# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2015

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

data_Dy
_database_code_depnum_ccdc_archive 'CCDC 1041404'
_audit_update_record             
;
2015-01-05 deposited with the CCDC.
2015-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H24 Dy N3 O10 P3, Cl O4, 3(H2 O)'
_chemical_formula_sum            'C9 H30 Cl Dy N3 O17 P3'
_chemical_formula_weight         743.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.1503(10)
_cell_length_b                   9.2244(10)
_cell_length_c                   15.1607(16)
_cell_angle_alpha                87.9626(18)
_cell_angle_beta                 76.3602(17)
_cell_angle_gamma                75.8111(18)
_cell_volume                     1205.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    4557
_cell_measurement_theta_min      2.441
_cell_measurement_theta_max      28.024

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.048
_exptl_crystal_F_000             738
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    3.492
_shelx_estimated_absorpt_T_min   0.375
_shelx_estimated_absorpt_T_max   0.845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.664
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6104
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.362
_diffrn_reflns_theta_max         25.244
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             4267
_reflns_number_gt                3930
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0333P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4267
_refine_ls_number_parameters     344
_refine_ls_number_restraints     120
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0252
_refine_ls_wR_factor_ref         0.0605
_refine_ls_wR_factor_gt          0.0599
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.020
_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_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 0.20032(2) 0.21265(2) 0.49895(2) 0.01661(7) Uani 1 1 d . . . . .
P1 P 0.46485(11) 0.03479(12) 0.64487(6) 0.0199(2) Uani 1 1 d . . . . .
P2 P -0.04130(11) 0.00073(11) 0.63233(6) 0.0193(2) Uani 1 1 d . . . . .
P3 P 0.03082(12) 0.54378(11) 0.64291(7) 0.0202(2) Uani 1 1 d . . . . .
C1 C 0.1220(5) 0.0186(5) 0.8756(2) 0.0262(9) Uani 1 1 d . . . . .
H1A H 0.1991 -0.0558 0.8978 0.031 Uiso 1 1 calc R U . . .
H1B H 0.0748 0.0973 0.9216 0.031 Uiso 1 1 calc R U . . .
C2 C -0.0003(5) -0.0521(5) 0.8566(3) 0.0258(9) Uani 1 1 d . . . . .
H2A H 0.0484 -0.1402 0.8175 0.031 Uiso 1 1 calc R U . . .
H2B H -0.0597 -0.0824 0.9129 0.031 Uiso 1 1 calc R U . . .
C3 C -0.2151(5) 0.1703(5) 0.8727(3) 0.0289(10) Uani 1 1 d . . . . .
H3A H -0.1783 0.1813 0.9265 0.035 Uiso 1 1 calc R U . . .
H3B H -0.3119 0.1399 0.8916 0.035 Uiso 1 1 calc R U . . .
C4 C -0.2425(4) 0.3190(5) 0.8251(3) 0.0298(10) Uani 1 1 d . . . . .
H4A H -0.3111 0.3181 0.7853 0.036 Uiso 1 1 calc R U . . .
H4B H -0.2935 0.3987 0.8701 0.036 Uiso 1 1 calc R U . . .
C5 C 0.0234(4) 0.3489(5) 0.8271(3) 0.0245(9) Uani 1 1 d . . . . .
H5A H 0.0331 0.4505 0.8323 0.029 Uiso 1 1 calc R U . . .
H5B H -0.0175 0.3176 0.8878 0.029 Uiso 1 1 calc R U . . .
C6 C 0.1838(4) 0.2493(4) 0.7914(3) 0.0241(9) Uani 1 1 d . . . . .
H6A H 0.2235 0.2798 0.7303 0.029 Uiso 1 1 calc R U . . .
H6B H 0.2506 0.2679 0.8285 0.029 Uiso 1 1 calc R U . . .
C7 C 0.3645(4) -0.0054(5) 0.7573(3) 0.0250(9) Uani 1 1 d . . . . .
H7A H 0.3662 -0.1110 0.7592 0.030 Uiso 1 1 calc R U . . .
H7B H 0.4216 0.0133 0.8003 0.030 Uiso 1 1 calc R U . . .
C8 C -0.1635(5) -0.0019(5) 0.7439(2) 0.0265(9) Uani 1 1 d . . . . .
H8A H -0.2672 0.0578 0.7450 0.032 Uiso 1 1 calc R U . . .
H8B H -0.1702 -0.1037 0.7584 0.032 Uiso 1 1 calc R U . . .
C9 C -0.1329(5) 0.4950(4) 0.7228(3) 0.0282(9) Uani 1 1 d . . . . .
H9A H -0.1786 0.5750 0.7681 0.034 Uiso 1 1 calc R U . . .
H9B H -0.2108 0.4900 0.6900 0.034 Uiso 1 1 calc R U . . .
N1 N 0.1980(3) 0.0831(4) 0.7884(2) 0.0208(7) Uani 1 1 d . . . . .
H1C H 0.1488 0.0663 0.7461 0.025 Uiso 1 1 d R U . . .
N2 N -0.1021(4) 0.0574(4) 0.8123(2) 0.0220(7) Uani 1 1 d . . . . .
N3 N -0.0944(3) 0.3505(4) 0.7705(2) 0.0215(7) Uani 1 1 d . . . . .
H3C H -0.0501 0.2761 0.7278 0.026 Uiso 1 1 d R U . . .
O1 O 0.3488(3) 0.0841(3) 0.58913(18) 0.0277(6) Uani 1 1 d . . . . .
O2 O 0.5885(3) -0.1047(3) 0.61465(17) 0.0247(6) Uani 1 1 d . . . . .
O3 O 0.5313(3) 0.1681(3) 0.66518(19) 0.0309(7) Uani 1 1 d . . . . .
H3D H 0.5674 0.2043 0.6172 0.046 Uiso 1 1 calc R U . . .
O4 O 0.0000(3) 0.1521(3) 0.62107(17) 0.0213(6) Uani 1 1 d . . . . .
O5 O 0.1136(3) -0.1162(3) 0.63368(18) 0.0272(6) Uani 1 1 d . . . . .
H5C H 0.0945 -0.1933 0.6566 0.041 Uiso 1 1 calc R U . . .
O6 O -0.1241(3) -0.0354(3) 0.56512(17) 0.0237(6) Uani 1 1 d . . . . .
O7 O 0.1397(3) 0.3975(3) 0.60524(17) 0.0238(6) Uani 1 1 d . . . . .
O8 O -0.0438(3) 0.6400(3) 0.57601(18) 0.0292(7) Uani 1 1 d . . . . .
O9 O 0.1051(3) 0.6314(3) 0.69591(17) 0.0261(6) Uani 1 1 d . . . . .
Cl1 Cl 0.67982(17) 0.72436(17) 0.98163(9) 0.0565(4) Uani 1 1 d D U . . .
O10 O 0.625(2) 0.8409(18) 1.0469(11) 0.076(4) Uani 0.41(2) 1 d D U P A 1
O11 O 0.8129(19) 0.617(3) 0.9933(15) 0.120(5) Uani 0.41(2) 1 d D U P A 1
O12 O 0.698(3) 0.751(3) 0.8901(6) 0.107(5) Uani 0.41(2) 1 d D U P A 1
O13 O 0.580(2) 0.6295(19) 0.9997(15) 0.095(4) Uani 0.41(2) 1 d D U P A 1
O10' O 0.6746(17) 0.8648(11) 1.0164(10) 0.078(3) Uani 0.59(2) 1 d D U P A 2
O11' O 0.8400(9) 0.6587(16) 0.9615(12) 0.114(4) Uani 0.59(2) 1 d D U P A 2
O12' O 0.622(2) 0.757(2) 0.9051(7) 0.116(4) Uani 0.59(2) 1 d D U P A 2
O13' O 0.5853(13) 0.6561(15) 1.0465(11) 0.099(4) Uani 0.59(2) 1 d D U P A 2
O1W O 0.3681(3) 0.3881(3) 0.4460(2) 0.0392(8) Uani 1 1 d . . . . .
H1WA H 0.3372 0.4728 0.4744 0.059 Uiso 1 1 d R U . . .
H1WB H 0.4232 0.3943 0.3926 0.059 Uiso 1 1 d R U . . .
O2W O 0.5852(4) 0.4121(6) 0.2906(3) 0.0804(14) Uani 1 1 d . . . . .
H2WA H 0.6641 0.4334 0.3029 0.121 Uiso 1 1 d R U . . .
H2WB H 0.6107 0.3816 0.2354 0.121 Uiso 1 1 d R U . . .
O3W O 0.6642(5) 0.2932(4) 0.5189(2) 0.0641(11) Uani 1 1 d . . . . .
H3WB H 0.7386 0.2285 0.4854 0.096 Uiso 1 1 d R U . . .
H3WA H 0.5939 0.3265 0.4902 0.096 Uiso 1 1 d R U . . .
O4W O 0.3359(7) 0.6605(6) 0.9005(4) 0.121(2) Uani 1 1 d . . . . .
H4WA H 0.4285 0.6705 0.8929 0.182 Uiso 1 1 d R U . . .
H4WB H 0.3359 0.5772 0.9265 0.182 Uiso 1 1 d 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
Dy1 O8 2.212(3) 2_566 ?
Dy1 O1 2.256(3) . ?
Dy1 O6 2.257(3) 2_556 ?
Dy1 O7 2.263(3) . ?
Dy1 O2 2.302(3) 2_656 ?
Dy1 O4 2.435(2) . ?
Dy1 O1W 2.483(3) . ?
P1 O1 1.486(3) . ?
P1 O2 1.493(3) . ?
P1 O3 1.568(3) . ?
P1 C7 1.808(4) . ?
P2 O6 1.495(3) . ?
P2 O4 1.527(3) . ?
P2 O5 1.561(3) . ?
P2 C8 1.797(4) . ?
P3 O8 1.500(3) . ?
P3 O7 1.506(3) . ?
P3 O9 1.527(3) . ?
P3 C9 1.830(4) . ?
C1 C2 1.511(5) . ?
C1 N1 1.516(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.458(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.445(5) . ?
C3 C4 1.521(6) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N3 1.502(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.513(5) . ?
C5 N3 1.525(5) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.508(5) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.512(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.468(5) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N3 1.499(5) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N1 H1C 0.9028 . ?
N3 H3C 0.9082 . ?
O2 Dy1 2.302(3) 2_656 ?
O3 H3D 0.8200 . ?
O5 H5C 0.8200 . ?
O6 Dy1 2.257(3) 2_556 ?
O8 Dy1 2.212(3) 2_566 ?
Cl1 O12 1.379(8) . ?
Cl1 O12' 1.381(7) . ?
Cl1 O13' 1.391(7) . ?
Cl1 O13 1.392(8) . ?
Cl1 O10 1.401(8) . ?
Cl1 O10' 1.401(7) . ?
Cl1 O11' 1.405(7) . ?
Cl1 O11 1.412(9) . ?
O1W H1WA 0.8564 . ?
O1W H1WB 0.8557 . ?
O2W H2WA 0.8547 . ?
O2W H2WB 0.8529 . ?
O3W H3WB 0.8586 . ?
O3W H3WA 0.8509 . ?
O4W H4WA 0.8548 . ?
O4W H4WB 0.8505 . ?

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
O8 Dy1 O1 172.95(10) 2_566 . ?
O8 Dy1 O6 81.28(10) 2_566 2_556 ?
O1 Dy1 O6 104.25(10) . 2_556 ?
O8 Dy1 O7 88.74(10) 2_566 . ?
O1 Dy1 O7 84.27(10) . . ?
O6 Dy1 O7 147.87(10) 2_556 . ?
O8 Dy1 O2 103.04(10) 2_566 2_656 ?
O1 Dy1 O2 82.78(9) . 2_656 ?
O6 Dy1 O2 75.22(9) 2_556 2_656 ?
O7 Dy1 O2 136.90(10) . 2_656 ?
O8 Dy1 O4 97.19(10) 2_566 . ?
O1 Dy1 O4 80.08(9) . . ?
O6 Dy1 O4 76.85(9) 2_556 . ?
O7 Dy1 O4 74.21(9) . . ?
O2 Dy1 O4 142.29(9) 2_656 . ?
O8 Dy1 O1W 83.61(10) 2_566 . ?
O1 Dy1 O1W 94.98(10) . . ?
O6 Dy1 O1W 136.40(9) 2_556 . ?
O7 Dy1 O1W 71.65(10) . . ?
O2 Dy1 O1W 68.80(10) 2_656 . ?
O4 Dy1 O1W 145.82(10) . . ?
O1 P1 O2 117.33(16) . . ?
O1 P1 O3 110.85(16) . . ?
O2 P1 O3 112.68(16) . . ?
O1 P1 C7 108.33(17) . . ?
O2 P1 C7 104.47(17) . . ?
O3 P1 C7 101.65(18) . . ?
O6 P2 O4 115.33(15) . . ?
O6 P2 O5 114.20(16) . . ?
O4 P2 O5 105.48(15) . . ?
O6 P2 C8 107.87(17) . . ?
O4 P2 C8 108.04(18) . . ?
O5 P2 C8 105.34(17) . . ?
O8 P3 O7 115.50(16) . . ?
O8 P3 O9 111.64(16) . . ?
O7 P3 O9 111.89(16) . . ?
O8 P3 C9 103.41(17) . . ?
O7 P3 C9 105.89(17) . . ?
O9 P3 C9 107.68(18) . . ?
C2 C1 N1 108.7(3) . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
N1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 108.3(3) . . ?
N2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
N2 C3 C4 110.1(3) . . ?
N2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 112.3(3) . . ?
N3 C4 H4A 109.2 . . ?
C3 C4 H4A 109.2 . . ?
N3 C4 H4B 109.2 . . ?
C3 C4 H4B 109.2 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 N3 116.0(3) . . ?
C6 C5 H5A 108.3 . . ?
N3 C5 H5A 108.3 . . ?
C6 C5 H5B 108.3 . . ?
N3 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
N1 C6 C5 117.2(3) . . ?
N1 C6 H6A 108.0 . . ?
C5 C6 H6A 108.0 . . ?
N1 C6 H6B 108.0 . . ?
C5 C6 H6B 108.0 . . ?
H6A C6 H6B 107.2 . . ?
N1 C7 P1 115.6(2) . . ?
N1 C7 H7A 108.4 . . ?
P1 C7 H7A 108.4 . . ?
N1 C7 H7B 108.4 . . ?
P1 C7 H7B 108.4 . . ?
H7A C7 H7B 107.4 . . ?
N2 C8 P2 110.9(3) . . ?
N2 C8 H8A 109.5 . . ?
P2 C8 H8A 109.5 . . ?
N2 C8 H8B 109.5 . . ?
P2 C8 H8B 109.5 . . ?
H8A C8 H8B 108.0 . . ?
N3 C9 P3 115.3(3) . . ?
N3 C9 H9A 108.4 . . ?
P3 C9 H9A 108.4 . . ?
N3 C9 H9B 108.4 . . ?
P3 C9 H9B 108.4 . . ?
H9A C9 H9B 107.5 . . ?
C6 N1 C7 112.4(3) . . ?
C6 N1 C1 115.4(3) . . ?
C7 N1 C1 109.3(3) . . ?
C6 N1 H1C 106.7 . . ?
C7 N1 H1C 106.4 . . ?
C1 N1 H1C 106.1 . . ?
C3 N2 C2 114.6(3) . . ?
C3 N2 C8 114.1(3) . . ?
C2 N2 C8 116.2(3) . . ?
C9 N3 C4 108.6(3) . . ?
C9 N3 C5 112.7(3) . . ?
C4 N3 C5 112.9(3) . . ?
C9 N3 H3C 108.3 . . ?
C4 N3 H3C 107.7 . . ?
C5 N3 H3C 106.5 . . ?
P1 O1 Dy1 164.61(18) . . ?
P1 O2 Dy1 144.49(16) . 2_656 ?
P1 O3 H3D 109.5 . . ?
P2 O4 Dy1 125.00(14) . . ?
P2 O5 H5C 109.5 . . ?
P2 O6 Dy1 147.19(17) . 2_556 ?
P3 O7 Dy1 146.23(16) . . ?
P3 O8 Dy1 167.53(19) . 2_566 ?
O12' Cl1 O13' 111.4(8) . . ?
O12 Cl1 O13 104.6(11) . . ?
O12 Cl1 O10 121.8(15) . . ?
O13 Cl1 O10 108.2(9) . . ?
O12' Cl1 O10' 104.1(10) . . ?
O13' Cl1 O10' 108.2(6) . . ?
O12' Cl1 O11' 113.1(8) . . ?
O13' Cl1 O11' 117.3(8) . . ?
O10' Cl1 O11' 101.2(10) . . ?
O12 Cl1 O11 107.8(11) . . ?
O13 Cl1 O11 96.3(14) . . ?
O10 Cl1 O11 114.6(13) . . ?
Dy1 O1W H1WA 114.4 . . ?
Dy1 O1W H1WB 127.8 . . ?
H1WA O1W H1WB 111.6 . . ?
H2WA O2W H2WB 107.6 . . ?
H3WB O3W H3WA 109.5 . . ?
H4WA O4W H4WB 105.4 . . ?

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
N1 C1 C2 N2 -52.2(4) . . . . ?
N2 C3 C4 N3 -42.3(5) . . . . ?
N3 C5 C6 N1 -65.1(4) . . . . ?
O1 P1 C7 N1 -29.0(3) . . . . ?
O2 P1 C7 N1 -154.8(3) . . . . ?
O3 P1 C7 N1 87.9(3) . . . . ?
O6 P2 C8 N2 -170.3(3) . . . . ?
O4 P2 C8 N2 -45.0(3) . . . . ?
O5 P2 C8 N2 67.3(3) . . . . ?
O8 P3 C9 N3 153.3(3) . . . . ?
O7 P3 C9 N3 31.4(3) . . . . ?
O9 P3 C9 N3 -88.4(3) . . . . ?
C5 C6 N1 C7 -176.3(3) . . . . ?
C5 C6 N1 C1 -50.1(4) . . . . ?
P1 C7 N1 C6 -60.4(4) . . . . ?
P1 C7 N1 C1 170.2(3) . . . . ?
C2 C1 N1 C6 120.0(4) . . . . ?
C2 C1 N1 C7 -112.2(4) . . . . ?
C4 C3 N2 C2 145.1(3) . . . . ?
C4 C3 N2 C8 -77.4(4) . . . . ?
C1 C2 N2 C3 -77.9(4) . . . . ?
C1 C2 N2 C8 145.5(3) . . . . ?
P2 C8 N2 C3 130.3(3) . . . . ?
P2 C8 N2 C2 -92.9(3) . . . . ?
P3 C9 N3 C4 -173.9(3) . . . . ?
P3 C9 N3 C5 60.3(4) . . . . ?
C3 C4 N3 C9 177.4(3) . . . . ?
C3 C4 N3 C5 -56.9(4) . . . . ?
C6 C5 N3 C9 -109.1(4) . . . . ?
C6 C5 N3 C4 127.5(4) . . . . ?
O2 P1 O1 Dy1 -117.1(6) . . . . ?
O3 P1 O1 Dy1 14.3(7) . . . . ?
C7 P1 O1 Dy1 125.0(6) . . . . ?
O1 P1 O2 Dy1 64.8(3) . . . 2_656 ?
O3 P1 O2 Dy1 -65.8(3) . . . 2_656 ?
C7 P1 O2 Dy1 -175.3(3) . . . 2_656 ?
O6 P2 O4 Dy1 -71.8(2) . . . . ?
O5 P2 O4 Dy1 55.2(2) . . . . ?
C8 P2 O4 Dy1 167.47(17) . . . . ?
O4 P2 O6 Dy1 164.6(2) . . . 2_556 ?
O5 P2 O6 Dy1 42.1(3) . . . 2_556 ?
C8 P2 O6 Dy1 -74.6(3) . . . 2_556 ?
O8 P3 O7 Dy1 -28.2(3) . . . . ?
O9 P3 O7 Dy1 -157.4(3) . . . . ?
C9 P3 O7 Dy1 85.5(3) . . . . ?
O7 P3 O8 Dy1 134.2(8) . . . 2_566 ?
O9 P3 O8 Dy1 -96.4(8) . . . 2_566 ?
C9 P3 O8 Dy1 19.1(9) . . . 2_566 ?

_refine_diff_density_max         0.811
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.104

_shelxl_version_number           2013-4



####################################################################### 
# 
# 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_Ho1
_database_code_depnum_ccdc_archive 'CCDC 1041405'
_audit_update_record             
;
2014-12-26 deposited with the CCDC.
2015-04-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C9 H24 Ho N3 O10 P3, Cl O4, 3(H2 O)'
_chemical_formula_sum            'C9 H32 Cl Ho N3 O17 P3'
_chemical_formula_weight         747.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
P P 0.1023 0.0942 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   9.1535(8)
_cell_length_b                   9.2424(8)
_cell_length_c                   15.2450(13)
_cell_angle_alpha                88.2040(10)
_cell_angle_beta                 76.2920(10)
_cell_angle_gamma                75.8130(10)
_cell_volume                     1214.29(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    5554
_cell_measurement_theta_min      2.362
_cell_measurement_theta_max      27.458

_exptl_crystal_description       rod-like
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_F_000             744
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.647
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_process_details   'SADABS(Bruker, 2000)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8250
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.375
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             5490
_reflns_number_gt                5128
_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       'SMART (Bruker, 2000)'
_computing_cell_refinement       SMART
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  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)+(0.0273P)²+1.6128P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5490
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0573
_refine_ls_wR_factor_gt          0.0558
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.011
_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_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
Ho1 Ho 0.20033(2) 0.21196(2) 0.49900(2) 0.01516(5) Uani 1 1 d . . . . .
P1 P 0.46428(9) 0.03587(9) 0.64397(5) 0.01876(15) Uani 1 1 d . . . . .
P2 P -0.04108(9) 0.00079(8) 0.63151(5) 0.01828(15) Uani 1 1 d . . . . .
P3 P 0.02961(9) 0.54451(8) 0.64162(5) 0.01911(15) Uani 1 1 d . . . . .
C1 C 0.1202(4) 0.0224(4) 0.8744(2) 0.0260(7) Uani 1 1 d . . . . .
H1A H 0.1971 -0.0517 0.8965 0.031 Uiso 1 1 calc R U . . .
H1B H 0.0734 0.1017 0.9200 0.031 Uiso 1 1 calc R U . . .
C2 C -0.0032(4) -0.0483(4) 0.8561(2) 0.0268(7) Uani 1 1 d . . . . .
H2A H 0.0451 -0.1374 0.8181 0.032 Uiso 1 1 calc R U . . .
H2B H -0.0632 -0.0764 0.9125 0.032 Uiso 1 1 calc R U . . .
C3 C -0.2186(4) 0.1740(4) 0.8713(2) 0.0298(7) Uani 1 1 d . . . . .
H3A H -0.1825 0.1859 0.9250 0.036 Uiso 1 1 calc R U . . .
H3B H -0.3153 0.1437 0.8899 0.036 Uiso 1 1 calc R U . . .
C4 C -0.2455(4) 0.3216(4) 0.8236(2) 0.0302(7) Uani 1 1 d . . . . .
H4A H -0.3138 0.3200 0.7839 0.036 Uiso 1 1 calc R U . . .
H4B H -0.2966 0.4018 0.8682 0.036 Uiso 1 1 calc R U . . .
C5 C 0.0210(4) 0.3523(4) 0.8252(2) 0.0247(6) Uani 1 1 d . . . . .
H5A H -0.0202 0.3216 0.8856 0.030 Uiso 1 1 calc R U . . .
H5B H 0.0304 0.4538 0.8303 0.030 Uiso 1 1 calc R U . . .
C6 C 0.1828(4) 0.2520(4) 0.7894(2) 0.0243(6) Uani 1 1 d . . . . .
H6A H 0.2226 0.2815 0.7285 0.029 Uiso 1 1 calc R U . . .
H6B H 0.2496 0.2711 0.8262 0.029 Uiso 1 1 calc R U . . .
C7 C 0.3632(4) -0.0029(4) 0.7566(2) 0.0248(6) Uani 1 1 d . . . . .
H7A H 0.3652 -0.1083 0.7588 0.030 Uiso 1 1 calc R U . . .
H7B H 0.4198 0.0169 0.7993 0.030 Uiso 1 1 calc R U . . .
C8 C -0.1655(4) -0.0009(4) 0.7434(2) 0.0254(7) Uani 1 1 d . . . . .
H8A H -0.2691 0.0587 0.7444 0.030 Uiso 1 1 calc R U . . .
H8B H -0.1721 -0.1023 0.7580 0.030 Uiso 1 1 calc R U . . .
C9 C -0.1354(4) 0.4968(4) 0.7208(2) 0.0272(7) Uani 1 1 d . . . . .
H9A H -0.1820 0.5772 0.7657 0.033 Uiso 1 1 calc R U . . .
H9B H -0.2125 0.4907 0.6880 0.033 Uiso 1 1 calc R U . . .
N1 N 0.1970(3) 0.0852(3) 0.78690(17) 0.0211(5) Uani 1 1 d . . . . .
H1C H 0.1477 0.0685 0.7446 0.025 Uiso 1 1 d R U . . .
N2 N -0.1039(3) 0.0597(3) 0.81122(18) 0.0232(5) Uani 1 1 d . . . . .
N3 N -0.0958(3) 0.3527(3) 0.76873(18) 0.0220(5) Uani 1 1 d . . . . .
H3C H -0.0516 0.2783 0.7261 0.026 Uiso 1 1 d R U . . .
O1 O 0.3480(3) 0.0850(3) 0.58829(16) 0.0274(5) Uani 1 1 d . . . . .
O2 O 0.5875(3) -0.1033(3) 0.61392(15) 0.0249(5) Uani 1 1 d . . . . .
O3 O 0.5307(3) 0.1698(3) 0.66404(16) 0.0293(5) Uani 1 1 d . . . . .
H3D H 0.5665 0.2057 0.6163 0.044 Uiso 1 1 calc R U . . .
O4 O 0.0001(3) 0.1516(2) 0.61988(14) 0.0209(4) Uani 1 1 d . . . . .
O5 O 0.1140(3) -0.1168(3) 0.63375(16) 0.0268(5) Uani 1 1 d . . . . .
H5C H 0.0942 -0.1933 0.6567 0.040 Uiso 1 1 calc R U . . .
O6 O -0.1238(3) -0.0355(2) 0.56464(15) 0.0235(5) Uani 1 1 d . . . . .
O7 O 0.1380(3) 0.3980(2) 0.60422(15) 0.0226(4) Uani 1 1 d . . . . .
O8 O -0.0445(3) 0.6411(3) 0.57474(16) 0.0291(5) Uani 1 1 d . . . . .
O9 O 0.1043(3) 0.6316(2) 0.69443(16) 0.0265(5) Uani 1 1 d . . . . .
Cl1 Cl 0.68101(16) 0.72410(16) 0.98186(9) 0.0623(3) Uani 1 1 d . . . . .
O10 O 0.636(3) 0.841(3) 1.044(2) 0.115(10) Uani 0.43(4) 1 d . . P A 1
O11 O 0.830(3) 0.631(4) 0.9959(18) 0.178(15) Uani 0.43(4) 1 d . . P A 1
O12 O 0.685(5) 0.758(3) 0.8897(14) 0.153(13) Uani 0.43(4) 1 d . . P A 1
O13 O 0.588(4) 0.627(4) 0.997(2) 0.141(11) Uani 0.43(4) 1 d . . P A 1
O10' O 0.667(3) 0.859(2) 1.0210(18) 0.115(7) Uani 0.57(4) 1 d . . P A 2
O11' O 0.835(2) 0.653(2) 0.955(2) 0.153(11) Uani 0.57(4) 1 d . . P A 2
O12' O 0.631(5) 0.758(4) 0.9086(18) 0.206(14) Uani 0.57(4) 1 d . . P A 2
O13' O 0.584(2) 0.650(2) 1.040(2) 0.128(9) Uani 0.57(4) 1 d . . P A 2
O1W O 0.3676(3) 0.3859(3) 0.44694(19) 0.0394(6) Uani 1 1 d . . . . .
H1WA H 0.3367 0.4706 0.4753 0.059 Uiso 1 1 d R U . . .
H1WB H 0.4227 0.3921 0.3935 0.059 Uiso 1 1 d R U . . .
O2W O 0.5844(4) 0.4119(5) 0.2929(3) 0.0819(13) Uani 1 1 d . . . . .
H2WA H 0.6633 0.4333 0.3052 0.123 Uiso 1 1 d R U . . .
H2WB H 0.6050 0.3815 0.2376 0.123 Uiso 1 1 d R U . . .
O3W O 0.6660(5) 0.2944(4) 0.5192(2) 0.0688(11) Uani 1 1 d . . . . .
H3WB H 0.7404 0.2297 0.4857 0.103 Uiso 1 1 d R U . . .
H3WA H 0.5957 0.3277 0.4904 0.103 Uiso 1 1 d R U . . .
O4W O 0.3394(9) 0.6644(6) 0.8966(4) 0.145(3) Uani 1 1 d . . . . .
H4WA H 0.4319 0.6744 0.8889 0.217 Uiso 1 1 d R U . . .
H4WB H 0.3394 0.5811 0.9225 0.217 Uiso 1 1 d 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
Ho1 O8 2.204(2) 2_566 ?
Ho1 O1 2.247(2) . ?
Ho1 O6 2.252(2) 2_556 ?
Ho1 O7 2.261(2) . ?
Ho1 O2 2.305(2) 2_656 ?
Ho1 O4 2.429(2) . ?
Ho1 O1W 2.472(2) . ?
P1 O2 1.489(2) . ?
P1 O1 1.492(2) . ?
P1 O3 1.574(2) . ?
P1 C7 1.817(3) . ?
P2 O6 1.495(2) . ?
P2 O4 1.526(2) . ?
P2 O5 1.569(2) . ?
P2 C8 1.815(3) . ?
P3 O7 1.505(2) . ?
P3 O8 1.507(2) . ?
P3 O9 1.528(2) . ?
P3 C9 1.833(3) . ?
C1 C2 1.517(5) . ?
C1 N1 1.522(4) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N2 1.456(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N2 1.456(4) . ?
C3 C4 1.520(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 N3 1.514(4) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 N3 1.523(4) . ?
C5 C6 1.526(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.515(4) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 N1 1.508(4) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 N2 1.472(4) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 N3 1.506(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
N1 H1C 0.9059 . ?
N3 H3C 0.9090 . ?
O2 Ho1 2.305(2) 2_656 ?
O3 H3D 0.8200 . ?
O5 H5C 0.8200 . ?
O6 Ho1 2.252(2) 2_556 ?
O8 Ho1 2.204(2) 2_566 ?
Cl1 O12' 1.31(2) . ?
Cl1 O13 1.36(3) . ?
Cl1 O10' 1.359(16) . ?
Cl1 O10 1.38(2) . ?
Cl1 O11' 1.371(18) . ?
Cl1 O13' 1.394(19) . ?
Cl1 O12 1.42(2) . ?
Cl1 O11 1.48(2) . ?
O1W H1WA 0.8570 . ?
O1W H1WB 0.8591 . ?
O2W H2WA 0.8556 . ?
O2W H2WB 0.8590 . ?
O3W H3WB 0.8586 . ?
O3W H3WA 0.8539 . ?
O4W H4WA 0.8550 . ?
O4W H4WB 0.8543 . ?

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
O8 Ho1 O1 172.64(9) 2_566 . ?
O8 Ho1 O6 81.38(8) 2_566 2_556 ?
O1 Ho1 O6 104.47(9) . 2_556 ?
O8 Ho1 O7 88.02(8) 2_566 . ?
O1 Ho1 O7 84.66(8) . . ?
O6 Ho1 O7 147.53(8) 2_556 . ?
O8 Ho1 O2 103.37(9) 2_566 2_656 ?
O1 Ho1 O2 82.63(8) . 2_656 ?
O6 Ho1 O2 75.48(8) 2_556 2_656 ?
O7 Ho1 O2 136.97(8) . 2_656 ?
O8 Ho1 O4 97.14(9) 2_566 . ?
O1 Ho1 O4 80.14(8) . . ?
O6 Ho1 O4 76.56(7) 2_556 . ?
O7 Ho1 O4 74.43(7) . . ?
O2 Ho1 O4 142.11(8) 2_656 . ?
O8 Ho1 O1W 83.58(9) 2_566 . ?
O1 Ho1 O1W 94.83(9) . . ?
O6 Ho1 O1W 136.54(9) 2_556 . ?
O7 Ho1 O1W 71.59(8) . . ?
O2 Ho1 O1W 68.78(9) 2_656 . ?
O4 Ho1 O1W 145.97(8) . . ?
O2 P1 O1 117.28(14) . . ?
O2 P1 O3 112.87(13) . . ?
O1 P1 O3 110.63(14) . . ?
O2 P1 C7 104.59(14) . . ?
O1 P1 C7 108.44(14) . . ?
O3 P1 C7 101.53(15) . . ?
O6 P2 O4 115.00(13) . . ?
O6 P2 O5 114.54(13) . . ?
O4 P2 O5 105.76(13) . . ?
O6 P2 C8 107.67(14) . . ?
O4 P2 C8 108.28(14) . . ?
O5 P2 C8 105.01(15) . . ?
O7 P3 O8 115.58(13) . . ?
O7 P3 O9 111.78(13) . . ?
O8 P3 O9 111.62(13) . . ?
O7 P3 C9 105.80(14) . . ?
O8 P3 C9 103.36(15) . . ?
O9 P3 C9 107.88(15) . . ?
C2 C1 N1 108.8(3) . . ?
C2 C1 H1A 109.9 . . ?
N1 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
N1 C1 H1B 109.9 . . ?
H1A C1 H1B 108.3 . . ?
N2 C2 C1 108.5(3) . . ?
N2 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N2 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
N2 C3 C4 110.1(3) . . ?
N2 C3 H3A 109.6 . . ?
C4 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C4 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
N3 C4 C3 112.3(3) . . ?
N3 C4 H4A 109.1 . . ?
C3 C4 H4A 109.1 . . ?
N3 C4 H4B 109.1 . . ?
C3 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
N3 C5 C6 115.8(3) . . ?
N3 C5 H5A 108.3 . . ?
C6 C5 H5A 108.3 . . ?
N3 C5 H5B 108.3 . . ?
C6 C5 H5B 108.3 . . ?
H5A C5 H5B 107.4 . . ?
N1 C6 C5 117.0(3) . . ?
N1 C6 H6A 108.0 . . ?
C5 C6 H6A 108.0 . . ?
N1 C6 H6B 108.0 . . ?
C5 C6 H6B 108.0 . . ?
H6A C6 H6B 107.3 . . ?
N1 C7 P1 115.4(2) . . ?
N1 C7 H7A 108.4 . . ?
P1 C7 H7A 108.4 . . ?
N1 C7 H7B 108.4 . . ?
P1 C7 H7B 108.4 . . ?
H7A C7 H7B 107.5 . . ?
N2 C8 P2 110.4(2) . . ?
N2 C8 H8A 109.6 . . ?
P2 C8 H8A 109.6 . . ?
N2 C8 H8B 109.6 . . ?
P2 C8 H8B 109.6 . . ?
H8A C8 H8B 108.1 . . ?
N3 C9 P3 114.8(2) . . ?
N3 C9 H9A 108.6 . . ?
P3 C9 H9A 108.6 . . ?
N3 C9 H9B 108.6 . . ?
P3 C9 H9B 108.6 . . ?
H9A C9 H9B 107.5 . . ?
C7 N1 C6 112.2(2) . . ?
C7 N1 C1 109.3(2) . . ?
C6 N1 C1 115.3(2) . . ?
C7 N1 H1C 106.7 . . ?
C6 N1 H1C 106.3 . . ?
C1 N1 H1C 106.5 . . ?
C2 N2 C3 114.4(3) . . ?
C2 N2 C8 116.5(3) . . ?
C3 N2 C8 113.8(3) . . ?
C9 N3 C4 108.2(2) . . ?
C9 N3 C5 112.9(2) . . ?
C4 N3 C5 112.8(3) . . ?
C9 N3 H3C 107.9 . . ?
C4 N3 H3C 107.7 . . ?
C5 N3 H3C 107.0 . . ?
P1 O1 Ho1 164.73(16) . . ?
P1 O2 Ho1 144.50(14) . 2_656 ?
P1 O3 H3D 109.5 . . ?
P2 O4 Ho1 125.41(12) . . ?
P2 O5 H5C 109.5 . . ?
P2 O6 Ho1 147.24(14) . 2_556 ?
P3 O7 Ho1 146.76(13) . . ?
P3 O8 Ho1 167.21(17) . 2_566 ?
O12' Cl1 O10' 104.2(17) . . ?
O13 Cl1 O10 114.0(17) . . ?
O12' Cl1 O11' 106.7(17) . . ?
O10' Cl1 O11' 109.4(13) . . ?
O12' Cl1 O13' 110.0(16) . . ?
O10' Cl1 O13' 108.0(13) . . ?
O11' Cl1 O13' 117.6(12) . . ?
O13 Cl1 O12 101.4(19) . . ?
O10 Cl1 O12 118.3(18) . . ?
O13 Cl1 O11 103(2) . . ?
O10 Cl1 O11 106.0(14) . . ?
O12 Cl1 O11 113(2) . . ?
Ho1 O1W H1WA 114.5 . . ?
Ho1 O1W H1WB 127.7 . . ?
H1WA O1W H1WB 111.5 . . ?
H2WA O2W H2WB 110.8 . . ?
H3WB O3W H3WA 109.3 . . ?
H4WA O4W H4WB 105.4 . . ?

_refine_diff_density_max         1.241
_refine_diff_density_min         -0.980
_refine_diff_density_rms         0.114

_shelxl_version_number           2013-4



