# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2017

####################################################################### 
# 
# 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_Compound6
_database_code_depnum_ccdc_archive 'CCDC 1534830'
_audit_update_record             
;
2017-05-11 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014


_chemical_name_systematic        
"[diaquatetraquis((2,6-dichlorophenyl)amino)phenyl)acetato-k2O,O')bis((mu-2,6-dichlorophenyl)amino)phenyl)acetato-k2O,O':kO)dimethanoldidysprosium(III)]"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C86 H72 Cl12 Dy2 N6 O16'
_chemical_formula_sum            'C86 H72 Cl12 Dy2 N6 O16'
_chemical_formula_weight         2195.89

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'
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.7378(5)
_cell_length_b                   33.4196(17)
_cell_length_c                   13.9653(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.6090(10)
_cell_angle_gamma                90
_cell_volume                     4377.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    105775
_cell_measurement_theta_min      2.255
_cell_measurement_theta_max      28.816

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.666
_exptl_crystal_F_000             2188
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    2.130
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7023
_exptl_absorpt_correction_T_max  0.8156
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            105775
_diffrn_reflns_av_unetI/netI     0.1366
_diffrn_reflns_av_R_equivalents  0.1950
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.255
_diffrn_reflns_theta_max         28.816
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11357
_reflns_number_gt                7377
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+13.2093P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11357
_refine_ls_number_parameters     551
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1351
_refine_ls_R_factor_gt           0.0655
_refine_ls_wR_factor_ref         0.0771
_refine_ls_wR_factor_gt          0.0656
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Dy1 Dy 0.30701(2) 0.00467(2) 0.02860(2) 0.00771(6) Uani 1 1 d . . . . .
Cl2A Cl 0.23172(15) 0.20288(4) 0.37576(10) 0.0256(3) Uani 1 1 d . . . . .
Cl2C Cl 0.15588(16) -0.11294(4) 0.18303(10) 0.0284(3) Uani 1 1 d . . . . .
Cl1B Cl -0.09600(15) 0.11530(4) -0.49261(10) 0.0268(3) Uani 1 1 d . . . . .
Cl2B Cl 0.36094(16) 0.14579(5) -0.18143(11) 0.0387(4) Uani 1 1 d . . . . .
Cl1C Cl 0.39615(16) -0.24037(4) 0.05020(11) 0.0328(4) Uani 1 1 d . . . . .
Cl1A Cl 0.54383(17) 0.06898(5) 0.37371(13) 0.0422(4) Uani 1 1 d . . . . .
C10A C 0.4958(6) 0.10909(17) 0.4354(4) 0.0281(14) Uani 1 1 d . . . . .
C9C C 0.2709(5) -0.17820(14) 0.1202(4) 0.0133(11) Uani 1 1 d . . . . .
C3B C 0.1362(5) 0.02237(14) -0.3604(3) 0.0130(11) Uani 1 1 d . . . . .
N1C N 0.3115(4) -0.15294(11) 0.0528(3) 0.0130(9) Uani 1 1 d . . . . .
H1C H 0.3749 -0.1341 0.0755 0.016 Uiso 1 1 calc R U . . .
N1B N 0.1438(4) 0.09251(11) -0.3140(3) 0.0188(10) Uani 1 1 d . . . . .
H1B H 0.1356 0.0856 -0.2550 0.023 Uiso 1 1 calc R U . . .
N1A N 0.3193(4) 0.12754(12) 0.2826(3) 0.0154(9) Uani 1 1 d . . . . .
H1A H 0.2742 0.1045 0.2699 0.018 Uiso 1 1 calc R U . . .
C4A C 0.2098(6) 0.17021(15) 0.0303(4) 0.0212(12) Uani 1 1 d . . . . .
H4A H 0.1425 0.1652 -0.0317 0.025 Uiso 1 1 calc R U . . .
C14C C 0.2000(5) -0.16340(14) 0.1870(4) 0.0150(11) Uani 1 1 d . . . . .
C7C C 0.1362(5) -0.18199(13) -0.0899(4) 0.0142(11) Uani 1 1 d . . . . .
H7C H 0.1003 -0.1982 -0.0462 0.017 Uiso 1 1 calc R U . . .
C9B C 0.1345(5) 0.13298(15) -0.3396(4) 0.0161(11) Uani 1 1 d . . . . .
C4B C 0.1625(5) -0.00734(15) -0.4220(3) 0.0185(11) Uani 1 1 d . . . . .
H4B H 0.1441 -0.0344 -0.4088 0.022 Uiso 1 1 calc R U . . .
C8B C 0.1660(5) 0.06193(14) -0.3796(3) 0.0133(11) Uani 1 1 d . . . . .
C6B C 0.2403(5) 0.04086(15) -0.5222(4) 0.0194(12) Uani 1 1 d . . . . .
H6B H 0.2723 0.0472 -0.5789 0.023 Uiso 1 1 calc R U . . .
C7B C 0.2195(5) 0.07125(15) -0.4604(4) 0.0184(12) Uani 1 1 d . . . . .
H7B H 0.2414 0.0982 -0.4726 0.022 Uiso 1 1 calc R U . . .
C5C C 0.1239(6) -0.15991(15) -0.2543(4) 0.0229(13) Uani 1 1 d . . . . .
H5C H 0.0782 -0.1601 -0.3236 0.027 Uiso 1 1 calc R U . . .
C3A C 0.2108(5) 0.14583(14) 0.1113(4) 0.0145(11) Uani 1 1 d . . . . .
C8A C 0.3123(5) 0.15357(14) 0.2018(4) 0.0144(11) Uani 1 1 d . . . . .
C8C C 0.2525(5) -0.15712(13) -0.0520(3) 0.0116(10) Uani 1 1 d . . . . .
C6C C 0.0729(5) -0.18315(15) -0.1905(4) 0.0190(12) Uani 1 1 d . . . . .
H6C H -0.0067 -0.2002 -0.2160 0.023 Uiso 1 1 calc R U . . .
C6A C 0.4025(6) 0.20941(15) 0.1284(4) 0.0231(13) Uani 1 1 d . . . . .
H6A H 0.4670 0.2312 0.1340 0.028 Uiso 1 1 calc R U . . .
C14B C 0.2245(6) 0.16183(16) -0.2821(4) 0.0238(13) Uani 1 1 d . . . . .
C12C C 0.1998(6) -0.22705(16) 0.2628(4) 0.0295(14) Uani 1 1 d . . . . .
H12C H 0.1758 -0.2436 0.3113 0.035 Uiso 1 1 calc R U . . .
C5B C 0.2153(5) 0.00146(16) -0.5028(3) 0.0205(11) Uani 1 1 d . . . . .
H5B H 0.2338 -0.0193 -0.5440 0.025 Uiso 1 1 calc R U . . .
C9A C 0.3923(5) 0.13570(15) 0.3808(4) 0.0160(11) Uani 1 1 d . . . . .
C7A C 0.4065(5) 0.18573(14) 0.2098(4) 0.0166(11) Uani 1 1 d . . . . .
H7A H 0.4735 0.1913 0.2716 0.020 Uiso 1 1 calc R U . . .
C61 C 0.3601(5) 0.16852(15) 0.4343(4) 0.0178(12) Uani 1 1 d . . . . .
C13A C 0.4257(6) 0.17390(18) 0.5339(4) 0.0313(15) Uani 1 1 d . . . . .
H13A H 0.4039 0.1968 0.5672 0.038 Uiso 1 1 calc R U . . .
C3C C 0.3102(5) -0.13428(13) -0.1155(3) 0.0118(11) Uani 1 1 d . . . . .
C13B C 0.2112(6) 0.20246(16) -0.3029(5) 0.0330(15) Uani 1 1 d . . . . .
H13B H 0.2720 0.2212 -0.2608 0.040 Uiso 1 1 calc R U . . .
C12A C 0.5226(7) 0.1463(2) 0.5855(5) 0.0423(18) Uani 1 1 d . . . . .
H12A H 0.5645 0.1496 0.6548 0.051 Uiso 1 1 calc R U . . .
C10C C 0.3049(6) -0.21894(15) 0.1284(4) 0.0208(12) Uani 1 1 d . . . . .
C10B C 0.0298(6) 0.14781(15) -0.4219(4) 0.0207(12) Uani 1 1 d . . . . .
C12B C 0.1083(7) 0.21509(17) -0.3858(5) 0.0323(15) Uani 1 1 d . . . . .
H12B H 0.1001 0.2427 -0.4020 0.039 Uiso 1 1 calc R U . . .
C13C C 0.1657(6) -0.18688(15) 0.2579(4) 0.0257(13) Uani 1 1 d . . . . .
H13C H 0.1191 -0.1756 0.3032 0.031 Uiso 1 1 calc R U . . .
C4C C 0.2429(6) -0.13610(14) -0.2165(4) 0.0201(12) Uani 1 1 d . . . . .
H4C H 0.2794 -0.1206 -0.2611 0.024 Uiso 1 1 calc R U . . .
C11A C 0.5584(6) 0.1141(2) 0.5362(4) 0.0383(17) Uani 1 1 d . . . . .
H11A H 0.6263 0.0952 0.5713 0.046 Uiso 1 1 calc R U . . .
C11B C 0.0175(6) 0.18816(16) -0.4453(4) 0.0254(13) Uani 1 1 d . . . . .
H11B H -0.0534 0.1972 -0.5022 0.031 Uiso 1 1 calc R U . . .
O1C O 0.3096(4) -0.06809(8) 0.0127(2) 0.0149(8) Uani 1 1 d . . . . .
O2A O 0.2790(3) 0.05762(9) 0.1410(2) 0.0164(8) Uani 1 1 d . . . . .
O2B O 0.2791(3) 0.02431(10) -0.1476(2) 0.0174(8) Uani 1 1 d . . . . .
C1B C 0.1598(5) 0.00683(14) -0.1763(3) 0.0122(10) Uani 1 1 d . . . . .
C1A C 0.1761(5) 0.07304(14) 0.0769(4) 0.0145(11) Uani 1 1 d . . . . .
C1C C 0.4084(5) -0.06965(13) -0.0283(3) 0.0103(10) Uani 1 1 d . . . . .
C2B C 0.0643(5) 0.01193(15) -0.2809(3) 0.0163(11) Uani 1 1 d . . . . .
H2B1 H 0.0107 -0.0133 -0.3004 0.020 Uiso 1 1 calc R U . . .
H2B2 H -0.0061 0.0331 -0.2796 0.020 Uiso 1 1 calc R U . . .
C2C C 0.4382(5) -0.10787(13) -0.0769(4) 0.0133(11) Uani 1 1 d . . . . .
H2C1 H 0.4782 -0.1009 -0.1328 0.016 Uiso 1 1 calc R U . . .
H2C2 H 0.5118 -0.1232 -0.0279 0.016 Uiso 1 1 calc R U . . .
C2A C 0.1084(5) 0.11124(14) 0.1003(4) 0.0192(12) Uani 1 1 d . . . . .
H2A1 H 0.0215 0.1170 0.0462 0.023 Uiso 1 1 calc R U . . .
H2A2 H 0.0799 0.1078 0.1627 0.023 Uiso 1 1 calc R U . . .
C5A C 0.3044(7) 0.20151(14) 0.0382(4) 0.0263(13) Uani 1 1 d . . . . .
H5A H 0.3023 0.2177 -0.0182 0.032 Uiso 1 1 calc R U . . .
C11C C 0.2684(6) -0.24327(16) 0.1975(4) 0.0270(14) Uani 1 1 d . . . . .
H11C H 0.2904 -0.2710 0.2001 0.032 Uiso 1 1 calc R U . . .
O1M O 0.4655(3) -0.01518(9) 0.1822(2) 0.0149(8) Uani 1 1 d . . . . .
O2C O 0.4829(3) -0.03850(9) -0.0317(2) 0.0113(7) Uani 1 1 d . . . . .
O1W O 0.1332(3) -0.02095(9) 0.1020(2) 0.0119(7) Uani 1 1 d . . . . .
O1B O 0.1141(3) -0.01466(9) -0.1166(2) 0.0128(8) Uani 1 1 d . . . . .
O1A O 0.1310(4) 0.05731(9) -0.0078(2) 0.0173(8) Uani 1 1 d . . . . .
C1M C 0.4442(6) -0.03356(18) 0.2687(4) 0.0317(14) Uani 1 1 d . . . . .
H1M1 H 0.3499 -0.0263 0.2757 0.048 Uiso 1 1 calc R U . . .
H1M2 H 0.5177 -0.0244 0.3273 0.048 Uiso 1 1 calc R U . . .
H1M3 H 0.4504 -0.0627 0.2630 0.048 Uiso 1 1 calc R U . . .
H1M H 0.5552 -0.0168 0.1836 0.048 Uiso 1 1 d . U . . .
H1WA H 0.0825 -0.0027 0.1185 0.048 Uiso 1 1 d . U . . .
H1WB H 0.0673 -0.0363 0.0700 0.048 Uiso 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Dy1 O2C 2.328(3) 3_655 ?
Dy1 O1W 2.362(3) . ?
Dy1 O1M 2.375(3) . ?
Dy1 O1A 2.413(3) . ?
Dy1 O2A 2.429(3) . ?
Dy1 O1C 2.443(3) . ?
Dy1 O1B 2.451(3) . ?
Dy1 O2B 2.490(3) . ?
Dy1 O2C 2.549(3) . ?
Dy1 C1A 2.786(5) . ?
Dy1 C1B 2.836(4) . ?
Dy1 C1C 2.863(4) . ?
Cl2A C61 1.732(5) . ?
Cl2C C14C 1.738(5) . ?
Cl1B C10B 1.734(5) . ?
Cl2B C14B 1.739(5) . ?
Cl1C C10C 1.737(5) . ?
Cl1A C10A 1.724(6) . ?
C10A C11A 1.385(8) . ?
C10A C9A 1.405(7) . ?
C9C C14C 1.393(6) . ?
C9C N1C 1.398(6) . ?
C9C C10C 1.399(7) . ?
C3B C4B 1.382(6) . ?
C3B C8B 1.395(6) . ?
C3B C2B 1.503(6) . ?
N1C C8C 1.428(6) . ?
N1C H1C 0.8800 . ?
N1B C9B 1.396(6) . ?
N1B C8B 1.427(6) . ?
N1B H1B 0.8800 . ?
N1A C9A 1.392(6) . ?
N1A C8A 1.411(6) . ?
N1A H1A 0.8800 . ?
C4A C5A 1.378(7) . ?
C4A C3A 1.392(7) . ?
C4A H4A 0.9500 . ?
C14C C13C 1.373(7) . ?
C7C C6C 1.374(7) . ?
C7C C8C 1.390(6) . ?
C7C H7C 0.9500 . ?
C9B C14B 1.402(7) . ?
C9B C10B 1.405(7) . ?
C4B C5B 1.392(6) . ?
C4B H4B 0.9500 . ?
C8B C7B 1.399(6) . ?
C6B C5B 1.379(7) . ?
C6B C7B 1.383(6) . ?
C6B H6B 0.9500 . ?
C7B H7B 0.9500 . ?
C5C C6C 1.372(7) . ?
C5C C4C 1.388(7) . ?
C5C H5C 0.9500 . ?
C3A C8A 1.403(7) . ?
C3A C2A 1.507(7) . ?
C8A C7A 1.398(6) . ?
C8C C3C 1.397(6) . ?
C6C H6C 0.9500 . ?
C6A C7A 1.377(7) . ?
C6A C5A 1.386(8) . ?
C6A H6A 0.9500 . ?
C14B C13B 1.387(7) . ?
C12C C11C 1.379(7) . ?
C12C C13C 1.380(7) . ?
C12C H12C 0.9500 . ?
C5B H5B 0.9500 . ?
C9A C61 1.409(7) . ?
C7A H7A 0.9500 . ?
C61 C13A 1.377(7) . ?
C13A C12A 1.376(8) . ?
C13A H13A 0.9500 . ?
C3C C4C 1.387(7) . ?
C3C C2C 1.504(6) . ?
C13B C12B 1.377(8) . ?
C13B H13B 0.9500 . ?
C12A C11A 1.373(9) . ?
C12A H12A 0.9500 . ?
C10C C11C 1.379(7) . ?
C10B C11B 1.385(7) . ?
C12B C11B 1.374(8) . ?
C12B H12B 0.9500 . ?
C13C H13C 0.9500 . ?
C4C H4C 0.9500 . ?
C11A H11A 0.9500 . ?
C11B H11B 0.9500 . ?
O1C C1C 1.247(5) . ?
O2A C1A 1.260(6) . ?
O2B C1B 1.265(5) . ?
C1B O1B 1.269(5) . ?
C1B C2B 1.516(6) . ?
C1A O1A 1.260(6) . ?
C1A C2A 1.512(6) . ?
C1C O2C 1.277(5) . ?
C1C C2C 1.511(6) . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C2C H2C1 0.9900 . ?
C2C H2C2 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
C5A H5A 0.9500 . ?
C11C H11C 0.9500 . ?
O1M C1M 1.420(5) . ?
O1M H1M 0.8694 . ?
O2C Dy1 2.328(3) 3_655 ?
O1W H1WA 0.8547 . ?
O1W H1WB 0.8480 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2C Dy1 O1W 153.73(10) 3_655 . ?
O2C Dy1 O1M 76.38(10) 3_655 . ?
O1W Dy1 O1M 82.79(10) . . ?
O2C Dy1 O1A 102.75(11) 3_655 . ?
O1W Dy1 O1A 78.72(11) . . ?
O1M Dy1 O1A 130.23(11) . . ?
O2C Dy1 O2A 83.42(10) 3_655 . ?
O1W Dy1 O2A 76.44(10) . . ?
O1M Dy1 O2A 77.21(11) . . ?
O1A Dy1 O2A 53.69(11) . . ?
O2C Dy1 O1C 117.06(11) 3_655 . ?
O1W Dy1 O1C 72.82(10) . . ?
O1M Dy1 O1C 77.52(11) . . ?
O1A Dy1 O1C 136.95(11) . . ?
O2A Dy1 O1C 142.15(10) . . ?
O2C Dy1 O1B 128.12(10) 3_655 . ?
O1W Dy1 O1B 77.54(10) . . ?
O1M Dy1 O1B 147.21(10) . . ?
O1A Dy1 O1B 71.05(10) . . ?
O2A Dy1 O1B 122.15(10) . . ?
O1C Dy1 O1B 71.75(11) . . ?
O2C Dy1 O2B 75.63(10) 3_655 . ?
O1W Dy1 O2B 128.60(11) . . ?
O1M Dy1 O2B 146.88(10) . . ?
O1A Dy1 O2B 73.59(11) . . ?
O2A Dy1 O2B 116.44(11) . . ?
O1C Dy1 O2B 100.01(11) . . ?
O1B Dy1 O2B 52.87(10) . . ?
O2C Dy1 O2C 67.40(11) 3_655 . ?
O1W Dy1 O2C 124.16(10) . . ?
O1M Dy1 O2C 78.98(10) . . ?
O1A Dy1 O2C 147.72(10) . . ?
O2A Dy1 O2C 145.88(10) . . ?
O1C Dy1 O2C 51.86(10) . . ?
O1B Dy1 O2C 90.64(10) . . ?
O2B Dy1 O2C 74.17(10) . . ?
O2C Dy1 C1A 93.11(12) 3_655 . ?
O1W Dy1 C1A 76.38(12) . . ?
O1M Dy1 C1A 103.82(13) . . ?
O1A Dy1 C1A 26.84(12) . . ?
O2A Dy1 C1A 26.85(12) . . ?
O1C Dy1 C1A 148.75(12) . . ?
O1B Dy1 C1A 96.77(13) . . ?
O2B Dy1 C1A 95.04(13) . . ?
O2C Dy1 C1A 159.35(11) . . ?
O2C Dy1 C1B 102.08(12) 3_655 . ?
O1W Dy1 C1B 102.74(12) . . ?
O1M Dy1 C1B 161.36(11) . . ?
O1A Dy1 C1B 68.39(11) . . ?
O2A Dy1 C1B 121.30(12) . . ?
O1C Dy1 C1B 87.04(12) . . ?
O1B Dy1 C1B 26.51(11) . . ?
O2B Dy1 C1B 26.47(11) . . ?
O2C Dy1 C1B 83.29(11) . . ?
C1A Dy1 C1B 94.80(14) . . ?
O2C Dy1 C1C 93.41(12) 3_655 . ?
O1W Dy1 C1C 98.44(12) . . ?
O1M Dy1 C1C 79.61(12) . . ?
O1A Dy1 C1C 148.49(12) . . ?
O2A Dy1 C1C 156.71(12) . . ?
O1C Dy1 C1C 25.64(11) . . ?
O1B Dy1 C1C 77.67(12) . . ?
O2B Dy1 C1C 84.74(12) . . ?
O2C Dy1 C1C 26.48(11) . . ?
C1A Dy1 C1C 173.21(14) . . ?
C1B Dy1 C1C 81.96(13) . . ?
C11A C10A C9A 122.0(6) . . ?
C11A C10A Cl1A 119.8(5) . . ?
C9A C10A Cl1A 118.2(4) . . ?
C14C C9C N1C 121.2(4) . . ?
C14C C9C C10C 116.1(4) . . ?
N1C C9C C10C 122.7(4) . . ?
C4B C3B C8B 118.6(4) . . ?
C4B C3B C2B 119.6(4) . . ?
C8B C3B C2B 121.6(4) . . ?
C9C N1C C8C 121.5(4) . . ?
C9C N1C H1C 119.3 . . ?
C8C N1C H1C 119.3 . . ?
C9B N1B C8B 122.7(4) . . ?
C9B N1B H1B 118.7 . . ?
C8B N1B H1B 118.7 . . ?
C9A N1A C8A 124.7(4) . . ?
C9A N1A H1A 117.7 . . ?
C8A N1A H1A 117.7 . . ?
C5A C4A C3A 121.4(5) . . ?
C5A C4A H4A 119.3 . . ?
C3A C4A H4A 119.3 . . ?
C13C C14C C9C 122.8(5) . . ?
C13C C14C Cl2C 118.1(4) . . ?
C9C C14C Cl2C 119.1(4) . . ?
C6C C7C C8C 120.1(4) . . ?
C6C C7C H7C 120.0 . . ?
C8C C7C H7C 120.0 . . ?
N1B C9B C14B 122.2(5) . . ?
N1B C9B C10B 122.3(5) . . ?
C14B C9B C10B 115.5(5) . . ?
C3B C4B C5B 121.6(5) . . ?
C3B C4B H4B 119.2 . . ?
C5B C4B H4B 119.2 . . ?
C3B C8B C7B 120.5(4) . . ?
C3B C8B N1B 118.7(4) . . ?
C7B C8B N1B 120.8(4) . . ?
C5B C6B C7B 121.0(5) . . ?
C5B C6B H6B 119.5 . . ?
C7B C6B H6B 119.5 . . ?
C6B C7B C8B 119.3(5) . . ?
C6B C7B H7B 120.4 . . ?
C8B C7B H7B 120.4 . . ?
C6C C5C C4C 119.3(5) . . ?
C6C C5C H5C 120.4 . . ?
C4C C5C H5C 120.4 . . ?
C4A C3A C8A 118.2(5) . . ?
C4A C3A C2A 120.4(5) . . ?
C8A C3A C2A 121.3(4) . . ?
C7A C8A C3A 120.1(5) . . ?
C7A C8A N1A 121.4(5) . . ?
C3A C8A N1A 118.5(4) . . ?
C7C C8C C3C 120.7(4) . . ?
C7C C8C N1C 120.7(4) . . ?
C3C C8C N1C 118.5(4) . . ?
C5C C6C C7C 120.5(5) . . ?
C5C C6C H6C 119.8 . . ?
C7C C6C H6C 119.8 . . ?
C7A C6A C5A 120.0(5) . . ?
C7A C6A H6A 120.0 . . ?
C5A C6A H6A 120.0 . . ?
C13B C14B C9B 123.0(5) . . ?
C13B C14B Cl2B 118.6(4) . . ?
C9B C14B Cl2B 118.4(4) . . ?
C11C C12C C13C 120.2(5) . . ?
C11C C12C H12C 119.9 . . ?
C13C C12C H12C 119.9 . . ?
C6B C5B C4B 119.0(5) . . ?
C6B C5B H5B 120.5 . . ?
C4B C5B H5B 120.5 . . ?
N1A C9A C10A 120.8(5) . . ?
N1A C9A C61 123.2(4) . . ?
C10A C9A C61 115.8(5) . . ?
C6A C7A C8A 120.3(5) . . ?
C6A C7A H7A 119.9 . . ?
C8A C7A H7A 119.9 . . ?
C13A C61 C9A 121.9(5) . . ?
C13A C61 Cl2A 118.0(4) . . ?
C9A C61 Cl2A 120.1(4) . . ?
C12A C13A C61 120.5(6) . . ?
C12A C13A H13A 119.8 . . ?
C61 C13A H13A 119.8 . . ?
C4C C3C C8C 117.4(4) . . ?
C4C C3C C2C 120.6(4) . . ?
C8C C3C C2C 121.9(4) . . ?
C12B C13B C14B 118.8(5) . . ?
C12B C13B H13B 120.6 . . ?
C14B C13B H13B 120.6 . . ?
C11A C12A C13A 119.6(6) . . ?
C11A C12A H12A 120.2 . . ?
C13A C12A H12A 120.2 . . ?
C11C C10C C9C 122.1(5) . . ?
C11C C10C Cl1C 117.9(4) . . ?
C9C C10C Cl1C 120.0(4) . . ?
C11B C10B C9B 122.3(5) . . ?
C11B C10B Cl1B 118.2(4) . . ?
C9B C10B Cl1B 119.4(4) . . ?
C11B C12B C13B 120.8(5) . . ?
C11B C12B H12B 119.6 . . ?
C13B C12B H12B 119.6 . . ?
C14C C13C C12C 119.3(5) . . ?
C14C C13C H13C 120.3 . . ?
C12C C13C H13C 120.3 . . ?
C3C C4C C5C 121.9(5) . . ?
C3C C4C H4C 119.0 . . ?
C5C C4C H4C 119.0 . . ?
C12A C11A C10A 120.2(6) . . ?
C12A C11A H11A 119.9 . . ?
C10A C11A H11A 119.9 . . ?
C12B C11B C10B 119.6(5) . . ?
C12B C11B H11B 120.2 . . ?
C10B C11B H11B 120.2 . . ?
C1C O1C Dy1 96.4(3) . . ?
C1A O2A Dy1 92.6(3) . . ?
C1B O2B Dy1 92.2(3) . . ?
O2B C1B O1B 120.5(4) . . ?
O2B C1B C2B 121.8(4) . . ?
O1B C1B C2B 117.7(4) . . ?
O2B C1B Dy1 61.3(2) . . ?
O1B C1B Dy1 59.6(2) . . ?
C2B C1B Dy1 171.1(3) . . ?
O2A C1A O1A 120.4(4) . . ?
O2A C1A C2A 120.1(5) . . ?
O1A C1A C2A 119.5(4) . . ?
O2A C1A Dy1 60.6(2) . . ?
O1A C1A Dy1 59.8(2) . . ?
C2A C1A Dy1 177.4(3) . . ?
O1C C1C O2C 120.0(4) . . ?
O1C C1C C2C 120.5(4) . . ?
O2C C1C C2C 119.6(4) . . ?
O1C C1C Dy1 58.0(2) . . ?
O2C C1C Dy1 62.9(2) . . ?
C2C C1C Dy1 168.7(3) . . ?
C3B C2B C1B 116.8(4) . . ?
C3B C2B H2B1 108.1 . . ?
C1B C2B H2B1 108.1 . . ?
C3B C2B H2B2 108.1 . . ?
C1B C2B H2B2 108.1 . . ?
H2B1 C2B H2B2 107.3 . . ?
C3C C2C C1C 114.6(4) . . ?
C3C C2C H2C1 108.6 . . ?
C1C C2C H2C1 108.6 . . ?
C3C C2C H2C2 108.6 . . ?
C1C C2C H2C2 108.6 . . ?
H2C1 C2C H2C2 107.6 . . ?
C3A C2A C1A 110.8(4) . . ?
C3A C2A H2A1 109.5 . . ?
C1A C2A H2A1 109.5 . . ?
C3A C2A H2A2 109.5 . . ?
C1A C2A H2A2 109.5 . . ?
H2A1 C2A H2A2 108.1 . . ?
C4A C5A C6A 120.0(5) . . ?
C4A C5A H5A 120.0 . . ?
C6A C5A H5A 120.0 . . ?
C12C C11C C10C 119.5(5) . . ?
C12C C11C H11C 120.2 . . ?
C10C C11C H11C 120.2 . . ?
C1M O1M Dy1 132.9(3) . . ?
C1M O1M H1M 109.2 . . ?
Dy1 O1M H1M 116.3 . . ?
C1C O2C Dy1 154.2(3) . 3_655 ?
C1C O2C Dy1 90.6(3) . . ?
Dy1 O2C Dy1 112.60(11) 3_655 . ?
Dy1 O1W H1WA 113.1 . . ?
Dy1 O1W H1WB 121.3 . . ?
H1WA O1W H1WB 99.3 . . ?
C1B O1B Dy1 93.9(3) . . ?
C1A O1A Dy1 93.3(3) . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?

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
O1W H1WA O1B 0.85 1.99 2.743(4) 145.7 3
O1W H1WB O1A 0.85 2.02 2.830(5) 159.7 3

_refine_diff_density_max         1.018
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.214

_shelxl_version_number           2014-3



# start Validation Reply Form
_vrf_RINTA01_Compound6           
;
PROBLEM: The value of Rint is greater than 0.18
RESPONSE: This value is slightly high owing to the quality
of singles crystals of the compound, which despite their well define
shape and morphology, do not show a very strong diffraction. Anyhow,
the quality of the measurement is high and most of parameters are 
comparable with those of the reamining isostructural specimens.
;
# end Validation Reply Form

_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Water and methanol'
_exptl_crystal_preparation       ', Magnetic properties,Luminescent'
####################################################################### 
# 
# 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_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1534829'
_audit_update_record             
;
2017-05-11 deposited with the CCDC.
2017-05-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014


_chemical_name_systematic        
"[diaquatetraquis((2,6-dichlorophenyl)amino)phenyl)acetato-k2O,O')bis((mu-2,6-dichlorophenyl)amino)phenyl)acetato-k2O,O':kO)dimethanoldipraseodymium(III)]"
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C86 H72 Cl12 N6 O16 Pr2'
_chemical_formula_sum            'C86 H72 Cl12 N6 O16 Pr2'
_chemical_formula_weight         2152.71

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'
Cl Cl 0.1484 0.1585 '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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.8700(4)
_cell_length_b                   33.5491(16)
_cell_length_c                   13.9418(6)
_cell_angle_alpha                90
_cell_angle_beta                 105.9068(12)
_cell_angle_gamma                90
_cell_volume                     4439.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    43628
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.73

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_F_000             2160
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.514
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6751
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            43628
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.230
_diffrn_reflns_theta_max         28.756
_diffrn_reflns_theta_full        26.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11416
_reflns_number_gt                10313
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0186P)²+4.2616P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11416
_refine_ls_number_parameters     552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0230
_refine_ls_wR_factor_ref         0.0519
_refine_ls_wR_factor_gt          0.0501
_refine_ls_goodness_of_fit_ref   1.061
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pr1 Pr 0.30697(2) 0.00498(2) 0.03160(2) 0.00815(3) Uani 1 1 d . . . . .
Cl2A Cl 0.23347(5) 0.20324(2) 0.37474(4) 0.02326(10) Uani 1 1 d . . . . .
Cl2C Cl 0.15887(6) -0.11314(2) 0.18401(4) 0.02527(10) Uani 1 1 d . . . . .
Cl1B Cl -0.09371(5) 0.11605(2) -0.49453(4) 0.02531(10) Uani 1 1 d . . . . .
Cl2B Cl 0.36239(6) 0.14521(2) -0.18385(4) 0.03658(13) Uani 1 1 d . . . . .
Cl1A Cl 0.54472(6) 0.07043(2) 0.37090(5) 0.03745(14) Uani 1 1 d . . . . .
C10A C 0.4968(2) 0.11053(7) 0.43348(16) 0.0253(4) Uani 1 1 d . . . . .
C9C C 0.27203(18) -0.17880(5) 0.12243(13) 0.0132(3) Uani 1 1 d . . . . .
N1C N 0.31221(15) -0.15411(4) 0.05393(11) 0.0137(3) Uani 1 1 d . . . . .
H1C H 0.3763 -0.1356 0.0757 0.016 Uiso 1 1 calc R U . . .
N1B N 0.14536(17) 0.09261(5) -0.31737(11) 0.0183(3) Uani 1 1 d . . . . .
H1B H 0.1363 0.0853 -0.2588 0.022 Uiso 1 1 calc R U . . .
N1A N 0.31862(16) 0.12852(4) 0.28086(11) 0.0162(3) Uani 1 1 d . . . . .
H1A H 0.2728 0.1058 0.2683 0.019 Uiso 1 1 calc R U . . .
C3B C 0.13818(18) 0.02299(6) -0.36566(13) 0.0153(3) Uani 1 1 d . . . . .
C6C C 0.13611(18) -0.18352(5) -0.08765(14) 0.0150(3) Uani 1 1 d . . . . .
H6C H 0.1023 -0.1998 -0.0435 0.018 Uiso 1 1 calc R U . . .
C7C C 0.25078(18) -0.15862(5) -0.05015(12) 0.0116(3) Uani 1 1 d . . . . .
C9B C 0.1364(2) 0.13301(6) -0.34186(14) 0.0181(4) Uani 1 1 d . . . . .
C2C C 0.30535(18) -0.13578(5) -0.11556(13) 0.0129(3) Uani 1 1 d . . . . .
C7B C 0.21998(19) 0.07224(6) -0.46451(13) 0.0180(4) Uani 1 1 d . . . . .
H7B H 0.2386 0.0992 -0.4772 0.022 Uiso 1 1 calc R U . . .
C4B C 0.16632(19) -0.00653(6) -0.42780(14) 0.0182(4) Uani 1 1 d . . . . .
H4B H 0.1485 -0.0336 -0.4154 0.022 Uiso 1 1 calc R U . . .
C14A C 0.3614(2) 0.16920(6) 0.43312(14) 0.0194(4) Uani 1 1 d . . . . .
C8A C 0.31286(19) 0.15456(5) 0.20005(13) 0.0144(3) Uani 1 1 d . . . . .
C14C C 0.20154(19) -0.16358(5) 0.18915(13) 0.0164(3) Uani 1 1 d . . . . .
C6A C 0.4055(2) 0.20939(6) 0.12540(15) 0.0232(4) Uani 1 1 d . . . . .
H6A H 0.4712 0.2305 0.1310 0.028 Uiso 1 1 calc R U . . .
C4A C 0.2105(2) 0.17155(6) 0.02789(14) 0.0209(4) Uani 1 1 d . . . . .
H4A H 0.1425 0.1668 -0.0340 0.025 Uiso 1 1 calc R U . . .
C10C C 0.3041(2) -0.21962(6) 0.13171(14) 0.0193(4) Uani 1 1 d . . . . .
C3C C 0.2374(2) -0.13757(5) -0.21726(14) 0.0191(4) Uani 1 1 d . . . . .
H3C H 0.2723 -0.1221 -0.2623 0.023 Uiso 1 1 calc R U . . .
C6B C 0.2438(2) 0.04223(6) -0.52652(14) 0.0197(4) Uani 1 1 d . . . . .
H6B H 0.2769 0.0488 -0.5824 0.024 Uiso 1 1 calc R U . . .
C5C C 0.0709(2) -0.18474(5) -0.18895(14) 0.0189(4) Uani 1 1 d . . . . .
H5C H -0.0081 -0.2017 -0.2139 0.023 Uiso 1 1 calc R U . . .
C7A C 0.4083(2) 0.18584(5) 0.20774(14) 0.0176(4) Uani 1 1 d . . . . .
H7A H 0.4756 0.1910 0.2697 0.021 Uiso 1 1 calc R U . . .
C9A C 0.39261(19) 0.13674(6) 0.37929(14) 0.0173(4) Uani 1 1 d . . . . .
C4C C 0.1201(2) -0.16144(6) -0.25414(14) 0.0217(4) Uani 1 1 d . . . . .
H4C H 0.0739 -0.1618 -0.3235 0.026 Uiso 1 1 calc R U . . .
C8B C 0.16857(18) 0.06267(5) -0.38346(13) 0.0151(3) Uani 1 1 d . . . . .
C14B C 0.2266(2) 0.16139(6) -0.28366(15) 0.0239(4) Uani 1 1 d . . . . .
C10B C 0.0317(2) 0.14824(6) -0.42309(14) 0.0196(4) Uani 1 1 d . . . . .
C11C C 0.2680(2) -0.24345(6) 0.20251(16) 0.0251(4) Uani 1 1 d . . . . .
H11C H 0.2894 -0.2711 0.2060 0.030 Uiso 1 1 calc R U . . .
C13C C 0.1671(2) -0.18671(6) 0.26114(15) 0.0243(4) Uani 1 1 d . . . . .
H13C H 0.1206 -0.1751 0.3057 0.029 Uiso 1 1 calc R U . . .
C3A C 0.21078(19) 0.14745(5) 0.10972(13) 0.0154(3) Uani 1 1 d . . . . .
C5A C 0.3068(2) 0.20214(6) 0.03484(15) 0.0247(4) Uani 1 1 d . . . . .
H5A H 0.3055 0.2180 -0.0218 0.030 Uiso 1 1 calc R U . . .
C12C C 0.2007(2) -0.22672(6) 0.26784(16) 0.0278(5) Uani 1 1 d . . . . .
H12C H 0.1777 -0.2428 0.3172 0.033 Uiso 1 1 calc R U . . .
C13B C 0.2136(2) 0.20194(7) -0.30377(18) 0.0314(5) Uani 1 1 d . . . . .
H13B H 0.2749 0.2203 -0.2611 0.038 Uiso 1 1 calc R U . . .
C12B C 0.1117(3) 0.21546(6) -0.38573(18) 0.0314(5) Uani 1 1 d . . . . .
H12B H 0.1040 0.2431 -0.4009 0.038 Uiso 1 1 calc R U . . .
C11B C 0.0203(2) 0.18864(6) -0.44604(16) 0.0258(4) Uani 1 1 d . . . . .
H11B H -0.0500 0.1978 -0.5029 0.031 Uiso 1 1 calc R U . . .
C5B C 0.2198(2) 0.00271(6) -0.50752(14) 0.0199(4) Uani 1 1 d . . . . .
H5B H 0.2396 -0.0178 -0.5485 0.024 Uiso 1 1 calc R U . . .
C1B C 0.16016(18) 0.00716(5) -0.18158(12) 0.0126(3) Uani 1 1 d . . . . .
C1A C 0.16944(18) 0.07507(5) 0.07866(13) 0.0146(3) Uani 1 1 d . . . . .
C11 C 0.40556(17) -0.07155(5) -0.02858(12) 0.0107(3) Uani 1 1 d . . . . .
C1C C 0.43373(18) -0.10972(5) -0.07798(13) 0.0138(3) Uani 1 1 d . . . . .
H1C1 H 0.4714 -0.1028 -0.1348 0.017 Uiso 1 1 calc R U . . .
H1C2 H 0.5071 -0.1251 -0.0295 0.017 Uiso 1 1 calc R U . . .
C2B C 0.06701(19) 0.01210(6) -0.28655(13) 0.0175(4) Uani 1 1 d . . . . .
H2B1 H 0.0152 -0.0132 -0.3066 0.021 Uiso 1 1 calc R U . . .
H2B2 H -0.0037 0.0329 -0.2857 0.021 Uiso 1 1 calc R U . . .
C2A C 0.10540(19) 0.11385(5) 0.09942(14) 0.0180(4) Uani 1 1 d . . . . .
H2A1 H 0.0762 0.1114 0.1617 0.022 Uiso 1 1 calc R U . . .
H2A2 H 0.0206 0.1198 0.0442 0.022 Uiso 1 1 calc R U . . .
O1B O 0.11556(13) -0.01442(4) -0.12186(9) 0.0132(2) Uani 1 1 d . . . . .
O1C O 0.31260(13) -0.07008(4) 0.01702(9) 0.0155(3) Uani 1 1 d . . . . .
O2C O 0.47804(12) -0.04030(3) -0.03447(9) 0.0125(2) Uani 1 1 d . . . . .
O2B O 0.27657(12) 0.02559(4) -0.15239(9) 0.0154(3) Uani 1 1 d . . . . .
O1A O 0.12271(13) 0.05826(4) -0.00566(9) 0.0161(3) Uani 1 1 d . . . . .
O2A O 0.27148(14) 0.05988(4) 0.14399(9) 0.0184(3) Uani 1 1 d . . . . .
O1W O 0.12636(12) -0.02207(4) 0.10694(9) 0.0136(2) Uani 1 1 d . . . . .
H1M H 0.5521 -0.0197 0.1896 0.016 Uiso 1 1 d . U . . .
H1WA H 0.0661 -0.0054 0.1223 0.020 Uiso 1 1 d . U . . .
H1WB H 0.0662 -0.0393 0.0707 0.020 Uiso 1 1 d . U . . .
Cl1C Cl 0.39433(6) -0.24133(2) 0.05432(4) 0.02949(11) Uani 1 1 d . . . . .
O1M O 0.47401(13) -0.01534(4) 0.19238(9) 0.0169(3) Uani 1 1 d . . . . .
C1M C 0.4520(2) -0.03550(7) 0.27717(15) 0.0278(5) Uani 1 1 d . . . . .
H1M1 H 0.3550 -0.0311 0.2799 0.042 Uiso 1 1 calc R U . . .
H1M2 H 0.5176 -0.0251 0.3380 0.042 Uiso 1 1 calc R U . . .
H1M3 H 0.4683 -0.0641 0.2717 0.042 Uiso 1 1 calc R U . . .
C13A C 0.4268(2) 0.17483(7) 0.53364(15) 0.0293(5) Uani 1 1 d . . . . .
H13A H 0.4046 0.1974 0.5675 0.035 Uiso 1 1 calc R U . . .
C11A C 0.5603(2) 0.11532(8) 0.53426(17) 0.0362(6) Uani 1 1 d . . . . .
H11A H 0.6285 0.0966 0.5690 0.043 Uiso 1 1 calc R U . . .
C12A C 0.5243(2) 0.14733(9) 0.58417(16) 0.0383(6) Uani 1 1 d . . . . .
H12A H 0.5668 0.1505 0.6537 0.046 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pr1 O2C 2.4213(11) 3_655 ?
Pr1 O1W 2.4760(11) . ?
Pr1 O1M 2.4863(12) . ?
Pr1 O1A 2.5009(12) . ?
Pr1 O2A 2.5042(12) . ?
Pr1 O1B 2.5207(12) . ?
Pr1 O1C 2.5281(12) . ?
Pr1 O2B 2.5935(12) . ?
Pr1 O2C 2.6192(12) . ?
Pr1 C1A 2.8794(17) . ?
Pr1 C1B 2.9288(17) . ?
Pr1 C11 2.9481(16) . ?
Cl2A C14A 1.732(2) . ?
Cl2C C14C 1.7406(18) . ?
Cl1B C10B 1.736(2) . ?
Cl2B C14B 1.733(2) . ?
Cl1A C10A 1.738(2) . ?
C10A C11A 1.382(3) . ?
C10A C9A 1.406(3) . ?
C9C N1C 1.401(2) . ?
C9C C14C 1.402(2) . ?
C9C C10C 1.403(2) . ?
N1C C7C 1.419(2) . ?
N1C H1C 0.8800 . ?
N1B C9B 1.394(2) . ?
N1B C8B 1.423(2) . ?
N1B H1B 0.8800 . ?
N1A C9A 1.394(2) . ?
N1A C8A 1.414(2) . ?
N1A H1A 0.8800 . ?
C3B C4B 1.393(3) . ?
C3B C8B 1.401(3) . ?
C3B C2B 1.506(2) . ?
C6C C5C 1.383(3) . ?
C6C C7C 1.389(2) . ?
C6C H6C 0.9500 . ?
C7C C2C 1.406(2) . ?
C9B C14B 1.401(3) . ?
C9B C10B 1.404(3) . ?
C2C C3C 1.394(3) . ?
C2C C1C 1.510(2) . ?
C7B C6B 1.389(3) . ?
C7B C8B 1.397(2) . ?
C7B H7B 0.9500 . ?
C4B C5B 1.390(3) . ?
C4B H4B 0.9500 . ?
C14A C13A 1.386(3) . ?
C14A C9A 1.404(3) . ?
C8A C7A 1.395(3) . ?
C8A C3A 1.401(3) . ?
C14C C13C 1.383(2) . ?
C6A C7A 1.387(3) . ?
C6A C5A 1.388(3) . ?
C6A H6A 0.9500 . ?
C4A C5A 1.384(3) . ?
C4A C3A 1.398(3) . ?
C4A H4A 0.9500 . ?
C10C C11C 1.390(3) . ?
C10C Cl1C 1.7363(19) . ?
C3C C4C 1.386(3) . ?
C3C H3C 0.9500 . ?
C6B C5B 1.385(3) . ?
C6B H6B 0.9500 . ?
C5C C4C 1.384(3) . ?
C5C H5C 0.9500 . ?
C7A H7A 0.9500 . ?
C4C H4C 0.9500 . ?
C14B C13B 1.388(3) . ?
C10B C11B 1.390(3) . ?
C11C C12C 1.385(3) . ?
C11C H11C 0.9500 . ?
C13C C12C 1.380(3) . ?
C13C H13C 0.9500 . ?
C3A C2A 1.514(3) . ?
C5A H5A 0.9500 . ?
C12C H12C 0.9500 . ?
C13B C12B 1.376(3) . ?
C13B H13B 0.9500 . ?
C12B C11B 1.384(3) . ?
C12B H12B 0.9500 . ?
C11B H11B 0.9500 . ?
C5B H5B 0.9500 . ?
C1B O2B 1.269(2) . ?
C1B O1B 1.270(2) . ?
C1B C2B 1.509(2) . ?
C1A O2A 1.265(2) . ?
C1A O1A 1.271(2) . ?
C1A C2A 1.509(2) . ?
C11 O1C 1.252(2) . ?
C11 O2C 1.2845(19) . ?
C11 C1C 1.515(2) . ?
C1C H1C1 0.9900 . ?
C1C H1C2 0.9900 . ?
C2B H2B1 0.9900 . ?
C2B H2B2 0.9900 . ?
C2A H2A1 0.9900 . ?
C2A H2A2 0.9900 . ?
O2C Pr1 2.4214(11) 3_655 ?
O1W H1WA 0.8846 . ?
O1W H1WB 0.8805 . ?
O1M C1M 1.429(2) . ?
O1M H1M 0.7955 . ?
C1M H1M1 0.9800 . ?
C1M H1M2 0.9800 . ?
C1M H1M3 0.9800 . ?
C13A C12A 1.379(3) . ?
C13A H13A 0.9500 . ?
C11A C12A 1.378(4) . ?
C11A H11A 0.9500 . ?
C12A H12A 0.9500 . ?

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
O2C Pr1 O1W 154.42(4) 3_655 . ?
O2C Pr1 O1M 75.98(4) 3_655 . ?
O1W Pr1 O1M 83.90(4) . . ?
O2C Pr1 O1A 103.75(4) 3_655 . ?
O1W Pr1 O1A 77.47(4) . . ?
O1M Pr1 O1A 130.39(4) . . ?
O2C Pr1 O2A 84.37(4) 3_655 . ?
O1W Pr1 O2A 76.33(4) . . ?
O1M Pr1 O2A 79.02(4) . . ?
O1A Pr1 O2A 52.11(4) . . ?
O2C Pr1 O1B 126.15(4) 3_655 . ?
O1W Pr1 O1B 78.83(4) . . ?
O1M Pr1 O1B 148.43(4) . . ?
O1A Pr1 O1B 71.04(4) . . ?
O2A Pr1 O1B 121.34(4) . . ?
O2C Pr1 O1C 116.77(4) 3_655 . ?
O1W Pr1 O1C 72.74(4) . . ?
O1M Pr1 O1C 77.04(4) . . ?
O1A Pr1 O1C 136.55(4) . . ?
O2A Pr1 O1C 142.45(4) . . ?
O1B Pr1 O1C 72.69(4) . . ?
O2C Pr1 O2B 75.47(4) 3_655 . ?
O1W Pr1 O2B 128.00(4) . . ?
O1M Pr1 O2B 146.42(4) . . ?
O1A Pr1 O2B 73.95(4) . . ?
O2A Pr1 O2B 115.13(4) . . ?
O1B Pr1 O2B 51.15(4) . . ?
O1C Pr1 O2B 100.67(4) . . ?
O2C Pr1 O2C 69.09(4) 3_655 . ?
O1W Pr1 O2C 123.03(4) . . ?
O1M Pr1 O2C 79.97(4) . . ?
O1A Pr1 O2C 147.54(4) . . ?
O2A Pr1 O2C 149.41(4) . . ?
O1B Pr1 O2C 87.55(4) . . ?
O1C Pr1 O2C 50.47(4) . . ?
O2B Pr1 O2C 73.61(4) . . ?
O2C Pr1 C1A 93.57(4) 3_655 . ?
O1W Pr1 C1A 76.32(4) . . ?
O1M Pr1 C1A 104.83(5) . . ?
O1A Pr1 C1A 26.13(5) . . ?
O2A Pr1 C1A 26.01(5) . . ?
O1B Pr1 C1A 96.53(4) . . ?
O1C Pr1 C1A 148.64(4) . . ?
O2B Pr1 C1A 94.22(5) . . ?
O2C Pr1 C1A 160.64(4) . . ?
O2C Pr1 C1B 101.07(4) 3_655 . ?
O1W Pr1 C1B 103.07(4) . . ?
O1M Pr1 C1B 160.59(4) . . ?
O1A Pr1 C1B 69.02(4) . . ?
O2A Pr1 C1B 120.09(4) . . ?
O1B Pr1 C1B 25.56(4) . . ?
O1C Pr1 C1B 87.65(4) . . ?
O2B Pr1 C1B 25.67(4) . . ?
O2C Pr1 C1B 81.08(4) . . ?
C1A Pr1 C1B 94.46(5) . . ?
O2C Pr1 C11 94.29(4) 3_655 . ?
O1W Pr1 C11 97.68(4) . . ?
O1M Pr1 C11 80.14(4) . . ?
O1A Pr1 C11 147.28(4) . . ?
O2A Pr1 C11 158.80(4) . . ?
O1B Pr1 C11 76.27(4) . . ?
O1C Pr1 C11 24.96(4) . . ?
O2B Pr1 C11 84.75(4) . . ?
O2C Pr1 C11 25.82(4) . . ?
C1A Pr1 C11 171.54(5) . . ?
C1B Pr1 C11 80.97(4) . . ?
C11A C10A C9A 122.3(2) . . ?
C11A C10A Cl1A 119.37(17) . . ?
C9A C10A Cl1A 118.31(16) . . ?
N1C C9C C14C 121.43(16) . . ?
N1C C9C C10C 122.75(16) . . ?
C14C C9C C10C 115.77(16) . . ?
C9C N1C C7C 120.83(14) . . ?
C9C N1C H1C 119.6 . . ?
C7C N1C H1C 119.6 . . ?
C9B N1B C8B 122.55(15) . . ?
C9B N1B H1B 118.7 . . ?
C8B N1B H1B 118.7 . . ?
C9A N1A C8A 123.89(15) . . ?
C9A N1A H1A 118.1 . . ?
C8A N1A H1A 118.1 . . ?
C4B C3B C8B 118.45(16) . . ?
C4B C3B C2B 119.69(17) . . ?
C8B C3B C2B 121.71(16) . . ?
C5C C6C C7C 120.38(17) . . ?
C5C C6C H6C 119.8 . . ?
C7C C6C H6C 119.8 . . ?
C6C C7C C2C 120.07(16) . . ?
C6C C7C N1C 121.66(15) . . ?
C2C C7C N1C 118.21(15) . . ?
N1B C9B C14B 122.08(18) . . ?
N1B C9B C10B 122.32(17) . . ?
C14B C9B C10B 115.51(18) . . ?
C3C C2C C7C 118.24(16) . . ?
C3C C2C C1C 120.12(15) . . ?
C7C C2C C1C 121.63(15) . . ?
C6B C7B C8B 119.86(18) . . ?
C6B C7B H7B 120.1 . . ?
C8B C7B H7B 120.1 . . ?
C5B C4B C3B 121.52(18) . . ?
C5B C4B H4B 119.2 . . ?
C3B C4B H4B 119.2 . . ?
C13A C14A C9A 122.5(2) . . ?
C13A C14A Cl2A 117.56(17) . . ?
C9A C14A Cl2A 119.93(14) . . ?
C7A C8A C3A 120.09(17) . . ?
C7A C8A N1A 121.65(16) . . ?
C3A C8A N1A 118.23(16) . . ?
C13C C14C C9C 122.86(17) . . ?
C13C C14C Cl2C 118.08(15) . . ?
C9C C14C Cl2C 119.04(13) . . ?
C7A C6A C5A 120.19(18) . . ?
C7A C6A H6A 119.9 . . ?
C5A C6A H6A 119.9 . . ?
C5A C4A C3A 121.60(18) . . ?
C5A C4A H4A 119.2 . . ?
C3A C4A H4A 119.2 . . ?
C11C C10C C9C 122.10(17) . . ?
C11C C10C Cl1C 118.36(15) . . ?
C9C C10C Cl1C 119.54(14) . . ?
C4C C3C C2C 121.50(17) . . ?
C4C C3C H3C 119.2 . . ?
C2C C3C H3C 119.2 . . ?
C5B C6B C7B 120.53(17) . . ?
C5B C6B H6B 119.7 . . ?
C7B C6B H6B 119.7 . . ?
C6C C5C C4C 120.32(17) . . ?
C6C C5C H5C 119.8 . . ?
C4C C5C H5C 119.8 . . ?
C6A C7A C8A 120.32(18) . . ?
C6A C7A H7A 119.8 . . ?
C8A C7A H7A 119.8 . . ?
N1A C9A C14A 123.19(17) . . ?
N1A C9A C10A 120.92(18) . . ?
C14A C9A C10A 115.69(18) . . ?
C5C C4C C3C 119.40(17) . . ?
C5C C4C H4C 120.3 . . ?
C3C C4C H4C 120.3 . . ?
C7B C8B C3B 120.28(17) . . ?
C7B C8B N1B 121.33(17) . . ?
C3B C8B N1B 118.39(16) . . ?
C13B C14B C9B 122.7(2) . . ?
C13B C14B Cl2B 118.53(17) . . ?
C9B C14B Cl2B 118.76(16) . . ?
C11B C10B C9B 122.40(19) . . ?
C11B C10B Cl1B 118.33(16) . . ?
C9B C10B Cl1B 119.20(15) . . ?
C12C C11C C10C 119.76(18) . . ?
C12C C11C H11C 120.1 . . ?
C10C C11C H11C 120.1 . . ?
C12C C13C C14C 119.53(18) . . ?
C12C C13C H13C 120.2 . . ?
C14C C13C H13C 120.2 . . ?
C4A C3A C8A 118.39(17) . . ?
C4A C3A C2A 120.37(17) . . ?
C8A C3A C2A 121.21(16) . . ?
C4A C5A C6A 119.38(18) . . ?
C4A C5A H5A 120.3 . . ?
C6A C5A H5A 120.3 . . ?
C13C C12C C11C 119.97(18) . . ?
C13C C12C H12C 120.0 . . ?
C11C C12C H12C 120.0 . . ?
C12B C13B C14B 119.8(2) . . ?
C12B C13B H13B 120.1 . . ?
C14B C13B H13B 120.1 . . ?
C13B C12B C11B 119.8(2) . . ?
C13B C12B H12B 120.1 . . ?
C11B C12B H12B 120.1 . . ?
C12B C11B C10B 119.7(2) . . ?
C12B C11B H11B 120.1 . . ?
C10B C11B H11B 120.1 . . ?
C6B C5B C4B 119.27(17) . . ?
C6B C5B H5B 120.4 . . ?
C4B C5B H5B 120.4 . . ?
O2B C1B O1B 120.89(15) . . ?
O2B C1B C2B 120.98(15) . . ?
O1B C1B C2B 118.03(15) . . ?
O2B C1B Pr1 62.25(9) . . ?
O1B C1B Pr1 58.95(9) . . ?
C2B C1B Pr1 170.91(12) . . ?
O2A C1A O1A 120.17(16) . . ?
O2A C1A C2A 120.13(16) . . ?
O1A C1A C2A 119.68(16) . . ?
O2A C1A Pr1 60.21(9) . . ?
O1A C1A Pr1 60.07(9) . . ?
C2A C1A Pr1 175.14(12) . . ?
O1C C11 O2C 119.90(15) . . ?
O1C C11 C1C 121.03(14) . . ?
O2C C11 C1C 119.07(14) . . ?
O1C C11 Pr1 58.41(8) . . ?
O2C C11 Pr1 62.64(8) . . ?
C1C C11 Pr1 168.90(12) . . ?
C2C C1C C11 113.95(14) . . ?
C2C C1C H1C1 108.8 . . ?
C11 C1C H1C1 108.8 . . ?
C2C C1C H1C2 108.8 . . ?
C11 C1C H1C2 108.8 . . ?
H1C1 C1C H1C2 107.7 . . ?
C3B C2B C1B 117.03(15) . . ?
C3B C2B H2B1 108.0 . . ?
C1B C2B H2B1 108.0 . . ?
C3B C2B H2B2 108.0 . . ?
C1B C2B H2B2 108.0 . . ?
H2B1 C2B H2B2 107.3 . . ?
C1A C2A C3A 110.32(14) . . ?
C1A C2A H2A1 109.6 . . ?
C3A C2A H2A1 109.6 . . ?
C1A C2A H2A2 109.6 . . ?
C3A C2A H2A2 109.6 . . ?
H2A1 C2A H2A2 108.1 . . ?
C1B O1B Pr1 95.48(10) . . ?
C11 O1C Pr1 96.64(10) . . ?
C11 O2C Pr1 154.08(11) . 3_655 ?
C11 O2C Pr1 91.54(9) . . ?
Pr1 O2C Pr1 110.90(4) 3_655 . ?
C1B O2B Pr1 92.09(10) . . ?
C1A O1A Pr1 93.79(10) . . ?
C1A O2A Pr1 93.79(10) . . ?
Pr1 O1W H1WA 118.8 . . ?
Pr1 O1W H1WB 116.5 . . ?
H1WA O1W H1WB 99.3 . . ?
C1M O1M Pr1 131.45(11) . . ?
C1M O1M H1M 108.8 . . ?
Pr1 O1M H1M 114.7 . . ?
O1M C1M H1M1 109.5 . . ?
O1M C1M H1M2 109.5 . . ?
H1M1 C1M H1M2 109.5 . . ?
O1M C1M H1M3 109.5 . . ?
H1M1 C1M H1M3 109.5 . . ?
H1M2 C1M H1M3 109.5 . . ?
C12A C13A C14A 119.4(2) . . ?
C12A C13A H13A 120.3 . . ?
C14A C13A H13A 120.3 . . ?
C12A C11A C10A 119.7(2) . . ?
C12A C11A H11A 120.1 . . ?
C10A C11A H11A 120.1 . . ?
C11A C12A C13A 120.3(2) . . ?
C11A C12A H12A 119.9 . . ?
C13A C12A H12A 119.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14C C9C N1C C7C -114.12(19) . . . . ?
C10C C9C N1C C7C 68.5(2) . . . . ?
C5C C6C C7C C2C -2.9(3) . . . . ?
C5C C6C C7C N1C 174.44(16) . . . . ?
C9C N1C C7C C6C 9.0(2) . . . . ?
C9C N1C C7C C2C -173.62(15) . . . . ?
C8B N1B C9B C14B -122.1(2) . . . . ?
C8B N1B C9B C10B 61.5(2) . . . . ?
C6C C7C C2C C3C 2.9(2) . . . . ?
N1C C7C C2C C3C -174.50(15) . . . . ?
C6C C7C C2C C1C -177.32(15) . . . . ?
N1C C7C C2C C1C 5.3(2) . . . . ?
C8B C3B C4B C5B -1.7(3) . . . . ?
C2B C3B C4B C5B 173.95(17) . . . . ?
C9A N1A C8A C7A 16.4(3) . . . . ?
C9A N1A C8A C3A -165.65(16) . . . . ?
N1C C9C C14C C13C -176.47(18) . . . . ?
C10C C9C C14C C13C 1.1(3) . . . . ?
N1C C9C C14C Cl2C 1.8(2) . . . . ?
C10C C9C C14C Cl2C 179.40(14) . . . . ?
N1C C9C C10C C11C 177.61(18) . . . . ?
C14C C9C C10C C11C 0.1(3) . . . . ?
N1C C9C C10C Cl1C -1.2(3) . . . . ?
C14C C9C C10C Cl1C -178.76(14) . . . . ?
C7C C2C C3C C4C -0.8(3) . . . . ?
C1C C2C C3C C4C 179.46(17) . . . . ?
C8B C7B C6B C5B -1.3(3) . . . . ?
C7C C6C C5C C4C 0.6(3) . . . . ?
C5A C6A C7A C8A 0.4(3) . . . . ?
C3A C8A C7A C6A -1.8(3) . . . . ?
N1A C8A C7A C6A 176.05(17) . . . . ?
C8A N1A C9A C14A 62.1(2) . . . . ?
C8A N1A C9A C10A -123.38(19) . . . . ?
C13A C14A C9A N1A 173.65(18) . . . . ?
Cl2A C14A C9A N1A -4.5(2) . . . . ?
C13A C14A C9A C10A -1.2(3) . . . . ?
Cl2A C14A C9A C10A -179.29(14) . . . . ?
C11A C10A C9A N1A -172.24(18) . . . . ?
Cl1A C10A C9A N1A 6.9(2) . . . . ?
C11A C10A C9A C14A 2.7(3) . . . . ?
Cl1A C10A C9A C14A -178.16(14) . . . . ?
C6C C5C C4C C3C 1.5(3) . . . . ?
C2C C3C C4C C5C -1.4(3) . . . . ?
C6B C7B C8B C3B -1.3(3) . . . . ?
C6B C7B C8B N1B 178.86(17) . . . . ?
C4B C3B C8B C7B 2.8(3) . . . . ?
C2B C3B C8B C7B -172.75(16) . . . . ?
C4B C3B C8B N1B -177.39(16) . . . . ?
C2B C3B C8B N1B 7.1(2) . . . . ?
C9B N1B C8B C7B 17.0(3) . . . . ?
C9B N1B C8B C3B -162.78(17) . . . . ?
N1B C9B C14B C13B -176.08(18) . . . . ?
C10B C9B C14B C13B 0.5(3) . . . . ?
N1B C9B C14B Cl2B 5.2(2) . . . . ?
C10B C9B C14B Cl2B -178.16(14) . . . . ?
N1B C9B C10B C11B 178.26(17) . . . . ?
C14B C9B C10B C11B 1.6(3) . . . . ?
N1B C9B C10B Cl1B 1.3(2) . . . . ?
C14B C9B C10B Cl1B -175.28(14) . . . . ?
C9C C10C C11C C12C -1.3(3) . . . . ?
Cl1C C10C C11C C12C 177.58(17) . . . . ?
C9C C14C C13C C12C -1.0(3) . . . . ?
Cl2C C14C C13C C12C -179.38(17) . . . . ?
C5A C4A C3A C8A -0.8(3) . . . . ?
C5A C4A C3A C2A -179.13(17) . . . . ?
C7A C8A C3A C4A 2.0(2) . . . . ?
N1A C8A C3A C4A -175.99(15) . . . . ?
C7A C8A C3A C2A -179.69(16) . . . . ?
N1A C8A C3A C2A 2.4(2) . . . . ?
C3A C4A C5A C6A -0.6(3) . . . . ?
C7A C6A C5A C4A 0.8(3) . . . . ?
C14C C13C C12C C11C -0.2(3) . . . . ?
C10C C11C C12C C13C 1.3(3) . . . . ?
C9B C14B C13B C12B -2.3(3) . . . . ?
Cl2B C14B C13B C12B 176.46(16) . . . . ?
C14B C13B C12B C11B 1.8(3) . . . . ?
C13B C12B C11B C10B 0.3(3) . . . . ?
C9B C10B C11B C12B -2.1(3) . . . . ?
Cl1B C10B C11B C12B 174.83(15) . . . . ?
C7B C6B C5B C4B 2.4(3) . . . . ?
C3B C4B C5B C6B -0.9(3) . . . . ?
C3C C2C C1C C11 104.50(18) . . . . ?
C7C C2C C1C C11 -75.3(2) . . . . ?
O1C C11 C1C C2C 30.9(2) . . . . ?
O2C C11 C1C C2C -148.66(15) . . . . ?
Pr1 C11 C1C C2C -52.8(6) . . . . ?
C4B C3B C2B C1B 99.5(2) . . . . ?
C8B C3B C2B C1B -85.0(2) . . . . ?
O2B C1B C2B C3B 27.0(2) . . . . ?
O1B C1B C2B C3B -156.35(16) . . . . ?
O2A C1A C2A C3A 65.7(2) . . . . ?
O1A C1A C2A C3A -112.52(18) . . . . ?
C4A C3A C2A C1A 95.2(2) . . . . ?
C8A C3A C2A C1A -83.1(2) . . . . ?
O2B C1B O1B Pr1 6.48(17) . . . . ?
C2B C1B O1B Pr1 -170.14(13) . . . . ?
O2C C11 O1C Pr1 12.53(16) . . . . ?
C1C C11 O1C Pr1 -167.02(13) . . . . ?
O1C C11 O2C Pr1 138.7(2) . . . 3_655 ?
C1C C11 O2C Pr1 -41.7(3) . . . 3_655 ?
Pr1 C11 O2C Pr1 150.7(3) . . . 3_655 ?
O1C C11 O2C Pr1 -12.01(16) . . . . ?
C1C C11 O2C Pr1 167.55(13) . . . . ?
O1B C1B O2B Pr1 -6.28(16) . . . . ?
C2B C1B O2B Pr1 170.24(14) . . . . ?
O2A C1A O1A Pr1 -3.84(17) . . . . ?
C2A C1A O1A Pr1 174.41(14) . . . . ?
O1A C1A O2A Pr1 3.83(17) . . . . ?
C2A C1A O2A Pr1 -174.41(14) . . . . ?
C9A C14A C13A C12A -1.3(3) . . . . ?
Cl2A C14A C13A C12A 176.82(16) . . . . ?
C9A C10A C11A C12A -1.7(3) . . . . ?
Cl1A C10A C11A C12A 179.15(17) . . . . ?
C10A C11A C12A C13A -0.9(3) . . . . ?
C14A C13A C12A C11A 2.4(3) . . . . ?

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
O1W H1WA O1B 0.88 1.91 2.7414(17) 155.8 3
O1W H1WB O1A 0.88 1.94 2.7583(17) 153.1 3

_refine_diff_density_max         0.823
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.073

_shelxl_version_number           2014-3



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Water and methanol'
