R U . . .
H1C H 0.7725 0.3317 0.7931 0.065 Uiso 1 1 calc R U . . .
C2 C 0.6142(10) 0.2657(4) 0.9481(8) 0.0330(18) Uani 1 1 d . . . . .
C3 C 0.7454(11) 0.2644(5) 1.0305(9) 0.045(2) Uani 1 1 d . . . . .
H3 H 0.8204 0.2965 1.0223 0.054 Uiso 1 1 calc R U . . .
C4 C 0.7662(13) 0.2154(6) 1.1259(10) 0.054(3) Uani 1 1 d . . . . .
H4 H 0.8562 0.2142 1.1821 0.065 Uiso 1 1 calc R U . . .
C5 C 0.6576(13) 0.1687(5) 1.1395(9) 0.052(2) Uani 1 1 d . . . . .
H5 H 0.6739 0.1357 1.2049 0.062 Uiso 1 1 calc R U . . .
C6 C 0.5234(12) 0.1694(5) 1.0576(8) 0.040(2) Uani 1 1 d . . . . .
C7 C 0.5019(9) 0.2179(4) 0.9599(7) 0.0303(17) Uani 1 1 d . . . . .
C8 C 0.4122(14) 0.1199(4) 1.0818(8) 0.049(3) Uani 1 1 d . . . . .
H8 H 0.4395 0.0877 1.1467 0.059 Uiso 1 1 calc R U . . .
C9 C 0.172(2) 0.0646(9) 1.0490(14) 0.115(8) Uani 1 1 d . . . . .
H9 H 0.1823 0.0315 0.9788 0.138 Uiso 1 1 calc R U . . .
C9A C 0.1934(17) 0.0269(7) 1.1609(15) 0.081(4) Uani 1 1 d . . . . .
H9A1 H 0.2973 0.0126 1.1746 0.121 Uiso 1 1 calc R U . . .
H9A2 H 0.1698 0.0532 1.2355 0.121 Uiso 1 1 calc R U . . .
H9A3 H 0.1284 -0.0119 1.1519 0.121 Uiso 1 1 calc R U . . .
C10 C 0.0189(17) 0.0900(8) 1.0151(19) 0.090(5) Uani 1 1 d . . . . .
H10A H -0.0494 0.0523 0.9952 0.108 Uiso 1 1 calc R U . . .
H10B H -0.0135 0.1136 1.0910 0.108 Uiso 1 1 calc R U . . .
C11 C -0.1119(12) 0.1464(5) 0.8318(12) 0.052(3) Uani 1 1 d . . . . .
H11 H -0.1994 0.1247 0.8525 0.063 Uiso 1 1 calc R U . . .
C12 C -0.1257(11) 0.1893(5) 0.7233(10) 0.046(2) Uani 1 1 d . . . . .
C13 C -0.2599(11) 0.1870(6) 0.6365(13) 0.062(3) Uani 1 1 d . . . . .
H13 H -0.3393 0.1598 0.6578 0.074 Uiso 1 1 calc R U . . .
C14 C -0.2769(12) 0.2225(7) 0.5254(13) 0.060(3) Uani 1 1 d . . . . .
H14 H -0.3675 0.2201 0.4701 0.072 Uiso 1 1 calc R U . . .
C15 C -0.1620(11) 0.2626(6) 0.4915(11) 0.052(3) Uani 1 1 d . . . . .
H15 H -0.1727 0.2865 0.4120 0.062 Uiso 1 1 calc R U . . .
C16 C -0.0311(10) 0.2674(5) 0.5755(9) 0.0369(19) Uani 1 1 d . . . . .
C17 C -0.0115(9) 0.2325(4) 0.6919(8) 0.0332(18) Uani 1 1 d . . . . .
C18 C 0.0889(10) 0.3298(6) 0.4226(8) 0.047(3) Uani 1 1 d . . . . .
H18A H 0.1785 0.3562 0.4160 0.071 Uiso 1 1 calc R U . . .
H18B H 0.0871 0.2925 0.3620 0.071 Uiso 1 1 calc R U . . .
H18C H 0.0008 0.3573 0.4007 0.071 Uiso 1 1 calc R U . . .
C19 C 0.4671(8) 0.4043(4) 0.5012(7) 0.0236(15) Uani 1 1 d . . . . .
C20 C 0.7534(9) 0.4389(4) 0.4943(8) 0.0296(17) Uani 1 1 d . . . . .
C21 C 0.7418(10) 0.4282(4) 0.2480(8) 0.0357(18) Uani 1 1 d . . . . .
C22 C 0.3318(10) 0.4889(5) 0.3248(8) 0.0341(18) Uani 1 1 d . . . . .
C23 C 0.5409(9) 0.5303(4) 0.5112(8) 0.0308(17) Uani 1 1 d . . . . .
C24 C 0.4920(10) 0.3653(4) 0.2764(8) 0.0313(17) Uani 1 1 d . . . . .
C25 C 0.6672(9) 0.5525(4) 0.3103(7) 0.0291(16) Uani 1 1 d . . . . .
C26 C 0.4991(11) 0.4789(4) 0.1506(8) 0.0374(19) Uani 1 1 d . . . . .
C27 C 0.1059(12) 0.5519(5) 0.6102(11) 0.052(3) Uani 1 1 d . . . . .
C28 C -0.0037(15) 0.5839(5) 0.5167(13) 0.061(3) Uani 1 1 d . . . . .
H28A H -0.0048 0.5622 0.4320 0.091 Uiso 1 1 calc R U . . .
H28B H 0.0223 0.6305 0.5083 0.091 Uiso 1 1 calc R U . . .
H28C H -0.1023 0.5804 0.5472 0.091 Uiso 1 1 calc R U . . .
Cu1 Cu 0.20162(12) 0.17389(5) 0.88501(10) 0.0365(2) Uani 1 1 d . . . . .
Dy1 Dy 0.30096(3) 0.31821(2) 0.75597(3) 0.02323(8) Uani 1 1 d . . . . .
N1 N 0.2814(12) 0.1166(4) 1.0224(7) 0.056(2) Uani 1 1 d . . . . .
N2 N 0.0088(11) 0.1343(4) 0.9044(8) 0.049(2) Uani 1 1 d . . . . .
N3 N 0.4104(8) 0.3721(4) 0.5744(6) 0.0298(15) Uani 1 1 d . . . . .
N4 N 0.8502(8) 0.4269(4) 0.5707(7) 0.0371(16) Uani 1 1 d . . . . .
N5 N 0.8366(10) 0.4119(5) 0.1896(8) 0.051(2) Uani 1 1 d . . . . .
N6 N 0.2089(10) 0.5022(4) 0.3046(9) 0.052(2) Uani 1 1 d . . . . .
N7 N 0.5341(10) 0.5690(4) 0.5913(7) 0.0448(19) Uani 1 1 d . . . . .
N8 N 0.4490(8) 0.3161(5) 0.2324(6) 0.0412(14) Uani 1 1 d . . . . .
N9 N 0.7211(10) 0.6023(4) 0.2849(7) 0.0377(17) Uani 1 1 d . . . . .
N10 N 0.4649(13) 0.4877(5) 0.0426(8) 0.057(3) Uani 1 1 d . . . . .
N11 N 0.1911(13) 0.5286(5) 0.6822(12) 0.076(3) Uani 1 1 d . . . . .
O1 O 0.5739(5) 0.3120(3) 0.8523(4) 0.0318(11) Uani 1 1 d . . . . .
O2 O 0.3799(7) 0.2239(3) 0.8783(5) 0.0316(12) Uani 1 1 d . . . . .
O1W O 0.2681(7) 0.3340(3) 0.9802(5) 0.0407(16) Uani 1 1 d D . . . .
O3 O 0.1171(7) 0.2405(3) 0.7688(6) 0.0323(14) Uani 1 1 d . . . . .
O2W O 0.0820(8) 0.3867(3) 0.7653(7) 0.0404(17) Uani 1 1 d . . . . .
O4 O 0.0893(6) 0.3055(3) 0.5524(5) 0.0350(14) Uani 1 1 d . . . . .
O3W O 0.3817(7) 0.4294(3) 0.8083(6) 0.0357(13) Uani 1 1 d . . . . .
O4W O 0.3738(7) 0.2345(3) 0.6153(5) 0.0303(12) Uani 1 1 d D . . . .
O5W O 0.3296(9) 0.1998(3) 0.3593(6) 0.0444(15) Uani 1 1 d D . . . .
O6W O 0.0909(8) 0.4286(4) 1.0569(8) 0.060(2) Uani 1 1 d . . . . .
Mo1 Mo 0.56280(7) 0.46063(3) 0.35409(5) 0.02343(14) Uani 1 1 d . . . . .
H1W H 0.323(9) 0.324(7) 1.049(6) 0.06(3) Uiso 1 1 d D . . . .
H2W H 0.205(11) 0.363(5) 0.993(13) 0.08(4) Uiso 1 1 d D . . . .
H7W H 0.376(11) 0.232(6) 0.5336(17) 0.04(3) Uiso 1 1 d D . . . .
H8W H 0.351(11) 0.198(3) 0.650(9) 0.04(3) Uiso 1 1 d D . . . .
H9W H 0.383(9) 0.166(3) 0.351(10) 0.04(3) Uiso 1 1 d D . . . .
H10W H 0.363(15) 0.233(4) 0.322(12) 0.09(5) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.447(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O1 1.385(10) . ?
C2 C3 1.386(12) . ?
C2 C7 1.419(13) . ?
C3 C4 1.397(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.383(17) . ?
C4 H4 0.9500 . ?
C5 C6 1.406(14) . ?
C5 H5 0.9500 . ?
C6 C7 1.407(11) . ?
C6 C8 1.461(15) . ?
C7 O2 1.322(10) . ?
C8 N1 1.276(15) . ?
C8 H8 0.9500 . ?
C9 C9A 1.383(18) . ?
C9 C10 1.48(3) . ?
C9 N1 1.494(15) . ?
C9 H9 1.0000 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10 N2 1.449(17) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.282(14) . ?
C11 C12 1.414(16) . ?
C11 H11 0.9500 . ?
C12 C17 1.419(12) . ?
C12 C13 1.432(15) . ?
C13 C14 1.350(18) . ?
C13 H13 0.9500 . ?
C14 C15 1.394(16) . ?
C14 H14 0.9500 . ?
C15 C16 1.396(13) . ?
C15 H15 0.9500 . ?
C16 O4 1.377(11) . ?
C16 C17 1.391(13) . ?
C17 O3 1.348(11) . ?
C18 O4 1.429(10) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N3 1.159(10) . ?
C19 Mo1 2.156(7) . ?
C20 N4 1.141(11) . ?
C20 Mo1 2.177(8) . ?
C21 N5 1.149(12) . ?
C21 Mo1 2.153(9) . ?
C22 N6 1.142(12) . ?
C22 Mo1 2.158(9) . ?
C23 N7 1.148(11) . ?
C23 Mo1 2.177(8) . ?
C24 N8 1.146(13) . ?
C24 Mo1 2.162(8) . ?
C25 N9 1.163(11) . ?
C25 Mo1 2.157(8) . ?
C26 N10 1.141(11) . ?
C26 Mo1 2.154(8) . ?
C27 N11 1.118(13) . ?
C27 C28 1.461(15) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
Cu1 O3 1.911(7) . ?
Cu1 O2 1.913(6) . ?
Cu1 N1 1.915(8) . ?
Cu1 N2 1.951(8) . ?
Cu1 N9 2.437(7) 2_646 ?
Cu1 Dy1 3.3752(10) . ?
Dy1 O3 2.305(6) . ?
Dy1 O2 2.360(5) . ?
Dy1 O4W 2.372(5) . ?
Dy1 O1W 2.390(5) . ?
Dy1 O3W 2.412(6) . ?
Dy1 O2W 2.430(7) . ?
Dy1 N3 2.468(7) . ?
Dy1 O1 2.567(5) . ?
Dy1 O4 2.703(5) . ?
N9 Cu1 2.437(7) 2_656 ?
O1W H1W 0.850(7) . ?
O1W H2W 0.850(7) . ?
O4W H7W 0.850(7) . ?
O4W H8W 0.848(7) . ?
O5W H9W 0.850(7) . ?
O5W H10W 0.850(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
O1 C2 C3 126.6(9) . . ?
O1 C2 C7 112.8(7) . . ?
C3 C2 C7 120.6(8) . . ?
C2 C3 C4 119.3(10) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C5 C4 C3 121.0(9) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 120.6(9) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C5 C6 C7 119.0(9) . . ?
C5 C6 C8 117.1(8) . . ?
C7 C6 C8 123.8(9) . . ?
O2 C7 C6 124.3(8) . . ?
O2 C7 C2 116.1(7) . . ?
C6 C7 C2 119.5(8) . . ?
N1 C8 C6 125.1(8) . . ?
N1 C8 H8 117.5 . . ?
C6 C8 H8 117.5 . . ?
C9A C9 C10 115.9(16) . . ?
C9A C9 N1 120.3(12) . . ?
C10 C9 N1 109.5(13) . . ?
C9A C9 H9 102.8 . . ?
C10 C9 H9 102.8 . . ?
N1 C9 H9 102.8 . . ?
C9 C9A H9A1 109.5 . . ?
C9 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C9 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
N2 C10 C9 112.4(12) . . ?
N2 C10 H10A 109.1 . . ?
C9 C10 H10A 109.1 . . ?
N2 C10 H10B 109.1 . . ?
C9 C10 H10B 109.1 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C12 125.4(9) . . ?
N2 C11 H11 117.3 . . ?
C12 C11 H11 117.3 . . ?
C11 C12 C17 123.8(9) . . ?
C11 C12 C13 118.3(9) . . ?
C17 C12 C13 117.8(10) . . ?
C14 C13 C12 121.9(10) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C15 120.3(10) . . ?
C13 C14 H14 119.9 . . ?
C15 C14 H14 119.9 . . ?
C14 C15 C16 119.4(11) . . ?
C14 C15 H15 120.3 . . ?
C16 C15 H15 120.3 . . ?
O4 C16 C17 113.9(7) . . ?
O4 C16 C15 124.5(9) . . ?
C17 C16 C15 121.6(9) . . ?
O3 C17 C16 118.1(7) . . ?
O3 C17 C12 123.0(8) . . ?
C16 C17 C12 118.9(8) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 Mo1 175.9(6) . . ?
N4 C20 Mo1 177.7(7) . . ?
N5 C21 Mo1 178.7(9) . . ?
N6 C22 Mo1 177.0(8) . . ?
N7 C23 Mo1 176.6(8) . . ?
N8 C24 Mo1 176.9(8) . . ?
N9 C25 Mo1 178.7(8) . . ?
N10 C26 Mo1 179.0(8) . . ?
N11 C27 C28 178.6(12) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 Cu1 O2 83.5(2) . . ?
O3 Cu1 N1 171.2(3) . . ?
O2 Cu1 N1 95.4(3) . . ?
O3 Cu1 N2 93.0(3) . . ?
O2 Cu1 N2 171.5(3) . . ?
N1 Cu1 N2 86.9(4) . . ?
O3 Cu1 N9 95.3(3) . 2_646 ?
O2 Cu1 N9 88.9(3) . 2_646 ?
N1 Cu1 N9 93.4(3) . 2_646 ?
N2 Cu1 N9 99.1(3) . 2_646 ?
O3 Cu1 Dy1 41.04(19) . . ?
O2 Cu1 Dy1 42.76(16) . . ?
N1 Cu1 Dy1 136.3(3) . . ?
N2 Cu1 Dy1 132.5(3) . . ?
N9 Cu1 Dy1 96.98(18) 2_646 . ?
O3 Dy1 O2 66.1(2) . . ?
O3 Dy1 O4W 78.3(2) . . ?
O2 Dy1 O4W 70.2(2) . . ?
O3 Dy1 O1W 82.6(2) . . ?
O2 Dy1 O1W 69.5(2) . . ?
O4W Dy1 O1W 139.6(2) . . ?
O3 Dy1 O3W 145.9(2) . . ?
O2 Dy1 O3W 124.7(2) . . ?
O4W Dy1 O3W 135.0(2) . . ?
O1W Dy1 O3W 73.9(2) . . ?
O3 Dy1 O2W 77.9(2) . . ?
O2 Dy1 O2W 130.0(2) . . ?
O4W Dy1 O2W 135.5(2) . . ?
O1W Dy1 O2W 72.5(2) . . ?
O3W Dy1 O2W 71.7(2) . . ?
O3 Dy1 N3 134.1(2) . . ?
O2 Dy1 N3 130.0(2) . . ?
O4W Dy1 N3 71.9(2) . . ?
O1W Dy1 N3 141.3(2) . . ?
O3W Dy1 N3 67.8(2) . . ?
O2W Dy1 N3 100.0(3) . . ?
O3 Dy1 O1 128.0(2) . . ?
O2 Dy1 O1 61.9(2) . . ?
O4W Dy1 O1 83.3(2) . . ?
O1W Dy1 O1 81.03(19) . . ?
O3W Dy1 O1 72.7(2) . . ?
O2W Dy1 O1 140.2(2) . . ?
N3 Dy1 O1 82.5(2) . . ?
O3 Dy1 O4 61.6(2) . . ?
O2 Dy1 O4 119.30(19) . . ?
O4W Dy1 O4 71.05(19) . . ?
O1W Dy1 O4 128.08(19) . . ?
O3W Dy1 O4 115.85(18) . . ?
O2W Dy1 O4 64.64(19) . . ?
N3 Dy1 O4 76.0(2) . . ?
O1 Dy1 O4 150.54(16) . . ?
O3 Dy1 Cu1 32.98(16) . . ?
O2 Dy1 Cu1 33.38(14) . . ?
O4W Dy1 Cu1 74.13(15) . . ?
O1W Dy1 Cu1 70.52(16) . . ?
O3W Dy1 Cu1 143.85(14) . . ?
O2W Dy1 Cu1 103.06(19) . . ?
N3 Dy1 Cu1 145.99(17) . . ?
O1 Dy1 Cu1 95.19(14) . . ?
O4 Dy1 Cu1 91.65(12) . . ?
C8 N1 C9 123.4(10) . . ?
C8 N1 Cu1 125.6(7) . . ?
C9 N1 Cu1 111.0(8) . . ?
C11 N2 C10 124.0(10) . . ?
C11 N2 Cu1 125.3(7) . . ?
C10 N2 Cu1 110.7(9) . . ?
C19 N3 Dy1 170.6(6) . . ?
C25 N9 Cu1 147.0(6) . 2_656 ?
C2 O1 C1 115.7(6) . . ?
C2 O1 Dy1 118.7(5) . . ?
C1 O1 Dy1 125.4(5) . . ?
C7 O2 Cu1 125.4(5) . . ?
C7 O2 Dy1 126.9(5) . . ?
Cu1 O2 Dy1 103.9(2) . . ?
Dy1 O1W H1W 132(7) . . ?
Dy1 O1W H2W 114(9) . . ?
H1W O1W H2W 112(10) . . ?
C17 O3 Cu1 123.3(5) . . ?
C17 O3 Dy1 129.2(5) . . ?
Cu1 O3 Dy1 106.0(3) . . ?
C16 O4 C18 115.6(7) . . ?
C16 O4 Dy1 115.3(5) . . ?
C18 O4 Dy1 129.0(5) . . ?
Dy1 O4W H7W 134(8) . . ?
Dy1 O4W H8W 105(7) . . ?
H7W O4W H8W 113(10) . . ?
H9W O5W H10W 112(10) . . ?
C21 Mo1 C26 72.1(3) . . ?
C21 Mo1 C19 125.4(3) . . ?
C26 Mo1 C19 134.0(3) . . ?
C21 Mo1 C25 77.6(3) . . ?
C26 Mo1 C25 74.0(3) . . ?
C19 Mo1 C25 145.4(3) . . ?
C21 Mo1 C22 141.2(3) . . ?
C26 Mo1 C22 70.3(4) . . ?
C19 Mo1 C22 77.5(3) . . ?
C25 Mo1 C22 100.4(3) . . ?
C21 Mo1 C24 75.4(3) . . ?
C26 Mo1 C24 75.7(3) . . ?
C19 Mo1 C24 70.3(3) . . ?
C25 Mo1 C24 144.3(3) . . ?
C22 Mo1 C24 86.6(3) . . ?
C21 Mo1 C23 135.3(3) . . ?
C26 Mo1 C23 125.6(3) . . ?
C19 Mo1 C23 75.0(3) . . ?
C25 Mo1 C23 71.0(3) . . ?
C22 Mo1 C23 76.6(3) . . ?
C24 Mo1 C23 144.0(3) . . ?
C21 Mo1 C20 72.0(3) . . ?
C26 Mo1 C20 142.8(3) . . ?
C19 Mo1 C20 76.9(3) . . ?
C25 Mo1 C20 88.9(3) . . ?
C22 Mo1 C20 146.6(3) . . ?
C24 Mo1 C20 104.5(3) . . ?
C23 Mo1 C20 76.3(3) . . ?

_refine_diff_density_max         0.912
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.092

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_11
_database_code_depnum_ccdc_archive 'CCDC 1060180'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H35 Cu La N11 O10 W'
_chemical_formula_weight         1083.98

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'
La La -0.2871 2.4523 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.2526(5)
_cell_length_b                   20.3849(11)
_cell_length_c                   10.4325(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.692(4)
_cell_angle_gamma                90
_cell_volume                     1954.30(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    28515
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      32.96

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_F_000             1052
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    4.613
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4225
_exptl_absorpt_correction_T_max  0.7064
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25998
_diffrn_reflns_av_unetI/netI     0.1111
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.431
_diffrn_reflns_theta_max         33.441
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measured_fraction_theta_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_point_group_measured_fraction_max 0.874
_diffrn_reflns_point_group_measured_fraction_full 0.879
_reflns_number_total             13356
_reflns_number_gt                9524
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_max     0.794
_reflns_Friedel_fraction_full    0.810

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0849P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(14)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         13356
_refine_ls_number_parameters     479
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0678
_refine_ls_wR_factor_ref         0.1694
_refine_ls_wR_factor_gt          0.1569
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_restrained_S_all      0.990
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.311(2) 0.6496(12) 0.160(2) 0.055(5) Uani 1 1 d . . . . .
H1A H 0.3449 0.6184 0.2279 0.083 Uiso 1 1 calc R U . . .
H1B H 0.2308 0.6757 0.1865 0.083 Uiso 1 1 calc R U . . .
H1C H 0.2767 0.6256 0.0804 0.083 Uiso 1 1 calc R U . . .
C2 C 0.393(2) 0.7385(9) 0.0409(17) 0.045(4) Uani 1 1 d . . . . .
C3 C 0.263(2) 0.7414(10) -0.0463(19) 0.049(4) Uani 1 1 d . . . . .
H3 H 0.1880 0.7098 -0.0427 0.058 Uiso 1 1 calc R U . . .
C4 C 0.248(2) 0.7914(14) -0.136(2) 0.062(6) Uani 1 1 d . . . . .
H4 H 0.1591 0.7946 -0.1914 0.075 Uiso 1 1 calc R U . . .
C5 C 0.357(3) 0.8376(13) -0.150(2) 0.072(7) Uani 1 1 d . . . . .
H5 H 0.3447 0.8694 -0.2171 0.086 Uiso 1 1 calc R U . . .
C6 C 0.485(2) 0.8364(10) -0.0645(16) 0.050(5) Uani 1 1 d . . . . .
C7 C 0.5043(19) 0.7862(8) 0.0298(13) 0.038(3) Uani 1 1 d . . . . .
C8 C 0.595(3) 0.8844(10) -0.0832(17) 0.057(6) Uani 1 1 d . . . . .
H8 H 0.5700 0.9178 -0.1453 0.069 Uiso 1 1 calc R U . . .
C9 C 0.824(4) 0.9388(19) -0.048(3) 0.098(12) Uani 1 1 d . . . . .
H9 H 0.8173 0.9710 0.0236 0.118 Uiso 1 1 calc R U . . .
C10 C 0.979(3) 0.9103(18) -0.023(5) 0.114(15) Uani 1 1 d . . . . .
H10A H 1.0016 0.8860 -0.1000 0.137 Uiso 1 1 calc R U . . .
H10B H 1.0498 0.9468 -0.0074 0.137 Uiso 1 1 calc R U . . .
C11 C 1.115(3) 0.8547(13) 0.157(3) 0.065(6) Uani 1 1 d . . . . .
H11 H 1.2007 0.8747 0.1326 0.078 Uiso 1 1 calc R U . . .
C12 C 1.131(2) 0.8126(13) 0.270(2) 0.061(6) Uani 1 1 d . . . . .
C13 C 1.261(2) 0.8140(15) 0.349(3) 0.076(8) Uani 1 1 d . . . . .
H13 H 1.3380 0.8408 0.3266 0.092 Uiso 1 1 calc R U . . .
C14 C 1.281(3) 0.778(2) 0.458(3) 0.085(10) Uani 1 1 d . . . . .
H14 H 1.3701 0.7817 0.5127 0.102 Uiso 1 1 calc R U . . .
C15 C 1.173(2) 0.7372(13) 0.491(3) 0.067(7) Uani 1 1 d . . . . .
H15 H 1.1896 0.7111 0.5671 0.081 Uiso 1 1 calc R U . . .
C16 C 1.0395(17) 0.7338(10) 0.413(2) 0.049(4) Uani 1 1 d . . . . .
C17 C 1.0143(17) 0.7712(9) 0.2970(19) 0.044(4) Uani 1 1 d . . . . .
C18 C 0.923(2) 0.6727(15) 0.5657(18) 0.060(6) Uani 1 1 d . . . . .
H18A H 0.8355 0.6460 0.5701 0.090 Uiso 1 1 calc R U . . .
H18B H 1.0096 0.6461 0.5910 0.090 Uiso 1 1 calc R U . . .
H18C H 0.9215 0.7102 0.6243 0.090 Uiso 1 1 calc R U . . .
C19 C 0.5208(17) 0.5968(9) 0.5006(13) 0.036(3) Uani 1 1 d . . . . .
C20 C 0.2481(17) 0.5583(8) 0.4997(15) 0.036(3) Uani 1 1 d . . . . .
C21 C 0.248(2) 0.5743(11) 0.7444(15) 0.046(4) Uani 1 1 d . . . . .
C22 C 0.656(2) 0.5148(10) 0.6807(17) 0.048(4) Uani 1 1 d . . . . .
C23 C 0.4541(17) 0.4689(10) 0.4962(16) 0.039(3) Uani 1 1 d . . . . .
C24 C 0.4962(19) 0.6344(8) 0.7193(14) 0.038(3) Uani 1 1 d . . . . .
C25 C 0.3229(18) 0.4512(8) 0.6895(14) 0.035(3) Uani 1 1 d . . . . .
C26 C 0.483(2) 0.5229(8) 0.8495(16) 0.043(4) Uani 1 1 d . . . . .
C27 C 0.884(3) 0.4507(13) 0.404(3) 0.071(7) Uani 1 1 d . . . . .
C28 C 0.989(3) 0.4205(15) 0.499(3) 0.082(8) Uani 1 1 d . . . . .
H28A H 0.9840 0.4410 0.5829 0.122 Uiso 1 1 calc R U . . .
H28B H 1.0873 0.4266 0.4734 0.122 Uiso 1 1 calc R U . . .
H28C H 0.9685 0.3736 0.5040 0.122 Uiso 1 1 calc R U . . .
Cu1 Cu 0.8006(3) 0.83013(11) 0.1106(2) 0.0434(5) Uani 1 1 d . . . . .
La1 La 0.70407(8) 0.68108(4) 0.24120(7) 0.02839(16) Uani 1 1 d . . . . .
N1 N 0.723(3) 0.8855(11) -0.0231(16) 0.067(6) Uani 1 1 d . . . . .
N2 N 0.995(2) 0.8669(10) 0.0874(19) 0.061(5) Uani 1 1 d . . . . .
N3 N 0.5821(17) 0.6264(8) 0.4283(12) 0.042(3) Uani 1 1 d . . . . .
N4 N 0.1539(15) 0.5707(9) 0.4185(15) 0.044(3) Uani 1 1 d . . . . .
N5 N 0.156(2) 0.5925(11) 0.7980(17) 0.059(5) Uani 1 1 d . . . . .
N6 N 0.776(2) 0.5003(13) 0.711(2) 0.074(7) Uani 1 1 d . . . . .
N7 N 0.467(2) 0.4291(9) 0.4152(14) 0.053(4) Uani 1 1 d . . . . .
N8 N 0.5376(18) 0.6839(9) 0.7626(14) 0.049(3) Uani 1 1 d . . . . .
N9 N 0.2675(18) 0.4022(9) 0.7164(15) 0.047(3) Uani 1 1 d . . . . .
N10 N 0.512(2) 0.5148(11) 0.9575(16) 0.065(5) Uani 1 1 d . . . . .
N11 N 0.801(3) 0.4724(13) 0.331(3) 0.105(10) Uani 1 1 d . . . . .
O1 O 0.4285(11) 0.6923(6) 0.1357(11) 0.038(2) Uani 1 1 d . . . . .
O2 O 0.6236(13) 0.7801(6) 0.1152(10) 0.037(2) Uani 1 1 d . . . . .
O1W O 0.7322(15) 0.6669(9) 0.0023(11) 0.055(4) Uani 1 1 d . . . . .
O3 O 0.8881(13) 0.7647(6) 0.2251(12) 0.041(2) Uani 1 1 d . . . . .
O2W O 0.9335(14) 0.6141(7) 0.2156(13) 0.044(3) Uani 1 1 d . . . . .
O4 O 0.9255(13) 0.6962(7) 0.4347(11) 0.045(3) Uani 1 1 d . . . . .
O3W O 0.6193(17) 0.5648(7) 0.1889(12) 0.050(3) Uani 1 1 d . . . . .
O4W O 0.6382(14) 0.7717(6) 0.3881(11) 0.039(2) Uani 1 1 d . . . . .
O5W O 0.6630(18) 0.7992(7) 0.6462(12) 0.053(3) Uani 1 1 d . . . . .
O6W O 0.9136(17) 0.5755(11) -0.0641(16) 0.073(5) Uani 1 1 d . . . . .
W1 W 0.42793(6) 0.53963(2) 0.64528(4) 0.02776(11) Uani 1 1 d . . . . .
C9A C 0.800(5) 0.9768(18) -0.164(5) 0.129(16) Uani 1 1 d . . . . .
H9A1 H 0.8770 1.0098 -0.1643 0.194 Uiso 1 1 calc R U . . .
H9A2 H 0.8014 0.9479 -0.2388 0.194 Uiso 1 1 calc R U . . .
H9A3 H 0.7053 0.9987 -0.1681 0.194 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.44(2) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 O1 1.38(2) . ?
C2 C3 1.42(2) . ?
C2 C7 1.43(3) . ?
C3 C4 1.38(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.40(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.39(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.42(2) . ?
C6 C8 1.44(3) . ?
C7 O2 1.341(19) . ?
C8 N1 1.28(3) . ?
C8 H8 0.9500 . ?
C9 C9A 1.43(5) . ?
C9 N1 1.47(3) . ?
C9 C10 1.54(5) . ?
C9 H9 1.0000 . ?
C10 N2 1.44(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N2 1.28(3) . ?
C11 C12 1.45(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.37(4) . ?
C12 C17 1.43(3) . ?
C13 C14 1.34(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.38(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.40(3) . ?
C15 H15 0.9500 . ?
C16 O4 1.34(2) . ?
C16 C17 1.43(3) . ?
C17 O3 1.32(2) . ?
C18 O4 1.45(2) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 N3 1.16(2) . ?
C19 W1 2.162(16) . ?
C20 N4 1.17(2) . ?
C20 W1 2.152(16) . ?
C21 N5 1.14(2) . ?
C21 W1 2.179(18) . ?
C22 N6 1.16(2) . ?
C22 W1 2.156(19) . ?
C23 N7 1.19(2) . ?
C23 W1 2.155(17) . ?
C24 N8 1.15(2) . ?
C24 W1 2.148(17) . ?
C25 N9 1.17(2) . ?
C25 W1 2.125(17) . ?
C26 N10 1.14(2) . ?
C26 W1 2.159(16) . ?
C27 N11 1.11(3) . ?
C27 C28 1.44(3) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
Cu1 N1 1.87(2) . ?
Cu1 O3 1.907(14) . ?
Cu1 O2 1.934(12) . ?
Cu1 N2 1.987(18) . ?
Cu1 N9 2.465(15) 2_656 ?
Cu1 La1 3.488(2) . ?
La1 O3 2.428(11) . ?
La1 O2 2.476(11) . ?
La1 O4W 2.520(11) . ?
La1 O3W 2.537(14) . ?
La1 O1W 2.553(11) . ?
La1 O2W 2.564(13) . ?
La1 N3 2.615(13) . ?
La1 O1 2.666(10) . ?
La1 O4 2.721(11) . ?
N9 Cu1 2.465(15) 2_646 ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
O1 C2 C3 126.9(19) . . ?
O1 C2 C7 114.1(14) . . ?
C3 C2 C7 118.9(17) . . ?
C4 C3 C2 118(2) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 123.4(19) . . ?
C3 C4 H4 118.3 . . ?
C5 C4 H4 118.3 . . ?
C6 C5 C4 119(2) . . ?
C6 C5 H5 120.4 . . ?
C4 C5 H5 120.4 . . ?
C5 C6 C7 119(2) . . ?
C5 C6 C8 117(2) . . ?
C7 C6 C8 123.4(19) . . ?
O2 C7 C6 123.8(18) . . ?
O2 C7 C2 115.3(15) . . ?
C6 C7 C2 120.9(16) . . ?
N1 C8 C6 125.3(18) . . ?
N1 C8 H8 117.4 . . ?
C6 C8 H8 117.4 . . ?
C9A C9 N1 120(3) . . ?
C9A C9 C10 113(3) . . ?
N1 C9 C10 107(3) . . ?
C9A C9 H9 104.9 . . ?
N1 C9 H9 104.9 . . ?
C10 C9 H9 104.9 . . ?
N2 C10 C9 112(2) . . ?
N2 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
N2 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 107.9 . . ?
N2 C11 C12 125(2) . . ?
N2 C11 H11 117.5 . . ?
C12 C11 H11 117.5 . . ?
C13 C12 C17 121(3) . . ?
C13 C12 C11 118(2) . . ?
C17 C12 C11 120(2) . . ?
C14 C13 C12 122(2) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 H13 119.2 . . ?
C13 C14 C15 121(2) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 H14 119.6 . . ?
C14 C15 C16 120(3) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
O4 C16 C15 126(2) . . ?
O4 C16 C17 113.0(15) . . ?
C15 C16 C17 121(2) . . ?
O3 C17 C12 126(2) . . ?
O3 C17 C16 118.3(15) . . ?
C12 C17 C16 115.5(18) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 W1 174.3(14) . . ?
N4 C20 W1 177.0(15) . . ?
N5 C21 W1 178.8(17) . . ?
N6 C22 W1 174.0(19) . . ?
N7 C23 W1 178.8(17) . . ?
N8 C24 W1 177.0(16) . . ?
N9 C25 W1 178.4(14) . . ?
N10 C26 W1 179.3(17) . . ?
N11 C27 C28 178(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 Cu1 O3 170.7(8) . . ?
N1 Cu1 O2 94.9(7) . . ?
O3 Cu1 O2 85.1(5) . . ?
N1 Cu1 N2 87.3(9) . . ?
O3 Cu1 N2 91.0(7) . . ?
O2 Cu1 N2 169.0(7) . . ?
N1 Cu1 N9 94.5(8) . 2_656 ?
O3 Cu1 N9 94.8(5) . 2_656 ?
O2 Cu1 N9 90.4(6) . 2_656 ?
N2 Cu1 N9 100.1(7) . 2_656 ?
N1 Cu1 La1 136.4(6) . . ?
O3 Cu1 La1 41.9(3) . . ?
O2 Cu1 La1 43.6(3) . . ?
N2 Cu1 La1 130.7(7) . . ?
N9 Cu1 La1 97.7(4) 2_656 . ?
O3 La1 O2 64.0(4) . . ?
O3 La1 O4W 75.4(4) . . ?
O2 La1 O4W 69.2(4) . . ?
O3 La1 O3W 147.4(4) . . ?
O2 La1 O3W 125.6(4) . . ?
O4W La1 O3W 136.5(4) . . ?
O3 La1 O1W 82.0(5) . . ?
O2 La1 O1W 68.4(5) . . ?
O4W La1 O1W 137.4(5) . . ?
O3W La1 O1W 75.4(5) . . ?
O3 La1 O2W 76.8(5) . . ?
O2 La1 O2W 125.5(4) . . ?
O4W La1 O2W 135.7(4) . . ?
O3W La1 O2W 73.7(5) . . ?
O1W La1 O2W 70.0(4) . . ?
O3 La1 N3 135.8(4) . . ?
O2 La1 N3 127.9(5) . . ?
O4W La1 N3 72.7(4) . . ?
O3W La1 N3 67.2(4) . . ?
O1W La1 N3 141.5(5) . . ?
O2W La1 N3 106.6(5) . . ?
O3 La1 O1 123.8(4) . . ?
O2 La1 O1 59.8(4) . . ?
O4W La1 O1 84.3(4) . . ?
O3W La1 O1 74.6(4) . . ?
O1W La1 O1 78.9(4) . . ?
O2W La1 O1 140.0(4) . . ?
N3 La1 O1 82.5(4) . . ?
O3 La1 O4 59.9(4) . . ?
O2 La1 O4 117.1(4) . . ?
O4W La1 O4 71.4(4) . . ?
O3W La1 O4 116.9(4) . . ?
O1W La1 O4 125.7(4) . . ?
O2W La1 O4 65.0(4) . . ?
N3 La1 O4 81.2(4) . . ?
O1 La1 O4 153.8(4) . . ?
O3 La1 Cu1 31.6(3) . . ?
O2 La1 Cu1 32.6(3) . . ?
O4W La1 Cu1 71.9(3) . . ?
O3W La1 Cu1 144.8(3) . . ?
O1W La1 Cu1 70.0(4) . . ?
O2W La1 Cu1 99.8(3) . . ?
N3 La1 Cu1 144.6(4) . . ?
O1 La1 Cu1 92.3(3) . . ?
O4 La1 Cu1 89.2(3) . . ?
C8 N1 C9 120(2) . . ?
C8 N1 Cu1 127.4(15) . . ?
C9 N1 Cu1 112.4(19) . . ?
C11 N2 C10 125(2) . . ?
C11 N2 Cu1 126.7(17) . . ?
C10 N2 Cu1 108.7(18) . . ?
C19 N3 La1 171.8(12) . . ?
C25 N9 Cu1 147.1(13) . 2_646 ?
C2 O1 C1 114.6(14) . . ?
C2 O1 La1 119.5(10) . . ?
C1 O1 La1 125.7(11) . . ?
C7 O2 Cu1 124.6(11) . . ?
C7 O2 La1 127.0(11) . . ?
Cu1 O2 La1 103.9(5) . . ?
C17 O3 Cu1 124.6(12) . . ?
C17 O3 La1 127.8(12) . . ?
Cu1 O3 La1 106.5(5) . . ?
C16 O4 C18 116.4(15) . . ?
C16 O4 La1 118.7(12) . . ?
C18 O4 La1 124.6(11) . . ?
C25 W1 C24 143.9(5) . . ?
C25 W1 C20 88.1(6) . . ?
C24 W1 C20 105.4(6) . . ?
C25 W1 C23 71.4(6) . . ?
C24 W1 C23 143.9(6) . . ?
C20 W1 C23 75.6(6) . . ?
C25 W1 C22 103.1(7) . . ?
C24 W1 C22 84.8(7) . . ?
C20 W1 C22 145.3(6) . . ?
C23 W1 C22 77.1(6) . . ?
C25 W1 C26 73.3(6) . . ?
C24 W1 C26 76.2(6) . . ?
C20 W1 C26 142.9(7) . . ?
C23 W1 C26 125.0(7) . . ?
C22 W1 C26 71.4(7) . . ?
C25 W1 C19 146.9(6) . . ?
C24 W1 C19 69.0(6) . . ?
C20 W1 C19 75.5(6) . . ?
C23 W1 C19 76.7(7) . . ?
C22 W1 C19 77.7(7) . . ?
C26 W1 C19 135.0(6) . . ?
C25 W1 C21 77.2(7) . . ?
C24 W1 C21 75.3(7) . . ?
C20 W1 C21 72.9(6) . . ?
C23 W1 C21 135.7(7) . . ?
C22 W1 C21 141.3(7) . . ?
C26 W1 C21 71.8(7) . . ?
C19 W1 C21 123.0(7) . . ?
C9 C9A H9A1 109.5 . . ?
C9 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C9 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?

_refine_diff_density_max         4.366
_refine_diff_density_min         -2.645
_refine_diff_density_rms         0.208

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_12
_database_code_depnum_ccdc_archive 'CCDC 1060181'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H35 Cu Gd N11 O10 W'
_chemical_formula_weight         1102.32

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'
Gd Gd -0.1653 3.9035 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.1369(3)
_cell_length_b                   20.3271(9)
_cell_length_c                   10.3756(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.597(3)
_cell_angle_gamma                90
_cell_volume                     1914.27(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12779
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      28.06

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_F_000             1066
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    5.326
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1524
_exptl_absorpt_correction_T_max  0.3761
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19642
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.215
_diffrn_reflns_theta_max         28.058
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.970
_reflns_number_total             9039
_reflns_number_gt                8106
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.898
_reflns_Friedel_fraction_max     0.947
_reflns_Friedel_fraction_full    0.941

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0015(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3433 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.032(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         9039
_refine_ls_number_parameters     480
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0318
_refine_ls_wR_factor_ref         0.0727
_refine_ls_wR_factor_gt          0.0712
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.000
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.3135(14) 0.6449(7) 0.1768(14) 0.070(4) Uani 1 1 d . . . . .
H1A H 0.3525 0.6145 0.2427 0.105 Uiso 1 1 calc R U . . .
H1B H 0.2362 0.6703 0.2079 0.105 Uiso 1 1 calc R U . . .
H1C H 0.2748 0.6211 0.1005 0.105 Uiso 1 1 calc R U . . .
C2 C 0.3922(13) 0.7366(5) 0.0501(10) 0.047(2) Uani 1 1 d . . . . .
C3 C 0.2608(15) 0.7380(7) -0.0306(13) 0.069(3) Uani 1 1 d . . . . .
H3 H 0.1883 0.7067 -0.0219 0.082 Uiso 1 1 calc R U . . .
C4 C 0.2385(19) 0.7864(8) -0.1242(15) 0.081(4) Uani 1 1 d . . . . .
H4 H 0.1510 0.7873 -0.1797 0.098 Uiso 1 1 calc R U . . .
C5 C 0.344(2) 0.8327(7) -0.1360(13) 0.081(5) Uani 1 1 d . . . . .
H5 H 0.3263 0.8655 -0.1983 0.098 Uiso 1 1 calc R U . . .
C6 C 0.4809(15) 0.8318(5) -0.0541(10) 0.056(3) Uani 1 1 d . . . . .
C7 C 0.5012(12) 0.7822(5) 0.0402(9) 0.044(2) Uani 1 1 d . . . . .
C8 C 0.592(2) 0.8798(6) -0.0767(11) 0.069(4) Uani 1 1 d . . . . .
H8 H 0.5651 0.9110 -0.1406 0.083 Uiso 1 1 calc R U . . .
C9 C 0.830(3) 0.9329(11) -0.0475(18) 0.140(11) Uani 1 1 d . . . . .
H9 H 0.8143 0.9638 0.0220 0.168 Uiso 1 1 calc R U . . .
C10 C 0.978(2) 0.9156(10) -0.002(3) 0.132(9) Uani 1 1 d . . . . .
H10A H 1.0312 0.9549 0.0294 0.159 Uiso 1 1 calc R U . . .
H10B H 1.0257 0.8982 -0.0736 0.159 Uiso 1 1 calc R U . . .
C11 C 1.1067(16) 0.8548(6) 0.1707(16) 0.070(4) Uani 1 1 d . . . . .
H11 H 1.1913 0.8755 0.1491 0.084 Uiso 1 1 calc R U . . .
C12 C 1.1244(13) 0.8118(6) 0.2797(13) 0.058(3) Uani 1 1 d . . . . .
C13 C 1.2558(16) 0.8132(9) 0.3647(19) 0.090(5) Uani 1 1 d . . . . .
H13 H 1.3328 0.8396 0.3437 0.107 Uiso 1 1 calc R U . . .
C14 C 1.2749(17) 0.7778(10) 0.4756(19) 0.094(5) Uani 1 1 d . . . . .
H14 H 1.3626 0.7802 0.5307 0.113 Uiso 1 1 calc R U . . .
C15 C 1.1611(15) 0.7379(8) 0.5052(15) 0.073(4) Uani 1 1 d . . . . .
H15 H 1.1723 0.7139 0.5820 0.087 Uiso 1 1 calc R U . . .
C16 C 1.0334(12) 0.7327(6) 0.4252(12) 0.050(3) Uani 1 1 d . . . . .
C17 C 1.0125(11) 0.7691(5) 0.3097(11) 0.045(2) Uani 1 1 d . . . . .
C18 C 0.9136(14) 0.6694(7) 0.5757(11) 0.069(4) Uani 1 1 d . . . . .
H18A H 0.8262 0.6437 0.5807 0.103 Uiso 1 1 calc R U . . .
H18B H 0.9989 0.6422 0.5969 0.103 Uiso 1 1 calc R U . . .
H18C H 0.9157 0.7053 0.6360 0.103 Uiso 1 1 calc R U . . .
C19 C 0.5358(11) 0.5958(4) 0.4990(8) 0.038(2) Uani 1 1 d . . . . .
C20 C 0.2546(11) 0.5609(5) 0.5045(9) 0.040(2) Uani 1 1 d . . . . .
C21 C 0.2628(13) 0.5729(6) 0.7488(10) 0.050(2) Uani 1 1 d . . . . .
C22 C 0.6675(13) 0.5118(5) 0.6731(10) 0.049(2) Uani 1 1 d . . . . .
C23 C 0.4615(13) 0.4713(5) 0.4874(10) 0.047(2) Uani 1 1 d . . . . .
C24 C 0.5131(13) 0.6339(4) 0.7231(9) 0.044(2) Uani 1 1 d . . . . .
C25 C 0.3363(12) 0.4484(5) 0.6885(9) 0.042(2) Uani 1 1 d . . . . .
C26 C 0.5057(14) 0.5214(5) 0.8475(9) 0.052(3) Uani 1 1 d . . . . .
C27 C 0.8994(18) 0.4469(7) 0.3865(16) 0.077(4) Uani 1 1 d . . . . .
C28 C 1.005(2) 0.4169(9) 0.4838(19) 0.101(6) Uani 1 1 d . . . . .
H28A H 1.0046 0.4400 0.5645 0.152 Uiso 1 1 calc R U . . .
H28B H 1.1016 0.4192 0.4562 0.152 Uiso 1 1 calc R U . . .
H28C H 0.9788 0.3717 0.4953 0.152 Uiso 1 1 calc R U . . .
Cu1 Cu 0.79877(16) 0.82700(6) 0.11780(13) 0.0506(3) Uani 1 1 d . . . . .
Gd1 Gd 0.70231(4) 0.68166(2) 0.24466(4) 0.03320(11) Uani 1 1 d . . . . .
N1 N 0.7192(17) 0.8836(5) -0.0193(10) 0.075(3) Uani 1 1 d . . . . .
N2 N 0.9879(14) 0.8677(5) 0.1002(12) 0.067(3) Uani 1 1 d . . . . .
N3 N 0.5898(11) 0.6264(4) 0.4252(8) 0.048(2) Uani 1 1 d . . . . .
N4 N 0.1573(11) 0.5726(5) 0.4267(10) 0.057(2) Uani 1 1 d . . . . .
N5 N 0.1683(13) 0.5888(6) 0.8052(11) 0.074(3) Uani 1 1 d . . . . .
N6 N 0.7923(14) 0.4990(6) 0.6935(12) 0.078(3) Uani 1 1 d . . . . .
N7 N 0.4696(14) 0.4331(6) 0.4086(11) 0.070(3) Uani 1 1 d . . . . .
N8 N 0.5567(12) 0.6831(5) 0.7675(9) 0.063(2) Uani 1 1 d . . . . .
N9 N 0.2849(13) 0.3991(5) 0.7132(9) 0.060(2) Uani 1 1 d . . . . .
N10 N 0.5388(16) 0.5130(6) 0.9553(10) 0.082(4) Uani 1 1 d . . . . .
N11 N 0.821(2) 0.4697(7) 0.3133(19) 0.126(7) Uani 1 1 d . . . . .
O1 O 0.4299(7) 0.6887(4) 0.1452(6) 0.0475(16) Uani 1 1 d . . . . .
O2 O 0.6238(8) 0.7757(3) 0.1210(6) 0.0444(16) Uani 1 1 d . . . . .
O1W O 0.7372(9) 0.6654(4) 0.0201(7) 0.061(2) Uani 1 1 d . . . . .
O3 O 0.8847(8) 0.7606(3) 0.2340(7) 0.0449(15) Uani 1 1 d . . . . .
O2W O 0.9215(10) 0.6120(4) 0.2377(9) 0.063(2) Uani 1 1 d . . . . .
O4 O 0.9136(8) 0.6946(4) 0.4468(7) 0.0509(17) Uani 1 1 d . . . . .
O3W O 0.6209(9) 0.5687(3) 0.1906(7) 0.0519(18) Uani 1 1 d . . . . .
O4W O 0.6271(9) 0.7667(3) 0.3851(7) 0.0489(17) Uani 1 1 d . . . . .
O5W O 0.6641(12) 0.8009(4) 0.6420(9) 0.073(2) Uani 1 1 d . . . . .
O6W O 0.9148(12) 0.5753(6) -0.0675(12) 0.096(4) Uani 1 1 d . . . . .
W1 W 0.44145(4) 0.53959(2) 0.64507(3) 0.03284(9) Uani 1 1 d . . . . .
C9A C 0.802(3) 0.9773(11) -0.152(2) 0.143(10) Uani 1 1 d . . . . .
H9A1 H 0.6979 0.9839 -0.1715 0.215 Uiso 1 1 calc R U . . .
H9A2 H 0.8491 1.0186 -0.1298 0.215 Uiso 1 1 calc R U . . .
H9A3 H 0.8406 0.9595 -0.2275 0.215 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.453(13) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C7 1.374(15) . ?
C2 C3 1.383(16) . ?
C2 O1 1.400(12) . ?
C3 C4 1.382(19) . ?
C3 H3 0.9300 . ?
C4 C5 1.36(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.430(19) . ?
C5 H5 0.9300 . ?
C6 C7 1.403(14) . ?
C6 C8 1.44(2) . ?
C7 O2 1.326(12) . ?
C8 N1 1.25(2) . ?
C8 H8 0.9300 . ?
C9 C9A 1.42(2) . ?
C9 C10 1.43(3) . ?
C9 N1 1.48(2) . ?
C9 H9 0.9800 . ?
C10 N2 1.43(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.265(19) . ?
C11 C12 1.42(2) . ?
C11 H11 0.9300 . ?
C12 C17 1.403(15) . ?
C12 C13 1.41(2) . ?
C13 C14 1.35(2) . ?
C13 H13 0.9300 . ?
C14 C15 1.38(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.356(17) . ?
C15 H15 0.9300 . ?
C16 O4 1.381(13) . ?
C16 C17 1.402(16) . ?
C17 O3 1.341(12) . ?
C18 O4 1.433(13) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N3 1.142(12) . ?
C19 W1 2.155(8) . ?
C20 N4 1.155(13) . ?
C20 W1 2.158(10) . ?
C21 N5 1.144(15) . ?
C21 W1 2.164(11) . ?
C22 N6 1.166(15) . ?
C22 W1 2.129(12) . ?
C23 N7 1.135(13) . ?
C23 W1 2.170(9) . ?
C24 N8 1.153(13) . ?
C24 W1 2.153(8) . ?
C25 N9 1.147(13) . ?
C25 W1 2.159(9) . ?
C26 N10 1.137(13) . ?
C26 W1 2.147(9) . ?
C27 N11 1.085(18) . ?
C27 C28 1.45(2) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Cu1 N1 1.907(11) . ?
Cu1 O2 1.913(7) . ?
Cu1 O3 1.917(7) . ?
Cu1 N2 1.944(11) . ?
Cu1 N9 2.473(10) 2_656 ?
Cu1 Gd1 3.3918(13) . ?
Gd1 O3 2.325(7) . ?
Gd1 O2 2.366(6) . ?
Gd1 O1W 2.411(7) . ?
Gd1 O4W 2.411(7) . ?
Gd1 O3W 2.458(7) . ?
Gd1 O2W 2.460(8) . ?
Gd1 N3 2.504(9) . ?
Gd1 O1 2.587(6) . ?
Gd1 O4 2.695(7) . ?
N9 Cu1 2.473(10) 2_646 ?
C9A H9A1 0.9600 . ?
C9A H9A2 0.9600 . ?
C9A H9A3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
C7 C2 C3 121.8(11) . . ?
C7 C2 O1 113.6(9) . . ?
C3 C2 O1 124.5(11) . . ?
C4 C3 C2 119.2(14) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C5 C4 C3 120.5(13) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C4 C5 C6 121.2(12) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 H5 119.4 . . ?
C7 C6 C5 117.4(12) . . ?
C7 C6 C8 124.0(11) . . ?
C5 C6 C8 118.5(11) . . ?
O2 C7 C2 116.9(8) . . ?
O2 C7 C6 123.2(10) . . ?
C2 C7 C6 119.9(10) . . ?
N1 C8 C6 126.7(10) . . ?
N1 C8 H8 116.7 . . ?
C6 C8 H8 116.7 . . ?
C9A C9 C10 120(2) . . ?
C9A C9 N1 121.2(19) . . ?
C10 C9 N1 114.4(16) . . ?
C9A C9 H9 97.4 . . ?
C10 C9 H9 97.4 . . ?
N1 C9 H9 97.4 . . ?
C9 C10 N2 112.9(14) . . ?
C9 C10 H10A 109.0 . . ?
N2 C10 H10A 109.0 . . ?
C9 C10 H10B 109.0 . . ?
N2 C10 H10B 109.0 . . ?
H10A C10 H10B 107.8 . . ?
N2 C11 C12 126.8(12) . . ?
N2 C11 H11 116.6 . . ?
C12 C11 H11 116.6 . . ?
C17 C12 C13 117.7(13) . . ?
C17 C12 C11 122.4(12) . . ?
C13 C12 C11 119.8(13) . . ?
C14 C13 C12 122.7(14) . . ?
C14 C13 H13 118.6 . . ?
C12 C13 H13 118.6 . . ?
C13 C14 C15 118.4(14) . . ?
C13 C14 H14 120.8 . . ?
C15 C14 H14 120.8 . . ?
C16 C15 C14 121.7(16) . . ?
C16 C15 H15 119.1 . . ?
C14 C15 H15 119.1 . . ?
C15 C16 O4 125.9(12) . . ?
C15 C16 C17 120.4(12) . . ?
O4 C16 C17 113.7(9) . . ?
O3 C17 C16 117.2(9) . . ?
O3 C17 C12 123.9(11) . . ?
C16 C17 C12 119.0(10) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 W1 177.4(8) . . ?
N4 C20 W1 178.0(9) . . ?
N5 C21 W1 178.1(12) . . ?
N6 C22 W1 176.5(11) . . ?
N7 C23 W1 176.6(11) . . ?
N8 C24 W1 177.1(10) . . ?
N9 C25 W1 177.7(10) . . ?
N10 C26 W1 178.6(11) . . ?
N11 C27 C28 179(2) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 Cu1 O2 95.4(4) . . ?
N1 Cu1 O3 170.8(4) . . ?
O2 Cu1 O3 83.5(3) . . ?
N1 Cu1 N2 86.5(6) . . ?
O2 Cu1 N2 171.1(4) . . ?
O3 Cu1 N2 93.1(4) . . ?
N1 Cu1 N9 92.8(4) . 2_656 ?
O2 Cu1 N9 89.1(3) . 2_656 ?
O3 Cu1 N9 96.3(3) . 2_656 ?
N2 Cu1 N9 99.5(4) . 2_656 ?
N1 Cu1 Gd1 136.1(4) . . ?
O2 Cu1 Gd1 42.5(2) . . ?
O3 Cu1 Gd1 41.3(2) . . ?
N2 Cu1 Gd1 132.9(4) . . ?
N9 Cu1 Gd1 97.2(2) 2_656 . ?
O3 Gd1 O2 65.9(2) . . ?
O3 Gd1 O1W 82.7(3) . . ?
O2 Gd1 O1W 69.7(3) . . ?
O3 Gd1 O4W 77.8(3) . . ?
O2 Gd1 O4W 70.1(2) . . ?
O1W Gd1 O4W 139.5(3) . . ?
O3 Gd1 O3W 146.4(3) . . ?
O2 Gd1 O3W 124.4(2) . . ?
O1W Gd1 O3W 73.8(3) . . ?
O4W Gd1 O3W 135.1(3) . . ?
O3 Gd1 O2W 78.8(3) . . ?
O2 Gd1 O2W 130.2(3) . . ?
O1W Gd1 O2W 72.2(3) . . ?
O4W Gd1 O2W 136.0(3) . . ?
O3W Gd1 O2W 71.4(3) . . ?
O3 Gd1 N3 134.7(3) . . ?
O2 Gd1 N3 130.0(3) . . ?
O1W Gd1 N3 140.6(3) . . ?
O4W Gd1 N3 72.5(3) . . ?
O3W Gd1 N3 67.2(3) . . ?
O2W Gd1 N3 99.7(3) . . ?
O3 Gd1 O1 127.2(2) . . ?
O2 Gd1 O1 61.4(2) . . ?
O1W Gd1 O1 81.4(2) . . ?
O4W Gd1 O1 82.7(2) . . ?
O3W Gd1 O1 73.1(2) . . ?
O2W Gd1 O1 140.3(3) . . ?
N3 Gd1 O1 82.2(3) . . ?
O3 Gd1 O4 61.1(2) . . ?
O2 Gd1 O4 119.2(2) . . ?
O1W Gd1 O4 127.1(3) . . ?
O4W Gd1 O4 71.8(2) . . ?
O3W Gd1 O4 116.1(2) . . ?
O2W Gd1 O4 64.3(2) . . ?
N3 Gd1 O4 77.3(3) . . ?
O1 Gd1 O4 151.1(2) . . ?
O3 Gd1 Cu1 32.95(18) . . ?
O2 Gd1 Cu1 33.11(18) . . ?
O1W Gd1 Cu1 71.1(2) . . ?
O4W Gd1 Cu1 73.41(17) . . ?
O3W Gd1 Cu1 144.13(17) . . ?
O2W Gd1 Cu1 104.0(2) . . ?
N3 Gd1 Cu1 145.9(2) . . ?
O1 Gd1 Cu1 94.48(15) . . ?
O4 Gd1 Cu1 91.27(16) . . ?
C8 N1 C9 124.8(13) . . ?
C8 N1 Cu1 125.0(9) . . ?
C9 N1 Cu1 110.2(12) . . ?
C11 N2 C10 123.0(14) . . ?
C11 N2 Cu1 124.8(9) . . ?
C10 N2 Cu1 112.2(12) . . ?
C19 N3 Gd1 172.9(7) . . ?
C25 N9 Cu1 147.5(8) . 2_646 ?
C2 O1 C1 117.2(8) . . ?
C2 O1 Gd1 117.8(6) . . ?
C1 O1 Gd1 124.9(6) . . ?
C7 O2 Cu1 125.5(6) . . ?
C7 O2 Gd1 127.2(6) . . ?
Cu1 O2 Gd1 104.4(3) . . ?
C17 O3 Cu1 122.9(6) . . ?
C17 O3 Gd1 129.9(6) . . ?
Cu1 O3 Gd1 105.8(3) . . ?
C16 O4 C18 115.9(9) . . ?
C16 O4 Gd1 116.0(6) . . ?
C18 O4 Gd1 127.9(7) . . ?
C22 W1 C26 70.7(5) . . ?
C22 W1 C24 86.4(4) . . ?
C26 W1 C24 75.4(4) . . ?
C22 W1 C19 77.1(4) . . ?
C26 W1 C19 133.9(4) . . ?
C24 W1 C19 70.4(4) . . ?
C22 W1 C20 145.6(4) . . ?
C26 W1 C20 143.3(4) . . ?
C24 W1 C20 105.0(4) . . ?
C19 W1 C20 76.6(4) . . ?
C22 W1 C25 101.1(4) . . ?
C26 W1 C25 74.1(4) . . ?
C24 W1 C25 144.0(4) . . ?
C19 W1 C25 145.6(3) . . ?
C20 W1 C25 88.7(4) . . ?
C22 W1 C21 142.2(4) . . ?
C26 W1 C21 72.8(4) . . ?
C24 W1 C21 75.5(4) . . ?
C19 W1 C21 124.7(4) . . ?
C20 W1 C21 71.9(4) . . ?
C25 W1 C21 77.6(4) . . ?
C22 W1 C23 76.6(4) . . ?
C26 W1 C23 126.2(4) . . ?
C24 W1 C23 143.6(4) . . ?
C19 W1 C23 74.6(4) . . ?
C20 W1 C23 75.4(4) . . ?
C25 W1 C23 71.7(4) . . ?
C21 W1 C23 135.1(4) . . ?
C9 C9A H9A1 109.5 . . ?
C9 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C9 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?

_refine_diff_density_max         0.870
_refine_diff_density_min         -1.154
_refine_diff_density_rms         0.103

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_13
_database_code_depnum_ccdc_archive 'CCDC 1060182'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H35 Cu N11 O10 Tb W'
_chemical_formula_weight         1103.99

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'
Tb Tb -0.1723 4.1537 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.1488(18)
_cell_length_b                   20.356(4)
_cell_length_c                   10.386(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.69(3)
_cell_angle_gamma                90
_cell_volume                     1921.0(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12871
_cell_measurement_theta_min      2.81
_cell_measurement_theta_max      28.44

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_F_000             1068
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    5.422
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7610
_exptl_absorpt_correction_T_max  1.0175
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16713
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_av_R_equivalents  0.0819
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.809
_diffrn_reflns_theta_max         26.994
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_point_group_measured_fraction_full 0.949
_reflns_number_total             7952
_reflns_number_gt                5939
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.874
_reflns_Friedel_fraction_max     0.910
_reflns_Friedel_fraction_full    0.913

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0219P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2216 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(12)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7952
_refine_ls_number_parameters     479
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.0806
_refine_ls_wR_factor_gt          0.0754
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_restrained_S_all      0.889
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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 0.687(2) 0.3535(10) 0.821(2) 0.069(6) Uani 1 1 d . . . . .
H1A H 0.6497 0.3843 0.7551 0.103 Uiso 1 1 calc R U . . .
H1B H 0.7283 0.3769 0.8968 0.103 Uiso 1 1 calc R U . . .
H1C H 0.7625 0.3271 0.7890 0.103 Uiso 1 1 calc R U . . .
C2 C 0.6108(19) 0.2648(9) 0.9474(15) 0.042(4) Uani 1 1 d . . . . .
C3 C 0.7378(19) 0.2621(11) 1.0279(18) 0.060(5) Uani 1 1 d . . . . .
H3 H 0.8110 0.2933 1.0228 0.072 Uiso 1 1 calc R U . . .
C4 C 0.757(3) 0.2100(13) 1.122(2) 0.084(8) Uani 1 1 d . . . . .
H4 H 0.8456 0.2068 1.1758 0.100 Uiso 1 1 calc R U . . .
C5 C 0.655(3) 0.1677(13) 1.133(2) 0.076(7) Uani 1 1 d . . . . .
H5 H 0.6712 0.1353 1.1964 0.092 Uiso 1 1 calc R U . . .
C6 C 0.523(2) 0.1689(10) 1.0545(16) 0.051(5) Uani 1 1 d . . . . .
C7 C 0.5008(18) 0.2178(8) 0.9599(13) 0.037(4) Uani 1 1 d . . . . .
C8 C 0.414(3) 0.1209(9) 1.0784(18) 0.061(6) Uani 1 1 d . . . . .
H8 H 0.4401 0.0906 1.1440 0.073 Uiso 1 1 calc R U . . .
C9 C 0.166(4) 0.0711(18) 1.050(3) 0.148(17) Uani 1 1 d . . . . .
H9 H 0.1756 0.0401 0.9792 0.178 Uiso 1 1 calc R U . . .
C10 C 0.023(3) 0.0873(16) 1.011(4) 0.117(11) Uani 1 1 d . . . . .
H10A H -0.0199 0.1074 1.0830 0.141 Uiso 1 1 calc R U . . .
H10B H -0.0327 0.0479 0.9857 0.141 Uiso 1 1 calc R U . . .
C11 C -0.106(3) 0.1438(10) 0.828(2) 0.075(7) Uani 1 1 d . . . . .
H11 H -0.1885 0.1205 0.8464 0.090 Uiso 1 1 calc R U . . .
C12 C -0.125(2) 0.1881(9) 0.719(2) 0.059(5) Uani 1 1 d . . . . .
C13 C -0.256(2) 0.1884(14) 0.629(3) 0.088(8) Uani 1 1 d . . . . .
H13 H -0.3345 0.1631 0.6497 0.106 Uiso 1 1 calc R U . . .
C14 C -0.274(2) 0.2206(15) 0.522(2) 0.089(9) Uani 1 1 d . . . . .
H14 H -0.3599 0.2156 0.4657 0.107 Uiso 1 1 calc R U . . .
C15 C -0.165(2) 0.2623(11) 0.490(2) 0.065(6) Uani 1 1 d . . . . .
H15 H -0.1797 0.2870 0.4141 0.078 Uiso 1 1 calc R U . . .
C16 C -0.0321(18) 0.2676(9) 0.5724(18) 0.046(4) Uani 1 1 d . . . . .
C17 C -0.0104(17) 0.2309(9) 0.6882(17) 0.047(4) Uani 1 1 d . . . . .
C18 C 0.087(2) 0.3315(12) 0.4243(16) 0.068(6) Uani 1 1 d . . . . .
H18A H 0.1761 0.3563 0.4211 0.102 Uiso 1 1 calc R U . . .
H18B H 0.0831 0.2966 0.3617 0.102 Uiso 1 1 calc R U . . .
H18C H 0.0037 0.3598 0.4049 0.102 Uiso 1 1 calc R U . . .
C19 C 0.4616(18) 0.4036(8) 0.5027(16) 0.038(4) Uani 1 1 d . . . . .
C20 C 0.7440(18) 0.4391(8) 0.4937(14) 0.040(4) Uani 1 1 d . . . . .
C21 C 0.737(2) 0.4268(8) 0.2494(15) 0.045(4) Uani 1 1 d . . . . .
C22 C 0.327(2) 0.4855(10) 0.3289(16) 0.050(5) Uani 1 1 d . . . . .
C23 C 0.536(2) 0.5283(9) 0.5107(17) 0.044(4) Uani 1 1 d . . . . .
C24 C 0.483(2) 0.3683(10) 0.2748(15) 0.051(5) Uani 1 1 d . . . . .
C25 C 0.6636(19) 0.5512(9) 0.3106(15) 0.042(4) Uani 1 1 d . . . . .
C26 C 0.4928(19) 0.4795(8) 0.1514(16) 0.050(4) Uani 1 1 d . . . . .
C27 C 0.101(3) 0.5537(11) 0.615(2) 0.075(7) Uani 1 1 d . . . . .
C28 C -0.007(3) 0.5855(12) 0.523(3) 0.095(9) Uani 1 1 d . . . . .
H28A H 0.0415 0.6056 0.4561 0.143 Uiso 1 1 calc R U . . .
H28B H -0.0575 0.6185 0.5669 0.143 Uiso 1 1 calc R U . . .
H28C H -0.0761 0.5534 0.4857 0.143 Uiso 1 1 calc R U . . .
Cu1 Cu 0.2017(3) 0.17346(12) 0.8817(2) 0.0488(6) Uani 1 1 d . . . . .
Tb1 Tb 0.29786(7) 0.31832(4) 0.75473(6) 0.03146(17) Uani 1 1 d . . . . .
N1 N 0.283(2) 0.1161(8) 1.0175(16) 0.075(5) Uani 1 1 d . . . . .
N2 N 0.0146(19) 0.1336(8) 0.9012(16) 0.060(4) Uani 1 1 d . . . . .
N3 N 0.4077(16) 0.3728(8) 0.5750(13) 0.046(4) Uani 1 1 d . . . . .
N4 N 0.8431(15) 0.4261(8) 0.5720(15) 0.053(4) Uani 1 1 d . . . . .
N5 N 0.8284(19) 0.4102(9) 0.1933(17) 0.071(5) Uani 1 1 d . . . . .
N6 N 0.205(2) 0.4995(12) 0.3040(19) 0.093(8) Uani 1 1 d . . . . .
N7 N 0.5296(18) 0.5663(8) 0.5908(15) 0.059(4) Uani 1 1 d . . . . .
N8 N 0.4424(16) 0.3177(9) 0.2315(12) 0.058(4) Uani 1 1 d . . . . .
N9 N 0.715(2) 0.6000(9) 0.2889(14) 0.063(4) Uani 1 1 d . . . . .
N10 N 0.456(2) 0.4872(9) 0.0435(14) 0.076(6) Uani 1 1 d . . . . .
N11 N 0.178(3) 0.5282(11) 0.685(3) 0.119(9) Uani 1 1 d . . . . .
O1 O 0.5713(10) 0.3123(6) 0.8524(9) 0.043(2) Uani 1 1 d . . . . .
O2 O 0.3764(12) 0.2258(6) 0.8771(10) 0.042(3) Uani 1 1 d . . . . .
O1W O 0.2628(12) 0.3345(6) 0.9789(10) 0.052(3) Uani 1 1 d . . . . .
O3 O 0.1186(12) 0.2390(6) 0.7670(12) 0.044(3) Uani 1 1 d . . . . .
O2W O 0.0821(14) 0.3886(7) 0.7600(13) 0.061(4) Uani 1 1 d . . . . .
O4 O 0.0860(11) 0.3044(6) 0.5506(10) 0.048(3) Uani 1 1 d . . . . .
O3W O 0.3796(14) 0.4302(6) 0.8100(11) 0.052(3) Uani 1 1 d . . . . .
O4W O 0.3739(13) 0.2340(6) 0.6148(11) 0.044(3) Uani 1 1 d . . . . .
O5W O 0.3358(17) 0.1975(8) 0.3574(13) 0.076(4) Uani 1 1 d . . . . .
O6W O 0.0821(16) 0.4246(8) 1.0664(15) 0.089(5) Uani 1 1 d . . . . .
W1 W 0.55699(6) 0.46040(3) 0.35455(5) 0.03061(14) Uani 1 1 d . . . . .
C9A C 0.195(3) 0.0248(17) 1.151(3) 0.137(13) Uani 1 1 d . . . . .
H9A1 H 0.2994 0.0179 1.1683 0.205 Uiso 1 1 calc R U . . .
H9A2 H 0.1580 0.0409 1.2276 0.205 Uiso 1 1 calc R U . . .
H9A3 H 0.1477 -0.0160 1.1253 0.205 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.421(19) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.35(2) . ?
C2 O1 1.398(19) . ?
C2 C7 1.40(3) . ?
C3 C4 1.44(3) . ?
C3 H3 0.9300 . ?
C4 C5 1.28(3) . ?
C4 H4 0.9300 . ?
C5 C6 1.38(3) . ?
C5 H5 0.9300 . ?
C6 C7 1.40(2) . ?
C6 C8 1.44(3) . ?
C7 O2 1.354(18) . ?
C8 N1 1.29(3) . ?
C8 H8 0.9300 . ?
C9 C10 1.37(4) . ?
C9 C9A 1.41(3) . ?
C9 N1 1.48(3) . ?
C9 H9 0.9800 . ?
C10 N2 1.48(3) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.28(3) . ?
C11 C12 1.44(3) . ?
C11 H11 0.9300 . ?
C12 C17 1.43(2) . ?
C12 C13 1.43(3) . ?
C13 C14 1.29(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.38(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.41(2) . ?
C15 H15 0.9300 . ?
C16 O4 1.36(2) . ?
C16 C17 1.41(3) . ?
C17 O3 1.37(2) . ?
C18 O4 1.425(19) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N3 1.134(17) . ?
C19 W1 2.187(16) . ?
C20 N4 1.17(2) . ?
C20 W1 2.151(16) . ?
C21 N5 1.12(2) . ?
C21 W1 2.191(17) . ?
C22 N6 1.15(2) . ?
C22 W1 2.149(19) . ?
C23 N7 1.14(2) . ?
C23 W1 2.157(17) . ?
C24 N8 1.17(2) . ?
C24 W1 2.13(2) . ?
C25 N9 1.13(2) . ?
C25 W1 2.164(18) . ?
C26 N10 1.14(2) . ?
C26 W1 2.159(17) . ?
C27 N11 1.08(3) . ?
C27 C28 1.44(3) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Cu1 O3 1.887(12) . ?
Cu1 N1 1.914(18) . ?
Cu1 N2 1.926(16) . ?
Cu1 O2 1.927(11) . ?
Cu1 Tb1 3.388(2) . ?
Tb1 O3 2.316(11) . ?
Tb1 O2 2.337(11) . ?
Tb1 O1W 2.409(10) . ?
Tb1 O4W 2.403(11) . ?
Tb1 O2W 2.444(12) . ?
Tb1 O3W 2.445(12) . ?
Tb1 N3 2.482(14) . ?
Tb1 O1 2.590(9) . ?
Tb1 O4 2.715(10) . ?
C9A H9A1 0.9600 . ?
C9A H9A2 0.9600 . ?
C9A H9A3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 126.7(18) . . ?
C3 C2 C7 119.3(17) . . ?
O1 C2 C7 114.0(14) . . ?
C2 C3 C4 119(2) . . ?
C2 C3 H3 120.7 . . ?
C4 C3 H3 120.7 . . ?
C5 C4 C3 121(2) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 122(2) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C7 C6 C5 118(2) . . ?
C7 C6 C8 124.1(17) . . ?
C5 C6 C8 118(2) . . ?
O2 C7 C6 125.0(16) . . ?
O2 C7 C2 114.6(14) . . ?
C6 C7 C2 120.3(15) . . ?
N1 C8 C6 126.1(17) . . ?
N1 C8 H8 117.0 . . ?
C6 C8 H8 117.0 . . ?
C10 C9 C9A 118(3) . . ?
C10 C9 N1 119(3) . . ?
C9A C9 N1 120(3) . . ?
C10 C9 H9 95.8 . . ?
C9A C9 H9 95.8 . . ?
N1 C9 H9 95.8 . . ?
C9 C10 N2 110(2) . . ?
C9 C10 H10A 109.7 . . ?
N2 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
N2 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
N2 C11 C12 125.8(19) . . ?
N2 C11 H11 117.1 . . ?
C12 C11 H11 117.1 . . ?
C17 C12 C13 115.5(19) . . ?
C17 C12 C11 122.1(19) . . ?
C13 C12 C11 122.2(19) . . ?
C14 C13 C12 126(2) . . ?
C14 C13 H13 117.2 . . ?
C12 C13 H13 117.2 . . ?
C13 C14 C15 120(2) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C16 120(2) . . ?
C14 C15 H15 120.1 . . ?
C16 C15 H15 120.1 . . ?
O4 C16 C15 126.2(18) . . ?
O4 C16 C17 113.5(14) . . ?
C15 C16 C17 120.2(17) . . ?
O3 C17 C12 123.0(18) . . ?
O3 C17 C16 118.3(14) . . ?
C12 C17 C16 118.7(16) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 W1 176.7(13) . . ?
N4 C20 W1 177.7(15) . . ?
N5 C21 W1 178.6(17) . . ?
N6 C22 W1 174.1(16) . . ?
N7 C23 W1 176.4(16) . . ?
N8 C24 W1 179.8(16) . . ?
N9 C25 W1 177.2(17) . . ?
N10 C26 W1 177.3(16) . . ?
N11 C27 C28 177(3) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O3 Cu1 N1 171.7(7) . . ?
O3 Cu1 N2 93.8(7) . . ?
N1 Cu1 N2 86.5(8) . . ?
O3 Cu1 O2 82.4(5) . . ?
N1 Cu1 O2 95.9(7) . . ?
N2 Cu1 O2 170.3(6) . . ?
O3 Cu1 Tb1 40.8(3) . . ?
N1 Cu1 Tb1 136.2(6) . . ?
N2 Cu1 Tb1 133.0(6) . . ?
O2 Cu1 Tb1 41.8(3) . . ?
O3 Tb1 O2 65.4(4) . . ?
O3 Tb1 O1W 82.4(4) . . ?
O2 Tb1 O1W 69.6(4) . . ?
O3 Tb1 O4W 78.0(4) . . ?
O2 Tb1 O4W 70.2(4) . . ?
O1W Tb1 O4W 139.6(4) . . ?
O3 Tb1 O2W 80.1(4) . . ?
O2 Tb1 O2W 131.1(4) . . ?
O1W Tb1 O2W 72.5(4) . . ?
O4W Tb1 O2W 136.3(4) . . ?
O3 Tb1 O3W 146.7(4) . . ?
O2 Tb1 O3W 123.8(4) . . ?
O1W Tb1 O3W 73.6(4) . . ?
O4W Tb1 O3W 134.8(4) . . ?
O2W Tb1 O3W 71.0(5) . . ?
O3 Tb1 N3 134.8(4) . . ?
O2 Tb1 N3 130.0(5) . . ?
O1W Tb1 N3 141.0(4) . . ?
O4W Tb1 N3 72.1(5) . . ?
O2W Tb1 N3 98.9(5) . . ?
O3W Tb1 N3 67.7(4) . . ?
O3 Tb1 O1 127.1(4) . . ?
O2 Tb1 O1 61.8(4) . . ?
O1W Tb1 O1 81.9(3) . . ?
O4W Tb1 O1 82.4(4) . . ?
O2W Tb1 O1 139.9(4) . . ?
O3W Tb1 O1 72.4(4) . . ?
N3 Tb1 O1 81.9(4) . . ?
O3 Tb1 O4 61.6(4) . . ?
O2 Tb1 O4 119.1(4) . . ?
O1W Tb1 O4 127.3(4) . . ?
O4W Tb1 O4 71.6(4) . . ?
O2W Tb1 O4 64.8(4) . . ?
O3W Tb1 O4 116.8(4) . . ?
N3 Tb1 O4 77.0(4) . . ?
O1 Tb1 O4 150.4(3) . . ?
O3 Tb1 Cu1 32.2(3) . . ?
O2 Tb1 Cu1 33.3(3) . . ?
O1W Tb1 Cu1 70.9(3) . . ?
O4W Tb1 Cu1 73.8(3) . . ?
O2W Tb1 Cu1 104.7(4) . . ?
O3W Tb1 Cu1 143.7(3) . . ?
N3 Tb1 Cu1 145.9(4) . . ?
O1 Tb1 Cu1 95.1(3) . . ?
O4 Tb1 Cu1 91.1(3) . . ?
C8 N1 C9 126.2(19) . . ?
C8 N1 Cu1 125.0(13) . . ?
C9 N1 Cu1 108.5(18) . . ?
C11 N2 C10 121.8(19) . . ?
C11 N2 Cu1 125.6(15) . . ?
C10 N2 Cu1 112.6(16) . . ?
C19 N3 Tb1 172.0(13) . . ?
C2 O1 C1 115.6(13) . . ?
C2 O1 Tb1 117.9(9) . . ?
C1 O1 Tb1 126.5(11) . . ?
C7 O2 Cu1 123.7(10) . . ?
C7 O2 Tb1 128.7(10) . . ?
Cu1 O2 Tb1 104.8(5) . . ?
C17 O3 Cu1 123.4(11) . . ?
C17 O3 Tb1 128.2(11) . . ?
Cu1 O3 Tb1 107.0(5) . . ?
C16 O4 C18 117.4(13) . . ?
C16 O4 Tb1 116.0(10) . . ?
C18 O4 Tb1 126.6(10) . . ?
C24 W1 C20 106.0(7) . . ?
C24 W1 C23 143.6(7) . . ?
C20 W1 C23 76.0(6) . . ?
C24 W1 C25 143.3(6) . . ?
C20 W1 C25 88.3(6) . . ?
C23 W1 C25 72.2(6) . . ?
C24 W1 C26 74.9(6) . . ?
C20 W1 C26 142.9(6) . . ?
C23 W1 C26 125.6(7) . . ?
C25 W1 C26 73.6(6) . . ?
C24 W1 C22 84.2(7) . . ?
C20 W1 C22 145.2(6) . . ?
C23 W1 C22 76.6(7) . . ?
C25 W1 C22 103.3(7) . . ?
C26 W1 C22 71.7(6) . . ?
C24 W1 C21 75.8(7) . . ?
C20 W1 C21 71.7(6) . . ?
C23 W1 C21 135.6(6) . . ?
C25 W1 C21 77.1(6) . . ?
C26 W1 C21 72.8(6) . . ?
C22 W1 C21 142.6(6) . . ?
C24 W1 C19 70.9(6) . . ?
C20 W1 C19 76.8(6) . . ?
C23 W1 C19 74.4(6) . . ?
C25 W1 C19 145.8(6) . . ?
C26 W1 C19 134.3(6) . . ?
C22 W1 C19 75.4(6) . . ?
C21 W1 C19 124.8(6) . . ?
C9 C9A H9A1 109.5 . . ?
C9 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C9 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?

_refine_diff_density_max         1.030
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.136

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_14
_database_code_depnum_ccdc_archive 'CCDC 1060183'
_audit_update_record             
;
2015-06-15 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H35 Cu Dy N11 O10 W'
_chemical_formula_weight         1107.57

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'
Dy Dy -0.1892 4.4098 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   9.1370(9)
_cell_length_b                   20.3334(14)
_cell_length_c                   10.3859(10)
_cell_angle_alpha                90
_cell_angle_beta                 96.566(8)
_cell_angle_gamma                90
_cell_volume                     1916.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    14729
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      27.34

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_F_000             1070
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    5.538
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4452
_exptl_absorpt_correction_T_max  0.5157
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20397
_diffrn_reflns_av_unetI/netI     0.2112
_diffrn_reflns_av_R_equivalents  0.1172
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.213
_diffrn_reflns_theta_max         27.338
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.986
_reflns_number_total             8525
_reflns_number_gt                4153
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.913
_reflns_Friedel_fraction_max     0.965
_reflns_Friedel_fraction_full    0.974

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     'w=1/[σ²(Fo²)] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00073(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1344 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.039(18)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         8525
_refine_ls_number_parameters     480
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0491
_refine_ls_wR_factor_ref         0.0909
_refine_ls_wR_factor_gt          0.0703
_refine_ls_goodness_of_fit_ref   0.695
_refine_ls_restrained_S_all      0.695
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.681(3) 0.3544(12) 0.821(2) 0.067(7) Uani 1 1 d . . . . .
H1A H 0.6418 0.3860 0.7576 0.100 Uiso 1 1 calc R U . . .
H1B H 0.7239 0.3769 0.8975 0.100 Uiso 1 1 calc R U . . .
H1C H 0.7554 0.3286 0.7862 0.100 Uiso 1 1 calc R U . . .
C2 C 0.610(3) 0.2640(12) 0.945(2) 0.052(7) Uani 1 1 d . . . . .
C3 C 0.741(3) 0.2638(13) 1.029(3) 0.067(7) Uani 1 1 d . . . . .
H3 H 0.8125 0.2960 1.0236 0.080 Uiso 1 1 calc R U . . .
C4 C 0.762(4) 0.2142(18) 1.121(3) 0.088(11) Uani 1 1 d . . . . .
H4 H 0.8512 0.2124 1.1745 0.106 Uiso 1 1 calc R U . . .
C5 C 0.656(4) 0.1677(13) 1.136(2) 0.084(10) Uani 1 1 d . . . . .
H5 H 0.6734 0.1356 1.1996 0.100 Uiso 1 1 calc R U . . .
C6 C 0.523(4) 0.1685(14) 1.056(2) 0.071(8) Uani 1 1 d . . . . .
C7 C 0.499(3) 0.2191(11) 0.959(2) 0.050(6) Uani 1 1 d . . . . .
C8 C 0.411(4) 0.1207(12) 1.078(3) 0.071(9) Uani 1 1 d . . . . .
H8 H 0.4352 0.0896 1.1429 0.085 Uiso 1 1 calc R U . . .
C9 C 0.170(7) 0.069(2) 1.046(3) 0.14(2) Uani 1 1 d . . . . .
H9 H 0.1840 0.0386 0.9754 0.173 Uiso 1 1 calc R U . . .
C10 C 0.020(7) 0.085(2) 1.004(6) 0.19(3) Uani 1 1 d . . . . .
H10A H -0.0270 0.1031 1.0760 0.222 Uiso 1 1 calc R U . . .
H10B H -0.0338 0.0462 0.9727 0.222 Uiso 1 1 calc R U . . .
C11 C -0.099(4) 0.1448(13) 0.834(3) 0.086(11) Uani 1 1 d . . . . .
H11 H -0.1826 0.1234 0.8570 0.104 Uiso 1 1 calc R U . . .
C12 C -0.120(3) 0.1886(14) 0.721(3) 0.074(8) Uani 1 1 d . . . . .
C13 C -0.255(4) 0.1874(16) 0.635(3) 0.089(10) Uani 1 1 d . . . . .
H13 H -0.3322 0.1613 0.6563 0.107 Uiso 1 1 calc R U . . .
C14 C -0.274(4) 0.2240(16) 0.520(4) 0.089(11) Uani 1 1 d . . . . .
H14 H -0.3605 0.2215 0.4628 0.107 Uiso 1 1 calc R U . . .
C15 C -0.160(3) 0.2631(16) 0.495(3) 0.084(9) Uani 1 1 d . . . . .
H15 H -0.1725 0.2880 0.4199 0.101 Uiso 1 1 calc R U . . .
C16 C -0.033(3) 0.2691(13) 0.570(3) 0.053(7) Uani 1 1 d . . . . .
C17 C -0.011(3) 0.2308(11) 0.688(2) 0.049(6) Uani 1 1 d . . . . .
C18 C 0.089(3) 0.3311(15) 0.423(2) 0.083(8) Uani 1 1 d . . . . .
H18A H 0.1781 0.3557 0.4181 0.124 Uiso 1 1 calc R U . . .
H18B H 0.0845 0.2955 0.3619 0.124 Uiso 1 1 calc R U . . .
H18C H 0.0056 0.3593 0.4028 0.124 Uiso 1 1 calc R U . . .
C19 C 0.461(3) 0.4042(11) 0.499(2) 0.048(6) Uani 1 1 d . . . . .
C20 C 0.743(3) 0.4404(10) 0.497(2) 0.050(6) Uani 1 1 d . . . . .
C21 C 0.732(3) 0.4281(11) 0.249(3) 0.057(6) Uani 1 1 d . . . . .
C22 C 0.351(4) 0.4865(13) 0.336(3) 0.072(9) Uani 1 1 d . . . . .
C23 C 0.538(3) 0.5286(12) 0.512(2) 0.051(7) Uani 1 1 d . . . . .
C24 C 0.487(3) 0.3662(11) 0.279(2) 0.064(8) Uani 1 1 d . . . . .
C25 C 0.663(3) 0.5527(12) 0.314(2) 0.050(6) Uani 1 1 d . . . . .
C26 C 0.492(2) 0.4782(10) 0.155(2) 0.053(6) Uani 1 1 d . . . . .
C27 C 0.101(4) 0.5534(15) 0.615(4) 0.092(11) Uani 1 1 d . . . . .
C28 C -0.008(5) 0.5837(15) 0.522(3) 0.109(12) Uani 1 1 d . . . . .
H28A H -0.0044 0.5638 0.4384 0.163 Uiso 1 1 calc R U . . .
H28B H 0.0117 0.6299 0.5164 0.163 Uiso 1 1 calc R U . . .
H28C H -0.1043 0.5773 0.5485 0.163 Uiso 1 1 calc R U . . .
Cu1 Cu 0.2021(4) 0.17388(15) 0.8816(3) 0.0603(10) Uani 1 1 d . . . . .
Dy1 Dy 0.29818(12) 0.31834(5) 0.75442(9) 0.0426(3) Uani 1 1 d . . . . .
N1 N 0.285(3) 0.1178(10) 1.0185(19) 0.076(7) Uani 1 1 d . . . . .
N2 N 0.018(3) 0.1337(11) 0.901(2) 0.068(6) Uani 1 1 d . . . . .
N3 N 0.403(3) 0.3736(10) 0.5750(19) 0.059(6) Uani 1 1 d . . . . .
N4 N 0.843(2) 0.4257(10) 0.569(2) 0.058(5) Uani 1 1 d . . . . .
N5 N 0.828(3) 0.4115(12) 0.192(2) 0.082(8) Uani 1 1 d . . . . .
N6 N 0.212(4) 0.5012(14) 0.306(2) 0.097(10) Uani 1 1 d . . . . .
N7 N 0.523(3) 0.5676(10) 0.594(2) 0.076(7) Uani 1 1 d . . . . .
N8 N 0.442(2) 0.3170(11) 0.2309(16) 0.071(5) Uani 1 1 d . . . . .
N9 N 0.716(3) 0.5998(11) 0.2857(18) 0.068(6) Uani 1 1 d . . . . .
N10 N 0.460(3) 0.4867(10) 0.0437(19) 0.100(10) Uani 1 1 d . . . . .
N11 N 0.179(4) 0.5299(15) 0.689(4) 0.144(15) Uani 1 1 d . . . . .
O1 O 0.5681(17) 0.3132(8) 0.8525(15) 0.058(4) Uani 1 1 d . . . . .
O2 O 0.3725(18) 0.2242(7) 0.8773(14) 0.049(4) Uani 1 1 d . . . . .
O1W O 0.2638(18) 0.3342(8) 0.9764(12) 0.069(5) Uani 1 1 d . . . . .
O3 O 0.1190(18) 0.2405(8) 0.7632(14) 0.049(4) Uani 1 1 d . . . . .
O2W O 0.083(2) 0.3885(9) 0.7581(17) 0.070(6) Uani 1 1 d . . . . .
O4 O 0.0885(19) 0.3051(7) 0.5520(14) 0.059(4) Uani 1 1 d . . . . .
O3W O 0.3785(19) 0.4302(7) 0.8079(15) 0.057(4) Uani 1 1 d . . . . .
O4W O 0.3760(17) 0.2355(7) 0.6162(14) 0.051(4) Uani 1 1 d . . . . .
O5W O 0.337(2) 0.1988(8) 0.3576(15) 0.075(5) Uani 1 1 d . . . . .
O6W O 0.086(2) 0.4235(11) 1.066(2) 0.103(7) Uani 1 1 d . . . . .
W1 W 0.55660(10) 0.46034(4) 0.35468(8) 0.0419(3) Uani 1 1 d . . . . .
C9A C 0.194(5) 0.027(2) 1.142(4) 0.164(17) Uani 1 1 d . . . . .
H9A1 H 0.2980 0.0196 1.1621 0.246 Uiso 1 1 calc R U . . .
H9A2 H 0.1548 0.0438 1.2175 0.246 Uiso 1 1 calc R U . . .
H9A3 H 0.1465 -0.0143 1.1177 0.246 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.40(2) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C7 1.39(4) . ?
C2 C3 1.40(4) . ?
C2 O1 1.41(3) . ?
C3 C4 1.39(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.38(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.39(4) . ?
C5 H5 0.9300 . ?
C6 C7 1.44(4) . ?
C6 C8 1.45(4) . ?
C7 O2 1.36(3) . ?
C8 N1 1.25(3) . ?
C8 H8 0.9300 . ?
C9 C9A 1.33(4) . ?
C9 C10 1.43(6) . ?
C9 N1 1.49(4) . ?
C9 H9 0.9800 . ?
C10 N2 1.45(4) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 N2 1.23(4) . ?
C11 C12 1.47(4) . ?
C11 H11 0.9300 . ?
C12 C17 1.39(3) . ?
C12 C13 1.43(4) . ?
C13 C14 1.40(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.36(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.33(3) . ?
C15 H15 0.9300 . ?
C16 O4 1.36(3) . ?
C16 C17 1.44(3) . ?
C17 O3 1.36(3) . ?
C18 O4 1.44(2) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 N3 1.18(2) . ?
C19 W1 2.15(2) . ?
C20 N4 1.15(3) . ?
C20 W1 2.17(3) . ?
C21 N5 1.17(3) . ?
C21 W1 2.14(3) . ?
C22 N6 1.31(4) . ?
C22 W1 1.94(4) . ?
C23 N7 1.18(3) . ?
C23 W1 2.16(2) . ?
C24 N8 1.17(3) . ?
C24 W1 2.14(2) . ?
C25 N9 1.13(3) . ?
C25 W1 2.18(2) . ?
C26 N10 1.17(3) . ?
C26 W1 2.12(2) . ?
C27 N11 1.09(4) . ?
C27 C28 1.45(5) . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
Cu1 O2 1.868(16) . ?
Cu1 N2 1.90(2) . ?
Cu1 N1 1.91(2) . ?
Cu1 O3 1.925(16) . ?
Cu1 N9 2.478(19) 2_646 ?
Cu1 Dy1 3.377(3) . ?
Dy1 O3 2.287(17) . ?
Dy1 O2 2.356(14) . ?
Dy1 O4W 2.374(14) . ?
Dy1 O1W 2.384(13) . ?
Dy1 O3W 2.434(15) . ?
Dy1 O2W 2.435(18) . ?
Dy1 N3 2.46(2) . ?
Dy1 O1 2.560(15) . ?
Dy1 O4 2.691(16) . ?
N9 Cu1 2.478(19) 2_656 ?
C9A H9A1 0.9600 . ?
C9A H9A2 0.9600 . ?
C9A H9A3 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
C7 C2 C3 121(2) . . ?
C7 C2 O1 113(2) . . ?
C3 C2 O1 125(2) . . ?
C4 C3 C2 118(3) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C5 C4 C3 122(3) . . ?
C5 C4 H4 118.9 . . ?
C3 C4 H4 118.9 . . ?
C4 C5 C6 120(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 119(3) . . ?
C5 C6 C8 119(3) . . ?
C7 C6 C8 122(3) . . ?
O2 C7 C2 118(2) . . ?
O2 C7 C6 123(2) . . ?
C2 C7 C6 119(3) . . ?
N1 C8 C6 126(3) . . ?
N1 C8 H8 117.2 . . ?
C6 C8 H8 117.2 . . ?
C9A C9 C10 117(4) . . ?
C9A C9 N1 121(4) . . ?
C10 C9 N1 118(4) . . ?
C9A C9 H9 97.1 . . ?
C10 C9 H9 97.1 . . ?
N1 C9 H9 97.1 . . ?
C9 C10 N2 108(4) . . ?
C9 C10 H10A 110.1 . . ?
N2 C10 H10A 110.1 . . ?
C9 C10 H10B 110.1 . . ?
N2 C10 H10B 110.1 . . ?
H10A C10 H10B 108.4 . . ?
N2 C11 C12 126(3) . . ?
N2 C11 H11 116.9 . . ?
C12 C11 H11 116.9 . . ?
C17 C12 C13 116(3) . . ?
C17 C12 C11 123(3) . . ?
C13 C12 C11 121(3) . . ?
C14 C13 C12 122(3) . . ?
C14 C13 H13 118.8 . . ?
C12 C13 H13 118.8 . . ?
C15 C14 C13 116(3) . . ?
C15 C14 H14 121.8 . . ?
C13 C14 H14 121.8 . . ?
C16 C15 C14 126(3) . . ?
C16 C15 H15 117.1 . . ?
C14 C15 H15 117.1 . . ?
C15 C16 O4 130(3) . . ?
C15 C16 C17 118(3) . . ?
O4 C16 C17 112(2) . . ?
O3 C17 C12 123(2) . . ?
O3 C17 C16 116(2) . . ?
C12 C17 C16 121(2) . . ?
O4 C18 H18A 109.5 . . ?
O4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N3 C19 W1 178(2) . . ?
N4 C20 W1 175.4(19) . . ?
N5 C21 W1 179(2) . . ?
N6 C22 W1 172(2) . . ?
N7 C23 W1 177(2) . . ?
N8 C24 W1 175(2) . . ?
N9 C25 W1 177(2) . . ?
N10 C26 W1 178(2) . . ?
N11 C27 C28 177(5) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O2 Cu1 N2 171.0(8) . . ?
O2 Cu1 N1 94.9(9) . . ?
N2 Cu1 N1 86.8(11) . . ?
O2 Cu1 O3 82.4(7) . . ?
N2 Cu1 O3 94.6(9) . . ?
N1 Cu1 O3 171.4(8) . . ?
O2 Cu1 N9 89.9(8) . 2_646 ?
N2 Cu1 N9 98.9(9) . 2_646 ?
N1 Cu1 N9 91.9(8) . 2_646 ?
O3 Cu1 N9 96.2(7) . 2_646 ?
O2 Cu1 Dy1 42.2(4) . . ?
N2 Cu1 Dy1 133.4(8) . . ?
N1 Cu1 Dy1 135.4(7) . . ?
O3 Cu1 Dy1 40.5(5) . . ?
N9 Cu1 Dy1 98.1(6) 2_646 . ?
O3 Dy1 O2 65.1(6) . . ?
O3 Dy1 O4W 78.4(5) . . ?
O2 Dy1 O4W 70.3(5) . . ?
O3 Dy1 O1W 83.1(5) . . ?
O2 Dy1 O1W 69.4(6) . . ?
O4W Dy1 O1W 139.7(5) . . ?
O3 Dy1 O3W 146.8(5) . . ?
O2 Dy1 O3W 125.1(6) . . ?
O4W Dy1 O3W 134.2(5) . . ?
O1W Dy1 O3W 73.9(5) . . ?
O3 Dy1 O2W 79.7(6) . . ?
O2 Dy1 O2W 130.6(6) . . ?
O4W Dy1 O2W 136.4(6) . . ?
O1W Dy1 O2W 73.1(6) . . ?
O3W Dy1 O2W 70.9(6) . . ?
O3 Dy1 N3 133.6(6) . . ?
O2 Dy1 N3 131.8(7) . . ?
O4W Dy1 N3 72.3(6) . . ?
O1W Dy1 N3 140.9(6) . . ?
O3W Dy1 N3 67.2(6) . . ?
O2W Dy1 N3 97.5(7) . . ?
O3 Dy1 O1 128.1(5) . . ?
O2 Dy1 O1 63.0(5) . . ?
O4W Dy1 O1 82.5(5) . . ?
O1W Dy1 O1 81.3(5) . . ?
O3W Dy1 O1 72.3(5) . . ?
O2W Dy1 O1 139.6(6) . . ?
N3 Dy1 O1 83.0(6) . . ?
O3 Dy1 O4 60.9(5) . . ?
O2 Dy1 O4 118.5(5) . . ?
O4W Dy1 O4 72.1(5) . . ?
O1W Dy1 O4 127.5(5) . . ?
O3W Dy1 O4 116.2(5) . . ?
O2W Dy1 O4 64.3(5) . . ?
N3 Dy1 O4 76.1(6) . . ?
O1 Dy1 O4 150.9(5) . . ?
O3 Dy1 Cu1 33.2(4) . . ?
O2 Dy1 Cu1 32.2(4) . . ?
O4W Dy1 Cu1 74.3(4) . . ?
O1W Dy1 Cu1 70.8(4) . . ?
O3W Dy1 Cu1 143.9(4) . . ?
O2W Dy1 Cu1 104.9(5) . . ?
N3 Dy1 Cu1 146.5(5) . . ?
O1 Dy1 Cu1 95.2(4) . . ?
O4 Dy1 Cu1 91.4(3) . . ?
C8 N1 C9 125(3) . . ?
C8 N1 Cu1 127.4(19) . . ?
C9 N1 Cu1 108(2) . . ?
C11 N2 C10 119(4) . . ?
C11 N2 Cu1 126(2) . . ?
C10 N2 Cu1 116(3) . . ?
C19 N3 Dy1 173.3(17) . . ?
C25 N9 Cu1 150.4(19) . 2_656 ?
C1 O1 C2 115.8(19) . . ?
C1 O1 Dy1 125.9(14) . . ?
C2 O1 Dy1 118.3(15) . . ?
C7 O2 Cu1 126.4(14) . . ?
C7 O2 Dy1 125.0(14) . . ?
Cu1 O2 Dy1 105.6(7) . . ?
C17 O3 Cu1 121.4(15) . . ?
C17 O3 Dy1 131.1(14) . . ?
Cu1 O3 Dy1 106.3(7) . . ?
C16 O4 C18 115(2) . . ?
C16 O4 Dy1 117.7(14) . . ?
C18 O4 Dy1 127.7(14) . . ?
C22 W1 C26 72.2(10) . . ?
C22 W1 C24 87.8(11) . . ?
C26 W1 C24 76.0(8) . . ?
C22 W1 C21 143.4(10) . . ?
C26 W1 C21 72.2(9) . . ?
C24 W1 C21 75.4(10) . . ?
C22 W1 C19 75.6(11) . . ?
C26 W1 C19 133.0(8) . . ?
C24 W1 C19 69.5(9) . . ?
C21 W1 C19 125.5(9) . . ?
C22 W1 C23 75.0(10) . . ?
C26 W1 C23 126.1(9) . . ?
C24 W1 C23 143.5(9) . . ?
C21 W1 C23 135.2(9) . . ?
C19 W1 C23 75.1(8) . . ?
C22 W1 C20 143.1(9) . . ?
C26 W1 C20 144.0(8) . . ?
C24 W1 C20 105.2(9) . . ?
C21 W1 C20 73.5(9) . . ?
C19 W1 C20 77.1(9) . . ?
C23 W1 C20 74.3(9) . . ?
C22 W1 C25 101.0(10) . . ?
C26 W1 C25 75.0(8) . . ?
C24 W1 C25 145.2(9) . . ?
C21 W1 C25 77.8(9) . . ?
C19 W1 C25 145.3(8) . . ?
C23 W1 C25 70.7(8) . . ?
C20 W1 C25 87.8(8) . . ?
C9 C9A H9A1 109.5 . . ?
C9 C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C9 C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?

_refine_diff_density_max         0.833
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.144

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound_15
_database_code_depnum_ccdc_archive 'CCDC 1060184'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H40 Cu2 La Mo N12 O8'
_chemical_formula_weight         1250.83

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'
La La -0.2871 2.4523 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_H-M_alt        'C 2 2 21'
_space_group_name_Hall           'C 2c 2'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'

_cell_length_a                   15.6813(10)
_cell_length_b                   19.0221(17)
_cell_length_c                   17.6117(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5253.4(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    28072
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      28.50

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             2484
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_exptl_absorpt_coefficient_mu    1.889
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_T_max  0.7351
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            30076
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_av_R_equivalents  0.0893
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.313
_diffrn_reflns_theta_max         28.496
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6641
_reflns_number_gt                4638
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0349P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 1591 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6641
_refine_ls_number_parameters     317
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0471
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0790
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_restrained_S_all      0.910
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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 -0.1965(7) 0.0021(8) 0.0938(6) 0.082(3) Uani 1 1 d . . . . .
H1A H -0.1895 0.0456 0.0670 0.122 Uiso 1 1 calc R U . . .
H1B H -0.2518 -0.0171 0.0830 0.122 Uiso 1 1 calc R U . . .
H1C H -0.1912 0.0103 0.1474 0.122 Uiso 1 1 calc R U . . .
C2 C -0.1330(6) -0.1126(4) 0.1034(5) 0.058(2) Uani 1 1 d . . . . .
C3 C -0.2018(7) -0.1411(6) 0.1421(6) 0.075(3) Uani 1 1 d . . . . .
H3 H -0.2524 -0.1159 0.1469 0.090 Uiso 1 1 calc R U . . .
C4 C -0.1941(10) -0.2081(7) 0.1736(7) 0.093(4) Uani 1 1 d . . . . .
H4 H -0.2404 -0.2280 0.1986 0.112 Uiso 1 1 calc R U . . .
C5 C -0.1224(10) -0.2433(6) 0.1683(7) 0.089(4) Uani 1 1 d . . . . .
H5 H -0.1184 -0.2870 0.1918 0.107 Uiso 1 1 calc R U . . .
C6 C -0.0517(7) -0.2178(5) 0.1286(5) 0.063(3) Uani 1 1 d . . . . .
C7 C -0.0575(5) -0.1510(4) 0.0938(4) 0.0474(19) Uani 1 1 d . . . . .
C8 C 0.0274(10) -0.2589(5) 0.1294(6) 0.083(4) Uani 1 1 d . . . . .
H8 H 0.0272 -0.3004 0.1573 0.099 Uiso 1 1 calc R U . . .
C9 C 0.1734(13) -0.2883(10) 0.0983(10) 0.149(8) Uani 1 1 d . . . . .
H9A H 0.1814 -0.3049 0.1499 0.179 Uiso 1 1 calc R U . . .
H9B H 0.1641 -0.3291 0.0663 0.179 Uiso 1 1 calc R U . . .
C10 C 0.2470(15) -0.2550(14) 0.0750(17) 0.218(14) Uani 1 1 d . . . . .
H10 H 0.2600 -0.2302 0.1224 0.262 Uiso 1 1 calc R U . . .
C11 C 0.3319(19) -0.2844(13) 0.0605(13) 0.233(14) Uani 1 1 d . . . . .
H11A H 0.3699 -0.2476 0.0449 0.349 Uiso 1 1 calc R U . . .
H11B H 0.3533 -0.3059 0.1060 0.349 Uiso 1 1 calc R U . . .
H11C H 0.3282 -0.3191 0.0210 0.349 Uiso 1 1 calc R U . . .
C12 C 0.2931(7) -0.1560(10) -0.0118(11) 0.116(6) Uani 1 1 d . . . . .
H12 H 0.3487 -0.1730 -0.0098 0.139 Uiso 1 1 calc R U . . .
C13 C 0.2815(10) -0.0975(9) -0.0525(10) 0.109(5) Uani 1 1 d . . . . .
C14 C 0.3608(10) -0.0706(11) -0.0903(14) 0.166(10) Uani 1 1 d . . . . .
H14 H 0.4119 -0.0946 -0.0830 0.199 Uiso 1 1 calc R U . . .
C15 C 0.3605(15) -0.0171(14) -0.1313(18) 0.229(17) Uani 1 1 d . . . . .
H15 H 0.4110 -0.0014 -0.1531 0.275 Uiso 1 1 calc R U . . .
C16 C 0.2831(15) 0.0200(8) -0.1448(12) 0.171(10) Uani 1 1 d . . . . .
H16 H 0.2838 0.0604 -0.1746 0.206 Uiso 1 1 calc R U . . .
C17 C 0.2060(9) -0.0036(8) -0.1138(7) 0.089(4) Uani 1 1 d . . . . .
C18 C 0.2088(7) -0.0636(6) -0.0643(7) 0.079(4) Uani 1 1 d . . . . .
C19 C 0.1098(13) 0.0588(7) -0.1932(7) 0.150(8) Uani 1 1 d . . . . .
H19A H 0.0537 0.0788 -0.1910 0.225 Uiso 1 1 calc R U . . .
H19B H 0.1506 0.0950 -0.2042 0.225 Uiso 1 1 calc R U . . .
H19C H 0.1118 0.0237 -0.2323 0.225 Uiso 1 1 calc R U . . .
C20 C -0.0116(6) 0.1093(4) 0.1722(4) 0.0506(19) Uani 1 1 d . . . . .
C21 C 0.1289(6) 0.1591(4) 0.2458(6) 0.060(2) Uani 1 1 d . . . . .
C23 C -0.0805(6) 0.2866(4) 0.2249(6) 0.067(3) Uani 1 1 d . . . . .
C24 C 0.0413(6) 0.2294(4) 0.1380(5) 0.059(2) Uani 1 1 d . . . . .
Cu1 Cu 0.11329(7) -0.16539(6) 0.02778(6) 0.0582(3) Uani 1 1 d . . . . .
La1 La 0.01855(4) 0.0000 0.0000 0.04622(17) Uani 1 2 d S T P . .
Mo1 Mo 0.0000 0.19631(4) 0.2500 0.0379(2) Uani 1 2 d S T P . .
N1 N 0.0952(7) -0.2432(5) 0.0959(5) 0.086(3) Uani 1 1 d . . . . .
N2 N 0.2323(7) -0.1946(6) 0.0279(6) 0.101(3) Uani 1 1 d . . . . .
N3 N -0.0208(6) 0.0662(3) 0.1277(4) 0.062(2) Uani 1 1 d . . . . .
N4 N 0.1992(6) 0.1388(4) 0.2474(7) 0.084(2) Uani 1 1 d . . . . .
N5 N -0.1220(7) 0.3340(5) 0.2126(7) 0.107(4) Uani 1 1 d . . . . .
N6 N 0.0622(7) 0.2415(5) 0.0775(5) 0.090(3) Uani 1 1 d . . . . .
O1 O -0.1312(4) -0.0472(3) 0.0696(3) 0.0600(15) Uani 1 1 d . . . . .
O2 O 0.0052(4) -0.1210(2) 0.0525(3) 0.0485(12) Uani 1 1 d . . . . .
O3 O 0.1347(4) -0.0814(3) -0.0294(3) 0.0605(15) Uani 1 1 d . . . . .
O4 O 0.1302(7) 0.0266(4) -0.1204(4) 0.091(3) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.452(12) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 O1 1.377(10) . ?
C2 C3 1.387(13) . ?
C2 C7 1.402(12) . ?
C3 C4 1.395(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.313(18) . ?
C4 H4 0.9300 . ?
C5 C6 1.398(16) . ?
C5 H5 0.9300 . ?
C6 C7 1.414(11) . ?
C6 C8 1.466(16) . ?
C7 O2 1.349(9) . ?
C8 N1 1.252(14) . ?
C8 H8 0.9300 . ?
C9 C10 1.38(3) . ?
C9 N1 1.496(16) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 N2 1.44(2) . ?
C10 C11 1.47(3) . ?
C10 H10 0.9800 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.34(2) . ?
C12 N2 1.392(19) . ?
C12 H12 0.9300 . ?
C13 C18 1.326(19) . ?
C13 C14 1.50(2) . ?
C14 C15 1.25(3) . ?
C14 H14 0.9300 . ?
C15 C16 1.42(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.401(19) . ?
C16 H16 0.9300 . ?
C17 O4 1.326(16) . ?
C17 C18 1.436(18) . ?
C18 O3 1.357(11) . ?
C19 O4 1.455(15) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 N3 1.144(9) . ?
C20 Mo1 2.156(7) . ?
C21 N4 1.169(11) . ?
C21 Mo1 2.143(10) . ?
C23 N5 1.132(11) . ?
C23 Mo1 2.177(9) . ?
C24 N6 1.138(11) . ?
C24 Mo1 2.169(9) . ?
Cu1 O3 1.918(6) . ?
Cu1 N1 1.926(10) . ?
Cu1 O2 1.944(5) . ?
Cu1 N2 1.947(10) . ?
Cu1 La1 3.5134(11) . ?
La1 O3 2.446(6) . ?
La1 O3 2.446(6) 3 ?
La1 O2 2.489(4) 3 ?
La1 O2 2.489(4) . ?
La1 N3 2.651(7) . ?
La1 N3 2.651(7) 3 ?
La1 O1 2.797(6) . ?
La1 O1 2.797(6) 3 ?
La1 O4 2.796(7) 3 ?
La1 O4 2.796(7) . ?
La1 Cu1 3.5134(11) 3 ?
Mo1 C21 2.143(10) 4 ?
Mo1 C20 2.156(7) 4 ?
Mo1 C24 2.169(9) 4 ?
Mo1 C23 2.177(9) 4 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 . . ?
O1 C2 C3 125.5(9) . . ?
O1 C2 C7 113.7(8) . . ?
C3 C2 C7 120.8(8) . . ?
C2 C3 C4 119.0(11) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 120.8(11) . . ?
C5 C4 H4 119.6 . . ?
C3 C4 H4 119.6 . . ?
C4 C5 C6 122.5(11) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C5 C6 C7 118.5(10) . . ?
C5 C6 C8 118.7(10) . . ?
C7 C6 C8 122.6(8) . . ?
O2 C7 C2 117.3(7) . . ?
O2 C7 C6 124.5(8) . . ?
C2 C7 C6 118.1(8) . . ?
N1 C8 C6 125.9(9) . . ?
N1 C8 H8 117.0 . . ?
C6 C8 H8 117.0 . . ?
C10 C9 N1 114.5(14) . . ?
C10 C9 H9A 108.6 . . ?
N1 C9 H9A 108.6 . . ?
C10 C9 H9B 108.6 . . ?
N1 C9 H9B 108.6 . . ?
H9A C9 H9B 107.6 . . ?
C9 C10 N2 113.9(14) . . ?
C9 C10 C11 130(2) . . ?
N2 C10 C11 110(2) . . ?
C9 C10 H10 98.2 . . ?
N2 C10 H10 98.2 . . ?
C11 C10 H10 98.2 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N2 128.0(11) . . ?
C13 C12 H12 116.0 . . ?
N2 C12 H12 116.0 . . ?
C18 C13 C12 127.4(15) . . ?
C18 C13 C14 118.5(18) . . ?
C12 C13 C14 114.1(18) . . ?
C15 C14 C13 122(2) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C14 C15 C16 120.3(17) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C17 C16 C15 120.7(19) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
O4 C17 C16 126.9(16) . . ?
O4 C17 C18 115.1(9) . . ?
C16 C17 C18 117.8(17) . . ?
C13 C18 O3 122.9(13) . . ?
C13 C18 C17 120.5(13) . . ?
O3 C18 C17 116.6(10) . . ?
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 . . ?
N3 C20 Mo1 175.3(8) . . ?
N4 C21 Mo1 176.7(10) . . ?
N5 C23 Mo1 179.1(11) . . ?
N6 C24 Mo1 174.7(8) . . ?
O3 Cu1 N1 173.1(4) . . ?
O3 Cu1 O2 84.7(2) . . ?
N1 Cu1 O2 93.8(3) . . ?
O3 Cu1 N2 94.0(4) . . ?
N1 Cu1 N2 85.5(5) . . ?
O2 Cu1 N2 163.7(3) . . ?
O3 Cu1 La1 41.85(17) . . ?
N1 Cu1 La1 135.4(3) . . ?
O2 Cu1 La1 43.38(14) . . ?
N2 Cu1 La1 131.4(4) . . ?
O3 La1 O3 83.7(3) . 3 ?
O3 La1 O2 124.70(18) . 3 ?
O3 La1 O2 63.66(17) 3 3 ?
O3 La1 O2 63.66(17) . . ?
O3 La1 O2 124.70(18) 3 . ?
O2 La1 O2 170.3(3) 3 . ?
O3 La1 N3 130.8(2) . . ?
O3 La1 N3 72.1(2) 3 . ?
O2 La1 N3 81.77(19) 3 . ?
O2 La1 N3 95.96(18) . . ?
O3 La1 N3 72.1(2) . 3 ?
O3 La1 N3 130.8(2) 3 3 ?
O2 La1 N3 95.96(18) 3 3 ?
O2 La1 N3 81.77(19) . 3 ?
N3 La1 N3 153.0(4) . 3 ?
O3 La1 O1 120.97(18) . . ?
O3 La1 O1 137.36(19) 3 . ?
O2 La1 O1 112.90(18) 3 . ?
O2 La1 O1 57.94(17) . . ?
N3 La1 O1 65.5(2) . . ?
N3 La1 O1 91.4(2) 3 . ?
O3 La1 O1 137.36(19) . 3 ?
O3 La1 O1 120.97(18) 3 3 ?
O2 La1 O1 57.94(17) 3 3 ?
O2 La1 O1 112.90(18) . 3 ?
N3 La1 O1 91.4(2) . 3 ?
N3 La1 O1 65.5(2) 3 3 ?
O1 La1 O1 65.8(3) . 3 ?
O3 La1 O4 65.1(2) . 3 ?
O3 La1 O4 59.2(2) 3 3 ?
O2 La1 O4 120.1(2) 3 3 ?
O2 La1 O4 66.6(2) . 3 ?
N3 La1 O4 65.7(3) . 3 ?
N3 La1 O4 134.7(2) 3 3 ?
O1 La1 O4 97.8(3) . 3 ?
O1 La1 O4 156.4(2) 3 3 ?
O3 La1 O4 59.2(2) . . ?
O3 La1 O4 65.1(2) 3 . ?
O2 La1 O4 66.6(2) 3 . ?
O2 La1 O4 120.1(2) . . ?
N3 La1 O4 134.7(2) . . ?
N3 La1 O4 65.7(3) 3 . ?
O1 La1 O4 156.4(2) . . ?
O1 La1 O4 97.8(3) 3 . ?
O4 La1 O4 102.5(4) 3 . ?
O3 La1 Cu1 31.55(13) . . ?
O3 La1 Cu1 102.85(13) 3 . ?
O2 La1 Cu1 156.24(13) 3 . ?
O2 La1 Cu1 32.44(12) . . ?
N3 La1 Cu1 113.92(17) . . ?
N3 La1 Cu1 77.97(14) 3 . ?
O1 La1 Cu1 90.36(12) . . ?
O1 La1 Cu1 134.72(13) 3 . ?
O4 La1 Cu1 57.81(14) 3 . ?
O4 La1 Cu1 90.18(19) . . ?
O3 La1 Cu1 102.85(13) . 3 ?
O3 La1 Cu1 31.55(13) 3 3 ?
O2 La1 Cu1 32.44(12) 3 3 ?
O2 La1 Cu1 156.24(13) . 3 ?
N3 La1 Cu1 77.97(14) . 3 ?
N3 La1 Cu1 113.92(17) 3 3 ?
O1 La1 Cu1 134.72(13) . 3 ?
O1 La1 Cu1 90.36(12) 3 3 ?
O4 La1 Cu1 90.18(19) 3 3 ?
O4 La1 Cu1 57.81(14) . 3 ?
Cu1 La1 Cu1 129.97(4) . 3 ?
C21 Mo1 C21 141.5(4) 4 . ?
C21 Mo1 C20 71.9(3) 4 . ?
C21 Mo1 C20 78.7(3) . . ?
C21 Mo1 C20 78.7(3) 4 4 ?
C21 Mo1 C20 71.9(3) . 4 ?
C20 Mo1 C20 79.7(4) . 4 ?
C21 Mo1 C24 114.1(4) 4 . ?
C21 Mo1 C24 77.5(4) . . ?
C20 Mo1 C24 70.7(3) . . ?
C20 Mo1 C24 140.8(3) 4 . ?
C21 Mo1 C24 77.5(4) 4 4 ?
C21 Mo1 C24 114.1(4) . 4 ?
C20 Mo1 C24 140.8(3) . 4 ?
C20 Mo1 C24 70.7(3) 4 4 ?
C24 Mo1 C24 146.3(4) . 4 ?
C21 Mo1 C23 143.1(3) 4 4 ?
C21 Mo1 C23 73.8(3) . 4 ?
C20 Mo1 C23 141.6(3) . 4 ?
C20 Mo1 C23 115.3(4) 4 4 ?
C24 Mo1 C23 77.5(4) . 4 ?
C24 Mo1 C23 76.1(3) 4 4 ?
C21 Mo1 C23 73.8(3) 4 . ?
C21 Mo1 C23 143.1(3) . . ?
C20 Mo1 C23 115.3(4) . . ?
C20 Mo1 C23 141.6(3) 4 . ?
C24 Mo1 C23 76.1(3) . . ?
C24 Mo1 C23 77.5(4) 4 . ?
C23 Mo1 C23 75.8(5) 4 . ?
C8 N1 C9 123.1(12) . . ?
C8 N1 Cu1 127.0(8) . . ?
C9 N1 Cu1 109.7(10) . . ?
C12 N2 C10 127.1(14) . . ?
C12 N2 Cu1 120.4(9) . . ?
C10 N2 Cu1 112.5(12) . . ?
C20 N3 La1 153.2(7) . . ?
C2 O1 C1 116.2(8) . . ?
C2 O1 La1 119.7(5) . . ?
C1 O1 La1 120.8(7) . . ?
C7 O2 Cu1 124.9(4) . . ?
C7 O2 La1 130.8(5) . . ?
Cu1 O2 La1 104.2(2) . . ?
C18 O3 Cu1 126.5(7) . . ?
C18 O3 La1 125.1(6) . . ?
Cu1 O3 La1 106.6(2) . . ?
C17 O4 C19 117.2(11) . . ?
C17 O4 La1 114.6(7) . . ?
C19 O4 La1 127.3(10) . . ?

_refine_diff_density_max         1.228
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.086

_shelxl_version_number           2014-3



_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1060185'
_audit_update_record             
;
2015-06-29 deposited with the CCDC.
2015-07-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H47 Cu2 Mo N13 O9 Pr'
_chemical_formula_weight         1325.92

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'
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'
Cu Cu 0.3201 1.2651 '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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.6875(8)
_cell_length_b                   21.6973(16)
_cell_length_c                   20.1860(14)
_cell_angle_alpha                90
_cell_angle_beta                 98.203(5)
_cell_angle_gamma                90
_cell_volume                     5500.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    29406
_cell_measurement_theta_min      2.14
_cell_measurement_theta_max      27.22

_exptl_crystal_description       prism
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_F_000             2652
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    1.920
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6031
_exptl_absorpt_correction_T_max  0.9133
_exptl_absorpt_process_details   
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            53689
_diffrn_reflns_av_unetI/netI     0.1787
_diffrn_reflns_av_R_equivalents  0.1673
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.136
_diffrn_reflns_theta_max         27.218
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             12187
_reflns_number_gt                5379
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Diamond 3.2 (Branderburg, 2014)'
_computing_publication_material  'WinGX (Farrugia, 2013)'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0820P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12187
_refine_ls_number_parameters     677
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1711
_refine_ls_R_factor_gt           0.0771
_refine_ls_wR_factor_ref         0.1914
_refine_ls_wR_factor_gt          0.1613
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_restrained_S_all      0.887
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.9747(12) 0.3483(6) 0.2620(8) 0.092(5) Uani 1 1 d . . . . .
H1A H 0.9286 0.3721 0.2860 0.139 Uiso 1 1 calc R U . . .
H1B H 1.0360 0.3725 0.2560 0.139 Uiso 1 1 calc R U . . .
H1C H 0.9371 0.3370 0.2191 0.139 Uiso 1 1 calc R U . . .
C2 C 1.0761(9) 0.2542(6) 0.2704(5) 0.056(3) Uani 1 1 d . . . . .
C3 C 1.1583(12) 0.2715(8) 0.2376(7) 0.081(4) Uani 1 1 d . . . . .
H3 H 1.1718 0.3132 0.2317 0.097 Uiso 1 1 calc R U . . .
C4 C 1.2223(11) 0.2271(11) 0.2129(7) 0.096(6) Uani 1 1 d . . . . .
H4 H 1.2784 0.2382 0.1903 0.115 Uiso 1 1 calc R U . . .
C5 C 1.1987(14) 0.1649(9) 0.2236(8) 0.093(5) Uani 1 1 d . . . . .
H5 H 1.2411 0.1350 0.2074 0.111 Uiso 1 1 calc R U . . .
C6 C 1.1191(10) 0.1459(7) 0.2556(7) 0.070(4) Uani 1 1 d . . . . .
C7 C 1.0554(9) 0.1898(6) 0.2823(6) 0.055(3) Uani 1 1 d . . . . .
C8 C 1.1018(12) 0.0790(7) 0.2620(7) 0.077(4) Uani 1 1 d . . . . .
H8 H 1.1516 0.0524 0.2479 0.092 Uiso 1 1 calc R U . . .
C9 C 1.0190(17) -0.0152(6) 0.2909(10) 0.099(5) Uani 0.714 1 d . . P A 1
H9 H 1.0440 -0.0347 0.2522 0.119 Uiso 0.714 1 calc R U P A 1
C10 C 0.9077(17) -0.0294(8) 0.2918(11) 0.112(6) Uani 0.714 1 d . . P A 1
H10A H 0.9009 -0.0710 0.3082 0.135 Uiso 0.714 1 calc R U P A 1
H10B H 0.8693 -0.0270 0.2468 0.135 Uiso 0.714 1 calc R U P A 1
C11 C 1.0822(18) -0.0368(9) 0.3532(11) 0.085(6) Uani 0.714 1 d . . P A 1
H11A H 1.1560 -0.0274 0.3524 0.128 Uiso 0.714 1 calc R U P A 1
H11B H 1.0583 -0.0166 0.3906 0.128 Uiso 0.714 1 calc R U P A 1
H11C H 1.0737 -0.0805 0.3572 0.128 Uiso 0.714 1 calc R U P A 1
C9A C 1.0190(17) -0.0152(6) 0.2909(10) 0.099(5) Uani 0.286 1 d . . P A 2
H9A1 H 1.0444 -0.0348 0.2529 0.119 Uiso 0.286 1 calc R U P A 2
H9A2 H 1.0620 -0.0294 0.3316 0.119 Uiso 0.286 1 calc R U P A 2
C10A C 0.9077(17) -0.0294(8) 0.2918(11) 0.112(6) Uani 0.286 1 d . . P A 2
H10C H 0.9080 -0.0691 0.3151 0.135 Uiso 0.286 1 calc R U P A 2
C11A C 0.861(5) -0.040(3) 0.233(3) 0.103(19) Uiso 0.286 1 d . . P A 2
H11D H 0.7877 -0.0495 0.2341 0.155 Uiso 0.286 1 calc R U P A 2
H11E H 0.8665 -0.0046 0.2052 0.155 Uiso 0.286 1 calc R U P A 2
H11F H 0.8948 -0.0747 0.2145 0.155 Uiso 0.286 1 calc R U P A 2
C12 C 0.7882(13) 0.0012(6) 0.3702(8) 0.078(4) Uani 1 1 d . . . . .
H12 H 0.7639 -0.0392 0.3671 0.093 Uiso 1 1 calc R U . . .
C13 C 0.7395(10) 0.0405(6) 0.4129(7) 0.060(3) Uani 1 1 d . . . . .
C14 C 0.6654(11) 0.0158(7) 0.4513(8) 0.076(4) Uani 1 1 d . . . . .
H14 H 0.6468 -0.0255 0.4454 0.091 Uiso 1 1 calc R U . . .
C15 C 0.6221(14) 0.0474(8) 0.4943(9) 0.096(5) Uani 1 1 d . . . . .
H15 H 0.5722 0.0288 0.5174 0.115 Uiso 1 1 calc R U . . .
C16 C 0.6496(11) 0.1112(8) 0.5073(8) 0.088(5) Uani 1 1 d . . . . .
H16 H 0.6204 0.1343 0.5390 0.106 Uiso 1 1 calc R U . . .
C17 C 0.7232(10) 0.1362(6) 0.4690(7) 0.065(4) Uani 1 1 d . . . . .
C18 C 0.7652(9) 0.1044(6) 0.4207(6) 0.054(3) Uani 1 1 d . . . . .
C19 C 0.7277(12) 0.2286(7) 0.5344(8) 0.090(5) Uani 1 1 d . . . . .
H19A H 0.7546 0.2700 0.5358 0.135 Uiso 1 1 calc R U . . .
H19B H 0.6515 0.2295 0.5312 0.135 Uiso 1 1 calc R U . . .
H19C H 0.7572 0.2072 0.5744 0.135 Uiso 1 1 calc R U . . .
C20 C 0.6576(9) 0.3192(6) 0.4080(7) 0.071(4) Uani 1 1 d . . . . .
H20A H 0.6412 0.2763 0.4116 0.107 Uiso 1 1 calc R U . . .
H20B H 0.6186 0.3427 0.4367 0.107 Uiso 1 1 calc R U . . .
H20C H 0.6380 0.3325 0.3625 0.107 Uiso 1 1 calc R U . . .
C21 C 0.8081(11) 0.3889(5) 0.4255(6) 0.063(3) Uani 1 1 d . . . . .
C22 C 0.7417(13) 0.4398(6) 0.4217(7) 0.082(4) Uani 1 1 d . . . . .
H22 H 0.6688 0.4350 0.4213 0.098 Uiso 1 1 calc R U . . .
C23 C 0.7856(14) 0.4986(6) 0.4185(8) 0.084(4) Uani 1 1 d . . . . .
H23 H 0.7420 0.5331 0.4181 0.101 Uiso 1 1 calc R U . . .
C24 C 0.8883(13) 0.5058(6) 0.4161(7) 0.078(4) Uani 1 1 d . . . . .
H24 H 0.9146 0.5452 0.4107 0.093 Uiso 1 1 calc R U . . .
C25 C 0.9594(12) 0.4553(5) 0.4214(7) 0.072(4) Uani 1 1 d . . . . .
C26 C 0.9149(10) 0.3951(5) 0.4255(5) 0.051(3) Uani 1 1 d . . . . .
C27 C 1.0707(13) 0.4670(6) 0.4174(7) 0.074(4) Uani 1 1 d . . . . .
H27 H 1.0903 0.5081 0.4145 0.089 Uiso 1 1 calc R U . . .
C28 C 1.2549(14) 0.4435(8) 0.4171(11) 0.105(6) Uani 0.72 1 d . . P B 3
H28 H 1.2893 0.4393 0.4635 0.126 Uiso 0.72 1 calc R U P B 3
C29 C 1.3049(13) 0.3952(9) 0.3780(9) 0.101(6) Uani 0.72 1 d . . P B 3
H29A H 1.2859 0.4020 0.3303 0.122 Uiso 0.72 1 calc R U P B 3
H29B H 1.3819 0.3962 0.3889 0.122 Uiso 0.72 1 calc R U P B 3
C30 C 1.288(3) 0.5024(13) 0.3950(17) 0.160(13) Uani 0.72 1 d . . P B 3
H30A H 1.3642 0.5036 0.3989 0.240 Uiso 0.72 1 calc R U P B 3
H30B H 1.2578 0.5087 0.3491 0.240 Uiso 0.72 1 calc R U P B 3
H30C H 1.2637 0.5343 0.4221 0.240 Uiso 0.72 1 calc R U P B 3
C28A C 1.2549(14) 0.4435(8) 0.4171(11) 0.105(6) Uani 0.28 1 d . . P B 4
H28A H 1.2917 0.4453 0.4626 0.126 Uiso 0.28 1 calc R U P B 4
H28B H 1.2600 0.4837 0.3966 0.126 Uiso 0.28 1 calc R U P B 4
C29A C 1.3049(13) 0.3952(9) 0.3780(9) 0.101(6) Uani 0.28 1 d . . P B 4
H29C H 1.2730 0.4014 0.3313 0.122 Uiso 0.28 1 calc R U P B 4
C30A C 1.416(3) 0.409(2) 0.380(2) 0.068(12) Uiso 0.28 1 d . . P B 4
H30D H 1.4233 0.4510 0.3644 0.101 Uiso 0.28 1 calc R U P B 4
H30E H 1.4519 0.4055 0.4246 0.101 Uiso 0.28 1 calc R U P B 4
H30F H 1.4469 0.3815 0.3510 0.101 Uiso 0.28 1 calc R U P B 4
C31 C 1.3215(11) 0.2843(8) 0.3934(7) 0.079(4) Uani 1 1 d . . . . .
H31 H 1.3871 0.2885 0.3784 0.095 Uiso 1 1 calc R U . . .
C32 C 1.2872(10) 0.2237(7) 0.4110(6) 0.067(4) Uani 1 1 d . . . . .
C33 C 1.3591(11) 0.1742(10) 0.4119(8) 0.094(5) Uani 1 1 d . . . . .
H33 H 1.4276 0.1819 0.4027 0.112 Uiso 1 1 calc R U . . .
C34 C 1.3316(14) 0.1156(9) 0.4257(9) 0.101(6) Uani 1 1 d . . . . .
H34 H 1.3807 0.0839 0.4246 0.122 Uiso 1 1 calc R U . . .
C35 C 1.2341(13) 0.1030(7) 0.4410(8) 0.086(5) Uani 1 1 d . . . . .
H35 H 1.2170 0.0628 0.4512 0.103 Uiso 1 1 calc R U . . .
C36 C 1.1582(9) 0.1495(6) 0.4417(6) 0.052(3) Uani 1 1 d . . . . .
C37 C 1.1842(9) 0.2110(5) 0.4272(5) 0.052(3) Uani 1 1 d . . . . .
C38 C 1.0344(13) 0.0951(6) 0.5023(7) 0.084(4) Uani 1 1 d . . . . .
H38A H 0.9596 0.0941 0.5054 0.125 Uiso 1 1 calc R U . . .
H38B H 1.0567 0.0553 0.4887 0.125 Uiso 1 1 calc R U . . .
H38C H 1.0734 0.1054 0.5452 0.125 Uiso 1 1 calc R U . . .
C39 C 0.7222(8) 0.2530(5) 0.2591(5) 0.046(3) Uani 1 1 d . . . . .
C40 C 0.7221(10) 0.1464(5) 0.2070(6) 0.056(3) Uani 1 1 d . . . . .
C41 C 0.5662(11) 0.1845(6) 0.2705(7) 0.069(4) Uani 1 1 d . . . . .
C42 C 0.5129(10) 0.2908(6) 0.2150(6) 0.057(3) Uani 1 1 d . . . . .
C43 C 0.6990(9) 0.2977(6) 0.1439(5) 0.051(3) Uani 1 1 d . . . . .
C44 C 0.6629(9) 0.1794(5) 0.0910(6) 0.048(3) Uani 1 1 d . . . . .
C45 C 0.4868(9) 0.1527(5) 0.1526(6) 0.053(3) Uani 1 1 d . . . . .
C46 C 0.5102(9) 0.2527(4) 0.0889(5) 0.047(3) Uani 1 1 d . . . . .
C47 C 0.412(4) -0.0056(15) 0.284(3) 0.204(18) Uani 1 1 d . . . . .
C48 C 0.500(3) 0.0237(12) 0.2797(13) 0.23(2) Uani 1 1 d . . . . .
H48A H 0.5015 0.0618 0.3041 0.348 Uiso 1 1 calc R U . . .
H48B H 0.5047 0.0322 0.2335 0.348 Uiso 1 1 calc R U . . .
H48C H 0.5599 -0.0012 0.2982 0.348 Uiso 1 1 calc R U . . .
N1 N 1.0247(9) 0.0557(5) 0.2851(6) 0.078(3) Uani 1 1 d . . . . .
N2 N 0.8615(11) 0.0146(5) 0.3355(6) 0.077(4) Uani 1 1 d . . . . .
N3 N 1.1445(10) 0.4273(5) 0.4173(6) 0.074(3) Uani 1 1 d . . . . .
N4 N 1.2617(11) 0.3348(6) 0.3982(5) 0.083(4) Uani 1 1 d . . . . .
N5 N 0.7837(7) 0.2651(4) 0.3059(4) 0.053(2) Uani 1 1 d . . . . .
N6 N 0.7884(10) 0.1112(5) 0.2252(5) 0.076(3) Uani 1 1 d . . . . .
N7 N 0.5477(10) 0.1675(6) 0.3220(6) 0.091(4) Uani 1 1 d . . . . .
N8 N 0.4665(9) 0.3290(5) 0.2356(6) 0.079(3) Uani 1 1 d . . . . .
N9 N 0.7428(11) 0.3361(6) 0.1256(6) 0.091(4) Uani 1 1 d . . . . .
N10 N 0.6886(9) 0.1595(4) 0.0432(6) 0.065(3) Uani 1 1 d . . . . .
N11 N 0.4153(8) 0.1176(5) 0.1402(6) 0.079(3) Uani 1 1 d . . . . .
N12 N 0.4644(8) 0.2675(4) 0.0386(5) 0.063(3) Uani 1 1 d . . . . .
N13 N 0.344(4) -0.031(2) 0.296(3) 0.31(3) Uani 1 1 d . . . . .
O1 O 1.0080(7) 0.2937(4) 0.2994(4) 0.063(2) Uani 1 1 d . . . . .
O2 O 0.9780(6) 0.1782(3) 0.3172(4) 0.0489(18) Uani 1 1 d . . . . .
O3 O 0.8358(6) 0.1341(3) 0.3870(4) 0.0525(19) Uani 1 1 d . . . . .
O4 O 0.7573(7) 0.1975(4) 0.4774(4) 0.065(2) Uani 1 1 d . . . . .
O5 O 0.7713(6) 0.3287(4) 0.4280(4) 0.059(2) Uani 1 1 d . . . . .
O6 O 0.9757(6) 0.3436(3) 0.4297(4) 0.0536(19) Uani 1 1 d . . . . .
O7 O 1.1079(5) 0.2518(3) 0.4262(3) 0.0503(19) Uani 1 1 d . . . . .
O8 O 1.0548(6) 0.1406(3) 0.4539(4) 0.059(2) Uani 1 1 d . . . . .
O9 O 0.946(3) 0.1907(13) 0.0943(16) 0.286(12) Uiso 1 1 d D . . . .
H9A H 0.9647 0.2220 0.0764 0.429 Uiso 1 1 calc R U . . .
Cu1 Cu 0.91544(12) 0.09739(6) 0.32204(7) 0.0557(4) Uani 1 1 d . . . . .
Cu2 Cu 1.12848(11) 0.33978(7) 0.42771(7) 0.0554(4) Uani 1 1 d . . . . .
Mo1 Mo 0.60988(7) 0.21970(4) 0.17829(4) 0.0411(2) Uani 1 1 d . . . . .
Pr1 Pr 0.91738(5) 0.23691(3) 0.40865(3) 0.04139(17) Uani 1 1 d . . . . .
C49 C 0.983(2) 0.1350(13) 0.0595(15) 0.214(13) Uiso 1 1 d D . . . .
H49A H 1.0594 0.1325 0.0680 0.321 Uiso 1 1 calc R U . . .
H49B H 0.9604 0.1383 0.0122 0.321 Uiso 1 1 calc R U . . .
H49C H 0.9530 0.0985 0.0762 0.321 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.437(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.365(17) . ?
C2 O1 1.403(14) . ?
C2 C7 1.448(17) . ?
C3 C4 1.40(2) . ?
C3 H3 0.9300 . ?
C4 C5 1.41(2) . ?
C4 H4 0.9300 . ?
C5 C6 1.34(2) . ?
C5 H5 0.9300 . ?
C6 C7 1.405(18) . ?
C6 C8 1.48(2) . ?
C7 O2 1.312(13) . ?
C8 N1 1.250(17) . ?
C8 H8 0.9300 . ?
C9 C10 1.45(2) . ?
C9 C11 1.47(2) . ?
C9 N1 1.546(18) . ?
C9 H9 0.9800 . ?
C10 N2 1.48(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C11A H11D 0.9600 . ?
C11A H11E 0.9600 . ?
C11A H11F 0.9600 . ?
C12 N2 1.274(18) . ?
C12 C13 1.41(2) . ?
C12 H12 0.9300 . ?
C13 C14 1.408(18) . ?
C13 C18 1.429(17) . ?
C14 C15 1.29(2) . ?
C14 H14 0.9300 . ?
C15 C16 1.44(2) . ?
C15 H15 0.9300 . ?
C16 C17 1.403(18) . ?
C16 H16 0.9300 . ?
C17 C18 1.365(18) . ?
C17 O4 1.401(15) . ?
C18 O3 1.361(13) . ?
C19 O4 1.429(16) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 O5 1.457(13) . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C26 1.361(17) . ?
C21 C22 1.385(17) . ?
C21 O5 1.390(14) . ?
C22 C23 1.396(19) . ?
C22 H22 0.9300 . ?
C23 C24 1.320(18) . ?
C23 H23 0.9300 . ?
C24 C25 1.414(18) . ?
C24 H24 0.9300 . ?
C25 C26 1.429(16) . ?
C25 C27 1.45(2) . ?
C26 O6 1.353(13) . ?
C27 N3 1.272(17) . ?
C27 H27 0.9300 . ?
C28 C30 1.44(3) . ?
C28 N3 1.445(19) . ?
C28 C29 1.51(2) . ?
C28 H28 0.9800 . ?
C29 N4 1.500(18) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30A H30D 0.9600 . ?
C30A H30E 0.9600 . ?
C30A H30F 0.9600 . ?
C31 N4 1.344(18) . ?
C31 C32 1.45(2) . ?
C31 H31 0.9300 . ?
C32 C33 1.407(19) . ?
C32 C37 1.418(17) . ?
C33 C34 1.36(2) . ?
C33 H33 0.9300 . ?
C34 C35 1.35(2) . ?
C34 H34 0.9300 . ?
C35 C36 1.396(17) . ?
C35 H35 0.9300 . ?
C36 O8 1.382(13) . ?
C36 C37 1.415(16) . ?
C37 O7 1.310(13) . ?
C38 O8 1.440(14) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N5 1.166(11) . ?
C39 Mo1 2.133(9) . ?
C40 N6 1.156(14) . ?
C40 Mo1 2.158(13) . ?
C41 N7 1.158(16) . ?
C41 Mo1 2.156(15) . ?
C42 N8 1.130(15) . ?
C42 Mo1 2.169(14) . ?
C43 N9 1.094(14) . ?
C43 Mo1 2.202(13) . ?
C44 N10 1.147(13) . ?
C44 Mo1 2.159(12) . ?
C45 N11 1.183(14) . ?
C45 Mo1 2.143(12) . ?
C46 N12 1.142(13) . ?
C46 Mo1 2.172(11) . ?
C47 N13 1.08(4) . ?
C47 C48 1.30(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
N1 Cu1 1.894(12) . ?
N2 Cu1 1.956(11) . ?
N3 Cu2 1.924(11) . ?
N4 Cu2 1.874(15) . ?
N5 Pr1 2.560(8) . ?
N6 Cu1 2.368(10) . ?
N10 Cu2 2.346(11) 4_565 ?
N12 Pr1 2.607(10) 4_565 ?
O1 Pr1 2.903(8) . ?
O2 Cu1 1.933(7) . ?
O2 Pr1 2.454(7) . ?
O3 Cu1 1.936(8) . ?
O3 Pr1 2.472(7) . ?
O4 Pr1 2.755(9) . ?
O5 Pr1 2.786(8) . ?
O6 Cu2 1.947(8) . ?
O6 Pr1 2.450(7) . ?
O7 Cu2 1.927(7) . ?
O7 Pr1 2.414(7) . ?
O8 Pr1 2.790(7) . ?
O9 C49 1.506(5) . ?
O9 H9A 0.8200 . ?
Cu1 Pr1 3.4941(14) . ?
Cu2 N10 2.346(11) 4_666 ?
Cu2 Pr1 3.4655(15) . ?
Pr1 N12 2.607(10) 4_666 ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
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 126.3(13) . . ?
C3 C2 C7 121.1(12) . . ?
O1 C2 C7 112.5(10) . . ?
C2 C3 C4 120.3(15) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 117.5(14) . . ?
C3 C4 H4 121.3 . . ?
C5 C4 H4 121.3 . . ?
C6 C5 C4 124.1(16) . . ?
C6 C5 H5 118.0 . . ?
C4 C5 H5 118.0 . . ?
C5 C6 C7 119.4(15) . . ?
C5 C6 C8 118.4(14) . . ?
C7 C6 C8 122.2(13) . . ?
O2 C7 C6 126.3(12) . . ?
O2 C7 C2 116.2(10) . . ?
C6 C7 C2 117.5(12) . . ?
N1 C8 C6 124.4(12) . . ?
N1 C8 H8 117.8 . . ?
C6 C8 H8 117.8 . . ?
C10 C9 C11 109.6(18) . . ?
C10 C9 N1 105.5(13) . . ?
C11 C9 N1 110.8(15) . . ?
C10 C9 H9 110.3 . . ?
C11 C9 H9 110.3 . . ?
N1 C9 H9 110.3 . . ?
C9 C10 N2 110.0(15) . . ?
C9 C10 H10A 109.7 . . ?
N2 C10 H10A 109.7 . . ?
C9 C10 H10B 109.7 . . ?
N2 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H11D C11A H11E 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
N2 C12 C13 127.9(13) . . ?
N2 C12 H12 116.1 . . ?
C13 C12 H12 116.1 . . ?
C14 C13 C12 119.4(13) . . ?
C14 C13 C18 118.0(13) . . ?
C12 C13 C18 122.6(12) . . ?
C15 C14 C13 123.4(15) . . ?
C15 C14 H14 118.3 . . ?
C13 C14 H14 118.3 . . ?
C14 C15 C16 121.2(16) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 115.7(16) . . ?
C17 C16 H16 122.1 . . ?
C15 C16 H16 122.1 . . ?
C18 C17 O4 114.9(11) . . ?
C18 C17 C16 123.8(13) . . ?
O4 C17 C16 121.3(14) . . ?
O3 C18 C17 118.1(11) . . ?
O3 C18 C13 124.0(12) . . ?
C17 C18 C13 117.6(12) . . ?
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 C22 121.3(12) . . ?
C26 C21 O5 115.6(10) . . ?
C22 C21 O5 123.1(13) . . ?
C21 C22 C23 119.1(15) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
C24 C23 C22 120.9(14) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 121.8(14) . . ?
C23 C24 H24 119.1 . . ?
C25 C24 H24 119.1 . . ?
C24 C25 C26 117.3(14) . . ?
C24 C25 C27 118.4(12) . . ?
C26 C25 C27 124.1(12) . . ?
O6 C26 C21 118.5(10) . . ?
O6 C26 C25 122.1(12) . . ?
C21 C26 C25 119.4(11) . . ?
N3 C27 C25 127.3(12) . . ?
N3 C27 H27 116.4 . . ?
C25 C27 H27 116.4 . . ?
C30 C28 N3 123(2) . . ?
C30 C28 C29 107(2) . . ?
N3 C28 C29 108.3(14) . . ?
C30 C28 H28 105.8 . . ?
N3 C28 H28 105.8 . . ?
C29 C28 H28 105.8 . . ?
N4 C29 C28 105.6(13) . . ?
N4 C29 H29A 110.6 . . ?
C28 C29 H29A 110.6 . . ?
N4 C29 H29B 110.6 . . ?
C28 C29 H29B 110.6 . . ?
H29A C29 H29B 108.8 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
N4 C31 C32 122.1(13) . . ?
N4 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C33 C32 C37 117.7(14) . . ?
C33 C32 C31 118.6(14) . . ?
C37 C32 C31 123.6(12) . . ?
C34 C33 C32 122.2(14) . . ?
C34 C33 H33 118.9 . . ?
C32 C33 H33 118.9 . . ?
C35 C34 C33 120.5(15) . . ?
C35 C34 H34 119.7 . . ?
C33 C34 H34 119.7 . . ?
C34 C35 C36 120.9(15) . . ?
C34 C35 H35 119.5 . . ?
C36 C35 H35 119.5 . . ?
O8 C36 C35 125.1(12) . . ?
O8 C36 C37 115.1(10) . . ?
C35 C36 C37 119.8(12) . . ?
O7 C37 C36 116.5(10) . . ?
O7 C37 C32 124.6(11) . . ?
C36 C37 C32 118.8(11) . . ?
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 173.0(9) . . ?
N6 C40 Mo1 173.8(10) . . ?
N7 C41 Mo1 176.0(12) . . ?
N8 C42 Mo1 176.8(11) . . ?
N9 C43 Mo1 178.6(11) . . ?
N10 C44 Mo1 177.4(10) . . ?
N11 C45 Mo1 176.4(11) . . ?
N12 C46 Mo1 173.7(10) . . ?
N13 C47 C48 171(8) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C8 N1 C9 118.6(13) . . ?
C8 N1 Cu1 127.5(10) . . ?
C9 N1 Cu1 113.7(10) . . ?
C12 N2 C10 124.4(13) . . ?
C12 N2 Cu1 125.6(10) . . ?
C10 N2 Cu1 109.5(11) . . ?
C27 N3 C28 123.3(13) . . ?
C27 N3 Cu2 125.3(10) . . ?
C28 N3 Cu2 111.0(10) . . ?
C31 N4 C29 117.5(15) . . ?
C31 N4 Cu2 127.9(10) . . ?
C29 N4 Cu2 114.7(11) . . ?
C39 N5 Pr1 153.1(8) . . ?
C40 N6 Cu1 136.4(9) . . ?
C44 N10 Cu2 138.0(9) . 4_565 ?
C46 N12 Pr1 154.0(9) . 4_565 ?
C2 O1 C1 116.0(10) . . ?
C2 O1 Pr1 113.1(6) . . ?
C1 O1 Pr1 129.1(9) . . ?
C7 O2 Cu1 123.0(7) . . ?
C7 O2 Pr1 130.1(7) . . ?
Cu1 O2 Pr1 104.9(3) . . ?
C18 O3 Cu1 126.0(7) . . ?
C18 O3 Pr1 128.8(7) . . ?
Cu1 O3 Pr1 104.2(3) . . ?
C17 O4 C19 115.7(11) . . ?
C17 O4 Pr1 118.1(8) . . ?
C19 O4 Pr1 123.8(8) . . ?
C21 O5 C20 116.6(9) . . ?
C21 O5 Pr1 115.7(7) . . ?
C20 O5 Pr1 120.8(6) . . ?
C26 O6 Cu2 126.5(7) . . ?
C26 O6 Pr1 127.9(7) . . ?
Cu2 O6 Pr1 103.5(3) . . ?
C37 O7 Cu2 124.9(7) . . ?
C37 O7 Pr1 129.4(7) . . ?
Cu2 O7 Pr1 105.4(3) . . ?
C36 O8 C38 118.9(9) . . ?
C36 O8 Pr1 113.7(6) . . ?
C38 O8 Pr1 124.9(8) . . ?
C49 O9 H9A 109.5 . . ?
N1 Cu1 O2 94.9(4) . . ?
N1 Cu1 O3 160.7(4) . . ?
O2 Cu1 O3 85.3(3) . . ?
N1 Cu1 N2 84.6(6) . . ?
O2 Cu1 N2 174.2(4) . . ?
O3 Cu1 N2 93.2(5) . . ?
N1 Cu1 N6 100.7(5) . . ?
O2 Cu1 N6 94.6(3) . . ?
O3 Cu1 N6 98.5(4) . . ?
N2 Cu1 N6 91.2(4) . . ?
N1 Cu1 Pr1 131.1(4) . . ?
O2 Cu1 Pr1 42.7(2) . . ?
O3 Cu1 Pr1 43.3(2) . . ?
N2 Cu1 Pr1 134.7(4) . . ?
N6 Cu1 Pr1 105.0(3) . . ?
N4 Cu2 N3 84.7(6) . . ?
N4 Cu2 O7 93.7(4) . . ?
N3 Cu2 O7 172.9(4) . . ?
N4 Cu2 O6 162.8(4) . . ?
N3 Cu2 O6 94.6(5) . . ?
O7 Cu2 O6 84.8(3) . . ?
N4 Cu2 N10 97.9(4) . 4_666 ?
N3 Cu2 N10 94.4(4) . 4_666 ?
O7 Cu2 N10 92.7(3) . 4_666 ?
O6 Cu2 N10 99.4(4) . 4_666 ?
N4 Cu2 Pr1 130.2(4) . . ?
N3 Cu2 Pr1 135.7(4) . . ?
O7 Cu2 Pr1 42.2(2) . . ?
O6 Cu2 Pr1 43.4(2) . . ?
N10 Cu2 Pr1 104.5(3) 4_666 . ?
C39 Mo1 C45 143.0(4) . . ?
C39 Mo1 C41 71.7(5) . . ?
C45 Mo1 C41 72.5(5) . . ?
C39 Mo1 C40 72.6(4) . . ?
C45 Mo1 C40 89.7(4) . . ?
C41 Mo1 C40 75.4(5) . . ?
C39 Mo1 C44 120.6(4) . . ?
C45 Mo1 C44 80.2(4) . . ?
C41 Mo1 C44 135.2(5) . . ?
C40 Mo1 C44 69.5(4) . . ?
C39 Mo1 C42 81.2(4) . . ?
C45 Mo1 C42 97.8(4) . . ?
C41 Mo1 C42 74.2(5) . . ?
C40 Mo1 C42 144.8(4) . . ?
C44 Mo1 C42 145.6(4) . . ?
C39 Mo1 C46 140.4(4) . . ?
C45 Mo1 C46 72.9(4) . . ?
C41 Mo1 C46 130.0(5) . . ?
C40 Mo1 C46 138.5(4) . . ?
C44 Mo1 C46 70.6(4) . . ?
C42 Mo1 C46 76.0(4) . . ?
C39 Mo1 C43 70.4(4) . . ?
C45 Mo1 C43 146.6(4) . . ?
C41 Mo1 C43 138.7(4) . . ?
C40 Mo1 C43 107.6(4) . . ?
C44 Mo1 C43 79.6(4) . . ?
C42 Mo1 C43 84.4(5) . . ?
C46 Mo1 C43 75.5(4) . . ?
O7 Pr1 O6 65.0(2) . . ?
O7 Pr1 O2 76.4(2) . . ?
O6 Pr1 O2 120.1(3) . . ?
O7 Pr1 O3 122.1(2) . . ?
O6 Pr1 O3 172.9(3) . . ?
O2 Pr1 O3 64.3(3) . . ?
O7 Pr1 N5 128.4(3) . . ?
O6 Pr1 N5 93.6(3) . . ?
O2 Pr1 N5 75.9(3) . . ?
O3 Pr1 N5 82.0(3) . . ?
O7 Pr1 N12 77.1(3) . 4_666 ?
O6 Pr1 N12 80.8(3) . 4_666 ?
O2 Pr1 N12 133.3(3) . 4_666 ?
O3 Pr1 N12 100.1(3) . 4_666 ?
N5 Pr1 N12 148.7(3) . 4_666 ?
O7 Pr1 O4 139.7(2) . . ?
O6 Pr1 O4 115.6(3) . . ?
O2 Pr1 O4 123.4(2) . . ?
O3 Pr1 O4 59.3(3) . . ?
N5 Pr1 O4 91.8(3) . . ?
N12 Pr1 O4 64.0(3) 4_666 . ?
O7 Pr1 O5 123.8(2) . . ?
O6 Pr1 O5 59.3(2) . . ?
O2 Pr1 O5 139.7(2) . . ?
O3 Pr1 O5 113.6(2) . . ?
N5 Pr1 O5 64.2(3) . . ?
N12 Pr1 O5 86.9(3) 4_666 . ?
O4 Pr1 O5 66.3(2) . . ?
O7 Pr1 O8 59.1(2) . . ?
O6 Pr1 O8 119.5(2) . . ?
O2 Pr1 O8 67.0(2) . . ?
O3 Pr1 O8 66.9(2) . . ?
N5 Pr1 O8 139.0(3) . . ?
N12 Pr1 O8 66.5(3) 4_666 . ?
O4 Pr1 O8 94.2(2) . . ?
O5 Pr1 O8 152.5(2) . . ?
O7 Pr1 O1 63.8(2) . . ?
O6 Pr1 O1 65.7(3) . . ?
O2 Pr1 O1 56.5(2) . . ?
O3 Pr1 O1 116.7(2) . . ?
N5 Pr1 O1 64.6(3) . . ?
N12 Pr1 O1 136.2(3) 4_666 . ?
O4 Pr1 O1 156.2(2) . . ?
O5 Pr1 O1 98.4(2) . . ?
O8 Pr1 O1 105.6(2) . . ?
O7 Pr1 Cu2 32.42(17) . . ?
O6 Pr1 Cu2 33.12(18) . . ?
O2 Pr1 Cu2 95.59(17) . . ?
O3 Pr1 Cu2 153.93(18) . . ?
N5 Pr1 Cu2 110.4(2) . . ?
N12 Pr1 Cu2 81.4(2) 4_666 . ?
O4 Pr1 Cu2 139.25(17) . . ?
O5 Pr1 Cu2 92.45(16) . . ?
O8 Pr1 Cu2 90.52(17) . . ?
O1 Pr1 Cu2 55.07(16) . . ?
O7 Pr1 Cu1 97.16(17) . . ?
O6 Pr1 Cu1 152.40(19) . . ?
O2 Pr1 Cu1 32.31(17) . . ?
O3 Pr1 Cu1 32.50(19) . . ?
N5 Pr1 Cu1 81.1(2) . . ?
N12 Pr1 Cu1 117.1(2) 4_666 . ?
O4 Pr1 Cu1 91.74(18) . . ?
O5 Pr1 Cu1 137.08(15) . . ?
O8 Pr1 Cu1 58.28(16) . . ?
O1 Pr1 Cu1 87.86(17) . . ?
Cu2 Pr1 Cu1 124.31(4) . . ?
O9 C49 H49A 109.5 . . ?
O9 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
O9 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?

_refine_diff_density_max         3.821
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.152

_shelxl_version_number           2014-3


_chemical_properties_physical    Photo-sensitive
_exptl_crystal_preparation       'Magnetic properties'
