# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1446950'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H7 O9 Sm'
_chemical_formula_sum            'C8 H7 O9 Sm'
_chemical_formula_weight         397.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc '

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

_cell_length_a                   8.2946(7)
_cell_length_b                   14.4178(13)
_cell_length_c                   8.6950(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.2390(10)
_cell_angle_gamma                90.00
_cell_volume                     1012.20(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2512
_cell_measurement_theta_min      2.52
_cell_measurement_theta_max      28.35

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             756
_exptl_absorpt_coefficient_mu    5.844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5171
_exptl_absorpt_correction_T_max  0.6521
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9537
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.52
_diffrn_reflns_theta_max         28.35
_reflns_number_total             2512
_reflns_number_gt                2486
_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)+(0.0199P)²+2.5853P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2512
_refine_ls_number_parameters     175
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0195
_refine_ls_R_factor_gt           0.0192
_refine_ls_wR_factor_ref         0.0504
_refine_ls_wR_factor_gt          0.0502
_refine_ls_goodness_of_fit_ref   1.244
_refine_ls_restrained_S_all      1.243
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.366084(16) 0.689464(9) 0.403738(14) 0.00414(6) Uani 1 1 d . . .
C1 C 0.6564(4) 0.68638(18) 0.7574(3) 0.0069(5) Uani 1 1 d . . .
C2 C 0.8383(4) 0.68906(19) 0.7704(4) 0.0093(5) Uani 1 1 d . . .
H2A H 0.9083 0.7033 0.8674 0.011 Uiso 1 1 calc R . .
C3 C 0.9040(3) 0.6715(2) 0.6468(3) 0.0082(5) Uani 1 1 d . . .
H3A H 0.8328 0.6540 0.5523 0.010 Uiso 1 1 calc R . .
C4 C 1.0844(3) 0.67831(18) 0.6507(3) 0.0066(5) Uani 1 1 d . . .
C5 C 0.4618(3) 0.60544(19) 0.1243(3) 0.0071(5) Uani 1 1 d . . .
C6 C 0.4744(4) 0.54386(19) -0.0112(3) 0.0089(5) Uani 1 1 d . . .
H6A H 0.4459 0.5674 -0.1134 0.011 Uiso 1 1 calc R . .
C7 C 0.0258(4) 0.5602(2) 0.1989(3) 0.0100(5) Uani 1 1 d . . .
C8 C -0.0344(4) 0.4978(2) 0.0622(3) 0.0102(5) Uani 1 1 d . . .
H8A H -0.1196 0.4560 0.0631 0.012 Uiso 1 1 calc R . .
O1 O 0.5663(2) 0.64501(14) 0.6393(2) 0.0075(4) Uani 1 1 d . . .
O1W O 0.3162(3) 0.52365(14) 0.4750(2) 0.0097(4) Uani 1 1 d D . .
O2 O 0.6039(2) 0.72570(14) 0.8655(2) 0.0081(4) Uani 1 1 d . . .
O3 O 1.1228(3) 0.66937(15) 0.5182(2) 0.0092(4) Uani 1 1 d . . .
O4 O 1.1875(3) 0.69199(13) 0.7792(2) 0.0088(4) Uani 1 1 d . . .
O5 O 0.5062(3) 0.57611(14) 0.2644(2) 0.0099(4) Uani 1 1 d . . .
O6 O 0.4000(3) 0.68557(13) 0.0953(2) 0.0076(4) Uani 1 1 d . . .
O7 O 0.1392(3) 0.61463(15) 0.2021(2) 0.0113(4) Uani 1 1 d . . .
O8 O -0.0528(3) 0.55137(18) 0.3128(3) 0.0172(5) Uani 1 1 d . . .
H1WB H 0.352(5) 0.503(3) 0.569(2) 0.027(12) Uiso 1 1 d D . .
H1WA H 0.353(5) 0.478(2) 0.429(5) 0.027(12) Uiso 1 1 d D . .
H8 H -0.001(7) 0.582(4) 0.385(7) 0.045(15) Uiso 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
Sm1 O4 2.357(2) 4_475 ?
Sm1 O2 2.4077(19) 4_575 ?
Sm1 O1 2.4096(19) . ?
Sm1 O6 2.4258(19) 4_576 ?
Sm1 O3 2.463(2) 1_455 ?
Sm1 O5 2.477(2) . ?
Sm1 O7 2.504(2) . ?
Sm1 O1W 2.527(2) . ?
Sm1 O6 2.761(2) . ?
Sm1 C5 2.981(3) . ?
C1 O2 1.258(3) . ?
C1 O1 1.272(3) . ?
C1 C2 1.488(4) . ?
C2 C3 1.336(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.492(4) . ?
C3 H3A 0.9300 . ?
C4 O4 1.257(3) . ?
C4 O3 1.270(3) . ?
C5 O5 1.262(3) . ?
C5 O6 1.266(3) . ?
C5 C6 1.498(4) . ?
C6 C6 1.334(6) 3_665 ?
C6 H6A 0.9300 . ?
C7 O7 1.220(4) . ?
C7 O8 1.311(4) . ?
C7 C8 1.483(4) . ?
C8 C8 1.335(6) 3_565 ?
C8 H8A 0.9300 . ?
O1W H1WB 0.859(10) . ?
O1W H1WA 0.864(10) . ?
O2 Sm1 2.4077(19) 4_576 ?
O3 Sm1 2.463(2) 1_655 ?
O4 Sm1 2.357(2) 4_676 ?
O6 Sm1 2.4258(19) 4_575 ?
O8 H8 0.80(6) . ?

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
O4 Sm1 O2 90.96(7) 4_475 4_575 ?
O4 Sm1 O1 145.27(7) 4_475 . ?
O2 Sm1 O1 79.97(7) 4_575 . ?
O4 Sm1 O6 74.86(7) 4_475 4_576 ?
O2 Sm1 O6 75.38(7) 4_575 4_576 ?
O1 Sm1 O6 70.42(7) . 4_576 ?
O4 Sm1 O3 77.52(7) 4_475 1_455 ?
O2 Sm1 O3 152.68(7) 4_575 1_455 ?
O1 Sm1 O3 95.39(7) . 1_455 ?
O6 Sm1 O3 77.70(7) 4_576 1_455 ?
O4 Sm1 O5 124.74(7) 4_475 . ?
O2 Sm1 O5 77.09(7) 4_575 . ?
O1 Sm1 O5 86.05(7) . . ?
O6 Sm1 O5 146.33(7) 4_576 . ?
O3 Sm1 O5 129.77(7) 1_455 . ?
O4 Sm1 O7 72.43(7) 4_475 . ?
O2 Sm1 O7 129.07(7) 4_575 . ?
O1 Sm1 O7 137.89(7) . . ?
O6 Sm1 O7 138.70(7) 4_576 . ?
O3 Sm1 O7 71.23(7) 1_455 . ?
O5 Sm1 O7 74.62(7) . . ?
O4 Sm1 O1W 132.65(7) 4_475 . ?
O2 Sm1 O1W 134.41(7) 4_575 . ?
O1 Sm1 O1W 70.10(7) . . ?
O6 Sm1 O1W 122.27(6) 4_576 . ?
O3 Sm1 O1W 66.07(7) 1_455 . ?
O5 Sm1 O1W 67.50(7) . . ?
O7 Sm1 O1W 67.98(7) . . ?
O4 Sm1 O6 76.20(6) 4_475 . ?
O2 Sm1 O6 66.87(6) 4_575 . ?
O1 Sm1 O6 128.09(6) . . ?
O6 Sm1 O6 131.34(4) 4_576 . ?
O3 Sm1 O6 131.71(6) 1_455 . ?
O5 Sm1 O6 49.29(6) . . ?
O7 Sm1 O6 62.51(6) . . ?
O1W Sm1 O6 106.13(6) . . ?
O4 Sm1 C5 100.19(7) 4_475 . ?
O2 Sm1 C5 73.40(7) 4_575 . ?
O1 Sm1 C5 108.94(7) . . ?
O6 Sm1 C5 148.30(7) 4_576 . ?
O3 Sm1 C5 132.64(7) 1_455 . ?
O5 Sm1 C5 24.59(7) . . ?
O7 Sm1 C5 63.38(7) . . ?
O1W Sm1 C5 84.53(7) . . ?
O6 Sm1 C5 25.10(7) . . ?
O2 C1 O1 125.1(3) . . ?
O2 C1 C2 116.8(2) . . ?
O1 C1 C2 118.2(2) . . ?
C3 C2 C1 121.8(3) . . ?
C3 C2 H2A 119.1 . . ?
C1 C2 H2A 119.1 . . ?
C2 C3 C4 124.1(3) . . ?
C2 C3 H3A 117.9 . . ?
C4 C3 H3A 117.9 . . ?
O4 C4 O3 124.1(3) . . ?
O4 C4 C3 120.3(2) . . ?
O3 C4 C3 115.5(2) . . ?
O5 C5 O6 120.9(2) . . ?
O5 C5 C6 120.2(2) . . ?
O6 C5 C6 118.8(2) . . ?
O5 C5 Sm1 54.74(13) . . ?
O6 C5 Sm1 67.68(14) . . ?
C6 C5 Sm1 164.07(19) . . ?
C6 C6 C5 121.6(3) 3_665 . ?
C6 C6 H6A 119.2 3_665 . ?
C5 C6 H6A 119.2 . . ?
O7 C7 O8 124.0(3) . . ?
O7 C7 C8 121.6(3) . . ?
O8 C7 C8 114.3(3) . . ?
C8 C8 C7 119.5(3) 3_565 . ?
C8 C8 H8A 120.2 3_565 . ?
C7 C8 H8A 120.2 . . ?
C1 O1 Sm1 136.45(17) . . ?
Sm1 O1W H1WB 122(3) . . ?
Sm1 O1W H1WA 121(3) . . ?
H1WB O1W H1WA 95(4) . . ?
C1 O2 Sm1 140.08(18) . 4_576 ?
C4 O3 Sm1 138.88(18) . 1_655 ?
C4 O4 Sm1 138.61(18) . 4_676 ?
C5 O5 Sm1 100.68(16) . . ?
C5 O6 Sm1 142.45(18) . 4_575 ?
C5 O6 Sm1 87.23(15) . . ?
Sm1 O6 Sm1 129.07(8) 4_575 . ?
C7 O7 Sm1 138.15(18) . . ?
C7 O8 H8 106(4) . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.554
_refine_diff_density_min         -1.787
_refine_diff_density_rms         0.160
####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1446951'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H12 O16 Tb2, 3(H2 O)'
_chemical_formula_sum            'C12 H18 O19 Tb2'
_chemical_formula_weight         784.12

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn '

loop_
_symmetry_equiv_pos_as_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                   9.4396(3)
_cell_length_b                   14.6880(4)
_cell_length_c                   14.7437(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.271(3)
_cell_angle_gamma                90.00
_cell_volume                     2043.70(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3635
_cell_measurement_theta_min      3.52
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.549
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1488
_exptl_absorpt_coefficient_mu    6.961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5153
_exptl_absorpt_correction_T_max  0.6805
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7846
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.52
_diffrn_reflns_theta_max         25.10
_reflns_number_total             3635
_reflns_number_gt                3242
_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)+(0.0249P)²+4.3002P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3635
_refine_ls_number_parameters     298
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0278
_refine_ls_wR_factor_ref         0.0672
_refine_ls_wR_factor_gt          0.0637
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001

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
Tb1 Tb -0.02489(3) 0.336296(16) 0.754278(17) 0.01200(9) Uani 1 1 d . . .
Tb2 Tb 0.18903(3) 0.154012(16) 0.593456(17) 0.01134(9) Uani 1 1 d . . .
O1 O 0.2120(4) 0.3537(2) 0.8239(3) 0.0204(9) Uani 1 1 d . . .
O2 O 0.2169(4) 0.2770(2) 0.6976(3) 0.0191(9) Uani 1 1 d . . .
O3 O 0.7067(4) 0.3731(3) 0.9325(2) 0.0193(9) Uani 1 1 d . . .
O4 O 0.7385(4) 0.3182(3) 0.7929(3) 0.0213(9) Uani 1 1 d . . .
O5 O -0.0857(4) 0.3442(2) 0.5954(3) 0.0235(9) Uani 1 1 d . . .
O6 O 0.0918(4) 0.2805(3) 0.5215(3) 0.0239(9) Uani 1 1 d . . .
O7 O -0.0798(4) 0.5248(3) 0.3047(3) 0.0237(9) Uani 1 1 d . . .
O8 O 0.1493(4) 0.5163(3) 0.2833(3) 0.0256(10) Uani 1 1 d . . .
O9 O 0.4329(4) 0.1122(3) 0.6317(3) 0.0229(9) Uani 1 1 d . . .
O10 O 0.4107(4) 0.2298(3) 0.5415(3) 0.0212(9) Uani 1 1 d . . .
O11 O 0.9611(4) 0.1852(2) 0.6869(2) 0.0181(8) Uani 1 1 d . . .
O12 O 0.9435(4) 0.1048(3) 0.5622(3) 0.0234(9) Uani 1 1 d . . .
C1 C 0.2820(6) 0.3138(4) 0.7641(4) 0.0164(12) Uani 1 1 d . . .
C2 C 0.4368(6) 0.3124(4) 0.7701(4) 0.0212(13) Uani 1 1 d . . .
H2A H 0.4880 0.2966 0.7193 0.025 Uiso 1 1 calc R . .
C3 C 0.5050(6) 0.3330(4) 0.8460(4) 0.0204(13) Uani 1 1 d . . .
H3A H 0.4505 0.3435 0.8968 0.024 Uiso 1 1 calc R . .
C4 C 0.6625(6) 0.3410(3) 0.8582(4) 0.0156(12) Uani 1 1 d . . .
C5 C -0.0086(6) 0.3349(3) 0.5272(4) 0.0171(12) Uani 1 1 d . . .
C6 C -0.0382(6) 0.3965(4) 0.4491(4) 0.0214(13) Uani 1 1 d . . .
H6A H -0.1248 0.4266 0.4457 0.026 Uiso 1 1 calc R . .
C7 C 0.0532(6) 0.4100(4) 0.3849(4) 0.0235(14) Uani 1 1 d . . .
H7A H 0.1296 0.3704 0.3804 0.028 Uiso 1 1 calc R . .
C8 C 0.0393(7) 0.4864(4) 0.3186(4) 0.0217(13) Uani 1 1 d . . .
C9 C 0.4872(6) 0.1712(4) 0.5815(4) 0.0176(12) Uani 1 1 d . . .
C10 C 0.6420(6) 0.1722(4) 0.5706(4) 0.0259(15) Uani 1 1 d . . .
H10A H 0.6780 0.1930 0.5162 0.031 Uiso 1 1 calc R . .
C11 C 0.7311(6) 0.1449(4) 0.6344(4) 0.0198(13) Uani 1 1 d . . .
H11A H 0.6931 0.1238 0.6882 0.024 Uiso 1 1 calc R . .
C12 C 0.8865(6) 0.1450(3) 0.6279(4) 0.0143(12) Uani 1 1 d . . .
O1W O -0.0104(4) 0.2224(3) 0.8698(3) 0.0264(10) Uani 1 1 d . . .
H1WB H -0.0439 0.1718 0.8514 0.032 Uiso 1 1 d R . .
H1WC H -0.0524 0.2388 0.9175 0.032 Uiso 1 1 d R . .
O2W O -0.0310(4) 0.4271(2) 0.8922(2) 0.0186(9) Uani 1 1 d . . .
O3W O 0.1904(4) 0.0758(3) 0.7367(3) 0.0299(10) Uani 1 1 d . . .
H3WB H 0.2540 0.0349 0.7406 0.036 Uiso 1 1 d R . .
H3WC H 0.1100 0.0536 0.7492 0.036 Uiso 1 1 d R . .
O4W O 0.2132(5) -0.0036(3) 0.5598(3) 0.0292(10) Uani 1 1 d . . .
H4WB H 0.1443 -0.0234 0.5274 0.035 Uiso 1 1 d R . .
H4WC H 0.2223 -0.0357 0.6076 0.035 Uiso 1 1 d R . .
O7W O -0.0640(5) 0.0360(3) 0.8338(4) 0.0532(14) Uani 1 1 d . . .
H7WC H -0.1514 0.0220 0.8325 0.064 Uiso 1 1 d R . .
H7WD H -0.0387 0.0480 0.8882 0.064 Uiso 1 1 d R . .
O6W O -0.3546(8) 0.5649(5) 0.4350(5) 0.105(3) Uani 1 1 d U . .
H6WA H -0.3329 0.5560 0.3801 0.126 Uiso 1 1 d R . .
H6WB H -0.2992 0.6052 0.4573 0.126 Uiso 1 1 d R . .
O5W O -0.3722(19) 0.4068(15) 0.5432(13) 0.352(10) Uani 1 1 d U . .
H5WB H -0.4304 0.3629 0.5469 0.422 Uiso 1 1 d R . .
H5WA H -0.2889 0.3886 0.5567 0.422 Uiso 1 1 d R . .


_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
Tb1 O4 2.332(4) 1_455 ?
Tb1 O1W 2.389(4) . ?
Tb1 O5 2.403(4) . ?
Tb1 O2W 2.434(4) . ?
Tb1 O11 2.434(4) 1_455 ?
Tb1 O7 2.436(4) 3_566 ?
Tb1 O1 2.453(4) . ?
Tb1 O8 2.519(4) 3_566 ?
Tb1 O2 2.598(4) . ?
Tb1 C8 2.819(6) 3_566 ?
Tb1 C1 2.916(5) . ?
Tb2 O6 2.319(4) . ?
Tb2 O4W 2.379(4) . ?
Tb2 O2 2.382(4) . ?
Tb2 O3W 2.404(4) . ?
Tb2 O3 2.416(4) 4_565 ?
Tb2 O9 2.436(4) . ?
Tb2 O12 2.461(4) 1_455 ?
Tb2 O10 2.505(4) . ?
Tb2 O11 2.621(3) 1_455 ?
Tb2 C9 2.835(6) . ?
Tb2 C12 2.915(5) 1_455 ?
O1 C1 1.258(6) . ?
O2 C1 1.266(6) . ?
O3 C4 1.255(7) . ?
O3 Tb2 2.416(4) 4_666 ?
O4 C4 1.260(6) . ?
O4 Tb1 2.332(3) 1_655 ?
O5 C5 1.262(6) . ?
O6 C5 1.244(6) . ?
O7 C8 1.270(7) . ?
O7 Tb1 2.436(4) 3_566 ?
O8 C8 1.251(7) . ?
O8 Tb1 2.519(4) 3_566 ?
O9 C9 1.256(6) . ?
O10 C9 1.262(7) . ?
O11 C12 1.255(6) . ?
O11 Tb1 2.434(4) 1_655 ?
O11 Tb2 2.621(3) 1_655 ?
O12 C12 1.264(6) . ?
O12 Tb2 2.461(4) 1_655 ?
C1 C2 1.463(7) . ?
C2 C3 1.314(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.498(8) . ?
C3 H3A 0.9300 . ?
C5 C6 1.485(7) . ?
C6 C7 1.310(8) . ?
C6 H6A 0.9300 . ?
C7 C8 1.492(8) . ?
C7 H7A 0.9300 . ?
C8 Tb1 2.819(6) 3_566 ?
C9 C10 1.474(8) . ?
C10 C11 1.311(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.472(7) . ?
C11 H11A 0.9300 . ?
C12 Tb2 2.915(5) 1_655 ?
O1W H1WB 0.8499 . ?
O1W H1WC 0.8500 . ?
O3W H3WB 0.8500 . ?
O3W H3WC 0.8501 . ?
O4W H4WB 0.8499 . ?
O4W H4WC 0.8500 . ?
O7W H7WC 0.8500 . ?
O7W H7WD 0.8499 . ?
O6W H6WA 0.8500 . ?
O6W H6WB 0.8501 . ?
O5W H5WB 0.8500 . ?
O5W H5WA 0.8499 . ?

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
O4 Tb1 O1W 77.68(14) 1_455 . ?
O4 Tb1 O5 91.94(14) 1_455 . ?
O1W Tb1 O5 137.54(13) . . ?
O4 Tb1 O2W 79.50(13) 1_455 . ?
O1W Tb1 O2W 77.88(13) . . ?
O5 Tb1 O2W 141.14(12) . . ?
O4 Tb1 O11 87.26(13) 1_455 1_455 ?
O1W Tb1 O11 69.75(13) . 1_455 ?
O5 Tb1 O11 68.71(12) . 1_455 ?
O2W Tb1 O11 146.98(12) . 1_455 ?
O4 Tb1 O7 125.50(13) 1_455 3_566 ?
O1W Tb1 O7 145.44(14) . 3_566 ?
O5 Tb1 O7 72.64(13) . 3_566 ?
O2W Tb1 O7 81.75(13) . 3_566 ?
O11 Tb1 O7 129.58(12) 1_455 3_566 ?
O4 Tb1 O1 141.14(13) 1_455 . ?
O1W Tb1 O1 74.75(14) . . ?
O5 Tb1 O1 126.81(13) . . ?
O2W Tb1 O1 68.38(12) . . ?
O11 Tb1 O1 107.84(12) 1_455 . ?
O7 Tb1 O1 71.88(13) 3_566 . ?
O4 Tb1 O8 72.98(13) 1_455 3_566 ?
O1W Tb1 O8 141.08(12) . 3_566 ?
O5 Tb1 O8 69.10(13) . 3_566 ?
O2W Tb1 O8 72.15(13) . 3_566 ?
O11 Tb1 O8 132.31(13) 1_455 3_566 ?
O7 Tb1 O8 52.58(13) 3_566 3_566 ?
O1 Tb1 O8 114.77(13) . 3_566 ?
O4 Tb1 O2 153.28(13) 1_455 . ?
O1W Tb1 O2 87.57(12) . . ?
O5 Tb1 O2 84.00(13) . . ?
O2W Tb1 O2 119.32(12) . . ?
O11 Tb1 O2 66.63(12) 1_455 . ?
O7 Tb1 O2 78.44(12) 3_566 . ?
O1 Tb1 O2 50.98(12) . . ?
O8 Tb1 O2 128.74(12) 3_566 . ?
O4 Tb1 C8 99.19(16) 1_455 3_566 ?
O1W Tb1 C8 156.93(15) . 3_566 ?
O5 Tb1 C8 64.85(14) . 3_566 ?
O2W Tb1 C8 79.08(14) . 3_566 ?
O11 Tb1 C8 133.25(15) 1_455 3_566 ?
O7 Tb1 C8 26.73(15) 3_566 3_566 ?
O1 Tb1 C8 95.70(16) . 3_566 ?
O8 Tb1 C8 26.34(14) 3_566 3_566 ?
O2 Tb1 C8 102.84(15) . 3_566 ?
O4 Tb1 C1 158.55(15) 1_455 . ?
O1W Tb1 C1 81.03(14) . . ?
O5 Tb1 C1 105.64(15) . . ?
O2W Tb1 C1 93.59(14) . . ?
O11 Tb1 C1 87.81(14) 1_455 . ?
O7 Tb1 C1 72.66(14) 3_566 . ?
O1 Tb1 C1 25.28(13) . . ?
O8 Tb1 C1 124.46(14) 3_566 . ?
O2 Tb1 C1 25.73(13) . . ?
C8 Tb1 C1 99.38(17) 3_566 . ?
O6 Tb2 O4W 136.30(14) . . ?
O6 Tb2 O2 73.99(14) . . ?
O4W Tb2 O2 149.61(13) . . ?
O6 Tb2 O3W 141.20(13) . . ?
O4W Tb2 O3W 73.70(14) . . ?
O2 Tb2 O3W 78.34(14) . . ?
O6 Tb2 O3 73.61(13) . 4_565 ?
O4W Tb2 O3 68.03(13) . 4_565 ?
O2 Tb2 O3 138.52(13) . 4_565 ?
O3W Tb2 O3 141.73(13) . 4_565 ?
O6 Tb2 O9 132.08(13) . . ?
O4W Tb2 O9 73.06(14) . . ?
O2 Tb2 O9 87.22(13) . . ?
O3W Tb2 O9 71.92(13) . . ?
O3 Tb2 O9 95.75(13) 4_565 . ?
O6 Tb2 O12 77.76(14) . 1_455 ?
O4W Tb2 O12 76.68(14) . 1_455 ?
O2 Tb2 O12 115.69(12) . 1_455 ?
O3W Tb2 O12 90.62(14) . 1_455 ?
O3 Tb2 O12 81.55(12) 4_565 1_455 ?
O9 Tb2 O12 148.24(14) . 1_455 ?
O6 Tb2 O10 80.14(13) . . ?
O4W Tb2 O10 106.50(13) . . ?
O2 Tb2 O10 77.23(12) . . ?
O3W Tb2 O10 119.53(14) . . ?
O3 Tb2 O10 72.32(13) 4_565 . ?
O9 Tb2 O10 52.52(12) . . ?
O12 Tb2 O10 149.60(13) 1_455 . ?
O6 Tb2 O11 77.26(12) . 1_455 ?
O4W Tb2 O11 111.28(13) . 1_455 ?
O2 Tb2 O11 66.98(12) . 1_455 ?
O3W Tb2 O11 67.05(12) . 1_455 ?
O3 Tb2 O11 128.37(12) 4_565 1_455 ?
O9 Tb2 O11 134.81(13) . 1_455 ?
O12 Tb2 O11 50.88(12) 1_455 1_455 ?
O10 Tb2 O11 141.65(12) . 1_455 ?
O6 Tb2 C9 106.48(15) . . ?
O4W Tb2 C9 88.50(15) . . ?
O2 Tb2 C9 82.92(14) . . ?
O3W Tb2 C9 96.37(15) . . ?
O3 Tb2 C9 82.15(14) 4_565 . ?
O9 Tb2 C9 26.19(14) . . ?
O12 Tb2 C9 161.17(14) 1_455 . ?
O10 Tb2 C9 26.42(14) . . ?
O11 Tb2 C9 147.64(14) 1_455 . ?
O6 Tb2 C12 74.73(14) . 1_455 ?
O4W Tb2 C12 95.21(15) . 1_455 ?
O2 Tb2 C12 90.98(14) . 1_455 ?
O3W Tb2 C12 79.14(14) . 1_455 ?
O3 Tb2 C12 104.64(14) 4_565 1_455 ?
O9 Tb2 C12 150.77(14) . 1_455 ?
O12 Tb2 C12 25.45(13) 1_455 1_455 ?
O10 Tb2 C12 154.38(13) . 1_455 ?
O11 Tb2 C12 25.51(13) 1_455 1_455 ?
C9 Tb2 C12 173.09(16) . 1_455 ?
C1 O1 Tb1 98.4(3) . . ?
C1 O2 Tb2 150.2(4) . . ?
C1 O2 Tb1 91.3(3) . . ?
Tb2 O2 Tb1 112.09(14) . . ?
C4 O3 Tb2 140.1(3) . 4_666 ?
C4 O4 Tb1 136.2(4) . 1_655 ?
C5 O5 Tb1 129.9(4) . . ?
C5 O6 Tb2 141.1(4) . . ?
C8 O7 Tb1 93.7(3) . 3_566 ?
C8 O8 Tb1 90.3(3) . 3_566 ?
C9 O9 Tb2 94.9(3) . . ?
C9 O10 Tb2 91.5(3) . . ?
C12 O11 Tb1 137.4(4) . 1_655 ?
C12 O11 Tb2 90.4(3) . 1_655 ?
Tb1 O11 Tb2 109.63(13) 1_655 1_655 ?
C12 O12 Tb2 97.8(3) . 1_655 ?
O1 C1 O2 119.3(5) . . ?
O1 C1 C2 120.2(5) . . ?
O2 C1 C2 120.5(5) . . ?
O1 C1 Tb1 56.4(3) . . ?
O2 C1 Tb1 63.0(3) . . ?
C2 C1 Tb1 174.3(4) . . ?
C3 C2 C1 121.2(5) . . ?
C3 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
C2 C3 C4 125.9(5) . . ?
C2 C3 H3A 117.1 . . ?
C4 C3 H3A 117.1 . . ?
O3 C4 O4 125.7(5) . . ?
O3 C4 C3 116.4(5) . . ?
O4 C4 C3 117.9(5) . . ?
O6 C5 O5 125.3(5) . . ?
O6 C5 C6 118.0(5) . . ?
O5 C5 C6 116.7(5) . . ?
C7 C6 C5 122.5(5) . . ?
C7 C6 H6A 118.8 . . ?
C5 C6 H6A 118.8 . . ?
C6 C7 C8 122.5(5) . . ?
C6 C7 H7A 118.7 . . ?
C8 C7 H7A 118.7 . . ?
O8 C8 O7 121.1(5) . . ?
O8 C8 C7 118.3(5) . . ?
O7 C8 C7 120.3(5) . . ?
O8 C8 Tb1 63.3(3) . 3_566 ?
O7 C8 Tb1 59.6(3) . 3_566 ?
C7 C8 Tb1 161.3(4) . 3_566 ?
O9 C9 O10 120.6(5) . . ?
O9 C9 C10 119.3(5) . . ?
O10 C9 C10 120.1(5) . . ?
O9 C9 Tb2 58.9(3) . . ?
O10 C9 Tb2 62.0(3) . . ?
C10 C9 Tb2 174.7(4) . . ?
C11 C10 C9 122.7(5) . . ?
C11 C10 H10A 118.6 . . ?
C9 C10 H10A 118.6 . . ?
C10 C11 C12 125.2(5) . . ?
C10 C11 H11A 117.4 . . ?
C12 C11 H11A 117.4 . . ?
O11 C12 O12 120.6(5) . . ?
O11 C12 C11 120.0(5) . . ?
O12 C12 C11 119.5(5) . . ?
O11 C12 Tb2 64.0(3) . 1_655 ?
O12 C12 Tb2 56.8(3) . 1_655 ?
C11 C12 Tb2 173.2(4) . 1_655 ?
Tb1 O1W H1WB 111.7 . . ?
Tb1 O1W H1WC 111.7 . . ?
H1WB O1W H1WC 109.6 . . ?
Tb2 O3W H3WB 112.7 . . ?
Tb2 O3W H3WC 112.8 . . ?
H3WB O3W H3WC 110.3 . . ?
Tb2 O4W H4WB 112.0 . . ?
Tb2 O4W H4WC 112.0 . . ?
H4WB O4W H4WC 109.8 . . ?
H7WC O7W H7WD 108.8 . . ?
H6WA O6W H6WB 108.4 . . ?
H5WB O5W H5WA 110.0 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.777
_refine_diff_density_min         -0.950
_refine_diff_density_rms         0.160
####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1446952'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C12 H14 Dy2 O16, 3(H2 O)'
_chemical_formula_sum            'C12 H20 Dy2 O19'
_chemical_formula_weight         793.28

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'
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   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   9.4254(5)
_cell_length_b                   14.5461(8)
_cell_length_c                   14.7326(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.9090(10)
_cell_angle_gamma                90.00
_cell_volume                     2019.63(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3552
_cell_measurement_theta_min      1.97
_cell_measurement_theta_max      25.09

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1504
_exptl_absorpt_coefficient_mu    7.441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2057
_exptl_absorpt_correction_T_max  0.3207
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14949
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         25.09
_reflns_number_total             3552
_reflns_number_gt                3445
_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)+(0.0198P)²+10.9251P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3552
_refine_ls_number_parameters     338
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0209
_refine_ls_wR_factor_ref         0.0529
_refine_ls_wR_factor_gt          0.0523
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_restrained_S_all      1.155
_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
Dy1 Dy 0.81229(2) 1.346512(13) 0.905959(13) 0.00531(7) Uani 1 1 d . . .
Dy2 Dy 1.02468(2) 1.164357(13) 0.744583(13) 0.00552(7) Uani 1 1 d . . .
O1W O 1.0112(3) 1.2786(2) 0.6303(2) 0.0124(6) Uani 1 1 d D . .
O1 O 0.5911(3) 1.2696(2) 0.9599(2) 0.0104(6) Uani 1 1 d . . .
O2W O 1.0309(3) 1.0742(2) 0.6074(2) 0.0100(6) Uani 1 1 d D . .
O2 O 0.5692(3) 1.3877(2) 0.8673(2) 0.0109(6) Uani 1 1 d . . .
O3W O 0.8115(3) 1.4255(2) 0.7638(2) 0.0138(7) Uani 1 1 d D . .
O3 O 0.0576(3) 1.3947(2) 0.9386(2) 0.0109(6) Uani 1 1 d . . .
O4W O 0.7880(4) 1.5034(2) 0.9392(2) 0.0127(7) Uani 1 1 d D . .
O4 O 0.0377(3) 1.3158(2) 0.8123(2) 0.0084(6) Uani 1 1 d . . .
O5 O 0.7836(3) 1.2223(2) 0.8035(2) 0.0099(6) Uani 1 1 d . . .
O5W O 0.3705(14) 1.0936(9) 0.9528(9) 0.193(5) Uani 1 1 d . . .
H5WA H 0.4132 1.1363 0.9817 0.231 Uiso 1 1 d R . .
H5WC H 0.2874 1.1110 0.9376 0.231 Uiso 1 1 d R . .
O6 O 0.7888(3) 1.1471(2) 0.6745(2) 0.0098(6) Uani 1 1 d . . .
O7W O 0.4340(4) 0.9638(2) 0.8335(3) 0.0260(8) Uani 1 1 d D . .
O7 O 0.2940(3) 1.1270(2) 0.5670(2) 0.0094(6) Uani 1 1 d . . .
O8 O 0.2607(3) 1.1830(2) 0.7063(2) 0.0104(6) Uani 1 1 d . . .
O9 O 0.9192(3) 1.0258(2) 0.8039(2) 0.0130(7) Uani 1 1 d . . .
O10 O 1.1484(3) 1.0162(2) 0.7807(2) 0.0131(7) Uani 1 1 d . . .
O11 O 1.0917(3) 0.7804(2) 1.0227(2) 0.0120(6) Uani 1 1 d . . .
O12 O 0.9119(3) 0.8450(2) 1.0970(2) 0.0118(7) Uani 1 1 d . . .
C1 C 0.5143(5) 1.3286(3) 0.9193(3) 0.0082(9) Uani 1 1 d . . .
C2 C 0.3585(5) 1.3291(3) 0.9318(3) 0.0110(9) Uani 1 1 d . . .
H2A H 0.3218 1.3122 0.9876 0.013 Uiso 1 1 calc R . .
C3 C 0.2711(5) 1.3533(3) 0.8651(3) 0.0103(9) Uani 1 1 d . . .
H3A H 0.3101 1.3705 0.8101 0.012 Uiso 1 1 calc R . .
C4 C 0.1149(5) 1.3546(3) 0.8727(3) 0.0081(9) Uani 1 1 d . . .
C5 C 0.7186(5) 1.1861(3) 0.7358(3) 0.0077(8) Uani 1 1 d . . .
C6 C 0.5613(5) 1.1865(3) 0.7308(3) 0.0111(9) Uani 1 1 d . . .
H6A H 0.5092 1.1985 0.7826 0.013 Uiso 1 1 calc R . .
C7 C 0.4950(5) 1.1697(3) 0.6525(3) 0.0107(9) Uani 1 1 d . . .
H7A H 0.5501 1.1632 0.6011 0.013 Uiso 1 1 calc R . .
C8 C 0.3390(5) 1.1606(3) 0.6414(3) 0.0085(9) Uani 1 1 d . . .
C9 C 1.0384(5) 0.9862(3) 0.8181(3) 0.0119(9) Uani 1 1 d . . .
C10 C 1.0524(5) 0.9106(3) 0.8845(3) 0.0121(9) Uani 1 1 d . . .
H10A H 1.1294 0.8709 0.8806 0.015 Uiso 1 1 calc R . .
C11 C 0.9587(5) 0.8974(3) 0.9496(3) 0.0117(9) Uani 1 1 d . . .
H11A H 0.8718 0.9276 0.9464 0.014 Uiso 1 1 calc R . .
C12 C 0.9901(5) 0.8349(3) 1.0282(3) 0.0088(9) Uani 1 1 d . . .
H3WB H 0.890(3) 1.437(4) 0.737(3) 0.022(15) Uiso 1 1 d D . .
H3WA H 0.756(5) 1.460(3) 0.733(3) 0.030(17) Uiso 1 1 d D . .
H4WB H 0.762(6) 1.547(3) 0.903(3) 0.016(14) Uiso 1 1 d D . .
H4WA H 0.838(5) 1.535(4) 0.977(3) 0.030(17) Uiso 1 1 d D . .
H2WB H 1.002(6) 1.0188(15) 0.616(4) 0.018(14) Uiso 1 1 d D . .
H2WA H 1.116(3) 1.078(4) 0.588(4) 0.032(17) Uiso 1 1 d D . .
H1WB H 1.030(6) 1.266(4) 0.5749(14) 0.020(15) Uiso 1 1 d D . .
H1WA H 1.037(6) 1.3347(14) 0.639(4) 0.015(14) Uiso 1 1 d D . .
H7WB H 0.469(6) 0.998(3) 0.875(3) 0.030(17) Uiso 1 1 d D . .
H7WA H 0.353(4) 0.985(5) 0.817(5) 0.05(2) Uiso 1 1 d D . .
O6W O 0.6501(6) 1.0670(3) 0.9311(4) 0.0616(15) Uani 1 1 d . . .
H6WC H 0.6594 1.0265 0.9723 0.074 Uiso 1 1 d R . .
H6WD H 0.5872 1.0483 0.8934 0.074 Uiso 1 1 d R . .


_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 O11 2.303(3) 3_777 ?
Dy1 O4W 2.346(3) . ?
Dy1 O5 2.367(3) . ?
Dy1 O3W 2.389(3) . ?
Dy1 O7 2.412(3) 4_686 ?
Dy1 O2 2.427(3) . ?
Dy1 O3 2.456(3) 1_655 ?
Dy1 O1 2.506(3) . ?
Dy1 O4 2.591(3) 1_655 ?
Dy1 C1 2.830(4) . ?
Dy1 C4 2.905(4) 1_655 ?
Dy2 O8 2.319(3) 1_655 ?
Dy2 O1W 2.368(3) . ?
Dy2 O12 2.403(3) 3_777 ?
Dy2 O2W 2.411(3) . ?
Dy2 O9 2.417(3) . ?
Dy2 O4 2.421(3) 1_655 ?
Dy2 O6 2.449(3) . ?
Dy2 O10 2.503(3) . ?
Dy2 O5 2.586(3) . ?
Dy2 C9 2.811(4) . ?
Dy2 C5 2.903(4) . ?
O1W H1WB 0.859(10) . ?
O1W H1WA 0.860(10) . ?
O1 C1 1.267(5) . ?
O2W H2WB 0.860(10) . ?
O2W H2WA 0.859(11) . ?
O2 C1 1.267(5) . ?
O3W H3WB 0.859(11) . ?
O3W H3WA 0.856(10) . ?
O3 C4 1.261(5) . ?
O3 Dy1 2.456(3) 1_455 ?
O4W H4WB 0.859(10) . ?
O4W H4WA 0.857(11) . ?
O4 C4 1.272(5) . ?
O4 Dy2 2.421(3) 1_455 ?
O4 Dy1 2.591(3) 1_455 ?
O5 C5 1.276(5) . ?
O5W H5WA 0.8500 . ?
O5W H5WC 0.8500 . ?
O6 C5 1.263(5) . ?
O7W H7WB 0.850(10) . ?
O7W H7WA 0.857(10) . ?
O7 C8 1.267(5) . ?
O7 Dy1 2.412(3) 4_585 ?
O8 C8 1.260(5) . ?
O8 Dy2 2.319(3) 1_455 ?
O9 C9 1.276(6) . ?
O10 C9 1.260(6) . ?
O11 C12 1.247(5) . ?
O11 Dy1 2.303(3) 3_777 ?
O12 C12 1.271(6) . ?
O12 Dy2 2.403(3) 3_777 ?
C1 C2 1.483(6) . ?
C2 C3 1.320(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.478(6) . ?
C3 H3A 0.9300 . ?
C4 Dy1 2.905(4) 1_455 ?
C5 C6 1.483(6) . ?
C6 C7 1.326(6) . ?
C6 H6A 0.9300 . ?
C7 C8 1.483(6) . ?
C7 H7A 0.9300 . ?
C9 C10 1.476(6) . ?
C10 C11 1.328(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.498(6) . ?
C11 H11A 0.9300 . ?
O6W H6WC 0.8499 . ?
O6W H6WD 0.8500 . ?

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
O11 Dy1 O4W 136.34(11) 3_777 . ?
O11 Dy1 O5 73.71(11) 3_777 . ?
O4W Dy1 O5 149.89(10) . . ?
O11 Dy1 O3W 141.43(11) 3_777 . ?
O4W Dy1 O3W 73.50(11) . . ?
O5 Dy1 O3W 79.01(11) . . ?
O11 Dy1 O7 73.29(10) 3_777 4_686 ?
O4W Dy1 O7 68.33(11) . 4_686 ?
O5 Dy1 O7 137.71(10) . 4_686 ?
O3W Dy1 O7 141.82(11) . 4_686 ?
O11 Dy1 O2 131.90(11) 3_777 . ?
O4W Dy1 O2 73.36(11) . . ?
O5 Dy1 O2 86.63(10) . . ?
O3W Dy1 O2 71.68(11) . . ?
O7 Dy1 O2 96.26(10) 4_686 . ?
O11 Dy1 O3 77.13(11) 3_777 1_655 ?
O4W Dy1 O3 77.08(11) . 1_655 ?
O5 Dy1 O3 116.11(10) . 1_655 ?
O3W Dy1 O3 91.40(11) . 1_655 ?
O7 Dy1 O3 81.01(10) 4_686 1_655 ?
O2 Dy1 O3 149.05(10) . 1_655 ?
O11 Dy1 O1 79.63(10) 3_777 . ?
O4W Dy1 O1 106.49(11) . . ?
O5 Dy1 O1 76.94(10) . . ?
O3W Dy1 O1 120.10(10) . . ?
O7 Dy1 O1 71.75(10) 4_686 . ?
O2 Dy1 O1 52.98(10) . . ?
O3 Dy1 O1 148.26(10) 1_655 . ?
O11 Dy1 O4 77.61(10) 3_777 1_655 ?
O4W Dy1 O4 111.25(11) . 1_655 ?
O5 Dy1 O4 67.37(10) . 1_655 ?
O3W Dy1 O4 66.87(10) . 1_655 ?
O7 Dy1 O4 128.57(10) 4_686 1_655 ?
O2 Dy1 O4 134.17(10) . 1_655 ?
O3 Dy1 O4 51.38(10) 1_655 1_655 ?
O1 Dy1 O4 141.74(9) . 1_655 ?
O11 Dy1 C1 106.13(12) 3_777 . ?
O4W Dy1 C1 88.54(12) . . ?
O5 Dy1 C1 82.57(11) . . ?
O3W Dy1 C1 96.64(12) . . ?
O7 Dy1 C1 81.95(11) 4_686 . ?
O2 Dy1 C1 26.49(11) . . ?
O3 Dy1 C1 160.85(11) 1_655 . ?
O1 Dy1 C1 26.60(11) . . ?
O4 Dy1 C1 147.59(11) 1_655 . ?
O11 Dy1 C4 74.31(11) 3_777 1_655 ?
O4W Dy1 C4 95.47(12) . 1_655 ?
O5 Dy1 C4 91.48(11) . 1_655 ?
O3W Dy1 C4 79.76(11) . 1_655 ?
O7 Dy1 C4 104.20(11) 4_686 1_655 ?
O2 Dy1 C4 151.22(11) . 1_655 ?
O3 Dy1 C4 25.50(11) 1_655 1_655 ?
O1 Dy1 C4 153.58(11) . 1_655 ?
O4 Dy1 C4 25.98(11) 1_655 1_655 ?
C1 Dy1 C4 173.57(12) . 1_655 ?
O8 Dy2 O1W 77.65(11) 1_655 . ?
O8 Dy2 O12 91.03(11) 1_655 3_777 ?
O1W Dy2 O12 137.74(10) . 3_777 ?
O8 Dy2 O2W 79.86(10) 1_655 . ?
O1W Dy2 O2W 77.72(10) . . ?
O12 Dy2 O2W 140.72(10) 3_777 . ?
O8 Dy2 O9 125.94(11) 1_655 . ?
O1W Dy2 O9 145.55(11) . . ?
O12 Dy2 O9 72.47(10) 3_777 . ?
O2W Dy2 O9 82.25(11) . . ?
O8 Dy2 O4 87.19(10) 1_655 1_655 ?
O1W Dy2 O4 69.89(10) . 1_655 ?
O12 Dy2 O4 68.98(10) 3_777 1_655 ?
O2W Dy2 O4 147.02(10) . 1_655 ?
O9 Dy2 O4 128.93(10) . 1_655 ?
O8 Dy2 O6 141.02(10) 1_655 . ?
O1W Dy2 O6 74.57(11) . . ?
O12 Dy2 O6 127.83(11) 3_777 . ?
O2W Dy2 O6 67.97(10) . . ?
O9 Dy2 O6 72.02(10) . . ?
O4 Dy2 O6 107.86(10) 1_655 . ?
O8 Dy2 O10 72.95(11) 1_655 . ?
O1W Dy2 O10 140.78(11) . . ?
O12 Dy2 O10 68.73(10) 3_777 . ?
O2W Dy2 O10 72.07(10) . . ?
O9 Dy2 O10 53.01(10) . . ?
O4 Dy2 O10 132.49(10) 1_655 . ?
O6 Dy2 O10 114.71(10) . . ?
O8 Dy2 O5 153.43(10) 1_655 . ?
O1W Dy2 O5 88.41(10) . . ?
O12 Dy2 O5 84.19(10) 3_777 . ?
O2W Dy2 O5 119.46(10) . . ?
O9 Dy2 O5 77.41(10) . . ?
O4 Dy2 O5 66.68(10) 1_655 . ?
O6 Dy2 O5 51.57(10) . . ?
O10 Dy2 O5 128.19(10) . . ?
O8 Dy2 C9 99.39(12) 1_655 . ?
O1W Dy2 C9 157.30(11) . . ?
O12 Dy2 C9 64.20(11) 3_777 . ?
O2W Dy2 C9 79.60(11) . . ?
O9 Dy2 C9 26.93(12) . . ?
O4 Dy2 C9 132.75(11) 1_655 . ?
O6 Dy2 C9 95.94(12) . . ?
O10 Dy2 C9 26.64(12) . . ?
O5 Dy2 C9 101.92(12) . . ?
O8 Dy2 C5 158.88(11) 1_655 . ?
O1W Dy2 C5 81.37(11) . . ?
O12 Dy2 C5 106.31(11) 3_777 . ?
O2W Dy2 C5 93.40(11) . . ?
O9 Dy2 C5 72.10(11) . . ?
O4 Dy2 C5 87.89(11) 1_655 . ?
O6 Dy2 C5 25.52(11) . . ?
O10 Dy2 C5 124.22(11) . . ?
O5 Dy2 C5 26.07(11) . . ?
C9 Dy2 C5 99.02(13) . . ?
Dy2 O1W H1WB 121(4) . . ?
Dy2 O1W H1WA 123(4) . . ?
H1WB O1W H1WA 107(5) . . ?
C1 O1 Dy1 91.1(3) . . ?
Dy2 O2W H2WB 112(4) . . ?
Dy2 O2W H2WA 106(4) . . ?
H2WB O2W H2WA 114(6) . . ?
C1 O2 Dy1 94.8(2) . . ?
Dy1 O3W H3WB 120(4) . . ?
Dy1 O3W H3WA 138(4) . . ?
H3WB O3W H3WA 99(5) . . ?
C4 O3 Dy1 97.5(2) . 1_455 ?
Dy1 O4W H4WB 128(4) . . ?
Dy1 O4W H4WA 127(4) . . ?
H4WB O4W H4WA 99(5) . . ?
C4 O4 Dy2 135.7(3) . 1_455 ?
C4 O4 Dy1 90.9(3) . 1_455 ?
Dy2 O4 Dy1 109.84(11) 1_455 1_455 ?
C5 O5 Dy1 149.6(3) . . ?
C5 O5 Dy2 91.0(2) . . ?
Dy1 O5 Dy2 111.77(11) . . ?
H5WA O5W H5WC 110.0 . . ?
C5 O6 Dy2 97.8(2) . . ?
H7WB O7W H7WA 109(6) . . ?
C8 O7 Dy1 139.6(3) . 4_585 ?
C8 O8 Dy2 136.8(3) . 1_455 ?
C9 O9 Dy2 94.0(3) . . ?
C9 O10 Dy2 90.4(3) . . ?
C12 O11 Dy1 140.9(3) . 3_777 ?
C12 O12 Dy2 129.0(3) . 3_777 ?
O2 C1 O1 120.6(4) . . ?
O2 C1 C2 119.1(4) . . ?
O1 C1 C2 120.3(4) . . ?
O2 C1 Dy1 58.7(2) . . ?
O1 C1 Dy1 62.3(2) . . ?
C2 C1 Dy1 173.6(3) . . ?
C3 C2 C1 121.0(4) . . ?
C3 C2 H2A 119.5 . . ?
C1 C2 H2A 119.5 . . ?
C2 C3 C4 123.9(4) . . ?
C2 C3 H3A 118.1 . . ?
C4 C3 H3A 118.1 . . ?
O3 C4 O4 119.7(4) . . ?
O3 C4 C3 120.2(4) . . ?
O4 C4 C3 120.0(4) . . ?
O3 C4 Dy1 57.0(2) . 1_455 ?
O4 C4 Dy1 63.1(2) . 1_455 ?
C3 C4 Dy1 173.8(3) . 1_455 ?
O6 C5 O5 119.6(4) . . ?
O6 C5 C6 120.1(4) . . ?
O5 C5 C6 120.3(4) . . ?
O6 C5 Dy2 56.7(2) . . ?
O5 C5 Dy2 63.0(2) . . ?
C6 C5 Dy2 174.0(3) . . ?
C7 C6 C5 119.9(4) . . ?
C7 C6 H6A 120.0 . . ?
C5 C6 H6A 120.0 . . ?
C6 C7 C8 124.4(4) . . ?
C6 C7 H7A 117.8 . . ?
C8 C7 H7A 117.8 . . ?
O8 C8 O7 124.4(4) . . ?
O8 C8 C7 119.0(4) . . ?
O7 C8 C7 116.6(4) . . ?
O10 C9 O9 120.0(4) . . ?
O10 C9 C10 118.9(4) . . ?
O9 C9 C10 120.9(4) . . ?
O10 C9 Dy2 62.9(2) . . ?
O9 C9 Dy2 59.1(2) . . ?
C10 C9 Dy2 160.9(3) . . ?
C11 C10 C9 122.2(4) . . ?
C11 C10 H10A 118.9 . . ?
C9 C10 H10A 118.9 . . ?
C10 C11 C12 121.4(4) . . ?
C10 C11 H11A 119.3 . . ?
C12 C11 H11A 119.3 . . ?
O11 C12 O12 125.6(4) . . ?
O11 C12 C11 118.5(4) . . ?
O12 C12 C11 115.9(4) . . ?
H6WC O6W H6WD 107.9 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         1.797
_refine_diff_density_min         -1.057
_refine_diff_density_rms         0.145
####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1446953'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H7 O8 Y'
_chemical_formula_sum            'C6 H7 O8 Y'
_chemical_formula_weight         296.03

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'
Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   9.4887(12)
_cell_length_b                   8.1086(11)
_cell_length_c                   12.2751(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.613(2)
_cell_angle_gamma                90.00
_cell_volume                     944.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1683
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.083
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_absorpt_coefficient_mu    6.200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_T_max  0.610
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6814
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         25.10
_reflns_number_total             1683
_reflns_number_gt                1602
_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)+(0.0367P)²+1.7504P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0165(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1683
_refine_ls_number_parameters     153
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0269
_refine_ls_wR_factor_ref         0.0762
_refine_ls_wR_factor_gt          0.0755
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_restrained_S_all      1.142
_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
Y1 Y 0.30907(3) 0.55650(3) 0.58101(2) 0.00567(16) Uani 1 1 d . . .
O6 O 0.0970(2) 0.6998(3) 0.51270(18) 0.0119(5) Uani 1 1 d . . .
O2W O 0.2612(2) 0.6116(3) 0.76434(17) 0.0097(4) Uani 1 1 d D . .
O1 O 0.4204(2) 0.3400(3) 0.67692(17) 0.0097(5) Uani 1 1 d . . .
O5 O 0.2569(2) 0.8529(3) 0.59634(17) 0.0113(5) Uani 1 1 d . . .
O1W O 0.1080(2) 0.3946(3) 0.63255(18) 0.0112(5) Uani 1 1 d D . .
C6 C 0.1438(3) 0.8408(4) 0.5406(2) 0.0102(6) Uani 1 1 d . . .
C1 C 0.5498(3) 0.3053(4) 0.6631(2) 0.0088(6) Uani 1 1 d . . .
C2 C 0.6295(3) 0.2338(4) 0.7581(2) 0.0106(6) Uani 1 1 d . . .
H2A H 0.5809 0.1764 0.8109 0.013 Uiso 1 1 calc R . .
C3 C 0.7680(3) 0.2500(4) 0.7692(2) 0.0109(6) Uani 1 1 d . . .
H3A H 0.8163 0.3047 0.7151 0.013 Uiso 1 1 calc R . .
C5 C 0.0688(3) 0.9967(4) 0.5087(3) 0.0125(6) Uani 1 1 d . . .
H5A H 0.1213 1.0927 0.5009 0.015 Uiso 1 1 calc R . .
O4 O 0.7842(2) 0.1438(3) 0.94945(17) 0.0123(5) Uani 1 1 d . . .
C4 C 0.8501(3) 0.1835(4) 0.8658(3) 0.0095(6) Uani 1 1 d . . .
O3 O 0.9809(2) 0.1684(3) 0.85404(18) 0.0120(5) Uani 1 1 d . . .
O2 O 0.6112(2) 0.3343(3) 0.57683(17) 0.0127(5) Uani 1 1 d . . .
H1WB H 0.057(4) 0.366(6) 0.577(2) 0.032(12) Uiso 1 1 d D . .
H1WA H 0.123(5) 0.312(4) 0.675(3) 0.030(12) Uiso 1 1 d D . .
H2WB H 0.244(5) 0.525(4) 0.802(4) 0.039(14) Uiso 1 1 d D . .
H2WA H 0.195(3) 0.681(4) 0.773(3) 0.018(10) 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
Y1 O2 2.279(2) 3_666 ?
Y1 O4 2.298(2) 4_565 ?
Y1 O3 2.311(2) 2_656 ?
Y1 O1 2.348(2) . ?
Y1 O2W 2.351(2) . ?
Y1 O1W 2.415(2) . ?
Y1 O6 2.451(2) . ?
Y1 O5 2.462(2) . ?
Y1 C6 2.824(3) . ?
O6 C6 1.270(4) . ?
O2W H2WB 0.856(10) . ?
O2W H2WA 0.854(10) . ?
O1 C1 1.275(4) . ?
O5 C6 1.261(4) . ?
O1W H1WB 0.861(10) . ?
O1W H1WA 0.856(10) . ?
C6 C5 1.497(4) . ?
C1 O2 1.245(4) . ?
C1 C2 1.491(4) . ?
C2 C3 1.324(4) . ?
C2 H2A 0.9300 . ?
C3 C4 1.500(4) . ?
C3 H3A 0.9300 . ?
C5 C5 1.317(6) 3_576 ?
C5 H5A 0.9300 . ?
O4 C4 1.259(4) . ?
O4 Y1 2.298(2) 4_666 ?
C4 O3 1.260(4) . ?
O3 Y1 2.311(2) 2_646 ?
O2 Y1 2.279(2) 3_666 ?

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
O2 Y1 O4 72.97(8) 3_666 4_565 ?
O2 Y1 O3 80.62(8) 3_666 2_656 ?
O4 Y1 O3 126.19(8) 4_565 2_656 ?
O2 Y1 O1 124.15(8) 3_666 . ?
O4 Y1 O1 81.95(8) 4_565 . ?
O3 Y1 O1 75.46(8) 2_656 . ?
O2 Y1 O2W 144.86(8) 3_666 . ?
O4 Y1 O2W 142.02(8) 4_565 . ?
O3 Y1 O2W 77.48(8) 2_656 . ?
O1 Y1 O2W 76.02(7) . . ?
O2 Y1 O1W 135.87(8) 3_666 . ?
O4 Y1 O1W 74.55(8) 4_565 . ?
O3 Y1 O1W 143.41(8) 2_656 . ?
O1 Y1 O1W 79.03(7) . . ?
O2W Y1 O1W 71.16(8) . . ?
O2 Y1 O6 79.28(8) 3_666 . ?
O4 Y1 O6 91.58(8) 4_565 . ?
O3 Y1 O6 128.58(8) 2_656 . ?
O1 Y1 O6 151.57(7) . . ?
O2W Y1 O6 93.35(8) . . ?
O1W Y1 O6 72.56(7) . . ?
O2 Y1 O5 75.99(8) 3_666 . ?
O4 Y1 O5 136.62(7) 4_565 . ?
O3 Y1 O5 76.33(7) 2_656 . ?
O1 Y1 O5 141.26(7) . . ?
O2W Y1 O5 72.34(7) . . ?
O1W Y1 O5 110.42(8) . . ?
O6 Y1 O5 53.03(7) . . ?
O2 Y1 C6 74.30(8) 3_666 . ?
O4 Y1 C6 114.07(8) 4_565 . ?
O3 Y1 C6 102.08(8) 2_656 . ?
O1 Y1 C6 159.73(8) . . ?
O2W Y1 C6 83.79(8) . . ?
O1W Y1 C6 92.93(8) . . ?
O6 Y1 C6 26.68(8) . . ?
O5 Y1 C6 26.47(8) . . ?
C6 O6 Y1 93.27(18) . . ?
Y1 O2W H2WB 114(3) . . ?
Y1 O2W H2WA 114(3) . . ?
H2WB O2W H2WA 108(4) . . ?
C1 O1 Y1 121.28(18) . . ?
C6 O5 Y1 93.03(17) . . ?
Y1 O1W H1WB 112(3) . . ?
Y1 O1W H1WA 118(3) . . ?
H1WB O1W H1WA 111(4) . . ?
O5 C6 O6 120.1(3) . . ?
O5 C6 C5 117.9(3) . . ?
O6 C6 C5 122.0(3) . . ?
O5 C6 Y1 60.50(15) . . ?
O6 C6 Y1 60.05(15) . . ?
C5 C6 Y1 173.0(2) . . ?
O2 C1 O1 123.2(3) . . ?
O2 C1 C2 120.0(3) . . ?
O1 C1 C2 116.8(3) . . ?
C3 C2 C1 121.5(3) . . ?
C3 C2 H2A 119.3 . . ?
C1 C2 H2A 119.3 . . ?
C2 C3 C4 122.5(3) . . ?
C2 C3 H3A 118.8 . . ?
C4 C3 H3A 118.8 . . ?
C5 C5 C6 122.5(4) 3_576 . ?
C5 C5 H5A 118.7 3_576 . ?
C6 C5 H5A 118.7 . . ?
C4 O4 Y1 135.28(19) . 4_666 ?
O4 C4 O3 125.6(3) . . ?
O4 C4 C3 118.5(3) . . ?
O3 C4 C3 115.8(3) . . ?
C4 O3 Y1 147.3(2) . 2_646 ?
C1 O2 Y1 166.1(2) . 3_666 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.116
####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1446954'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H7 Ho O8'
_chemical_formula_sum            'C6 H7 Ho O8'
_chemical_formula_weight         372.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   9.4773(10)
_cell_length_b                   8.1182(9)
_cell_length_c                   12.2797(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.566(2)
_cell_angle_gamma                90.00
_cell_volume                     944.43(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1649
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      25.09

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_absorpt_coefficient_mu    8.400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1558
_exptl_absorpt_correction_T_max  0.2546
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4920
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         25.09
_reflns_number_total             1649
_reflns_number_gt                1570
_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)+(0.0413P)²+3.1969P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1649
_refine_ls_number_parameters     160
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0734
_refine_ls_wR_factor_gt          0.0724
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.122
_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
Ho1 Ho 0.30932(3) 0.05653(3) 0.580854(17) 0.00330(13) Uani 1 1 d . . .
O1 O 0.5188(4) 0.1684(5) 0.6461(3) 0.0121(9) Uani 1 1 d . . .
O1W O 0.1081(4) -0.1051(5) 0.6328(3) 0.0118(9) Uani 1 1 d D . .
O2W O 0.2613(4) 0.1119(5) 0.7646(3) 0.0089(8) Uani 1 1 d D . .
O2 O 0.7164(4) 0.1437(5) 0.5511(3) 0.0129(9) Uani 1 1 d . . .
O3 O 1.0797(4) 0.3403(5) 0.8226(3) 0.0085(8) Uani 1 1 d . . .
O4 O 0.8890(4) 0.3341(5) 0.9235(3) 0.0135(9) Uani 1 1 d . . .
O5 O 0.2561(5) 0.3519(5) 0.5963(3) 0.0122(9) Uani 1 1 d . . .
O6 O 0.0975(4) 0.2012(5) 0.5125(3) 0.0138(9) Uani 1 1 d . . .
C1 C 0.6505(6) 0.1831(7) 0.6350(4) 0.0082(12) Uani 1 1 d . . .
C2 C 0.7324(6) 0.2499(7) 0.7302(5) 0.0094(12) Uani 1 1 d . . .
H2 H 0.674(7) 0.292(8) 0.785(5) 0.009(16) Uiso 1 1 d . . .
C3 C 0.8704(7) 0.2332(7) 0.7423(5) 0.0113(12) Uani 1 1 d . . .
H3 H 0.928(8) 0.186(9) 0.695(6) 0.03(2) Uiso 1 1 d . . .
C4 C 0.9503(6) 0.3046(7) 0.8365(4) 0.0072(11) Uani 1 1 d . . .
C5 C 0.1430(6) 0.3404(7) 0.5406(4) 0.0084(12) Uani 1 1 d . . .
C6 C 0.0686(7) 0.4972(8) 0.5088(5) 0.0140(12) Uani 1 1 d . . .
H6A H 0.1212 0.5931 0.5014 0.017 Uiso 1 1 calc R . .
H2WB H 0.184(4) 0.160(8) 0.782(5) 0.015(18) Uiso 1 1 d D . .
H1WB H 0.125(8) -0.191(6) 0.672(5) 0.03(2) Uiso 1 1 d D . .
H2WA H 0.243(8) 0.032(6) 0.808(5) 0.02(2) Uiso 1 1 d D . .
H1WA H 0.043(7) -0.120(12) 0.584(5) 0.05(3) 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
Ho1 O4 2.274(4) 4_565 ?
Ho1 O2 2.303(4) 3_656 ?
Ho1 O1 2.306(4) . ?
Ho1 O3 2.351(4) 2_646 ?
Ho1 O2W 2.357(4) . ?
Ho1 O1W 2.415(4) . ?
Ho1 O6 2.454(4) . ?
Ho1 O5 2.459(4) . ?
Ho1 C5 2.828(6) . ?
O1 C1 1.265(7) . ?
O1W H1WB 0.859(10) . ?
O1W H1WA 0.859(10) . ?
O2W H2WB 0.859(10) . ?
O2W H2WA 0.861(10) . ?
O2 C1 1.261(7) . ?
O2 Ho1 2.303(4) 3_656 ?
O3 C4 1.276(7) . ?
O3 Ho1 2.351(4) 2_656 ?
O4 C4 1.253(7) . ?
O4 Ho1 2.274(4) 4_666 ?
O5 C5 1.259(7) . ?
O6 C5 1.254(7) . ?
C1 C2 1.488(8) . ?
C2 C3 1.319(9) . ?
C2 H2 0.95(6) . ?
C3 C4 1.483(8) . ?
C3 H3 0.89(8) . ?
C5 C6 1.502(9) . ?
C6 C6 1.313(13) 3_566 ?
C6 H6A 0.9300 . ?

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
O4 Ho1 O2 73.09(15) 4_565 3_656 ?
O4 Ho1 O1 80.74(15) 4_565 . ?
O2 Ho1 O1 126.58(14) 3_656 . ?
O4 Ho1 O3 124.48(14) 4_565 2_646 ?
O2 Ho1 O3 82.25(14) 3_656 2_646 ?
O1 Ho1 O3 75.53(14) . 2_646 ?
O4 Ho1 O2W 144.70(15) 4_565 . ?
O2 Ho1 O2W 142.04(14) 3_656 . ?
O1 Ho1 O2W 77.24(14) . . ?
O3 Ho1 O2W 75.81(14) 2_646 . ?
O4 Ho1 O1W 136.00(14) 4_565 . ?
O2 Ho1 O1W 74.51(14) 3_656 . ?
O1 Ho1 O1W 143.18(14) . . ?
O3 Ho1 O1W 78.84(14) 2_646 . ?
O2W Ho1 O1W 71.12(14) . . ?
O4 Ho1 O6 79.04(15) 4_565 . ?
O2 Ho1 O6 91.55(14) 3_656 . ?
O1 Ho1 O6 128.21(15) . . ?
O3 Ho1 O6 151.69(14) 2_646 . ?
O2W Ho1 O6 93.37(14) . . ?
O1W Ho1 O6 72.89(14) . . ?
O4 Ho1 O5 76.02(14) 4_565 . ?
O2 Ho1 O5 136.43(14) 3_656 . ?
O1 Ho1 O5 76.44(14) . . ?
O3 Ho1 O5 141.20(13) 2_646 . ?
O2W Ho1 O5 72.23(13) . . ?
O1W Ho1 O5 110.14(15) . . ?
O6 Ho1 O5 52.56(14) . . ?
O4 Ho1 C5 74.32(15) 4_565 . ?
O2 Ho1 C5 113.85(15) 3_656 . ?
O1 Ho1 C5 102.13(16) . . ?
O3 Ho1 C5 159.43(14) 2_646 . ?
O2W Ho1 C5 83.72(14) . . ?
O1W Ho1 C5 92.78(16) . . ?
O6 Ho1 C5 26.28(16) . . ?
O5 Ho1 C5 26.39(15) . . ?
C1 O1 Ho1 147.4(4) . . ?
Ho1 O1W H1WB 117(5) . . ?
Ho1 O1W H1WA 117(6) . . ?
H1WB O1W H1WA 113(8) . . ?
Ho1 O2W H2WB 120(5) . . ?
Ho1 O2W H2WA 120(5) . . ?
H2WB O2W H2WA 91(7) . . ?
C1 O2 Ho1 135.1(4) . 3_656 ?
C4 O3 Ho1 121.3(3) . 2_656 ?
C4 O4 Ho1 166.2(4) . 4_666 ?
C5 O5 Ho1 93.4(3) . . ?
C5 O6 Ho1 93.7(3) . . ?
O2 C1 O1 125.2(5) . . ?
O2 C1 C2 118.3(5) . . ?
O1 C1 C2 116.4(5) . . ?
C3 C2 C1 123.1(5) . . ?
C3 C2 H2 124(4) . . ?
C1 C2 H2 113(4) . . ?
C2 C3 C4 122.1(5) . . ?
C2 C3 H3 126(5) . . ?
C4 C3 H3 112(5) . . ?
O4 C4 O3 122.8(5) . . ?
O4 C4 C3 120.0(5) . . ?
O3 C4 C3 117.1(5) . . ?
O6 C5 O5 119.9(5) . . ?
O6 C5 C6 122.4(5) . . ?
O5 C5 C6 117.7(5) . . ?
O6 C5 Ho1 60.0(3) . . ?
O5 C5 Ho1 60.2(3) . . ?
C6 C5 Ho1 172.6(4) . . ?
C6 C6 C5 121.9(8) 3_566 . ?
C6 C6 H6A 119.1 3_566 . ?
C5 C6 H6A 119.1 . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         1.568
_refine_diff_density_min         -2.365
_refine_diff_density_rms         0.256
####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 1446955'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H7 Er O8'
_chemical_formula_sum            'C6 H7 Er O8'
_chemical_formula_weight         374.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   9.4562(9)
_cell_length_b                   8.0842(8)
_cell_length_c                   12.2466(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4540(10)
_cell_angle_gamma                90.00
_cell_volume                     935.90(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1664
_cell_measurement_theta_min      2.69
_cell_measurement_theta_max      25.09

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             700
_exptl_absorpt_coefficient_mu    8.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1397
_exptl_absorpt_correction_T_max  0.2209
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6959
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.69
_diffrn_reflns_theta_max         25.09
_reflns_number_total             1664
_reflns_number_gt                1651
_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)+(0.0155P)²+6.3143P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1664
_refine_ls_number_parameters     152
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0491
_refine_ls_wR_factor_gt          0.0489
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_restrained_S_all      1.213
_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
Er1 Er 0.309119(19) 0.44362(2) 0.581035(15) 0.00352(9) Uani 1 1 d . . .
O6 O 0.0973(3) 0.3000(4) 0.5130(3) 0.0097(7) Uani 1 1 d . . .
O1 O 0.5185(3) 0.3327(4) 0.6456(3) 0.0102(7) Uani 1 1 d . . .
O1W O 0.2615(3) 0.3876(4) 0.7645(3) 0.0079(6) Uani 1 1 d D . .
O5 O 0.2576(3) 0.1476(4) 0.5967(3) 0.0097(7) Uani 1 1 d . . .
O2 O 0.7168(3) 0.3564(4) 0.5500(3) 0.0104(7) Uani 1 1 d . . .
O2W O 0.1077(3) 0.6048(4) 0.6328(3) 0.0089(7) Uani 1 1 d D . .
C5 C 0.1442(5) 0.1592(6) 0.5405(3) 0.0076(9) Uani 1 1 d . . .
C6 C 0.0693(5) 0.0033(6) 0.5086(4) 0.0097(9) Uani 1 1 d . . .
H6A H 0.1221 -0.0928 0.5006 0.012 Uiso 1 1 calc R . .
C2 C 0.7315(5) 0.2495(6) 0.7300(4) 0.0087(9) Uani 1 1 d . . .
H2A H 0.6830 0.1938 0.7838 0.010 Uiso 1 1 calc R . .
C1 C 0.6500(5) 0.3163(6) 0.6341(4) 0.0076(9) Uani 1 1 d . . .
O4 O 0.8879(3) 0.1655(4) 0.9236(3) 0.0113(7) Uani 1 1 d . . .
O3 O 1.0799(3) 0.1592(4) 0.8231(2) 0.0070(6) Uani 1 1 d . . .
C4 C 0.9495(5) 0.1943(5) 0.8368(4) 0.0065(9) Uani 1 1 d . . .
C3 C 0.8709(5) 0.2665(6) 0.7416(4) 0.0089(9) Uani 1 1 d . . .
H3A H 0.9201 0.3247 0.6892 0.011 Uiso 1 1 calc R . .
H2WB H 0.054(5) 0.628(7) 0.578(3) 0.017(15) Uiso 1 1 d D . .
H2WA H 0.127(7) 0.691(5) 0.671(5) 0.029(18) Uiso 1 1 d D . .
H1WB H 0.187(4) 0.331(7) 0.776(5) 0.024(16) Uiso 1 1 d D . .
H1WA H 0.252(9) 0.473(6) 0.805(6) 0.05(3) 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
Er1 O4 2.263(3) 4_565 ?
Er1 O2 2.286(3) 3_666 ?
Er1 O1 2.295(3) . ?
Er1 O3 2.335(3) 2_656 ?
Er1 O1W 2.346(3) . ?
Er1 O2W 2.406(3) . ?
Er1 O6 2.443(3) . ?
Er1 O5 2.450(3) . ?
Er1 C5 2.815(5) . ?
O6 C5 1.264(6) . ?
O1 C1 1.263(5) . ?
O1W H1WB 0.858(10) . ?
O1W H1WA 0.859(10) . ?
O5 C5 1.263(6) . ?
O2 C1 1.265(6) . ?
O2 Er1 2.286(3) 3_666 ?
O2W H2WB 0.858(10) . ?
O2W H2WA 0.856(10) . ?
C5 C6 1.492(7) . ?
C6 C6 1.324(9) 3_556 ?
C6 H6A 0.9300 . ?
C2 C3 1.329(6) . ?
C2 C1 1.489(6) . ?
C2 H2A 0.9300 . ?
O4 C4 1.248(5) . ?
O4 Er1 2.263(3) 4_666 ?
O3 C4 1.280(5) . ?
O3 Er1 2.335(3) 2_646 ?
C4 C3 1.486(6) . ?
C3 H3A 0.9300 . ?

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
O4 Er1 O2 73.13(12) 4_565 3_666 ?
O4 Er1 O1 80.89(12) 4_565 . ?
O2 Er1 O1 126.46(11) 3_666 . ?
O4 Er1 O3 124.47(11) 4_565 2_656 ?
O2 Er1 O3 82.19(11) 3_666 2_656 ?
O1 Er1 O3 75.27(11) . 2_656 ?
O4 Er1 O1W 144.64(12) 4_565 . ?
O2 Er1 O1W 142.04(11) 3_666 . ?
O1 Er1 O1W 77.25(11) . . ?
O3 Er1 O1W 75.94(11) 2_656 . ?
O4 Er1 O2W 135.68(11) 4_565 . ?
O2 Er1 O2W 74.37(11) 3_666 . ?
O1 Er1 O2W 143.34(11) . . ?
O3 Er1 O2W 79.16(11) 2_656 . ?
O1W Er1 O2W 71.32(11) . . ?
O4 Er1 O6 78.98(11) 4_565 . ?
O2 Er1 O6 91.39(11) 3_666 . ?
O1 Er1 O6 128.62(11) . . ?
O3 Er1 O6 151.65(10) 2_656 . ?
O1W Er1 O6 93.41(11) . . ?
O2W Er1 O6 72.52(11) . . ?
O4 Er1 O5 75.88(11) 4_565 . ?
O2 Er1 O5 136.66(11) 3_666 . ?
O1 Er1 O5 76.28(11) . . ?
O3 Er1 O5 140.99(11) 2_656 . ?
O1W Er1 O5 72.16(11) . . ?
O2W Er1 O5 110.37(11) . . ?
O6 Er1 O5 53.11(11) . . ?
O4 Er1 C5 73.99(12) 4_565 . ?
O2 Er1 C5 113.87(12) 3_666 . ?
O1 Er1 C5 102.16(13) . . ?
O3 Er1 C5 159.69(12) 2_656 . ?
O1W Er1 C5 83.82(12) . . ?
O2W Er1 C5 92.87(12) . . ?
O6 Er1 C5 26.64(12) . . ?
O5 Er1 C5 26.61(12) . . ?
C5 O6 Er1 93.3(3) . . ?
C1 O1 Er1 147.8(3) . . ?
Er1 O1W H1WB 116(4) . . ?
Er1 O1W H1WA 115(6) . . ?
H1WB O1W H1WA 103(7) . . ?
C5 O5 Er1 93.0(3) . . ?
C1 O2 Er1 134.9(3) . 3_666 ?
Er1 O2W H2WB 112(4) . . ?
Er1 O2W H2WA 115(4) . . ?
H2WB O2W H2WA 112(6) . . ?
O5 C5 O6 119.9(4) . . ?
O5 C5 C6 118.1(4) . . ?
O6 C5 C6 122.0(4) . . ?
O5 C5 Er1 60.3(2) . . ?
O6 C5 Er1 60.0(2) . . ?
C6 C5 Er1 173.0(3) . . ?
C6 C6 C5 122.5(6) 3_556 . ?
C6 C6 H6A 118.8 3_556 . ?
C5 C6 H6A 118.8 . . ?
C3 C2 C1 122.6(4) . . ?
C3 C2 H2A 118.7 . . ?
C1 C2 H2A 118.7 . . ?
O1 C1 O2 125.3(4) . . ?
O1 C1 C2 116.2(4) . . ?
O2 C1 C2 118.4(4) . . ?
C4 O4 Er1 165.9(3) . 4_666 ?
C4 O3 Er1 121.4(3) . 2_646 ?
O4 C4 O3 122.9(4) . . ?
O4 C4 C3 120.4(4) . . ?
O3 C4 C3 116.7(4) . . ?
C2 C3 C4 121.3(4) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.09
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.580
_refine_diff_density_min         -1.748
_refine_diff_density_rms         0.153
####################################################################### 
# 
# 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_3d
_database_code_depnum_ccdc_archive 'CCDC 1446956'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 H7 O8 Tm'
_chemical_formula_sum            'C6 H7 O8 Tm'
_chemical_formula_weight         376.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tm Tm -0.3139 5.2483 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn '

loop_
_symmetry_equiv_pos_as_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                   9.394(4)
_cell_length_b                   8.142(4)
_cell_length_c                   12.262(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.581(8)
_cell_angle_gamma                90.00
_cell_volume                     937.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1662
_cell_measurement_theta_min      2.70
_cell_measurement_theta_max      25.10

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_absorpt_coefficient_mu    9.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1099
_exptl_absorpt_correction_T_max  0.1945
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 7.31
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6536
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0215
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.70
_diffrn_reflns_theta_max         25.10
_reflns_number_total             1662
_reflns_number_gt                1641
_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)+(0.0516P)²+5.8435P] 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         1662
_refine_ls_number_parameters     136
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0282
_refine_ls_wR_factor_ref         0.0875
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   1.195
_refine_ls_restrained_S_all      1.195
_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
Tm1 Tm 0.69002(3) 0.55824(3) 0.419177(19) 0.00893(15) Uani 1 1 d . . .
O1 O 0.4794(5) 0.6670(6) 0.3549(4) 0.0218(11) Uani 1 1 d . . .
O6 O 0.7455(6) 0.8516(6) 0.4029(4) 0.0249(11) Uani 1 1 d . . .
O5 O 0.9014(5) 0.6982(7) 0.4884(4) 0.0272(12) Uani 1 1 d . . .
C1 C 0.3469(7) 0.6788(7) 0.3655(5) 0.0143(13) Uani 1 1 d . . .
C3 C 0.1278(7) 0.7298(8) 0.2566(5) 0.0172(13) Uani 1 1 d . . .
H3A H 0.0776 0.6705 0.3077 0.021 Uiso 1 1 calc R . .
C2 C 0.2661(7) 0.7469(9) 0.2697(5) 0.0186(14) Uani 1 1 d . . .
H2A H 0.3156 0.8037 0.2170 0.022 Uiso 1 1 calc R . .
C5 C 0.8573(8) 0.8401(8) 0.4579(6) 0.0211(15) Uani 1 1 d . . .
C6 C 0.9302(9) 0.9970(10) 0.4911(7) 0.0296(16) Uani 1 1 d . . .
H6A H 0.8764 1.0919 0.4992 0.035 Uiso 1 1 calc R . .
O2 O 0.2812(5) 0.6361(6) 0.4479(4) 0.0231(11) Uani 1 1 d . . .
O2W O 0.7373(5) 0.6124(6) 0.2365(4) 0.0189(10) Uani 1 1 d . . .
H2wA H 0.7912 0.6993 0.2189 0.023 Uiso 1 1 d R . .
H2wB H 0.7013 0.5463 0.1838 0.023 Uiso 1 1 d R . .
O1W O 0.8907(5) 0.3973(6) 0.3675(4) 0.0222(10) Uani 1 1 d . . .
H1WA H 0.9780 0.4427 0.3676 0.027 Uiso 1 1 d R . .
H1WB H 0.8788 0.2916 0.3478 0.027 Uiso 1 1 d R . .
O4 O 0.1115(5) 0.8309(6) 0.0748(4) 0.0226(11) Uani 1 1 d . . .
C4 C 0.0499(7) 0.8037(7) 0.1615(5) 0.0130(12) Uani 1 1 d . . .
O3 O -0.0809(5) 0.8416(5) 0.1748(4) 0.0156(9) 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
Tm1 O4 2.254(5) 4_676 ?
Tm1 O2 2.282(5) 3_666 ?
Tm1 O1 2.288(5) . ?
Tm1 O3 2.330(4) 2_545 ?
Tm1 O2W 2.337(4) . ?
Tm1 O1W 2.395(5) . ?
Tm1 O5 2.422(5) . ?
Tm1 O6 2.454(5) . ?
Tm1 C5 2.814(7) . ?
O1 C1 1.259(8) . ?
O6 C5 1.236(9) . ?
O5 C5 1.279(9) . ?
C1 O2 1.248(8) . ?
C1 C2 1.488(9) . ?
C3 C2 1.312(10) . ?
C3 C4 1.487(8) . ?
C3 H3A 0.9300 . ?
C2 H2A 0.9300 . ?
C5 C6 1.501(11) . ?
C6 C6 1.324(16) 3_776 ?
C6 H6A 0.9300 . ?
O2 Tm1 2.282(5) 3_666 ?
O2W H2wA 0.9000 . ?
O2W H2wB 0.9000 . ?
O1W H1WA 0.9000 . ?
O1W H1WB 0.9000 . ?
O4 C4 1.244(8) . ?
O4 Tm1 2.254(5) 4_575 ?
C4 O3 1.281(8) . ?
O3 Tm1 2.330(4) 2 ?

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
O4 Tm1 O2 73.02(18) 4_676 3_666 ?
O4 Tm1 O1 80.60(19) 4_676 . ?
O2 Tm1 O1 126.78(18) 3_666 . ?
O4 Tm1 O3 124.92(17) 4_676 2_545 ?
O2 Tm1 O3 82.54(18) 3_666 2_545 ?
O1 Tm1 O3 75.99(17) . 2_545 ?
O4 Tm1 O2W 144.22(18) 4_676 . ?
O2 Tm1 O2W 142.48(17) 3_666 . ?
O1 Tm1 O2W 77.42(18) . . ?
O3 Tm1 O2W 76.19(16) 2_545 . ?
O4 Tm1 O1W 136.18(18) 4_676 . ?
O2 Tm1 O1W 74.41(18) 3_666 . ?
O1 Tm1 O1W 143.12(18) . . ?
O3 Tm1 O1W 78.09(16) 2_545 . ?
O2W Tm1 O1W 71.20(18) . . ?
O4 Tm1 O5 78.40(18) 4_676 . ?
O2 Tm1 O5 89.78(19) 3_666 . ?
O1 Tm1 O5 129.1(2) . . ?
O3 Tm1 O5 151.05(17) 2_545 . ?
O2W Tm1 O5 94.11(18) . . ?
O1W Tm1 O5 72.95(18) . . ?
O4 Tm1 O6 75.76(18) 4_676 . ?
O2 Tm1 O6 135.36(18) 3_666 . ?
O1 Tm1 O6 77.22(18) . . ?
O3 Tm1 O6 142.04(16) 2_545 . ?
O2W Tm1 O6 72.09(16) . . ?
O1W Tm1 O6 109.91(18) . . ?
O5 Tm1 O6 52.89(18) . . ?
O4 Tm1 C5 74.02(19) 4_676 . ?
O2 Tm1 C5 113.0(2) 3_666 . ?
O1 Tm1 C5 102.5(2) . . ?
O3 Tm1 C5 159.58(18) 2_545 . ?
O2W Tm1 C5 83.58(18) . . ?
O1W Tm1 C5 92.9(2) . . ?
O5 Tm1 C5 27.0(2) . . ?
O6 Tm1 C5 26.0(2) . . ?
C1 O1 Tm1 147.4(4) . . ?
C5 O6 Tm1 93.5(4) . . ?
C5 O5 Tm1 93.8(4) . . ?
O2 C1 O1 125.1(6) . . ?
O2 C1 C2 119.4(6) . . ?
O1 C1 C2 115.5(6) . . ?
C2 C3 C4 121.2(6) . . ?
C2 C3 H3A 119.4 . . ?
C4 C3 H3A 119.4 . . ?
C3 C2 C1 122.6(6) . . ?
C3 C2 H2A 118.7 . . ?
C1 C2 H2A 118.7 . . ?
O6 C5 O5 119.4(6) . . ?
O6 C5 C6 117.2(6) . . ?
O5 C5 C6 123.2(7) . . ?
O6 C5 Tm1 60.5(3) . . ?
O5 C5 Tm1 59.2(3) . . ?
C6 C5 Tm1 171.4(5) . . ?
C6 C6 C5 121.3(10) 3_776 . ?
C6 C6 H6A 119.4 3_776 . ?
C5 C6 H6A 119.4 . . ?
C1 O2 Tm1 136.0(4) . 3_666 ?
Tm1 O2W H2wA 120.1 . . ?
Tm1 O2W H2wB 119.9 . . ?
H2wA O2W H2wB 120.0 . . ?
Tm1 O1W H1WA 119.9 . . ?
Tm1 O1W H1WB 120.1 . . ?
H1WA O1W H1WB 120.0 . . ?
C4 O4 Tm1 164.9(5) . 4_575 ?
O4 C4 O3 122.4(6) . . ?
O4 C4 C3 120.7(6) . . ?
O3 C4 C3 116.8(5) . . ?
C4 O3 Tm1 122.0(4) . 2 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.10
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.390
_refine_diff_density_min         -1.914
_refine_diff_density_rms         0.264
