# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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data_1
_database_code_depnum_ccdc_archive 'CCDC 899841'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H30 Cl4 Dy0.87 N2 O7 Yb1.13'
_chemical_formula_weight         841.13

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'
Cl Cl 0.1484 0.1585 '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'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/m

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

_cell_length_a                   15.469(4)
_cell_length_b                   9.292(2)
_cell_length_c                   8.889(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.463(3)
_cell_angle_gamma                90.00
_cell_volume                     1266.9(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             801
_exptl_absorpt_coefficient_mu    7.150
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.4567
_exptl_absorpt_correction_T_max  0.6345
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3640
_diffrn_reflns_av_R_equivalents  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         26.49
_reflns_number_total             1354
_reflns_number_gt                1283
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0200P)²+1.5604P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1354
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0218
_refine_ls_wR_factor_ref         0.0499
_refine_ls_wR_factor_gt          0.0490
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.384587(13) 0.0000 1.02516(2) 0.01533(9) Uani 0.43 2 d SP . 1
Yb1 Yb 0.384587(13) 0.0000 1.02516(2) 0.01533(9) Uani 0.57 2 d SP . 2
Cl1 Cl 0.37090(7) 0.23233(14) 1.19536(13) 0.0431(3) Uani 1 1 d . . .
O1 O 0.4783(2) 0.0000 0.8583(3) 0.0147(7) Uani 1 2 d S . .
O2 O 0.31898(16) 0.1562(3) 0.8356(3) 0.0199(5) Uani 1 1 d . . .
H2O H 0.2669 0.1860 0.8269 0.024 Uiso 1 1 d R . .
C1 C 0.4615(3) 0.0000 0.6957(5) 0.0181(11) Uani 1 2 d S . .
H1 H 0.5188 0.0000 0.6552 0.022 Uiso 1 2 calc SR . .
C2 C 0.4122(2) 0.1359(4) 0.6390(4) 0.0206(8) Uani 1 1 d . . .
H2A H 0.4429 0.2208 0.6876 0.025 Uiso 1 1 calc R . .
H2B H 0.4128 0.1443 0.5281 0.025 Uiso 1 1 calc R . .
C3 C 0.3183(2) 0.1372(4) 0.6721(4) 0.0198(8) Uani 1 1 d . . .
H3 H 0.2877 0.2212 0.6187 0.024 Uiso 1 1 calc R . .
C4 C 0.2700(3) 0.0000 0.6178(6) 0.0229(12) Uani 1 2 d S . .
H4A H 0.2603 0.0000 0.5055 0.027 Uiso 1 2 calc SR . .
H4B H 0.2121 0.0000 0.6541 0.027 Uiso 1 2 calc SR . .
N1 N 0.2284(3) 0.0000 1.0521(5) 0.0342(11) Uani 0.50 2 d SP A 1
C5 C 0.1528(6) 0.0000 1.0575(11) 0.016(2) Uani 0.50 2 d SP A 1
C6 C 0.0576(7) 0.0000 1.0419(15) 0.038(3) Uani 0.50 2 d SP . 1
H6A H 0.0386 0.0000 1.1405 0.057 Uiso 0.50 2 d SPR . 1
H6B H 0.0360 0.0844 0.9873 0.057 Uiso 0.50 1 d PR . 1
O1W O 0.2284(3) 0.0000 1.0521(5) 0.0342(11) Uani 0.50 2 d SP B 2
H1WA H 0.2032 -0.0719 1.0043 0.041 Uiso 0.25 1 d PR B 2
H1WB H 0.2214 0.0000 1.1446 0.041 Uiso 0.50 2 d SPR B 2
N2 N 0.1207(7) 0.0000 1.2855(12) 0.036(2) Uani 0.50 2 d SP . .
C7 C 0.0712(8) 0.0000 1.3658(12) 0.025(2) Uani 0.50 2 d SP . .
C8 C 0.007(2) 0.0000 1.476(3) 0.042(5) Uani 0.50 2 d SP . .
H8A H -0.0254 -0.0813 1.4338 0.063 Uiso 0.50 1 d PR . .
H8B H 0.0266 0.0000 1.5831 0.063 Uiso 0.50 2 d SPR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.01065(14) 0.02274(14) 0.01275(13) 0.000 0.00207(8) 0.000
Yb1 0.01065(14) 0.02274(14) 0.01275(13) 0.000 0.00207(8) 0.000
Cl1 0.0278(6) 0.0620(8) 0.0357(6) -0.0273(5) -0.0108(5) 0.0252(5)
O1 0.0111(17) 0.0227(18) 0.0097(15) 0.000 -0.0004(13) 0.000
O2 0.0155(13) 0.0253(14) 0.0188(12) -0.0008(11) 0.0017(10) 0.0074(10)
C1 0.012(2) 0.032(3) 0.012(2) 0.000 0.0064(19) 0.000
C2 0.021(2) 0.028(2) 0.0125(16) 0.0036(15) 0.0014(14) -0.0026(15)
C3 0.0194(19) 0.026(2) 0.0129(16) 0.0042(15) -0.0014(14) 0.0027(15)
C4 0.012(3) 0.039(3) 0.017(3) 0.000 -0.002(2) 0.000
N1 0.019(2) 0.060(3) 0.024(2) 0.000 0.0029(18) 0.000
C5 0.005(5) 0.018(5) 0.025(5) 0.000 0.003(4) 0.000
C6 0.019(7) 0.049(8) 0.045(8) 0.000 0.004(5) 0.000
O1W 0.019(2) 0.060(3) 0.024(2) 0.000 0.0029(18) 0.000
N2 0.034(6) 0.038(6) 0.038(6) 0.000 0.019(5) 0.000
C7 0.033(6) 0.019(5) 0.023(5) 0.000 0.005(5) 0.000
C8 0.047(13) 0.054(7) 0.030(17) 0.000 0.024(10) 0.000

_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
Dy1 O1 2.205(3) . ?
Dy1 O1 2.236(3) 5_657 ?
Dy1 O2 2.352(2) 6 ?
Dy1 O2 2.352(2) . ?
Dy1 N1 2.459(4) . ?
Dy1 Cl1 2.6604(12) . ?
Dy1 Cl1 2.6604(12) 6 ?
Dy1 Dy1 3.6556(9) 5_657 ?
O1 C1 1.435(5) . ?
O1 Yb1 2.236(3) 5_657 ?
O1 Dy1 2.236(3) 5_657 ?
O2 C3 1.463(4) . ?
O2 H2O 0.8461 . ?
C1 C2 1.527(4) 6 ?
C1 C2 1.527(4) . ?
C1 Yb1 3.208(5) 5_657 ?
C1 H1 1.0000 . ?
C2 C3 1.520(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.524(5) . ?
C3 H3 1.0000 . ?
C4 C3 1.524(5) 6 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N1 C5 1.176(10) . ?
N1 H1WA 0.8573 . ?
N1 H1WB 0.8440 . ?
C5 C6 1.461(14) . ?
C5 H1WA 1.1716 . ?
C5 H1WB 1.2292 . ?
C6 C6 1.84(2) 5_557 ?
C6 H6A 0.9603 . ?
C6 H6B 0.9596 . ?
N2 C7 1.112(14) . ?
C7 C8 1.481(19) . ?
C7 C8 1.97(2) 5_558 ?
C8 C8 0.50(3) 5_558 ?
C8 C7 1.97(2) 5_558 ?
C8 H8A 0.9587 . ?
C8 H8B 0.9587 . ?

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 Dy1 O1 69.19(13) . 5_657 ?
O1 Dy1 O2 77.19(9) . 6 ?
O1 Dy1 O2 128.83(8) 5_657 6 ?
O1 Dy1 O2 77.19(9) . . ?
O1 Dy1 O2 128.83(8) 5_657 . ?
O2 Dy1 O2 76.20(12) 6 . ?
O1 Dy1 N1 143.70(13) . . ?
O1 Dy1 N1 147.11(13) 5_657 . ?
O2 Dy1 N1 74.43(10) 6 . ?
O2 Dy1 N1 74.43(10) . . ?
O1 Dy1 Cl1 119.37(4) . . ?
O1 Dy1 Cl1 82.94(5) 5_657 . ?
O2 Dy1 Cl1 148.14(7) 6 . ?
O2 Dy1 Cl1 81.25(7) . . ?
N1 Dy1 Cl1 78.05(6) . . ?
O1 Dy1 Cl1 119.37(4) . 6 ?
O1 Dy1 Cl1 82.94(5) 5_657 6 ?
O2 Dy1 Cl1 81.25(7) 6 6 ?
O2 Dy1 Cl1 148.14(7) . 6 ?
N1 Dy1 Cl1 78.05(6) . 6 ?
Cl1 Dy1 Cl1 108.48(6) . 6 ?
O1 Dy1 Dy1 34.87(8) . 5_657 ?
O1 Dy1 Dy1 34.32(8) 5_657 5_657 ?
O2 Dy1 Dy1 104.46(6) 6 5_657 ?
O2 Dy1 Dy1 104.46(6) . 5_657 ?
N1 Dy1 Dy1 178.57(10) . 5_657 ?
Cl1 Dy1 Dy1 102.75(3) . 5_657 ?
Cl1 Dy1 Dy1 102.75(3) 6 5_657 ?
C1 O1 Dy1 128.9(3) . . ?
C1 O1 Yb1 120.3(3) . 5_657 ?
Dy1 O1 Yb1 110.81(13) . 5_657 ?
C1 O1 Dy1 120.3(3) . 5_657 ?
Dy1 O1 Dy1 110.81(13) . 5_657 ?
Yb1 O1 Dy1 0.000(11) 5_657 5_657 ?
C3 O2 Dy1 125.8(2) . . ?
C3 O2 H2O 93.7 . . ?
Dy1 O2 H2O 125.8 . . ?
O1 C1 C2 110.5(2) . 6 ?
O1 C1 C2 110.5(2) . . ?
C2 C1 C2 111.7(4) 6 . ?
O1 C1 Yb1 37.00(18) . 5_657 ?
C2 C1 Yb1 122.9(2) 6 5_657 ?
C2 C1 Yb1 122.9(2) . 5_657 ?
O1 C1 H1 108.0 . . ?
C2 C1 H1 108.0 6 . ?
C2 C1 H1 108.0 . . ?
Yb1 C1 H1 71.0 5_657 . ?
C3 C2 C1 113.0(3) . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
O2 C3 C2 108.0(3) . . ?
O2 C3 C4 110.8(3) . . ?
C2 C3 C4 112.0(3) . . ?
O2 C3 H3 108.7 . . ?
C2 C3 H3 108.7 . . ?
C4 C3 H3 108.7 . . ?
C3 C4 C3 113.5(4) . 6 ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 6 . ?
C3 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 6 . ?
H4A C4 H4B 107.7 . . ?
C5 N1 Dy1 176.8(6) . . ?
C5 N1 H1WA 68.3 . . ?
Dy1 N1 H1WA 109.9 . . ?
C5 N1 H1WB 72.9 . . ?
Dy1 N1 H1WB 110.3 . . ?
H1WA N1 H1WB 112.1 . . ?
N1 C5 C6 172.3(11) . . ?
N1 C5 H1WA 42.8 . . ?
C6 C5 H1WA 132.6 . . ?
N1 C5 H1WB 41.0 . . ?
C6 C5 H1WB 146.7 . . ?
H1WA C5 H1WB 71.9 . . ?
C5 C6 C6 161.7(14) . 5_557 ?
C5 C6 H6A 109.8 . . ?
C6 C6 H6A 88.5 5_557 . ?
C5 C6 H6B 109.1 . . ?
C6 C6 H6B 62.6 5_557 . ?
H6A C6 H6B 109.5 . . ?
N2 C7 C8 178.5(19) . . ?
N2 C7 C8 174.6(16) . 5_558 ?
C8 C7 C8 4(3) . 5_558 ?
C8 C8 C7 165(10) 5_558 . ?
C8 C8 C7 11(8) 5_558 5_558 ?
C7 C8 C7 176(3) . 5_558 ?
C8 C8 H8A 93.4 5_558 . ?
C7 C8 H8A 95.9 . . ?
C7 C8 H8A 86.4 5_558 . ?
C8 C8 H8B 44.3 5_558 . ?
C7 C8 H8B 120.6 . . ?
C7 C8 H8B 55.6 5_558 . ?
H8A C8 H8B 118.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2O Cl1 0.85 2.25 3.093(3) 179.3 7_557
O1W H1WB N2 0.84 2.12 2.825(11) 140.6 .

_diffrn_measured_fraction_theta_max 0.967
_diffrn_reflns_theta_full        26.49
_diffrn_measured_fraction_theta_full 0.967
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.134


data_2
_database_code_depnum_ccdc_archive 'CCDC 899842'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H30 Cl4 Dy2 N2 O7'
_chemical_formula_weight         829.22

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'
Cl Cl 0.1484 0.1585 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/m

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

_cell_length_a                   15.546(2)
_cell_length_b                   9.2831(14)
_cell_length_c                   8.8893(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.267(2)
_cell_angle_gamma                90.00
_cell_volume                     1272.6(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             792
_exptl_absorpt_coefficient_mu    6.284
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3062
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.31
_diffrn_reflns_theta_max         27.00
_reflns_number_total             1436
_reflns_number_gt                1360
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0226P)²+0.1132P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1436
_refine_ls_number_parameters     97
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0208
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0472
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.061
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.384300(11) 0.0000 1.02738(2) 0.01432(8) Uani 1 2 d S . .
Cl1 Cl 0.37112(6) 0.23553(12) 1.19782(10) 0.0384(3) Uani 1 1 d . A .
O1 O 0.47780(17) 0.0000 0.8575(3) 0.0134(6) Uani 1 2 d S . .
O2 O 0.31843(13) 0.1567(2) 0.8344(2) 0.0177(5) Uani 1 1 d . A .
H2O H 0.2663 0.1865 0.8257 0.021 Uiso 1 1 d R . .
C1 C 0.4611(3) 0.0000 0.6948(5) 0.0174(10) Uani 1 2 d S . .
H1 H 0.5182 0.0000 0.6543 0.021 Uiso 1 2 calc SR A .
C2 C 0.4126(2) 0.1361(4) 0.6382(3) 0.0195(7) Uani 1 1 d . A .
H2A H 0.4430 0.2210 0.6869 0.023 Uiso 1 1 calc R . .
H2B H 0.4134 0.1446 0.5274 0.023 Uiso 1 1 calc R . .
C3 C 0.3191(2) 0.1372(4) 0.6714(3) 0.0178(7) Uani 1 1 d . . .
H3 H 0.2889 0.2212 0.6176 0.021 Uiso 1 1 calc R A .
C4 C 0.2707(3) 0.0000 0.6165(5) 0.0199(10) Uani 1 2 d S . .
H4A H 0.2614 0.0000 0.5043 0.024 Uiso 1 2 calc SR . .
H4B H 0.2131 0.0000 0.6528 0.024 Uiso 1 2 calc SR . .
N1 N 0.2270(2) 0.0000 1.0553(4) 0.0315(10) Uani 0.50 2 d SP A 1
C5 C 0.1524(5) 0.0000 1.0612(8) 0.0076(15) Uani 0.50 2 d SPU A 1
C6 C 0.0564(6) 0.0000 1.0462(13) 0.038(3) Uani 0.50 2 d SP . 1
H6A H 0.0373 0.0000 1.1448 0.056 Uiso 0.50 2 d SPR . 1
H6B H 0.0348 0.0844 0.9916 0.056 Uiso 0.50 1 d PR . 1
O1W O 0.2270(2) 0.0000 1.0553(4) 0.0315(10) Uani 0.50 2 d SP A 2
H1WA H 0.2020 -0.0719 1.0086 0.038 Uiso 0.25 1 d PR A 2
H1WB H 0.2201 0.0000 1.1490 0.038 Uiso 0.50 2 d SPR A 2
N2 N 0.1215(6) 0.0000 1.2872(10) 0.032(2) Uani 0.50 2 d SP . .
C7 C 0.0709(6) 0.0000 1.3712(11) 0.025(2) Uani 0.50 2 d SP . .
C8 C 0.0077(19) 0.0000 1.480(3) 0.046(5) Uani 0.50 2 d SPU . .
H8A H -0.0251 -0.0813 1.4372 0.069 Uiso 0.50 1 d PR . .
H8B H 0.0269 0.0000 1.5866 0.069 Uiso 0.50 2 d SPR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Dy1 0.00962(12) 0.02047(14) 0.01289(12) 0.000 0.00145(7) 0.000
Cl1 0.0246(4) 0.0557(7) 0.0315(5) -0.0245(4) -0.0101(4) 0.0225(4)
O1 0.0118(14) 0.0169(17) 0.0115(13) 0.000 0.0012(11) 0.000
O2 0.0147(10) 0.0236(13) 0.0146(10) -0.0014(9) 0.0016(8) 0.0052(9)
C1 0.013(2) 0.026(3) 0.013(2) 0.000 0.0009(16) 0.000
C2 0.0219(17) 0.0231(19) 0.0132(14) 0.0045(13) 0.0009(12) -0.0036(14)
C3 0.0189(16) 0.0213(18) 0.0127(14) 0.0036(12) 0.0000(11) 0.0016(13)
C4 0.012(2) 0.031(3) 0.016(2) 0.000 0.0003(16) 0.000
N1 0.0178(19) 0.052(3) 0.0238(19) 0.000 -0.0001(15) 0.000
C5 0.0071(17) 0.0078(17) 0.0080(17) 0.000 0.0017(10) 0.000
C6 0.015(5) 0.050(8) 0.048(7) 0.000 0.007(4) 0.000
O1W 0.0178(19) 0.052(3) 0.0238(19) 0.000 -0.0001(15) 0.000
N2 0.030(5) 0.029(5) 0.036(5) 0.000 0.004(4) 0.000
C7 0.025(5) 0.021(6) 0.029(5) 0.000 0.001(4) 0.000
C8 0.042(8) 0.047(6) 0.051(10) 0.000 0.010(7) 0.000

_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
Dy1 O1 2.225(3) . ?
Dy1 O1 2.256(3) 5_657 ?
Dy1 O2 2.380(2) 6 ?
Dy1 O2 2.380(2) . ?
Dy1 N1 2.489(4) . ?
Dy1 Cl1 2.6826(10) . ?
Dy1 Cl1 2.6826(10) 6 ?
Dy1 Dy1 3.6907(7) 5_657 ?
O1 C1 1.436(5) . ?
O1 Dy1 2.256(3) 5_657 ?
O2 C3 1.462(4) . ?
O2 H2O 0.8501 . ?
C1 C2 1.524(4) 6 ?
C1 C2 1.524(4) . ?
C1 H1 1.0000 . ?
C2 C3 1.519(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.527(4) . ?
C3 H3 1.0000 . ?
C4 C3 1.527(4) 6 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N1 C5 1.168(8) . ?
N1 H1WA 0.8534 . ?
N1 H1WB 0.8526 . ?
C5 C6 1.482(12) . ?
C5 H1WA 1.1615 . ?
C5 H1WB 1.2286 . ?
C6 C6 1.839(18) 5_557 ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
N2 C7 1.150(13) . ?
C7 C8 1.46(3) . ?
C7 C8 1.91(3) 5_558 ?
C8 C8 0.46(4) 5_558 ?
C8 C7 1.91(3) 5_558 ?
C8 H8A 0.9600 . ?
C8 H8B 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 Dy1 O1 69.08(11) . 5_657 ?
O1 Dy1 O2 76.65(7) . 6 ?
O1 Dy1 O2 128.65(7) 5_657 6 ?
O1 Dy1 O2 76.65(7) . . ?
O1 Dy1 O2 128.65(7) 5_657 . ?
O2 Dy1 O2 75.38(10) 6 . ?
O1 Dy1 N1 143.36(11) . . ?
O1 Dy1 N1 147.57(11) 5_657 . ?
O2 Dy1 N1 74.54(8) 6 . ?
O2 Dy1 N1 74.54(8) . . ?
O1 Dy1 Cl1 119.12(3) . . ?
O1 Dy1 Cl1 83.10(4) 5_657 . ?
O2 Dy1 Cl1 148.07(5) 6 . ?
O2 Dy1 Cl1 81.50(6) . . ?
N1 Dy1 Cl1 78.31(5) . . ?
O1 Dy1 Cl1 119.12(3) . 6 ?
O1 Dy1 Cl1 83.10(4) 5_657 6 ?
O2 Dy1 Cl1 81.50(6) 6 6 ?
O2 Dy1 Cl1 148.07(5) . 6 ?
N1 Dy1 Cl1 78.31(5) . 6 ?
Cl1 Dy1 Cl1 109.18(5) . 6 ?
O1 Dy1 Dy1 34.81(6) . 5_657 ?
O1 Dy1 Dy1 34.27(7) 5_657 5_657 ?
O2 Dy1 Dy1 104.04(5) 6 5_657 ?
O2 Dy1 Dy1 104.04(5) . 5_657 ?
N1 Dy1 Dy1 178.17(8) . 5_657 ?
Cl1 Dy1 Dy1 102.70(2) . 5_657 ?
Cl1 Dy1 Dy1 102.70(2) 6 5_657 ?
C1 O1 Dy1 129.3(2) . . ?
C1 O1 Dy1 119.8(2) . 5_657 ?
Dy1 O1 Dy1 110.92(11) . 5_657 ?
C3 O2 Dy1 125.63(18) . . ?
C3 O2 H2O 94.4 . . ?
Dy1 O2 H2O 125.6 . . ?
O1 C1 C2 110.6(2) . 6 ?
O1 C1 C2 110.6(2) . . ?
C2 C1 C2 112.0(3) 6 . ?
O1 C1 H1 107.8 . . ?
C2 C1 H1 107.8 6 . ?
C2 C1 H1 107.8 . . ?
C3 C2 C1 112.8(3) . . ?
C3 C2 H2A 109.0 . . ?
C1 C2 H2A 109.0 . . ?
C3 C2 H2B 109.0 . . ?
C1 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
O2 C3 C2 108.7(2) . . ?
O2 C3 C4 110.8(3) . . ?
C2 C3 C4 112.1(3) . . ?
O2 C3 H3 108.4 . . ?
C2 C3 H3 108.4 . . ?
C4 C3 H3 108.4 . . ?
C3 C4 C3 113.0(3) . 6 ?
C3 C4 H4A 109.0 . . ?
C3 C4 H4A 109.0 6 . ?
C3 C4 H4B 109.0 . . ?
C3 C4 H4B 109.0 6 . ?
H4A C4 H4B 107.8 . . ?
C5 N1 Dy1 176.8(4) . . ?
C5 N1 H1WA 68.1 . . ?
Dy1 N1 H1WA 110.2 . . ?
C5 N1 H1WB 73.0 . . ?
Dy1 N1 H1WB 110.1 . . ?
H1WA N1 H1WB 111.7 . . ?
N1 C5 C6 172.4(8) . . ?
N1 C5 H1WA 43.0 . . ?
C6 C5 H1WA 132.6 . . ?
N1 C5 H1WB 41.6 . . ?
C6 C5 H1WB 146.1 . . ?
H1WA C5 H1WB 72.3 . . ?
C5 C6 C6 158.8(13) . 5_557 ?
C5 C6 H6A 110.0 . . ?
C6 C6 H6A 91.2 5_557 . ?
C5 C6 H6B 109.2 . . ?
C6 C6 H6B 61.4 5_557 . ?
H6A C6 H6B 109.5 . . ?
N2 C7 C8 179.2(14) . . ?
N2 C7 C8 176.7(12) . 5_558 ?
C8 C7 C8 3(2) . 5_558 ?
C8 C8 C7 169(9) 5_558 . ?
C8 C8 C7 8(7) 5_558 5_558 ?
C7 C8 C7 177(2) . 5_558 ?
C8 C8 H8A 90.4 5_558 . ?
C7 C8 H8A 96.2 . . ?
C7 C8 H8A 85.4 5_558 . ?
C8 C8 H8B 49.1 5_558 . ?
C7 C8 H8B 120.1 . . ?
C7 C8 H8B 57.3 5_558 . ?
H8A C8 H8B 118.2 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2O Cl1 0.85 2.24 3.091(2) 179.8 7_557
O1W H1WB N2 0.85 2.08 2.792(11) 140.3 .

_diffrn_measured_fraction_theta_max 0.966
_diffrn_reflns_theta_full        27.00
_diffrn_measured_fraction_theta_full 0.966
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.124


data_3
_database_code_depnum_ccdc_archive 'CCDC 899843'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C16 H30 Cl4 N2 O7 Yb2'
_chemical_formula_weight         850.30

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   C2/m

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

_cell_length_a                   15.378(3)
_cell_length_b                   9.2501(16)
_cell_length_c                   8.8674(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.534(2)
_cell_angle_gamma                90.00
_cell_volume                     1250.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.258
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             808
_exptl_absorpt_coefficient_mu    7.898
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.2878
_exptl_absorpt_correction_T_max  0.5056
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            3500
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         26.00
_reflns_number_total             1301
_reflns_number_gt                1271
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F² against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F², conventional R-factors R are based
on F, with F set to zero for negative F². The threshold expression of
F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F² are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0291P)²+2.2487P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1301
_refine_ls_number_parameters     97
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_gt           0.0190
_refine_ls_wR_factor_ref         0.0495
_refine_ls_wR_factor_gt          0.0492
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_restrained_S_all      1.112
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Yb1 Yb 0.384843(12) 0.0000 1.02364(2) 0.01431(9) Uani 1 2 d S . .
Cl1 Cl 0.37122(7) 0.23132(13) 1.19367(12) 0.0403(3) Uani 1 1 d . A .
O1 O 0.4784(2) 0.0000 0.8592(4) 0.0147(7) Uani 1 2 d S . .
O2 O 0.31937(15) 0.1566(3) 0.8370(3) 0.0191(5) Uani 1 1 d . A .
H2O H 0.2671 0.1864 0.8283 0.023 Uiso 1 1 d R . .
C1 C 0.4617(3) 0.0000 0.6957(5) 0.0177(10) Uani 1 2 d S . .
H1 H 0.5194 0.0000 0.6554 0.021 Uiso 1 2 calc SR A .
C2 C 0.4124(2) 0.1357(4) 0.6391(4) 0.0203(7) Uani 1 1 d . A .
H2A H 0.4434 0.2210 0.6874 0.024 Uiso 1 1 calc R . .
H2B H 0.4128 0.1439 0.5278 0.024 Uiso 1 1 calc R . .
C3 C 0.3181(2) 0.1376(4) 0.6725(4) 0.0191(7) Uani 1 1 d . . .
H3 H 0.2873 0.2220 0.6191 0.023 Uiso 1 1 calc R A .
C4 C 0.2694(3) 0.0000 0.6182(6) 0.0201(10) Uani 1 2 d S . .
H4A H 0.2595 0.0000 0.5056 0.024 Uiso 1 2 calc SR . .
H4B H 0.2113 0.0000 0.6549 0.024 Uiso 1 2 calc SR . .
N1 N 0.2297(3) 0.0000 1.0508(5) 0.0310(10) Uani 0.50 2 d SP A 1
C5 C 0.1540(6) 0.0000 1.0526(12) 0.019(2) Uani 0.50 2 d SP A 1
C6 C 0.0576(7) 0.0000 1.0445(15) 0.035(3) Uani 0.50 2 d SP . 1
H6A H 0.0385 0.0000 1.1431 0.053 Uiso 0.50 2 d SPR . 1
H6B H 0.0360 0.0844 0.9898 0.053 Uiso 0.50 1 d PR . 1
O1W O 0.2297(3) 0.0000 1.0508(5) 0.0310(10) Uani 0.50 2 d SP A 2
H1WA H 0.2204 0.0000 1.1477 0.037 Uiso 0.50 2 d SPR A 2
H1WB H 0.2131 -0.0732 1.0042 0.037 Uiso 0.25 1 d PR A 2
N2 N 0.1223(7) 0.0000 1.2848(11) 0.029(2) Uani 0.50 2 d SP . .
C7 C 0.0708(7) 0.0000 1.3666(12) 0.024(2) Uani 0.50 2 d SP . .
C8 C 0.004(2) 0.0000 1.4718(19) 0.039(5) Uani 0.50 2 d SP . .
H8A H -0.0284 -0.0813 1.4294 0.059 Uiso 0.50 1 d PR . .
H8B H 0.0236 0.0000 1.5788 0.059 Uiso 0.50 2 d SPR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Yb1 0.01056(13) 0.02084(14) 0.01143(13) 0.000 0.00112(8) 0.000
Cl1 0.0262(5) 0.0588(7) 0.0320(5) -0.0260(5) -0.0104(4) 0.0231(5)
O1 0.0126(16) 0.0186(16) 0.0120(16) 0.000 -0.0011(12) 0.000
O2 0.0143(11) 0.0251(13) 0.0176(12) -0.0021(10) 0.0004(9) 0.0058(10)
C1 0.013(2) 0.031(3) 0.010(2) 0.000 0.0031(17) 0.000
C2 0.0187(17) 0.0282(19) 0.0137(17) 0.0036(14) 0.0010(13) -0.0032(15)
C3 0.0182(17) 0.0236(18) 0.0142(17) 0.0051(14) -0.0027(13) 0.0008(14)
C4 0.015(2) 0.030(3) 0.015(2) 0.000 -0.0003(18) 0.000
N1 0.014(2) 0.060(3) 0.018(2) 0.000 0.0013(16) 0.000
C5 0.013(5) 0.024(5) 0.022(5) 0.000 0.007(4) 0.000
C6 0.014(5) 0.046(7) 0.045(8) 0.000 0.003(5) 0.000
O1W 0.014(2) 0.060(3) 0.018(2) 0.000 0.0013(16) 0.000
N2 0.036(5) 0.026(5) 0.028(5) 0.000 0.006(4) 0.000
C7 0.028(6) 0.017(5) 0.026(6) 0.000 0.001(5) 0.000
C8 0.050(10) 0.048(7) 0.021(15) 0.000 0.005(12) 0.000

_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
Yb1 O1 2.178(3) . ?
Yb1 O1 2.220(3) 5_657 ?
Yb1 O2 2.327(2) 6 ?
Yb1 O2 2.327(2) . ?
Yb1 N1 2.429(4) . ?
Yb1 Cl1 2.6416(11) . ?
Yb1 Cl1 2.6416(11) 6 ?
Yb1 C1 3.198(5) 5_657 ?
Yb1 Yb1 3.6207(7) 5_657 ?
Yb1 H1WB 2.7100 . ?
O1 C1 1.439(5) . ?
O1 Yb1 2.220(3) 5_657 ?
O2 C3 1.466(4) . ?
O2 H2O 0.8433 . ?
C1 C2 1.518(4) 6 ?
C1 C2 1.518(4) . ?
C1 Yb1 3.198(5) 5_657 ?
C1 H1 1.0000 . ?
C2 C3 1.518(5) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.522(4) . ?
C3 H3 1.0000 . ?
C4 C3 1.522(4) 6 ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
N1 C5 1.167(11) . ?
N1 H1WA 0.8896 . ?
N1 H1WB 0.8163 . ?
C5 C6 1.475(14) . ?
C5 H1WA 1.2370 . ?
C5 H1WB 1.2539 . ?
C6 C6 1.84(2) 5_557 ?
C6 H6A 0.9578 . ?
C6 H6B 0.9554 . ?
N2 C7 1.143(15) . ?
C7 C8 1.47(2) . ?
C7 C8 1.95(2) 5_558 ?
C8 C8 0.53(3) 5_558 ?
C8 C7 1.95(2) 5_558 ?
C8 H8A 0.9541 . ?
C8 H8B 0.9558 . ?

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 Yb1 O1 69.19(13) . 5_657 ?
O1 Yb1 O2 77.64(9) . 6 ?
O1 Yb1 O2 128.89(8) 5_657 6 ?
O1 Yb1 O2 77.64(9) . . ?
O1 Yb1 O2 128.89(8) 5_657 . ?
O2 Yb1 O2 76.98(12) 6 . ?
O1 Yb1 N1 144.07(13) . . ?
O1 Yb1 N1 146.74(12) 5_657 . ?
O2 Yb1 N1 74.43(9) 6 . ?
O2 Yb1 N1 74.43(9) . . ?
O1 Yb1 Cl1 119.39(4) . . ?
O1 Yb1 Cl1 82.77(5) 5_657 . ?
O2 Yb1 Cl1 148.31(6) 6 . ?
O2 Yb1 Cl1 80.94(6) . . ?
N1 Yb1 Cl1 77.94(6) . . ?
O1 Yb1 Cl1 119.39(4) . 6 ?
O1 Yb1 Cl1 82.77(5) 5_657 6 ?
O2 Yb1 Cl1 80.94(6) 6 6 ?
O2 Yb1 Cl1 148.31(6) . 6 ?
N1 Yb1 Cl1 77.94(6) . 6 ?
Cl1 Yb1 Cl1 108.19(6) . 6 ?
O1 Yb1 C1 92.06(12) . 5_657 ?
O1 Yb1 C1 22.87(12) 5_657 5_657 ?
O2 Yb1 C1 139.47(7) 6 5_657 ?
O2 Yb1 C1 139.47(7) . 5_657 ?
N1 Yb1 C1 123.87(13) . 5_657 ?
Cl1 Yb1 C1 70.21(5) . 5_657 ?
Cl1 Yb1 C1 70.21(5) 6 5_657 ?
O1 Yb1 Yb1 34.97(8) . 5_657 ?
O1 Yb1 Yb1 34.22(8) 5_657 5_657 ?
O2 Yb1 Yb1 104.84(6) 6 5_657 ?
O2 Yb1 Yb1 104.84(6) . 5_657 ?
N1 Yb1 Yb1 179.04(10) . 5_657 ?
Cl1 Yb1 Yb1 102.60(2) . 5_657 ?
Cl1 Yb1 Yb1 102.60(2) 6 5_657 ?
C1 Yb1 Yb1 57.09(8) 5_657 5_657 ?
O1 Yb1 H1WB 132.9 . . ?
O1 Yb1 H1WB 152.3 5_657 . ?
O2 Yb1 H1WB 58.1 6 . ?
O2 Yb1 H1WB 77.5 . . ?
N1 Yb1 H1WB 17.2 . . ?
Cl1 Yb1 H1WB 95.1 . . ?
Cl1 Yb1 H1WB 71.6 6 . ?
C1 Yb1 H1WB 131.6 5_657 . ?
Yb1 Yb1 H1WB 162.3 5_657 . ?
C1 O1 Yb1 128.9(3) . . ?
C1 O1 Yb1 120.3(3) . 5_657 ?
Yb1 O1 Yb1 110.81(13) . 5_657 ?
C3 O2 Yb1 125.5(2) . . ?
C3 O2 H2O 93.4 . . ?
Yb1 O2 H2O 125.9 . . ?
O1 C1 C2 110.4(2) . 6 ?
O1 C1 C2 110.4(2) . . ?
C2 C1 C2 111.6(4) 6 . ?
O1 C1 Yb1 36.83(18) . 5_657 ?
C2 C1 Yb1 122.9(2) 6 5_657 ?
C2 C1 Yb1 122.9(2) . 5_657 ?
O1 C1 H1 108.1 . . ?
C2 C1 H1 108.1 6 . ?
C2 C1 H1 108.1 . . ?
Yb1 C1 H1 71.2 5_657 . ?
C3 C2 C1 113.2(3) . . ?
C3 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
C3 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.8 . . ?
O2 C3 C2 107.9(3) . . ?
O2 C3 C4 110.9(3) . . ?
C2 C3 C4 111.8(3) . . ?
O2 C3 H3 108.7 . . ?
C2 C3 H3 108.7 . . ?
C4 C3 H3 108.7 . . ?
C3 C4 C3 113.5(4) . 6 ?
C3 C4 H4A 108.9 . . ?
C3 C4 H4A 108.9 6 . ?
C3 C4 H4B 108.9 . . ?
C3 C4 H4B 108.9 6 . ?
H4A C4 H4B 107.7 . . ?
C5 N1 Yb1 175.2(6) . . ?
C5 N1 H1WA 72.5 . . ?
Yb1 N1 H1WA 112.3 . . ?
C5 N1 H1WB 76.1 . . ?
Yb1 N1 H1WB 101.3 . . ?
H1WA N1 H1WB 114.2 . . ?
N1 C5 C6 176.4(11) . . ?
N1 C5 H1WA 43.3 . . ?
C6 C5 H1WA 140.3 . . ?
N1 C5 H1WB 39.2 . . ?
C6 C5 H1WB 138.8 . . ?
H1WA C5 H1WB 70.2 . . ?
C5 C6 C6 157.6(14) . 5_557 ?
C5 C6 H6A 112.4 . . ?
C6 C6 H6A 89.9 5_557 . ?
C5 C6 H6B 107.8 . . ?
C6 C6 H6B 62.1 5_557 . ?
H6A C6 H6B 109.6 . . ?
N2 C7 C8 179.9(16) . . ?
N2 C7 C8 172.4(14) . 5_558 ?
C8 C7 C8 8(2) . 5_558 ?
C8 C8 C7 151(9) 5_558 . ?
C8 C8 C7 22(7) 5_558 5_558 ?
C7 C8 C7 172(2) . 5_558 ?
C8 C8 H8A 100.8 5_558 . ?
C7 C8 H8A 97.2 . . ?
C7 C8 H8A 87.5 5_558 . ?
C8 C8 H8B 32.1 5_558 . ?
C7 C8 H8B 118.6 . . ?
C7 C8 H8B 53.7 5_558 . ?
H8A C8 H8B 118.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2O Cl1 0.84 2.24 3.087(3) 179.3 7_557
O1W H1WA N2 0.89 2.06 2.817(11) 142.5 .

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.748
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.129


#_eof
#End of Crystallographic Information File





