# 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 
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data_Compound-1a
_database_code_depnum_ccdc_archive 'CCDC 1477300'
_audit_update_record             
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_audit_creation_date             2016-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        Compound-1a
_chemical_formula_moiety         'C10 H16 Co N2 O10 P2, 2.5(H2 O)'
_chemical_formula_sum            'C10 H21 Co N2 O12.50 P2'
_chemical_formula_weight         490.16
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9975(11)
_cell_length_b                   10.0662(10)
_cell_length_c                   18.303(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.790(3)
_cell_angle_gamma                90
_cell_volume                     1949.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2672
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.915
_cell_measurement_theta_min      2.312
_shelx_estimated_absorpt_T_max   0.978
_shelx_estimated_absorpt_T_min   0.860
_exptl_absorpt_coefficient_mu    1.109
_exptl_absorpt_correction_T_max  0.9503
_exptl_absorpt_correction_T_min  0.8978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_av_unetI/netI     0.0771
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            14597
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         1.957
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2942
_reflns_number_total             4698
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4698
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0383
_refine_ls_restrained_S_all      0.883
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0831
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O11B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Sof(O11B)=1-FVAR(1)
 Sof(O11A)=FVAR(1)
 Sof(O12A)=Sof(H12C)=Sof(H12D)=1-FVAR(2)
 Sof(O12B)=Sof(H12A)=Sof(H12B)=FVAR(2)
 Fixed Sof: O13(0.5) H13A(0.5) H13B(0.5)
4.a Riding coordinates:
 O10(H10A,H10B), O9(H9A,H9B), O7(H7A,H7B), O4(H4), O1(H1), O11A(H11A,H11B)
4.b Free rotating group:
 O8(H8A,H8B), O12B(H12A,H12B), O12A(H12C,H12D), O13(H13A,H13B)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1A), C3(H3), C8(H8), C7(H7), C4(H4A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Co1 Co 0.31257(4) 0.39885(4) 0.63976(2) 0.01891(10) Uani 1 1 d . . . . .
P1 P 0.18304(7) 0.09703(7) 0.35689(4) 0.01977(16) Uani 1 1 d . . . . .
P2 P 0.48393(7) 0.95087(7) 0.69371(4) 0.02132(17) Uani 1 1 d . . . . .
O10 O 0.49589(17) 0.31732(17) 0.66000(10) 0.0226(4) Uani 1 1 d . . . . .
H10A H 0.5038 0.2255 0.6582 0.034 Uiso 1 1 d R . . . .
H10B H 0.5567 0.3439 0.6977 0.034 Uiso 1 1 d R . . . .
O6 O 0.53522(19) 1.05589(18) 0.65125(12) 0.0279(5) Uani 1 1 d . . . . .
O9 O 0.34612(18) 0.4471(2) 0.75243(11) 0.0299(5) Uani 1 1 d . . . . .
H9A H 0.2848 0.4428 0.7731 0.045 Uiso 1 1 d R . . . .
H9B H 0.4238 0.4444 0.7902 0.045 Uiso 1 1 d R . . . .
O3 O 0.19190(18) 0.11019(19) 0.27623(11) 0.0275(5) Uani 1 1 d . . . . .
O8 O 0.1253(2) 0.4746(2) 0.62319(12) 0.0321(5) Uani 1 1 d . . . . .
H8A H 0.1081 0.5487 0.6046 0.048 Uiso 1 1 d G . . . .
H8B H 0.1053 0.4945 0.6682 0.048 Uiso 1 1 d G . . . .
O5 O 0.38158(19) 0.99297(19) 0.72618(11) 0.0304(5) Uani 1 1 d . . . . .
O7 O 0.2410(2) 0.21328(19) 0.65156(12) 0.0343(5) Uani 1 1 d . . . . .
H7A H 0.1588 0.2014 0.6440 0.051 Uiso 1 1 d R . . . .
H7B H 0.2810 0.1373 0.6782 0.051 Uiso 1 1 d R . . . .
O4 O 0.59377(19) 0.88997(19) 0.75938(11) 0.0328(5) Uani 1 1 d . . . . .
H4 H 0.6705 0.8865 0.7496 0.049 Uiso 1 1 d R . . . .
O1 O 0.27392(19) -0.01297(18) 0.40015(11) 0.0305(5) Uani 1 1 d . . . . .
H1 H 0.3391 -0.0354 0.3805 0.046 Uiso 1 1 d R . . . .
O2 O 0.05486(19) 0.0682(2) 0.36707(12) 0.0352(5) Uani 1 1 d . . . . .
N2 N 0.3707(2) 0.5853(2) 0.60757(12) 0.0186(5) Uani 1 1 d . . . . .
N1 N 0.2873(2) 0.3751(2) 0.52157(12) 0.0194(5) Uani 1 1 d . . . . .
C9 C 0.4338(2) 0.8145(3) 0.62863(15) 0.0195(6) Uani 1 1 d . . . . .
C2 C 0.2388(3) 0.2506(3) 0.40516(15) 0.0197(6) Uani 1 1 d . . . . .
C5 C 0.3186(3) 0.4812(3) 0.48495(15) 0.0187(6) Uani 1 1 d . . . . .
C10 C 0.4063(3) 0.6897(3) 0.65311(16) 0.0212(6) Uani 1 1 d . . . . .
H10 H 0.4133 0.6783 0.7056 0.025 Uiso 1 1 calc R . . . .
C1 C 0.2494(3) 0.2638(3) 0.48219(15) 0.0217(6) Uani 1 1 d . . . . .
H1A H 0.2284 0.1895 0.5084 0.026 Uiso 1 1 calc R . . . .
C6 C 0.3607(2) 0.6005(3) 0.53262(15) 0.0193(6) Uani 1 1 d . . . . .
C3 C 0.2709(3) 0.3599(3) 0.36818(16) 0.0249(7) Uani 1 1 d . . . . .
H3 H 0.2649 0.3555 0.3155 0.030 Uiso 1 1 calc R . . . .
C8 C 0.4217(3) 0.8284(3) 0.55139(16) 0.0269(7) Uani 1 1 d . . . . .
H8 H 0.4383 0.9117 0.5317 0.032 Uiso 1 1 calc R . . . .
C7 C 0.3856(3) 0.7209(3) 0.50310(16) 0.0285(7) Uani 1 1 d . . . . .
H7 H 0.3779 0.7298 0.4504 0.034 Uiso 1 1 calc R . . . .
C4 C 0.3117(3) 0.4754(3) 0.40820(16) 0.0256(7) Uani 1 1 d . . . . .
H4A H 0.3348 0.5502 0.3833 0.031 Uiso 1 1 calc R . . . .
O11A O -0.0156(5) 0.2076(6) 0.6147(13) 0.080(4) Uani 0.83(4) 1 d . . P A 1
H11A H -0.0347 0.1241 0.6237 0.120 Uiso 1 1 d R . . . .
H11B H -0.0668 0.2512 0.6303 0.120 Uiso 1 1 d R . . . .
O12B O 0.0780(4) 0.7331(5) 0.5585(3) 0.0529(19) Uani 0.604(9) 1 d . . P B 1
H12A H 0.0525 0.7235 0.5094 0.079 Uiso 0.604(9) 1 d G . P B 1
H12B H 0.0172 0.7668 0.5746 0.079 Uiso 0.604(9) 1 d G . P B 1
O12A O 0.0587(8) 0.6365(8) 0.5106(4) 0.058(3) Uani 0.396(9) 1 d . . P B 2
H12C H 0.0291 0.6426 0.4615 0.087 Uiso 0.396(9) 1 d G . P B 2
H12D H 0.1081 0.7037 0.5275 0.087 Uiso 0.396(9) 1 d G . P B 2
O13 O 0.0833(10) 0.9139(12) 0.5280(5) 0.144(3) Uani 0.5 1 d . . P C 2
H13A H 0.1648 0.9192 0.5470 0.216 Uiso 0.5 1 d G . P C 2
H13B H 0.0466 0.9218 0.5643 0.216 Uiso 0.5 1 d G . P C 2
O11B O -0.002(3) 0.208(2) 0.6532(16) 0.028(8) Uani 0.17(4) 1 d . U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O10 2.1140(19) . ?
Co1 O9 2.0518(19) . ?
Co1 O8 2.139(2) . ?
Co1 O7 2.0613(19) . ?
Co1 N2 2.118(2) . ?
Co1 N1 2.118(2) . ?
P1 O3 1.512(2) . ?
P1 O1 1.556(2) . ?
P1 O2 1.500(2) . ?
P1 C2 1.803(3) . ?
P2 O6 1.509(2) . ?
P2 O5 1.471(2) . ?
P2 O4 1.578(2) . ?
P2 C9 1.803(3) . ?
O10 H10A 0.9297 . ?
O10 H10B 0.8624 . ?
O9 H9A 0.8587 . ?
O9 H9B 0.9418 . ?
O8 H8A 0.8192 . ?
O8 H8B 0.9304 . ?
O7 H7A 0.8841 . ?
O7 H7B 0.9487 . ?
O4 H4 0.9095 . ?
O1 H1 0.9137 . ?
N2 C10 1.332(3) . ?
N2 C6 1.355(3) . ?
N1 C5 1.354(3) . ?
N1 C1 1.336(3) . ?
C9 C10 1.395(4) . ?
C9 C8 1.391(4) . ?
C2 C1 1.389(4) . ?
C2 C3 1.387(4) . ?
C5 C6 1.483(4) . ?
C5 C4 1.387(4) . ?
C10 H10 0.9500 . ?
C1 H1A 0.9500 . ?
C6 C7 1.384(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.382(4) . ?
C8 H8 0.9500 . ?
C8 C7 1.385(4) . ?
C7 H7 0.9500 . ?
C4 H4A 0.9500 . ?
O11A H11A 0.8924 . ?
O11A H11B 0.8230 . ?
O12B H12A 0.8701 . ?
O12B H12B 0.8700 . ?
O12A H12C 0.8699 . ?
O12A H12D 0.8698 . ?
O13 H13A 0.8701 . ?
O13 H13B 0.8701 . ?
O11B H11A 1.0165 . ?
O11B H11B 0.8459 . ?

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
O10 Co1 O8 177.22(8) . . ?
O10 Co1 N2 92.70(8) . . ?
O10 Co1 N1 89.36(8) . . ?
O9 Co1 O10 90.78(7) . . ?
O9 Co1 O8 87.77(8) . . ?
O9 Co1 O7 94.50(8) . . ?
O9 Co1 N2 94.86(8) . . ?
O9 Co1 N1 172.23(8) . . ?
O7 Co1 O10 90.18(8) . . ?
O7 Co1 O8 87.57(9) . . ?
O7 Co1 N2 170.17(9) . . ?
O7 Co1 N1 93.27(8) . . ?
N2 Co1 O8 89.79(8) . . ?
N2 Co1 N1 77.38(8) . . ?
N1 Co1 O8 92.40(8) . . ?
O3 P1 O1 110.86(11) . . ?
O3 P1 C2 107.44(12) . . ?
O1 P1 C2 105.96(12) . . ?
O2 P1 O3 116.80(12) . . ?
O2 P1 O1 107.14(12) . . ?
O2 P1 C2 108.10(12) . . ?
O6 P2 O4 110.39(12) . . ?
O6 P2 C9 106.46(12) . . ?
O5 P2 O6 116.14(11) . . ?
O5 P2 O4 108.39(12) . . ?
O5 P2 C9 110.86(12) . . ?
O4 P2 C9 103.93(12) . . ?
Co1 O10 H10A 118.3 . . ?
Co1 O10 H10B 121.0 . . ?
H10A O10 H10B 106.1 . . ?
Co1 O9 H9A 118.8 . . ?
Co1 O9 H9B 127.5 . . ?
H9A O9 H9B 109.9 . . ?
Co1 O8 H8A 119.2 . . ?
Co1 O8 H8B 113.7 . . ?
H8A O8 H8B 95.0 . . ?
Co1 O7 H7A 120.6 . . ?
Co1 O7 H7B 130.3 . . ?
H7A O7 H7B 106.4 . . ?
P2 O4 H4 115.0 . . ?
P1 O1 H1 116.1 . . ?
C10 N2 Co1 125.75(18) . . ?
C10 N2 C6 118.3(2) . . ?
C6 N2 Co1 115.74(18) . . ?
C5 N1 Co1 115.85(17) . . ?
C1 N1 Co1 125.49(17) . . ?
C1 N1 C5 118.6(2) . . ?
C10 C9 P2 121.9(2) . . ?
C8 C9 P2 121.5(2) . . ?
C8 C9 C10 116.6(3) . . ?
C1 C2 P1 120.2(2) . . ?
C3 C2 P1 122.6(2) . . ?
C3 C2 C1 117.2(2) . . ?
N1 C5 C6 115.4(2) . . ?
N1 C5 C4 121.1(2) . . ?
C4 C5 C6 123.5(2) . . ?
N2 C10 C9 124.2(2) . . ?
N2 C10 H10 117.9 . . ?
C9 C10 H10 117.9 . . ?
N1 C1 C2 123.7(3) . . ?
N1 C1 H1A 118.1 . . ?
C2 C1 H1A 118.1 . . ?
N2 C6 C5 115.5(2) . . ?
N2 C6 C7 121.6(3) . . ?
C7 C6 C5 122.9(2) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C9 C8 H8 119.9 . . ?
C7 C8 C9 120.1(3) . . ?
C7 C8 H8 119.9 . . ?
C6 C7 C8 119.2(3) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C5 C4 H4A 120.2 . . ?
C3 C4 C5 119.5(3) . . ?
C3 C4 H4A 120.2 . . ?
H11A O11A H11B 102.8 . . ?
H12A O12B H12B 109.5 . . ?
H12C O12A H12D 109.5 . . ?
H13A O13 H13B 109.5 . . ?
H11A O11B H11B 91.7 . . ?

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
Co1 N2 C10 C9 -174.3(2) . . . . ?
Co1 N2 C6 C5 -4.0(3) . . . . ?
Co1 N2 C6 C7 174.6(2) . . . . ?
Co1 N1 C5 C6 -2.6(3) . . . . ?
Co1 N1 C5 C4 177.0(2) . . . . ?
Co1 N1 C1 C2 -177.3(2) . . . . ?
P1 C2 C1 N1 -178.5(2) . . . . ?
P1 C2 C3 C4 179.3(2) . . . . ?
P2 C9 C10 N2 -179.0(2) . . . . ?
P2 C9 C8 C7 178.6(2) . . . . ?
O6 P2 C9 C10 166.2(2) . . . . ?
O6 P2 C9 C8 -13.2(3) . . . . ?
O3 P1 C2 C1 -175.7(2) . . . . ?
O3 P1 C2 C3 5.3(3) . . . . ?
O5 P2 C9 C10 -66.6(3) . . . . ?
O5 P2 C9 C8 114.0(2) . . . . ?
O4 P2 C9 C10 49.6(2) . . . . ?
O4 P2 C9 C8 -129.8(2) . . . . ?
O1 P1 C2 C1 -57.1(3) . . . . ?
O1 P1 C2 C3 123.8(2) . . . . ?
O2 P1 C2 C1 57.5(3) . . . . ?
O2 P1 C2 C3 -121.6(2) . . . . ?
N2 C6 C7 C8 0.1(4) . . . . ?
N1 C5 C6 N2 4.4(4) . . . . ?
N1 C5 C6 C7 -174.2(3) . . . . ?
N1 C5 C4 C3 0.7(4) . . . . ?
C9 C8 C7 C6 0.6(5) . . . . ?
C2 C3 C4 C5 -0.8(4) . . . . ?
C5 N1 C1 C2 -0.7(4) . . . . ?
C5 C6 C7 C8 178.6(3) . . . . ?
C10 N2 C6 C5 -179.0(2) . . . . ?
C10 N2 C6 C7 -0.4(4) . . . . ?
C10 C9 C8 C7 -0.8(4) . . . . ?
C1 N1 C5 C6 -179.6(2) . . . . ?
C1 N1 C5 C4 0.0(4) . . . . ?
C1 C2 C3 C4 0.2(4) . . . . ?
C6 N2 C10 C9 0.2(4) . . . . ?
C6 C5 C4 C3 -179.7(3) . . . . ?
C3 C2 C1 N1 0.6(4) . . . . ?
C8 C9 C10 N2 0.5(4) . . . . ?
C4 C5 C6 N2 -175.2(3) . . . . ?
C4 C5 C6 C7 6.2(4) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound-1b
_database_code_depnum_ccdc_archive 'CCDC 1477301'
_audit_update_record             
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_audit_creation_date             2016-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        Compound-1b
_chemical_formula_moiety         'C10 H16 N2 Ni O10 P2, 2.5(H2 O)'
_chemical_formula_sum            'C10 H21 N2 Ni O12.50 P2'
_chemical_formula_weight         489.94
_chemical_melting_point          ?
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'
Ni Ni 0.3393 1.1124 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.9582(16)
_cell_length_b                   10.0015(11)
_cell_length_c                   18.204(2)
_cell_angle_alpha                90
_cell_angle_beta                 105.491(5)
_cell_angle_gamma                90
_cell_volume                     1922.6(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1521
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      26.110
_cell_measurement_theta_min      2.322
_shelx_estimated_absorpt_T_max   0.964
_shelx_estimated_absorpt_T_min   0.886
_exptl_absorpt_coefficient_mu    1.241
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0470 before and 0.0426 after correction.
The Ratio of minimum to maximum transmission is 0.9227.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9961
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.963
_diffrn_reflns_theta_min         1.967
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3098
_reflns_number_total             4605
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0449
_refine_ls_restrained_S_all      0.985
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0455P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1036
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Sof(O12A)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(O12B)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Fixed Sof: O13(0.5) H13A(0.5) H13B(0.5)
3.a Riding coordinates:
 O9(H9A,H9B)
3.b Free rotating group:
 O12B(H12A,H12B), O12A(H12C,H12D), O11(H11A,H11B), O13(H13A,H13B)
3.c Rotating group:
 O8(H8A,H8B), O10(H10A,H10B), O7(H7A,H7B)
3.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C1(H1), C4(H4), C8(H8), C3(H3)
3.e Idealised tetrahedral OH refined as rotating group:
 O6(H6), O2(H2)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ni00 Ni 0.68556(4) 0.09806(4) 0.36105(2) 0.01491(12) Uani 1 1 d . . . . .
P2 P 0.81816(9) 0.40533(8) 0.64221(5) 0.01687(18) Uani 1 1 d . . . . .
P1 P 0.51299(9) -0.45246(8) 0.30441(5) 0.01664(19) Uani 1 1 d . . . . .
O5 O 0.8108(2) 0.3917(2) 0.72375(12) 0.0196(5) Uani 1 1 d . . . . .
N2 N 0.6280(3) -0.0857(2) 0.39095(14) 0.0142(6) Uani 1 1 d . . . . .
O6 O 0.7260(2) 0.5168(2) 0.59930(13) 0.0230(5) Uani 1 1 d . . . . .
H6 H 0.6679 0.5283 0.6208 0.035 Uiso 1 1 calc GR . . . .
O2 O 0.4029(2) -0.3913(2) 0.23877(12) 0.0220(5) Uani 1 1 d . . . . .
H2 H 0.3360 -0.3885 0.2530 0.033 Uiso 1 1 calc GR . . . .
C5 C 0.6379(3) -0.1003(3) 0.46639(17) 0.0172(7) Uani 1 1 d . . . . .
C2 C 0.5643(3) -0.3158(3) 0.36979(17) 0.0161(7) Uani 1 1 d . . . . .
C10 C 0.7504(3) 0.2380(3) 0.51585(18) 0.0180(7) Uani 1 1 d . . . . .
H10 H 0.7722 0.3124 0.4895 0.022 Uiso 1 1 calc R . . . .
O4 O 0.9458(2) 0.4341(2) 0.63095(13) 0.0265(6) Uani 1 1 d . . . . .
N1 N 0.7113(3) 0.1258(2) 0.47670(14) 0.0153(6) Uani 1 1 d . . . . .
C9 C 0.7608(3) 0.2510(3) 0.59342(18) 0.0170(7) Uani 1 1 d . . . . .
O8 O 0.6541(2) 0.0494(2) 0.24815(13) 0.0239(5) Uani 1 1 d . . . . .
H8A H 0.7216 0.0630 0.2325 0.036 Uiso 1 1 d GR . . . .
H8B H 0.5930 0.0977 0.2203 0.036 Uiso 1 1 d GR . . . .
O3 O 0.6162(2) -0.4945(2) 0.27002(13) 0.0223(5) Uani 1 1 d . . . . .
C6 C 0.6796(3) 0.0193(3) 0.51339(18) 0.0158(7) Uani 1 1 d . . . . .
C7 C 0.6877(3) 0.0247(3) 0.59070(18) 0.0198(7) Uani 1 1 d . . . . .
H7 H 0.6652 -0.0508 0.6160 0.024 Uiso 1 1 calc R . . . .
C1 C 0.5927(3) -0.1904(3) 0.34465(18) 0.0162(7) Uani 1 1 d . . . . .
H1 H 0.5866 -0.1792 0.2920 0.019 Uiso 1 1 calc R . . . .
C4 C 0.6134(4) -0.2221(3) 0.49588(18) 0.0239(8) Uani 1 1 d . . . . .
H4 H 0.6216 -0.2315 0.5489 0.029 Uiso 1 1 calc R . . . .
C8 C 0.7290(3) 0.1417(3) 0.63073(18) 0.0216(8) Uani 1 1 d . . . . .
H8 H 0.7353 0.1465 0.6837 0.026 Uiso 1 1 calc R . . . .
O1 O 0.4637(2) -0.5590(2) 0.34774(13) 0.0213(5) Uani 1 1 d . . . . .
C3 C 0.5768(4) -0.3296(3) 0.44737(18) 0.0219(8) Uani 1 1 d . . . . .
H3 H 0.5600 -0.4134 0.4672 0.026 Uiso 1 1 calc R . . . .
O10 O 0.7570(2) 0.2836(2) 0.34732(13) 0.0251(6) Uani 1 1 d . . . . .
H10A H 0.7061 0.3289 0.3089 0.038 Uiso 1 1 d GR . . . .
H10B H 0.8322 0.2778 0.3372 0.038 Uiso 1 1 d GR . . . .
O7 O 0.8696(2) 0.0252(2) 0.37800(13) 0.0232(5) Uani 1 1 d . . . . .
H7A H 0.8856 -0.0400 0.4123 0.035 Uiso 1 1 d GR . . . .
H7B H 0.9064 0.0150 0.3345 0.035 Uiso 1 1 d GR . . . .
O9 O 0.5063(2) 0.1778(2) 0.34066(12) 0.0181(5) Uani 1 1 d . . . . .
H9A H 0.4450 0.1565 0.3011 0.027 Uiso 1 1 d R . . . .
H9B H 0.5010 0.2643 0.3546 0.027 Uiso 1 1 d R . . . .
O12B O 1.0777(6) 0.2288(6) 0.5554(4) 0.042(2) Uani 0.583(12) 1 d . . P A 1
H12A H 1.0341 0.2880 0.5726 0.063 Uiso 0.583(12) 1 d G . P A 1
H12B H 1.0571 0.2318 0.5058 0.063 Uiso 0.583(12) 1 d G . P A 1
O12A O 1.0622(8) 0.1432(9) 0.5113(4) 0.049(3) Uani 0.417(12) 1 d . . P A 2
H12C H 1.0790 0.2274 0.5209 0.073 Uiso 0.417(12) 1 d G . P A 2
H12D H 1.0166 0.1343 0.4644 0.073 Uiso 0.417(12) 1 d G . P A 2
O11 O 1.0119(4) 0.2885(3) 0.3756(3) 0.0826(15) Uani 1 1 d . . . . .
H11A H 1.0484 0.2424 0.3469 0.124 Uiso 1 1 d G . . . .
H11B H 1.0336 0.3722 0.3751 0.124 Uiso 1 1 d G . . . .
O13 O 1.0921(9) 0.4227(10) 0.5295(5) 0.089(3) Uani 0.5 1 d . . P B 2
H13A H 1.0417 0.4019 0.4853 0.133 Uiso 0.5 1 d G . P B 2
H13B H 1.0478 0.4524 0.5592 0.133 Uiso 0.5 1 d G . P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni00 N2 2.063(2) . ?
Ni00 N1 2.067(2) . ?
Ni00 O8 2.050(2) . ?
Ni00 O10 2.055(2) . ?
Ni00 O7 2.088(2) . ?
Ni00 O9 2.060(2) . ?
P2 O5 1.514(2) . ?
P2 O6 1.565(2) . ?
P2 O4 1.495(3) . ?
P2 C9 1.808(3) . ?
P1 O2 1.577(2) . ?
P1 C2 1.801(3) . ?
P1 O3 1.492(2) . ?
P1 O1 1.509(2) . ?
N2 C5 1.356(4) . ?
N2 C1 1.335(4) . ?
O6 H6 0.8400 . ?
O2 H2 0.8400 . ?
C5 C6 1.470(4) . ?
C5 C4 1.386(4) . ?
C2 C1 1.398(4) . ?
C2 C3 1.389(4) . ?
C10 H10 0.9500 . ?
C10 N1 1.336(4) . ?
C10 C9 1.392(4) . ?
N1 C6 1.352(4) . ?
C9 C8 1.380(4) . ?
O8 H8A 0.8709 . ?
O8 H8B 0.8710 . ?
C6 C7 1.387(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.389(4) . ?
C1 H1 0.9500 . ?
C4 H4 0.9500 . ?
C4 C3 1.381(4) . ?
C8 H8 0.9500 . ?
C3 H3 0.9500 . ?
O10 H10A 0.8925 . ?
O10 H10B 0.8938 . ?
O7 H7A 0.8875 . ?
O7 H7B 0.9850 . ?
O9 H9A 0.8697 . ?
O9 H9B 0.9080 . ?
O12B H12A 0.8701 . ?
O12B H12B 0.8702 . ?
O12A H12C 0.8699 . ?
O12A H12D 0.8700 . ?
O11 H11A 0.8701 . ?
O11 H11B 0.8700 . ?
O13 H13A 0.8704 . ?
O13 H13B 0.8693 . ?

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
N2 Ni00 N1 79.59(10) . . ?
N2 Ni00 O7 90.07(10) . . ?
N1 Ni00 O7 91.88(10) . . ?
O8 Ni00 N2 94.11(10) . . ?
O8 Ni00 N1 173.69(10) . . ?
O8 Ni00 O10 93.44(9) . . ?
O8 Ni00 O7 87.83(9) . . ?
O8 Ni00 O9 90.83(9) . . ?
O10 Ni00 N2 171.83(10) . . ?
O10 Ni00 N1 92.85(10) . . ?
O10 Ni00 O7 87.09(10) . . ?
O10 Ni00 O9 90.23(9) . . ?
O9 Ni00 N2 92.78(10) . . ?
O9 Ni00 N1 89.75(10) . . ?
O9 Ni00 O7 176.94(9) . . ?
O5 P2 O6 110.95(13) . . ?
O5 P2 C9 107.57(14) . . ?
O6 P2 C9 105.65(15) . . ?
O4 P2 O5 116.64(14) . . ?
O4 P2 O6 107.26(14) . . ?
O4 P2 C9 108.21(15) . . ?
O2 P1 C2 104.33(14) . . ?
O3 P1 O2 107.69(13) . . ?
O3 P1 C2 110.69(15) . . ?
O3 P1 O1 115.94(13) . . ?
O1 P1 O2 111.18(14) . . ?
O1 P1 C2 106.42(14) . . ?
C5 N2 Ni00 114.6(2) . . ?
C1 N2 Ni00 126.1(2) . . ?
C1 N2 C5 119.1(3) . . ?
P2 O6 H6 109.5 . . ?
P1 O2 H2 109.5 . . ?
N2 C5 C6 115.5(3) . . ?
N2 C5 C4 121.0(3) . . ?
C4 C5 C6 123.5(3) . . ?
C1 C2 P1 121.5(2) . . ?
C3 C2 P1 121.7(2) . . ?
C3 C2 C1 116.8(3) . . ?
N1 C10 H10 118.4 . . ?
N1 C10 C9 123.2(3) . . ?
C9 C10 H10 118.4 . . ?
C10 N1 Ni00 126.4(2) . . ?
C10 N1 C6 119.1(3) . . ?
C6 N1 Ni00 114.5(2) . . ?
C10 C9 P2 120.1(2) . . ?
C8 C9 P2 122.3(2) . . ?
C8 C9 C10 117.5(3) . . ?
Ni00 O8 H8A 111.2 . . ?
Ni00 O8 H8B 110.4 . . ?
H8A O8 H8B 108.1 . . ?
N1 C6 C5 115.8(3) . . ?
N1 C6 C7 121.0(3) . . ?
C7 C6 C5 123.2(3) . . ?
C6 C7 H7 120.4 . . ?
C6 C7 C8 119.3(3) . . ?
C8 C7 H7 120.4 . . ?
N2 C1 C2 123.3(3) . . ?
N2 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C5 C4 H4 120.3 . . ?
C3 C4 C5 119.3(3) . . ?
C3 C4 H4 120.3 . . ?
C9 C8 C7 119.9(3) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.0 . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(3) . . ?
C4 C3 H3 119.8 . . ?
Ni00 O10 H10A 112.0 . . ?
Ni00 O10 H10B 111.6 . . ?
H10A O10 H10B 106.7 . . ?
Ni00 O7 H7A 111.2 . . ?
Ni00 O7 H7B 120.2 . . ?
H7A O7 H7B 116.3 . . ?
Ni00 O9 H9A 122.9 . . ?
Ni00 O9 H9B 116.6 . . ?
H9A O9 H9B 111.8 . . ?
H12A O12B H12B 109.5 . . ?
H12C O12A H12D 109.4 . . ?
H11A O11 H11B 109.5 . . ?
H13A O13 H13B 109.5 . . ?

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
Ni00 N2 C5 C6 3.9(4) . . . . ?
Ni00 N2 C5 C4 -174.3(3) . . . . ?
Ni00 N2 C1 C2 174.7(2) . . . . ?
Ni00 N1 C6 C5 2.7(4) . . . . ?
Ni00 N1 C6 C7 -177.8(3) . . . . ?
P2 C9 C8 C7 -178.8(3) . . . . ?
P1 C2 C1 N2 178.3(3) . . . . ?
P1 C2 C3 C4 -178.4(3) . . . . ?
O5 P2 C9 C10 176.5(3) . . . . ?
O5 P2 C9 C8 -5.1(3) . . . . ?
N2 C5 C6 N1 -4.4(5) . . . . ?
N2 C5 C6 C7 176.1(3) . . . . ?
N2 C5 C4 C3 -0.8(5) . . . . ?
O6 P2 C9 C10 57.9(3) . . . . ?
O6 P2 C9 C8 -123.7(3) . . . . ?
O2 P1 C2 C1 -49.9(3) . . . . ?
O2 P1 C2 C3 129.6(3) . . . . ?
C5 N2 C1 C2 0.4(5) . . . . ?
C5 C6 C7 C8 179.5(3) . . . . ?
C5 C4 C3 C2 -0.2(6) . . . . ?
C10 N1 C6 C5 -179.8(3) . . . . ?
C10 N1 C6 C7 -0.3(5) . . . . ?
C10 C9 C8 C7 -0.4(5) . . . . ?
O4 P2 C9 C10 -56.7(3) . . . . ?
O4 P2 C9 C8 121.7(3) . . . . ?
N1 C10 C9 P2 178.6(3) . . . . ?
N1 C10 C9 C8 0.1(5) . . . . ?
N1 C6 C7 C8 0.1(5) . . . . ?
C9 C10 N1 Ni00 177.4(2) . . . . ?
C9 C10 N1 C6 0.2(5) . . . . ?
O3 P1 C2 C1 65.7(3) . . . . ?
O3 P1 C2 C3 -114.8(3) . . . . ?
C6 C5 C4 C3 -178.8(3) . . . . ?
C6 C7 C8 C9 0.3(5) . . . . ?
C1 N2 C5 C6 178.9(3) . . . . ?
C1 N2 C5 C4 0.7(5) . . . . ?
C1 C2 C3 C4 1.2(5) . . . . ?
C4 C5 C6 N1 173.7(3) . . . . ?
C4 C5 C6 C7 -5.8(6) . . . . ?
O1 P1 C2 C1 -167.5(3) . . . . ?
O1 P1 C2 C3 12.0(3) . . . . ?
C3 C2 C1 N2 -1.3(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound-2
_database_code_depnum_ccdc_archive 'CCDC 1477302'
_audit_update_record             
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT973_Compound-2          
;
PROBLEM: Check Calcd Positive Residual Density on     Gd1       2.73 eA-3
RESPONSE: Disordered GD atom with occupancy < 5%
;
# Added during the CSD deposition process: Saturday 09 July 2016 08:37 AM
# end Validation Reply Form


_audit_creation_date             2016-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        Compound-2
_chemical_formula_moiety         
'C30 H40 Gd2 N6 O24 P6, 0.5(O2), 12(H2 O), 4(Cl), 0.5(H2 O2)'
_chemical_formula_sum            'C30 H65 Cl4 Gd2 N6 O38 P6'
_chemical_formula_weight         1760.00
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.362(3)
_cell_length_b                   10.819(3)
_cell_length_c                   14.686(4)
_cell_angle_alpha                104.138(7)
_cell_angle_beta                 100.605(7)
_cell_angle_gamma                98.755(7)
_cell_volume                     1535.5(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4532
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.226
_cell_measurement_theta_min      2.537
_shelx_estimated_absorpt_T_max   0.748
_shelx_estimated_absorpt_T_min   0.303
_exptl_absorpt_coefficient_mu    2.573
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1081 before and 0.0802 after correction.
The Ratio of minimum to maximum transmission is 0.6056.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.903
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             877
_exptl_crystal_size_max          0.61
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0852
_diffrn_reflns_av_unetI/netI     0.1134
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.955
_diffrn_reflns_theta_min         1.984
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5311
_reflns_number_total             7328
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.855
_refine_diff_density_min         -2.118
_refine_diff_density_rms         0.222
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7328
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0573
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0752P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1597
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(O19B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
3. Others
 Sof(O19B)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(O19A)=Sof(H19A)=Sof(H19B)=FVAR(1)
 Sof(O20B)=Sof(H20C)=Sof(H20D)=1-FVAR(2)
 Sof(O20A)=Sof(H20A)=Sof(H20B)=FVAR(2)
 Fixed Sof: O18(0.5) H17(0.5)
4.a Riding coordinates:
 O3(H3), O5(H5), O7(H7), O10(H10A,H10B), O13(H13A), O20A(H20A,H20B), O19A(H19A,
 H19B), O19B(H19C,H19D), O20B(H20C,H20D)
4.b Free rotating group:
 O12(H12A,H12B), O16(H16A,H16B), O14(H14A,H14B), O15(H15A,H15B)
4.c Rotating group:
 O11(H11A,H11B), O17(H17)
4.d Aromatic/amide H refined with riding coordinates:
 N3(H3A), C11(H11), C13(H13), C14(H14), C0AA(H0AA), C1(H1A), C4(H4), C7(H7A),
 C8(H8), C10(H10)
4.e Fitted hexagon refined as free rotating group:
 N3(C11,C12,C13,C14,C15)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.74524(3) 0.49679(3) 1.01879(2) 0.01834(12) Uani 1 1 d . . . . .
P1 P 0.95293(16) 0.58629(17) 0.85302(12) 0.0167(4) Uani 1 1 d . . . . .
P2 P 0.6330(2) 0.20494(18) 0.09649(13) 0.0273(4) Uani 1 1 d . . . . .
P3 P 0.43504(16) 0.35893(17) 0.81296(12) 0.0162(4) Uani 1 1 d . . . . .
O1 O 0.8532(5) 0.5406(5) 0.9042(4) 0.0344(14) Uani 1 1 d . . . . .
O2 O 1.0866(5) 0.5541(6) 0.8792(4) 0.0396(15) Uani 1 1 d . . . . .
O3 O 0.9640(7) 0.7326(5) 0.8596(4) 0.0504(18) Uani 1 1 d . . . . .
H3 H 1.0430 0.7702 0.8790 0.076 Uiso 1 1 d R . . . .
O4 O 0.5048(6) 0.0997(5) 0.0661(4) 0.0342(13) Uani 1 1 d . . . . .
O5 O 0.7485(6) 0.1460(5) 0.0629(4) 0.0349(13) Uani 1 1 d . . . . .
H5 H 0.7430 0.0725 0.0696 0.052 Uiso 1 1 d R . . . .
O6 O 0.6170(4) 0.3230(4) 0.0621(3) 0.0183(10) Uani 1 1 d . . . . .
O7 O 0.4072(5) 0.2062(5) 0.7826(4) 0.0370(14) Uani 1 1 d . . . . .
H7 H 0.4538 0.1560 0.7591 0.055 Uiso 1 1 d R . . . .
O8 O 0.5576(5) 0.4193(5) 0.8919(3) 0.0270(12) Uani 1 1 d . . . . .
O9 O 0.3073(4) 0.3972(5) 0.8333(3) 0.0207(10) Uani 1 1 d . . . . .
O10 O 0.7985(5) 0.2833(5) 0.9291(4) 0.0310(12) Uani 1 1 d . . . . .
H10A H 0.8761 0.2988 0.9169 0.046 Uiso 1 1 d R . . . .
H10B H 0.7397 0.2488 0.8760 0.046 Uiso 1 1 d R . . . .
O11 O 0.6605(5) 0.6864(5) 0.9900(4) 0.0295(12) Uani 1 1 d . . . . .
H11A H 0.6892 0.7544 1.0415 0.044 Uiso 1 1 d GR . . . .
H11B H 0.5719 0.6698 0.9764 0.044 Uiso 1 1 d GR . . . .
O12 O 0.9307(6) 0.6990(6) 1.1006(4) 0.0402(14) Uani 1 1 d . . . . .
H12A H 0.9314 0.7742 1.0891 0.060 Uiso 1 1 d G . . . .
H12B H 0.9376 0.7099 1.1622 0.060 Uiso 1 1 d G . . . .
N1 N 0.8551(5) 0.5116(6) 0.5627(4) 0.0204(12) Uani 1 1 d . . . . .
H1 H 0.861(7) 0.551(7) 0.517(6) 0.03(2) Uiso 1 1 d . . . . .
N2 N 0.7853(5) 0.4158(6) 0.3746(4) 0.0226(13) Uani 1 1 d . . . . .
N3 N 0.5542(5) 0.5614(5) 0.6327(4) 0.055(2) Uani 1 1 d . . . . .
H3A H 0.6028 0.6359 0.6383 0.066 Uiso 1 1 calc R . . . .
C11 C 0.5386(4) 0.5237(4) 0.7146(3) 0.0309(18) Uani 1 1 d G . . . .
H11 H 0.5807 0.5791 0.7755 0.037 Uiso 1 1 calc R . . . .
C12 C 0.4601(4) 0.4032(4) 0.7055(3) 0.0176(14) Uani 1 1 d G . . . .
C13 C 0.3972(5) 0.3204(4) 0.6145(3) 0.040(2) Uani 1 1 d G . . . .
H13 H 0.3446 0.2397 0.6084 0.048 Uiso 1 1 calc R . . . .
C14 C 0.4128(5) 0.3580(6) 0.5325(2) 0.050(3) Uani 1 1 d G . . . .
H14 H 0.3707 0.3026 0.4716 0.060 Uiso 1 1 calc R . . . .
C15 C 0.4913(6) 0.4785(7) 0.5416(3) 0.054(3) Uani 1 1 d G U . . .
C0AA C 0.8090(6) 0.3805(7) 0.6929(5) 0.0203(14) Uani 1 1 d . . . . .
H0AA H 0.7918 0.3356 0.7373 0.024 Uiso 1 1 calc R . . . .
C1 C 0.9044(6) 0.5723(6) 0.6571(5) 0.0178(14) Uani 1 1 d . . . . .
H1A H 0.9526 0.6578 0.6766 0.021 Uiso 1 1 calc R . . . .
C2 C 0.8833(6) 0.5075(7) 0.7256(5) 0.0163(13) Uani 1 1 d . . . . .
C4 C 0.7608(7) 0.3203(7) 0.5960(5) 0.0241(15) Uani 1 1 d . . . . .
H4 H 0.7119 0.2350 0.5751 0.029 Uiso 1 1 calc R . . . .
C5 C 0.7850(6) 0.3869(7) 0.5297(5) 0.0194(14) Uani 1 1 d . . . . .
C6 C 0.7414(6) 0.3333(7) 0.4229(5) 0.0202(14) Uani 1 1 d . . . . .
C7 C 0.6626(8) 0.2113(7) 0.3789(5) 0.0309(18) Uani 1 1 d . . . . .
H7A H 0.6333 0.1583 0.4153 0.037 Uiso 1 1 calc R . . . .
C8 C 0.6275(8) 0.1684(7) 0.2778(5) 0.0279(17) Uani 1 1 d . . . . .
H8 H 0.5759 0.0856 0.2459 0.034 Uiso 1 1 calc R . . . .
C9 C 0.6714(7) 0.2525(7) 0.2258(5) 0.0233(15) Uani 1 1 d . . . . .
C10 C 0.7498(6) 0.3740(7) 0.2783(5) 0.0207(14) Uani 1 1 d . . . . .
H10 H 0.7796 0.4300 0.2440 0.025 Uiso 1 1 calc R . . . .
O18 O 1.0192(19) 0.9314(16) 1.0051(14) 0.109(8) Uani 0.5 1 d . . . A 1
O16 O 1.1965(7) 1.0609(8) 0.8790(8) 0.082(3) Uani 1 1 d . . . . .
H16A H 1.1390 1.0656 0.9136 0.124 Uiso 1 1 d G . . . .
H16B H 1.1613 1.0652 0.8231 0.124 Uiso 1 1 d G . . . .
O13 O 0.9490(6) 0.6976(6) 0.4868(4) 0.0387(15) Uani 1 1 d . . . . .
H13A H 0.9805 0.7714 0.5280 0.058 Uiso 1 1 d R . . . .
H13B H 0.931(10) 0.694(10) 0.435(7) 0.058 Uiso 1 1 d R . . . .
O14 O 1.0750(5) 1.2615(6) 0.6954(4) 0.0396(14) Uani 1 1 d . . . . .
H14A H 1.1380 1.3164 0.7380 0.059 Uiso 1 1 d G . . . .
H14B H 1.0915 1.1856 0.6883 0.059 Uiso 1 1 d G . . . .
O20A O 0.7570(17) 0.863(2) 0.7089(15) 0.104(8) Uani 0.55(2) 1 d . . . B 2
H20A H 0.8331 0.8573 0.6964 0.156 Uiso 0.55(2) 1 d R . . B 2
H20B H 0.7328 0.9288 0.6944 0.156 Uiso 0.55(2) 1 d R . . B 2
Cl1 Cl 0.6210(4) 0.0993(4) 0.7208(3) 0.1065(13) Uani 1 1 d . . . . .
O17 O 0.5000 0.0000 0.5000 0.150(7) Uani 1 2 d S T P . .
H17 H 0.4218 0.0184 0.5182 0.224 Uiso 0.5 1 d GR . . . .
Cl2 Cl 1.0306(3) 0.9538(2) 0.6585(2) 0.0636(7) Uani 1 1 d . . . . .
O19A O 0.7442(17) 0.8748(15) 0.9018(16) 0.039(7) Uani 0.40(3) 1 d . . . C 2
H19A H 0.8097 0.8428 0.8862 0.058 Uiso 0.40(3) 1 d R . . C 2
H19B H 0.6845 0.8150 0.9064 0.058 Uiso 0.40(3) 1 d R . . C 2
O19B O 0.7099(18) 0.854(2) 0.8317(19) 0.133(9) Uani 0.60(3) 1 d . U . C 1
H19C H 0.7728 0.9176 0.8657 0.199 Uiso 0.60(3) 1 d R . . C 1
H19D H 0.6421 0.8543 0.8566 0.199 Uiso 0.60(3) 1 d R . . C 1
O15 O 0.2186(9) 0.0134(9) 0.5109(7) 0.086(3) Uani 1 1 d . . . . .
H15A H 0.1594 -0.0362 0.5261 0.129 Uiso 1 1 d G . . . .
H15B H 0.1817 0.0401 0.4649 0.129 Uiso 1 1 d G . . . .
O20B O 0.7079(19) 0.798(2) 0.6261(15) 0.079(8) Uani 0.45(2) 1 d . . . B 1
H20C H 0.7104 0.8240 0.6861 0.118 Uiso 0.45(2) 1 d R . . B 1
H20D H 0.7736 0.8430 0.6136 0.118 Uiso 0.45(2) 1 d R . . B 1


_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
Gd1 O1 2.288(5) . ?
Gd1 O2 2.306(5) 2_767 ?
Gd1 O6 2.417(4) 1_556 ?
Gd1 O8 2.316(5) . ?
Gd1 O9 2.395(5) 2_667 ?
Gd1 O10 2.558(5) . ?
Gd1 O11 2.448(5) . ?
Gd1 O12 2.551(6) . ?
P1 O1 1.479(5) . ?
P1 O2 1.484(5) . ?
P1 O3 1.547(6) . ?
P1 C2 1.813(7) . ?
P2 O4 1.527(6) . ?
P2 O5 1.543(6) . ?
P2 O6 1.504(5) . ?
P2 C9 1.792(7) . ?
P3 O7 1.568(5) . ?
P3 O8 1.490(5) . ?
P3 O9 1.505(5) . ?
P3 C12 1.808(4) . ?
O2 Gd1 2.306(5) 2_767 ?
O3 H3 0.8201 . ?
O5 H5 0.8195 . ?
O6 Gd1 2.417(4) 1_554 ?
O7 H7 0.8357 . ?
O9 Gd1 2.395(5) 2_667 ?
O10 H10A 0.8567 . ?
O10 H10B 0.8564 . ?
O11 H11A 0.8833 . ?
O11 H11B 0.8824 . ?
O12 H12A 0.8703 . ?
O12 H12B 0.8711 . ?
N1 H1 0.89(8) . ?
N1 C1 1.345(8) . ?
N1 C5 1.355(9) . ?
N2 C6 1.346(9) . ?
N2 C10 1.336(8) . ?
N3 H3A 0.8600 . ?
N3 C11 1.3900 . ?
N3 C15 1.3900 . ?
C11 H11 0.9300 . ?
C11 C12 1.3900 . ?
C12 C13 1.3900 . ?
C13 H13 0.9300 . ?
C13 C14 1.3900 . ?
C14 H14 0.9300 . ?
C14 C15 1.3900 . ?
C15 C15 1.441(6) 2_666 ?
C0AA H0AA 0.9300 . ?
C0AA C2 1.390(9) . ?
C0AA C4 1.373(9) . ?
C1 H1A 0.9300 . ?
C1 C2 1.389(9) . ?
C4 H4 0.9300 . ?
C4 C5 1.381(10) . ?
C5 C6 1.488(9) . ?
C6 C7 1.374(10) . ?
C7 H7A 0.9300 . ?
C7 C8 1.401(10) . ?
C8 H8 0.9300 . ?
C8 C9 1.399(10) . ?
C9 C10 1.390(9) . ?
C10 H10 0.9300 . ?
O18 O18 1.63(4) 2_777 ?
O16 H16A 0.8506 . ?
O16 H16B 0.8501 . ?
O13 H13A 0.8492 . ?
O13 H13B 0.74(10) . ?
O14 H14A 0.8485 . ?
O14 H14B 0.8494 . ?
O20A H20A 0.8506 . ?
O20A H20B 0.8491 . ?
O17 H17 0.9330 . ?
O19A H19A 0.8506 . ?
O19A H19B 0.8497 . ?
O19B H19C 0.8503 . ?
O19B H19D 0.8499 . ?
O15 H15A 0.8508 . ?
O15 H15B 0.8491 . ?
O20B H20C 0.8503 . ?
O20B H20D 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
O1 Gd1 O2 101.3(2) . 2_767 ?
O1 Gd1 O6 143.13(18) . 1_556 ?
O1 Gd1 O8 84.58(17) . . ?
O1 Gd1 O9 141.26(18) . 2_667 ?
O1 Gd1 O10 72.71(19) . . ?
O1 Gd1 O11 78.45(19) . . ?
O1 Gd1 O12 72.41(18) . . ?
O2 Gd1 O6 79.70(19) 2_767 1_556 ?
O2 Gd1 O8 146.8(2) 2_767 . ?
O2 Gd1 O9 83.25(17) 2_767 2_667 ?
O2 Gd1 O10 71.63(19) 2_767 . ?
O2 Gd1 O11 140.3(2) 2_767 . ?
O2 Gd1 O12 70.4(2) 2_767 . ?
O6 Gd1 O10 72.79(16) 1_556 . ?
O6 Gd1 O11 123.99(16) 1_556 . ?
O6 Gd1 O12 138.68(17) 1_556 . ?
O8 Gd1 O6 76.64(16) . 1_556 ?
O8 Gd1 O9 112.51(17) . 2_667 ?
O8 Gd1 O10 79.30(17) . . ?
O8 Gd1 O11 72.91(18) . . ?
O8 Gd1 O12 140.90(19) . . ?
O9 Gd1 O6 75.61(16) 2_667 1_556 ?
O9 Gd1 O10 142.42(17) 2_667 . ?
O9 Gd1 O11 74.41(17) 2_667 . ?
O9 Gd1 O12 73.15(17) 2_667 . ?
O11 Gd1 O10 141.44(17) . . ?
O11 Gd1 O12 71.79(19) . . ?
O12 Gd1 O10 120.93(18) . . ?
O1 P1 O2 115.0(3) . . ?
O1 P1 O3 111.7(4) . . ?
O1 P1 C2 106.3(3) . . ?
O2 P1 O3 111.9(4) . . ?
O2 P1 C2 108.0(3) . . ?
O3 P1 C2 103.0(3) . . ?
O4 P2 O5 109.7(3) . . ?
O4 P2 C9 105.0(3) . . ?
O5 P2 C9 108.3(3) . . ?
O6 P2 O4 113.6(3) . . ?
O6 P2 O5 111.3(3) . . ?
O6 P2 C9 108.7(3) . . ?
O7 P3 C12 104.8(3) . . ?
O8 P3 O7 112.9(3) . . ?
O8 P3 O9 115.5(3) . . ?
O8 P3 C12 109.0(3) . . ?
O9 P3 O7 106.7(3) . . ?
O9 P3 C12 107.3(2) . . ?
P1 O1 Gd1 164.6(3) . . ?
P1 O2 Gd1 153.5(3) . 2_767 ?
P1 O3 H3 109.4 . . ?
P2 O5 H5 109.5 . . ?
P2 O6 Gd1 141.0(3) . 1_554 ?
P3 O7 H7 129.4 . . ?
P3 O8 Gd1 175.0(3) . . ?
P3 O9 Gd1 131.0(3) . 2_667 ?
Gd1 O10 H10A 109.4 . . ?
Gd1 O10 H10B 109.8 . . ?
H10A O10 H10B 109.1 . . ?
Gd1 O11 H11A 111.1 . . ?
Gd1 O11 H11B 110.7 . . ?
H11A O11 H11B 107.8 . . ?
Gd1 O12 H12A 124.6 . . ?
Gd1 O12 H12B 104.9 . . ?
H12A O12 H12B 108.3 . . ?
C1 N1 H1 123(5) . . ?
C1 N1 C5 122.7(6) . . ?
C5 N1 H1 114(5) . . ?
C10 N2 C6 116.9(6) . . ?
C11 N3 H3A 120.0 . . ?
C11 N3 C15 120.0 . . ?
C15 N3 H3A 120.0 . . ?
N3 C11 H11 120.0 . . ?
N3 C11 C12 120.0 . . ?
C12 C11 H11 120.0 . . ?
C11 C12 P3 119.3(3) . . ?
C13 C12 P3 120.6(3) . . ?
C13 C12 C11 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C13 C14 C15 120.0 . . ?
C15 C14 H14 120.0 . . ?
N3 C15 C15 118.4(9) . 2_666 ?
C14 C15 N3 120.0 . . ?
C14 C15 C15 121.6(9) . 2_666 ?
C2 C0AA H0AA 119.5 . . ?
C4 C0AA H0AA 119.5 . . ?
C4 C0AA C2 120.9(6) . . ?
N1 C1 H1A 120.0 . . ?
N1 C1 C2 120.1(6) . . ?
C2 C1 H1A 120.0 . . ?
C0AA C2 P1 121.5(5) . . ?
C1 C2 P1 120.7(5) . . ?
C1 C2 C0AA 117.8(6) . . ?
C0AA C4 H4 120.1 . . ?
C0AA C4 C5 119.8(7) . . ?
C5 C4 H4 120.1 . . ?
N1 C5 C4 118.6(6) . . ?
N1 C5 C6 115.8(6) . . ?
C4 C5 C6 125.6(6) . . ?
N2 C6 C5 113.7(6) . . ?
N2 C6 C7 123.8(6) . . ?
C7 C6 C5 122.5(6) . . ?
C6 C7 H7A 120.7 . . ?
C6 C7 C8 118.6(7) . . ?
C8 C7 H7A 120.7 . . ?
C7 C8 H8 120.6 . . ?
C9 C8 C7 118.8(7) . . ?
C9 C8 H8 120.6 . . ?
C8 C9 P2 121.8(5) . . ?
C10 C9 P2 120.7(6) . . ?
C10 C9 C8 117.4(6) . . ?
N2 C10 C9 124.5(6) . . ?
N2 C10 H10 117.8 . . ?
C9 C10 H10 117.8 . . ?
H16A O16 H16B 109.5 . . ?
H13A O13 H13B 119.0 . . ?
H14A O14 H14B 109.7 . . ?
H20A O20A H20B 109.5 . . ?
H19A O19A H19B 109.5 . . ?
H19C O19B H19D 109.5 . . ?
H15A O15 H15B 109.4 . . ?
H20C O20B H20D 109.4 . . ?

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
O5 H5 O16 0.82 1.92 2.685(9) 155.2 2_766
N1 H1 O13 0.89(8) 1.90(8) 2.672(8) 145(7) .
C14 H14 O20B 0.93 1.56 2.49(2) 174.8 2_666
O14 H14A O9 0.85 1.96 2.780(7) 162.8 1_665
O19A H19B O11 0.85 2.09 2.785(16) 139.3 .

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
P2 C9 C10 N2 -178.6(5) . . . . ?
P3 C12 C13 C14 177.3(3) . . . . ?
O1 P1 O2 Gd1 -24.1(10) . . . 2_767 ?
O1 P1 C2 C0AA -36.5(6) . . . . ?
O1 P1 C2 C1 144.3(5) . . . . ?
O2 P1 O1 Gd1 50.1(16) . . . . ?
O2 P1 C2 C0AA 87.4(6) . . . . ?
O2 P1 C2 C1 -91.7(6) . . . . ?
O3 P1 O1 Gd1 -78.8(15) . . . . ?
O3 P1 O2 Gd1 104.8(9) . . . 2_767 ?
O3 P1 C2 C0AA -154.1(6) . . . . ?
O3 P1 C2 C1 26.8(6) . . . . ?
O4 P2 O6 Gd1 -152.2(4) . . . 1_554 ?
O4 P2 C9 C8 25.1(7) . . . . ?
O4 P2 C9 C10 -156.8(6) . . . . ?
O5 P2 O6 Gd1 -27.9(5) . . . 1_554 ?
O5 P2 C9 C8 -92.1(7) . . . . ?
O5 P2 C9 C10 86.1(6) . . . . ?
O6 P2 C9 C8 146.9(6) . . . . ?
O6 P2 C9 C10 -35.0(7) . . . . ?
O7 P3 O9 Gd1 111.9(4) . . . 2_667 ?
O7 P3 C12 C11 -153.5(3) . . . . ?
O7 P3 C12 C13 29.2(4) . . . . ?
O8 P3 O9 Gd1 -14.5(5) . . . 2_667 ?
O8 P3 C12 C11 -32.4(4) . . . . ?
O8 P3 C12 C13 150.3(3) . . . . ?
O9 P3 C12 C11 93.3(3) . . . . ?
O9 P3 C12 C13 -83.9(3) . . . . ?
N1 C1 C2 P1 178.3(5) . . . . ?
N1 C1 C2 C0AA -0.9(9) . . . . ?
N1 C5 C6 N2 3.5(9) . . . . ?
N1 C5 C6 C7 -175.9(7) . . . . ?
N2 C6 C7 C8 1.2(12) . . . . ?
N3 C11 C12 P3 -177.3(3) . . . . ?
N3 C11 C12 C13 0.0 . . . . ?
C11 N3 C15 C14 0.0 . . . . ?
C11 N3 C15 C15 179.4(8) . . . 2_666 ?
C11 C12 C13 C14 0.0 . . . . ?
C12 P3 O9 Gd1 -136.2(3) . . . 2_667 ?
C12 C13 C14 C15 0.0 . . . . ?
C13 C14 C15 N3 0.0 . . . . ?
C13 C14 C15 C15 -179.3(8) . . . 2_666 ?
C15 N3 C11 C12 0.0 . . . . ?
C0AA C4 C5 N1 -0.8(10) . . . . ?
C0AA C4 C5 C6 178.7(7) . . . . ?
C1 N1 C5 C4 1.4(10) . . . . ?
C1 N1 C5 C6 -178.2(6) . . . . ?
C2 P1 O1 Gd1 169.6(14) . . . . ?
C2 P1 O2 Gd1 -142.6(8) . . . 2_767 ?
C2 C0AA C4 C5 -0.6(11) . . . . ?
C4 C0AA C2 P1 -177.7(5) . . . . ?
C4 C0AA C2 C1 1.4(10) . . . . ?
C4 C5 C6 N2 -176.0(6) . . . . ?
C4 C5 C6 C7 4.5(11) . . . . ?
C5 N1 C1 C2 -0.6(10) . . . . ?
C5 C6 C7 C8 -179.4(7) . . . . ?
C6 N2 C10 C9 0.1(10) . . . . ?
C6 C7 C8 C9 -1.4(12) . . . . ?
C7 C8 C9 P2 179.2(6) . . . . ?
C7 C8 C9 C10 1.0(11) . . . . ?
C8 C9 C10 N2 -0.3(11) . . . . ?
C9 P2 O6 Gd1 91.3(5) . . . 1_554 ?
C10 N2 C6 C5 180.0(6) . . . . ?
C10 N2 C6 C7 -0.6(10) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound-3a
_database_code_depnum_ccdc_archive 'CCDC 1477303'
_audit_update_record             
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_audit_creation_date             2016-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        Compound-3a
_chemical_formula_moiety         'C30 H28 Co Gd N6 O20 P6, 6.25(H2 O), 0.25(O)'
_chemical_formula_sum            'C30 H40.50 Co Gd N6 O26.50 P6'
_chemical_formula_weight         1311.18
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.1648(18)
_cell_length_b                   17.1628(12)
_cell_length_c                   23.0284(18)
_cell_angle_alpha                90
_cell_angle_beta                 116.436(2)
_cell_angle_gamma                90
_cell_volume                     8905.9(11)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    6060
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.848
_cell_measurement_theta_min      2.571
_shelx_estimated_absorpt_T_max   0.846
_shelx_estimated_absorpt_T_min   0.405
_exptl_absorpt_coefficient_mu    2.167
_exptl_absorpt_correction_T_max  1.0204
_exptl_absorpt_correction_T_min  0.8405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.956
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5244
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            29738
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.946
_diffrn_reflns_theta_min         1.491
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7646
_reflns_number_total             10663
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.786
_refine_diff_density_min         -1.761
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     737
_refine_ls_number_reflns         10663
_refine_ls_number_restraints     54
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0470
_refine_ls_restrained_S_all      0.979
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0636P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1250
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(P1X) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(O17) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4X) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.005
Uanis(O4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O27A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2X) \\sim Ueq, Uanis(O3X) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.001
3. Others
 Sof(P2)=Sof(O4)=Sof(H4)=1-FVAR(1)
 Sof(P1X)=Sof(O4A)=Sof(H4AA)=FVAR(1)
 Sof(O16)=Sof(O18)=Sof(O17)=Sof(H17)=1-FVAR(2)
 Sof(O2X)=Sof(H2X)=Sof(O4X)=Sof(O3X)=FVAR(2)
 Sof(O19A)=Sof(H19C)=Sof(H19D)=Sof(O20A)=Sof(H20C)=Sof(H20D)=1-FVAR(3)
 Sof(O19)=Sof(H19A)=Sof(H19B)=Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(3)
 Fixed Sof: H26A(0.5) H26B(0.5) O28(0.25) H28A(0.25) H28B(0.25) O29(0.25)
 O27(0.5) H27A(0.5) H27B(0.5) H25A(0.5) H25B(0.5) O27A(0.5) H27C(0.5) H27D(0.5)
4.a Riding coordinates:
 O3(H3), O26(H26A,H26B), O28(H28A,H28B), O22(H22A,H22B), O21(H21A,H21B),
 O23(H23A,H23B), O27(H27A,H27B), O25(H25A,H25B), O4A(H4AA), O27A(H27C,H27D),
 O19A(H19C,H19D)
4.b Free rotating group:
 O24(H24A,H24B)
4.c Rotating group:
 O19(H19A,H19B), O20(H20A,H20B), O20A(H20C,H20D)
4.d Aromatic/amide H refined with riding coordinates:
 C11(H11A), C1(H1), C14(H14), C21(H21), C17(H17A), C24(H24), C10(H10),
 C30(H30), C13(H13A), C27(H27), C3(H3A), C4(H4A), C28(H28), C8(H8), C7(H7),
 C23(H23), C18(H18), C20(H20)
4.e Idealised tetrahedral OH refined as rotating group:
 O11(H11), O13(H13), O17(H17), O2X(H2X), O9(H9), O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Gd01 Gd 0.26122(2) 0.59435(2) 0.03297(2) 0.01897(8) Uani 1 1 d . . . . .
Co02 Co 0.35951(3) 0.72734(3) 0.34232(3) 0.01173(14) Uani 1 1 d . . . . .
P1X P 0.3147(7) 0.8933(9) 0.5383(7) 0.021(4) Uani 0.101(5) 1 d . U . A 2
P5 P 0.23720(6) 0.91975(7) 0.11926(6) 0.0171(3) Uani 1 1 d . . . . .
P3 P 0.40688(7) 0.69100(8) 0.12594(7) 0.0204(3) Uani 1 1 d . . . . .
P4 P 0.38926(6) 0.54082(8) 0.56101(6) 0.0169(3) Uani 1 1 d . . . . .
P1 P 0.20434(6) 0.52278(8) 0.14279(7) 0.0189(3) Uani 1 1 d . . . . .
P6 P 0.58041(7) 0.75900(8) 0.57310(7) 0.0219(3) Uani 1 1 d . . . . .
P2 P 0.33999(8) 0.92243(10) 0.53209(8) 0.0252(5) Uani 0.899(5) 1 d . . . A 1
O14 O 0.24628(17) 0.8748(2) 0.06827(18) 0.0234(8) Uani 1 1 d . . . . .
O10 O 0.44564(17) 0.4997(2) 0.60527(19) 0.0270(9) Uani 1 1 d . . . . .
O11 O 0.38374(19) 0.6235(2) 0.5850(2) 0.0282(9) Uani 1 1 d . . . . .
H11 H 0.4174 0.6443 0.6028 0.042 Uiso 1 1 calc GR . . . .
O7 O 0.34626(17) 0.6670(2) 0.07526(19) 0.0258(9) Uani 1 1 d . . . . .
O13 O 0.24063(17) 1.0097(2) 0.10937(19) 0.0260(9) Uani 1 1 d . . . . .
H13 H 0.2553 1.0177 0.0835 0.039 Uiso 1 1 calc GR . . . .
O12 O 0.33238(17) 0.4985(2) 0.54637(19) 0.0252(9) Uani 1 1 d . . . . .
O15 O 0.18262(16) 0.8999(2) 0.12650(19) 0.0259(9) Uani 1 1 d . . . . .
O3 O 0.22398(17) 0.4444(2) 0.17951(19) 0.0252(9) Uani 1 1 d . . . . .
H3 H 0.1961 0.4259 0.1858 0.038 Uiso 1 1 d R . . . .
O16 O 0.63942(18) 0.7947(3) 0.5856(2) 0.0296(11) Uani 0.910(6) 1 d . . . B 1
O1 O 0.24655(17) 0.5446(2) 0.11498(18) 0.0255(9) Uani 1 1 d . . . . .
O5 O 0.29381(19) 0.9801(2) 0.5268(2) 0.0352(10) Uani 1 1 d . . . . .
O8 O 0.4176(2) 0.7767(2) 0.1334(2) 0.0345(10) Uani 1 1 d . . . . .
O2 O 0.13975(18) 0.5164(3) 0.0963(2) 0.0370(10) Uani 1 1 d . . . . .
O18 O 0.5570(2) 0.7776(3) 0.6209(2) 0.0312(12) Uani 0.910(6) 1 d . . . B 1
O17 O 0.58042(19) 0.6695(2) 0.5625(2) 0.0303(12) Uani 0.910(6) 1 d . U . B 1
H17 H 0.6153 0.6543 0.5736 0.045 Uiso 0.910(6) 1 calc GR . . B 1
O19 O 0.2547(5) 0.7097(5) 0.1017(4) 0.013(3) Uani 0.52(3) 1 d . . . C 1
H19A H 0.2740 0.6987 0.1433 0.020 Uiso 0.52(3) 1 d GR . . C 1
H19B H 0.2172 0.7192 0.0917 0.020 Uiso 0.52(3) 1 d GR . . C 1
O20 O 0.1634(4) 0.6483(8) -0.0157(5) 0.021(3) Uani 0.52(3) 1 d . . . C 1
H20A H 0.1509 0.6533 -0.0577 0.031 Uiso 0.52(3) 1 d GR . . C 1
H20B H 0.1639 0.6946 0.0012 0.031 Uiso 0.52(3) 1 d GR . . C 1
O2X O 0.5421(17) 0.678(2) 0.5879(19) 0.016(9) Uani 0.090(6) 1 d . U . B 2
H2X H 0.5584 0.6674 0.6275 0.024 Uiso 0.090(6) 1 calc GR . . B 2
O4X O 0.6310(16) 0.730(2) 0.5657(19) 0.015(9) Uani 0.090(6) 1 d . U . B 2
O3X O 0.5842(17) 0.823(2) 0.6154(19) 0.017(9) Uani 0.090(6) 1 d . U . B 2
O9 O 0.45682(17) 0.6495(2) 0.11528(19) 0.0245(8) Uani 1 1 d . . . . .
H9 H 0.4462 0.6038 0.1022 0.037 Uiso 1 1 calc GR . . . .
O24 O 0.6691(2) 0.5793(4) 0.7360(3) 0.0586(15) Uani 1 1 d . . . . .
H24A H 0.6755 0.5812 0.7019 0.088 Uiso 1 1 d G . . . .
H24B H 0.7028 0.5812 0.7708 0.088 Uiso 1 1 d G . . . .
O4 O 0.3908(2) 0.9626(3) 0.5203(2) 0.0350(12) Uani 0.899(5) 1 d . . . A 1
H4 H 0.3758 0.9947 0.4897 0.052 Uiso 0.899(5) 1 calc GR . . A 1
O6 O 0.3676(2) 0.8730(3) 0.5897(2) 0.0492(13) Uani 1 1 d . . . . .
N1 N 0.28283(18) 0.6805(2) 0.2875(2) 0.0140(8) Uani 1 1 d . . . . .
N3 N 0.39599(17) 0.6748(2) 0.29550(19) 0.0115(8) Uani 1 1 d . . . . .
N4 N 0.37976(18) 0.6338(2) 0.3945(2) 0.0129(8) Uani 1 1 d . . . . .
N6 N 0.34688(18) 0.8209(2) 0.29082(19) 0.0120(8) Uani 1 1 d . . . . .
N5 N 0.43438(18) 0.7771(2) 0.39869(19) 0.0127(8) Uani 1 1 d . . . . .
N2 N 0.3167(2) 0.7740(2) 0.3860(2) 0.0172(9) Uani 1 1 d . . . . .
C11 C 0.3986(2) 0.7007(3) 0.2417(2) 0.0133(10) Uani 1 1 d . . . . .
H11A H 0.3899 0.7538 0.2297 0.016 Uiso 1 1 calc R . . . .
C15 C 0.4129(2) 0.6002(3) 0.3158(2) 0.0106(9) Uani 1 1 d . . . . .
C1 C 0.2699(2) 0.6289(3) 0.2387(2) 0.0157(10) Uani 1 1 d . . . . .
H1 H 0.3004 0.6155 0.2270 0.019 Uiso 1 1 calc R . . . .
C14 C 0.4296(2) 0.5494(3) 0.2802(2) 0.0154(10) Uani 1 1 d . . . . .
H14 H 0.4414 0.4976 0.2947 0.018 Uiso 1 1 calc R . . . .
C29 C 0.5254(2) 0.7939(3) 0.4947(3) 0.0183(11) Uani 1 1 d . . . . .
C21 C 0.3008(2) 0.8370(3) 0.2336(2) 0.0146(10) Uani 1 1 d . . . . .
H21 H 0.2674 0.8032 0.2177 0.018 Uiso 1 1 calc R . . . .
C17 C 0.4299(2) 0.5118(3) 0.4096(2) 0.0142(10) Uani 1 1 d . . . . .
H17A H 0.4485 0.4737 0.3950 0.017 Uiso 1 1 calc R . . . .
C12 C 0.4137(2) 0.6522(3) 0.2031(2) 0.0165(10) Uani 1 1 d . . . . .
C22 C 0.3001(2) 0.9012(3) 0.1967(2) 0.0136(9) Uani 1 1 d . . . . .
C24 C 0.3952(2) 0.9362(3) 0.2814(3) 0.0191(11) Uani 1 1 d . . . . .
H24 H 0.4282 0.9706 0.2989 0.023 Uiso 1 1 calc R . . . .
C10 C 0.3391(2) 0.8229(3) 0.4365(3) 0.0187(11) Uani 1 1 d . . . . .
H10 H 0.3802 0.8349 0.4548 0.022 Uiso 1 1 calc R . . . .
C26 C 0.4400(2) 0.8494(3) 0.3787(2) 0.0164(10) Uani 1 1 d . . . . .
C30 C 0.4773(2) 0.7501(3) 0.4541(2) 0.0168(10) Uani 1 1 d . . . . .
H30 H 0.4745 0.6979 0.4661 0.020 Uiso 1 1 calc R . . . .
C5 C 0.2390(2) 0.6999(3) 0.3045(3) 0.0205(11) Uani 1 1 d . . . . .
C13 C 0.4287(2) 0.5760(3) 0.2228(2) 0.0184(11) Uani 1 1 d . . . . .
H13A H 0.4385 0.5414 0.1969 0.022 Uiso 1 1 calc R . . . .
C27 C 0.4870(3) 0.8973(3) 0.4175(3) 0.0304(14) Uani 1 1 d . . . . .
H27 H 0.4900 0.9485 0.4036 0.036 Uiso 1 1 calc R . . . .
C9 C 0.3054(3) 0.8567(3) 0.4633(3) 0.0264(13) Uani 1 1 d . . . . .
C3 C 0.1703(3) 0.6172(3) 0.2216(3) 0.0243(12) Uani 1 1 d . . . . .
H3A H 0.1313 0.5966 0.1986 0.029 Uiso 1 1 calc R . . . .
C4 C 0.1827(3) 0.6695(3) 0.2716(3) 0.0286(13) Uani 1 1 d . . . . .
H4A H 0.1524 0.6844 0.2834 0.034 Uiso 1 1 calc R . . . .
C28 C 0.5290(3) 0.8703(3) 0.4761(3) 0.0320(14) Uani 1 1 d . . . . .
H28 H 0.5602 0.9034 0.5039 0.038 Uiso 1 1 calc R . . . .
C6 C 0.2585(3) 0.7545(3) 0.3593(3) 0.0236(12) Uani 1 1 d . . . . .
C8 C 0.2465(3) 0.8375(4) 0.4357(4) 0.0426(17) Uani 1 1 d . . . . .
H8 H 0.2217 0.8597 0.4527 0.051 Uiso 1 1 calc R . . . .
C7 C 0.2221(3) 0.7869(4) 0.3840(4) 0.0406(17) Uani 1 1 d . . . . .
H7 H 0.1811 0.7743 0.3654 0.049 Uiso 1 1 calc R . . . .
C16 C 0.4077(2) 0.5790(3) 0.3748(2) 0.0111(9) Uani 1 1 d . . . . .
C19 C 0.3953(2) 0.5554(3) 0.4864(2) 0.0114(9) Uani 1 1 d . . . . .
C23 C 0.3488(2) 0.9500(3) 0.2208(2) 0.0177(11) Uani 1 1 d . . . . .
H23 H 0.3504 0.9932 0.1958 0.021 Uiso 1 1 calc R . . . .
C2 C 0.2150(2) 0.5946(3) 0.2049(2) 0.0158(10) Uani 1 1 d . . . . .
C18 C 0.4246(2) 0.5007(3) 0.4668(2) 0.0145(10) Uani 1 1 d . . . . .
H18 H 0.4410 0.4555 0.4923 0.017 Uiso 1 1 calc R . . . .
C20 C 0.3735(2) 0.6211(3) 0.4481(2) 0.0145(10) Uani 1 1 d . . . . .
H20 H 0.3531 0.6589 0.4608 0.017 Uiso 1 1 calc R . . . .
C25 C 0.3928(2) 0.8715(3) 0.3158(2) 0.0135(10) Uani 1 1 d . . . . .
O26 O 0.5000 1.1529(4) 0.7500 0.079(3) Uani 1 2 d S T P D 2
H26A H 0.5088 1.1916 0.7772 0.118 Uiso 0.5 1 d R . . D 2
H26B H 0.5283 1.1186 0.7648 0.118 Uiso 0.5 1 d R . . D 2
O28 O 0.4360(9) 1.0354(14) 0.6599(11) 0.066(7) Uani 0.25 1 d . . . E 1
H28A H 0.4364 1.0674 0.6894 0.098 Uiso 0.25 1 d R . . E 1
H28B H 0.4718 1.0185 0.6710 0.098 Uiso 0.25 1 d R . . E 1
O29 O 0.5222(9) 0.9945(12) 0.7800(12) 0.063(7) Uani 0.25 1 d . U . F 2
O22 O 0.5845(3) 0.6840(4) 0.7311(3) 0.0791(19) Uani 1 1 d . . . . .
H22A H 0.5872 0.7318 0.7446 0.119 Uiso 1 1 d R . . . .
H22B H 0.6189 0.6614 0.7508 0.119 Uiso 1 1 d R . . . .
O21 O 0.4358(2) 0.7482(3) 0.5764(3) 0.0519(13) Uani 1 1 d . . . . .
H21A H 0.4714 0.7286 0.5937 0.078 Uiso 1 1 d R . . . .
H21B H 0.4294 0.7718 0.6061 0.078 Uiso 1 1 d R . . . .
O23 O 0.5097(3) 0.9211(3) 0.6339(4) 0.098(3) Uani 1 1 d . . . . .
H23A H 0.5341 0.9188 0.6165 0.147 Uiso 1 1 d R . . . .
H23B H 0.4734 0.9170 0.6038 0.147 Uiso 1 1 d R . . . .
O27 O 0.5578(6) 0.8148(10) 0.7903(8) 0.108(6) Uani 0.5 1 d . . . G 2
H27A H 0.5222 0.8319 0.7654 0.162 Uiso 0.5 1 d R . . G 2
H27B H 0.5833 0.8523 0.7978 0.162 Uiso 0.5 1 d R . . G 2
O25 O 0.5000 0.6028(5) 0.7500 0.138(5) Uani 1 2 d S TU P . .
H25A H 0.4870 0.6327 0.7714 0.207 Uiso 0.5 1 d R . . . .
H25B H 0.5333 0.6213 0.7529 0.207 Uiso 0.5 1 d R . . . .
O4A O 0.2723(18) 0.880(2) 0.570(2) 0.030(10) Uani 0.101(5) 1 d . U . A 2
H4AA H 0.2877 0.8482 0.6009 0.045 Uiso 0.101(5) 1 d R . . A 2
O27A O 0.4399(8) 0.8922(12) 0.7243(9) 0.131(7) Uani 0.5 1 d . U . H 1
H27C H 0.4265 0.8460 0.7094 0.197 Uiso 0.5 1 d R . . H 1
H27D H 0.4256 0.9260 0.6928 0.197 Uiso 0.5 1 d R . . H 1
O19A O 0.2298(12) 0.7101(8) 0.064(2) 0.085(11) Uani 0.48(3) 1 d . . . C 2
H19C H 0.2523 0.7487 0.0640 0.127 Uiso 0.48(3) 1 d R . . C 2
H19D H 0.2335 0.7034 0.1033 0.127 Uiso 0.48(3) 1 d R . . C 2
O20A O 0.1516(9) 0.6185(14) -0.0447(17) 0.074(9) Uani 0.48(3) 1 d . . . C 2
H20C H 0.1329 0.6525 -0.0270 0.111 Uiso 0.48(3) 1 d GR . . C 2
H20D H 0.1285 0.5723 -0.0558 0.111 Uiso 0.48(3) 1 d GR . . C 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd01 O14 2.315(4) 7_565 ?
Gd01 O7 2.287(4) . ?
Gd01 O12 2.312(4) 6_565 ?
Gd01 O1 2.248(4) . ?
Gd01 O5 2.442(4) 4_545 ?
Gd01 O19 2.585(9) . ?
Gd01 O20 2.391(10) . ?
Gd01 O19A 2.365(14) . ?
Gd01 O20A 2.57(2) . ?
Co02 N1 1.948(4) . ?
Co02 N3 1.923(4) . ?
Co02 N4 1.933(4) . ?
Co02 N6 1.936(4) . ?
Co02 N5 1.946(4) . ?
Co02 N2 1.945(4) . ?
P1X O5 1.562(15) . ?
P1X O6 1.376(16) . ?
P1X C9 1.754(16) . ?
P1X O4A 1.56(4) . ?
P5 O14 1.505(4) . ?
P5 O13 1.568(4) . ?
P5 O15 1.495(4) . ?
P5 C22 1.809(5) . ?
P3 O7 1.508(4) . ?
P3 O8 1.492(4) . ?
P3 O9 1.556(4) . ?
P3 C12 1.832(5) . ?
P4 O10 1.504(4) . ?
P4 O11 1.551(4) . ?
P4 O12 1.504(4) . ?
P4 C19 1.809(5) . ?
P1 O3 1.548(4) . ?
P1 O1 1.511(4) . ?
P1 O2 1.500(4) . ?
P1 C2 1.815(5) . ?
P6 O16 1.510(4) . ?
P6 O18 1.495(5) . ?
P6 O17 1.555(4) . ?
P6 O2X 1.80(4) . ?
P6 O4X 1.45(4) . ?
P6 O3X 1.44(4) . ?
P6 C29 1.819(5) . ?
P2 O5 1.489(4) . ?
P2 O4 1.579(5) . ?
P2 O6 1.464(5) . ?
P2 C9 1.821(6) . ?
O14 Gd01 2.315(4) 7_565 ?
O11 H11 0.8400 . ?
O13 H13 0.8400 . ?
O12 Gd01 2.312(4) 6_566 ?
O3 H3 0.8385 . ?
O5 Gd01 2.442(4) 4 ?
O17 H17 0.8400 . ?
O19 H19A 0.8818 . ?
O19 H19B 0.8820 . ?
O20 H20A 0.8788 . ?
O20 H20B 0.8815 . ?
O2X H2X 0.8400 . ?
O9 H9 0.8400 . ?
O24 H24A 0.8700 . ?
O24 H24B 0.8704 . ?
O4 H4 0.8400 . ?
N1 C1 1.352(6) . ?
N1 C5 1.365(6) . ?
N3 C11 1.346(6) . ?
N3 C15 1.364(6) . ?
N4 C16 1.368(6) . ?
N4 C20 1.329(6) . ?
N6 C21 1.341(6) . ?
N6 C25 1.353(6) . ?
N5 C26 1.351(6) . ?
N5 C30 1.334(6) . ?
N2 C10 1.337(7) . ?
N2 C6 1.354(7) . ?
C11 H11A 0.9500 . ?
C11 C12 1.387(6) . ?
C15 C14 1.385(6) . ?
C15 C16 1.466(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.380(7) . ?
C14 H14 0.9500 . ?
C14 C13 1.389(7) . ?
C29 C30 1.377(7) . ?
C29 C28 1.394(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.387(6) . ?
C17 H17A 0.9500 . ?
C17 C16 1.373(6) . ?
C17 C18 1.394(7) . ?
C12 C13 1.381(7) . ?
C22 C23 1.381(7) . ?
C24 H24 0.9500 . ?
C24 C23 1.384(7) . ?
C24 C25 1.382(7) . ?
C10 H10 0.9500 . ?
C10 C9 1.379(7) . ?
C26 C27 1.391(7) . ?
C26 C25 1.456(7) . ?
C30 H30 0.9500 . ?
C5 C4 1.378(8) . ?
C5 C6 1.471(8) . ?
C13 H13A 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.373(8) . ?
C9 C8 1.367(9) . ?
C3 H3A 0.9500 . ?
C3 C4 1.382(8) . ?
C3 C2 1.397(7) . ?
C4 H4A 0.9500 . ?
C28 H28 0.9500 . ?
C6 C7 1.389(7) . ?
C8 H8 0.9500 . ?
C8 C7 1.379(9) . ?
C7 H7 0.9500 . ?
C19 C18 1.387(6) . ?
C19 C20 1.386(6) . ?
C23 H23 0.9500 . ?
C18 H18 0.9500 . ?
C20 H20 0.9500 . ?
O26 H26A 0.8705 . ?
O26 H26B 0.8686 . ?
O28 H28A 0.8710 . ?
O28 H28B 0.8682 . ?
O29 O29 1.34(5) 2_656 ?
O22 H22A 0.8701 . ?
O22 H22B 0.8696 . ?
O21 H21A 0.8703 . ?
O21 H21B 0.8703 . ?
O23 H23A 0.8684 . ?
O23 H23B 0.8706 . ?
O27 H27A 0.8702 . ?
O27 H27B 0.8695 . ?
O25 H25A 0.8702 . ?
O25 H25B 0.8702 . ?
O4A H4AA 0.8397 . ?
O27A H27C 0.8695 . ?
O27A H27D 0.8705 . ?
O19A H19C 0.8717 . ?
O19A H19D 0.8727 . ?
O20A H20C 0.9469 . ?
O20A H20D 0.9487 . ?

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
O14 Gd01 O5 81.08(13) 7_565 4_545 ?
O14 Gd01 O19 116.2(2) 7_565 . ?
O14 Gd01 O20 80.4(2) 7_565 . ?
O14 Gd01 O19A 103.0(9) 7_565 . ?
O14 Gd01 O20A 71.4(5) 7_565 . ?
O7 Gd01 O14 86.85(13) . 7_565 ?
O7 Gd01 O12 78.27(13) . 6_565 ?
O7 Gd01 O5 150.08(14) . 4_545 ?
O7 Gd01 O19 67.9(3) . . ?
O7 Gd01 O20 124.1(4) . . ?
O7 Gd01 O19A 77.8(6) . . ?
O7 Gd01 O20A 136.1(5) . . ?
O12 Gd01 O14 90.18(13) 6_565 7_565 ?
O12 Gd01 O5 74.52(14) 6_565 4_545 ?
O12 Gd01 O19 134.6(3) 6_565 . ?
O12 Gd01 O20 154.7(3) 6_565 . ?
O12 Gd01 O19A 151.9(9) 6_565 . ?
O12 Gd01 O20A 137.1(8) 6_565 . ?
O1 Gd01 O14 164.32(14) . 7_565 ?
O1 Gd01 O7 108.79(14) . . ?
O1 Gd01 O12 91.91(14) . 6_565 ?
O1 Gd01 O5 84.51(14) . 4_545 ?
O1 Gd01 O19 72.4(2) . . ?
O1 Gd01 O20 91.2(3) . . ?
O1 Gd01 O19A 82.1(7) . . ?
O1 Gd01 O20A 96.8(4) . . ?
O5 Gd01 O19 141.8(3) 4_545 . ?
O5 Gd01 O20A 64.7(7) 4_545 . ?
O20 Gd01 O5 80.8(3) . 4_545 ?
O20 Gd01 O19 70.0(3) . . ?
O19A Gd01 O5 131.6(6) . 4_545 ?
O19A Gd01 O20A 71.0(6) . . ?
N3 Co02 N1 91.47(17) . . ?
N3 Co02 N4 84.26(16) . . ?
N3 Co02 N6 91.99(16) . . ?
N3 Co02 N5 91.03(16) . . ?
N3 Co02 N2 174.85(18) . . ?
N4 Co02 N1 88.33(17) . . ?
N4 Co02 N6 174.52(17) . . ?
N4 Co02 N5 92.34(17) . . ?
N4 Co02 N2 94.21(16) . . ?
N6 Co02 N1 95.77(17) . . ?
N6 Co02 N5 83.73(17) . . ?
N6 Co02 N2 89.87(16) . . ?
N5 Co02 N1 177.46(16) . . ?
N2 Co02 N1 83.56(18) . . ?
N2 Co02 N5 93.95(17) . . ?
O5 P1X C9 106.7(9) . . ?
O5 P1X O4A 88.1(16) . . ?
O6 P1X O5 120.7(11) . . ?
O6 P1X C9 114.3(10) . . ?
O6 P1X O4A 99.2(18) . . ?
O4A P1X C9 126.5(18) . . ?
O14 P5 O13 110.7(2) . . ?
O14 P5 C22 108.0(2) . . ?
O13 P5 C22 103.6(2) . . ?
O15 P5 O14 115.9(2) . . ?
O15 P5 O13 110.7(2) . . ?
O15 P5 C22 107.1(2) . . ?
O7 P3 O9 111.3(2) . . ?
O7 P3 C12 106.1(2) . . ?
O8 P3 O7 115.3(2) . . ?
O8 P3 O9 110.6(2) . . ?
O8 P3 C12 108.2(2) . . ?
O9 P3 C12 104.7(2) . . ?
O10 P4 O11 113.2(2) . . ?
O10 P4 O12 116.2(2) . . ?
O10 P4 C19 104.8(2) . . ?
O11 P4 C19 105.7(2) . . ?
O12 P4 O11 107.2(2) . . ?
O12 P4 C19 109.2(2) . . ?
O3 P1 C2 105.1(2) . . ?
O1 P1 O3 109.4(2) . . ?
O1 P1 C2 106.3(2) . . ?
O2 P1 O3 107.9(2) . . ?
O2 P1 O1 117.3(2) . . ?
O2 P1 C2 110.2(2) . . ?
O16 P6 O17 111.2(3) . . ?
O16 P6 C29 107.8(3) . . ?
O18 P6 O16 116.7(3) . . ?
O18 P6 O17 110.7(3) . . ?
O18 P6 C29 106.5(2) . . ?
O17 P6 C29 102.9(2) . . ?
O2X P6 C29 101.8(13) . . ?
O4X P6 O2X 109.1(19) . . ?
O4X P6 C29 108.6(15) . . ?
O3X P6 O2X 110(2) . . ?
O3X P6 O4X 123(2) . . ?
O3X P6 C29 102.3(16) . . ?
O5 P2 O4 111.0(3) . . ?
O5 P2 C9 106.7(3) . . ?
O4 P2 C9 103.4(3) . . ?
O6 P2 O5 119.8(3) . . ?
O6 P2 O4 108.3(3) . . ?
O6 P2 C9 106.3(3) . . ?
P5 O14 Gd01 134.1(2) . 7_565 ?
P4 O11 H11 109.5 . . ?
P3 O7 Gd01 155.6(2) . . ?
P5 O13 H13 109.5 . . ?
P4 O12 Gd01 165.1(2) . 6_566 ?
P1 O3 H3 109.6 . . ?
P1 O1 Gd01 149.2(2) . . ?
P1X O5 Gd01 157.7(6) . 4 ?
P2 O5 Gd01 143.7(3) . 4 ?
P6 O17 H17 109.5 . . ?
Gd01 O19 H19A 110.3 . . ?
Gd01 O19 H19B 109.5 . . ?
H19A O19 H19B 109.2 . . ?
Gd01 O20 H20A 110.0 . . ?
Gd01 O20 H20B 109.4 . . ?
H20A O20 H20B 109.1 . . ?
P6 O2X H2X 109.5 . . ?
P3 O9 H9 109.5 . . ?
H24A O24 H24B 109.5 . . ?
P2 O4 H4 109.5 . . ?
C1 N1 Co02 127.7(3) . . ?
C1 N1 C5 118.1(4) . . ?
C5 N1 Co02 114.1(3) . . ?
C11 N3 Co02 126.4(3) . . ?
C11 N3 C15 119.4(4) . . ?
C15 N3 Co02 113.6(3) . . ?
C16 N4 Co02 113.4(3) . . ?
C20 N4 Co02 127.3(3) . . ?
C20 N4 C16 119.1(4) . . ?
C21 N6 Co02 127.4(3) . . ?
C21 N6 C25 119.1(4) . . ?
C25 N6 Co02 113.3(3) . . ?
C26 N5 Co02 113.1(3) . . ?
C30 N5 Co02 128.0(3) . . ?
C30 N5 C26 118.8(4) . . ?
C10 N2 Co02 126.3(4) . . ?
C10 N2 C6 120.1(4) . . ?
C6 N2 Co02 113.6(3) . . ?
N3 C11 H11A 119.0 . . ?
N3 C11 C12 122.1(4) . . ?
C12 C11 H11A 119.0 . . ?
N3 C15 C14 121.1(4) . . ?
N3 C15 C16 114.1(4) . . ?
C14 C15 C16 124.6(4) . . ?
N1 C1 H1 118.0 . . ?
N1 C1 C2 124.0(5) . . ?
C2 C1 H1 118.0 . . ?
C15 C14 H14 120.7 . . ?
C15 C14 C13 118.5(4) . . ?
C13 C14 H14 120.7 . . ?
C30 C29 P6 123.0(4) . . ?
C30 C29 C28 117.5(5) . . ?
C28 C29 P6 119.3(4) . . ?
N6 C21 H21 118.8 . . ?
N6 C21 C22 122.4(4) . . ?
C22 C21 H21 118.8 . . ?
C16 C17 H17A 120.6 . . ?
C16 C17 C18 118.7(4) . . ?
C18 C17 H17A 120.6 . . ?
C11 C12 P3 118.0(4) . . ?
C13 C12 P3 123.8(4) . . ?
C13 C12 C11 118.0(4) . . ?
C21 C22 P5 120.7(4) . . ?
C23 C22 P5 121.3(4) . . ?
C23 C22 C21 118.0(5) . . ?
C23 C24 H24 120.5 . . ?
C25 C24 H24 120.5 . . ?
C25 C24 C23 118.9(5) . . ?
N2 C10 H10 118.4 . . ?
N2 C10 C9 123.2(5) . . ?
C9 C10 H10 118.4 . . ?
N5 C26 C27 120.8(5) . . ?
N5 C26 C25 114.5(4) . . ?
C27 C26 C25 124.6(5) . . ?
N5 C30 C29 123.5(5) . . ?
N5 C30 H30 118.2 . . ?
C29 C30 H30 118.2 . . ?
N1 C5 C4 121.1(5) . . ?
N1 C5 C6 113.4(5) . . ?
C4 C5 C6 125.5(5) . . ?
C14 C13 H13A 119.7 . . ?
C12 C13 C14 120.6(4) . . ?
C12 C13 H13A 119.7 . . ?
C26 C27 H27 120.2 . . ?
C28 C27 C26 119.6(5) . . ?
C28 C27 H27 120.2 . . ?
C10 C9 P1X 138.8(7) . . ?
C10 C9 P2 119.9(5) . . ?
C8 C9 P1X 100.7(7) . . ?
C8 C9 P2 123.5(4) . . ?
C8 C9 C10 116.6(5) . . ?
C4 C3 H3A 120.0 . . ?
C4 C3 C2 120.0(5) . . ?
C2 C3 H3A 120.0 . . ?
C5 C4 C3 119.9(5) . . ?
C5 C4 H4A 120.0 . . ?
C3 C4 H4A 120.0 . . ?
C29 C28 H28 120.2 . . ?
C27 C28 C29 119.5(5) . . ?
C27 C28 H28 120.2 . . ?
N2 C6 C5 115.3(4) . . ?
N2 C6 C7 119.4(5) . . ?
C7 C6 C5 125.2(6) . . ?
C9 C8 H8 119.2 . . ?
C9 C8 C7 121.7(5) . . ?
C7 C8 H8 119.2 . . ?
C6 C7 H7 120.5 . . ?
C8 C7 C6 119.0(6) . . ?
C8 C7 H7 120.5 . . ?
N4 C16 C15 114.0(4) . . ?
N4 C16 C17 121.3(4) . . ?
C17 C16 C15 124.6(4) . . ?
C18 C19 P4 119.8(4) . . ?
C20 C19 P4 122.7(4) . . ?
C20 C19 C18 117.4(4) . . ?
C22 C23 C24 120.0(4) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C1 C2 P1 119.6(4) . . ?
C1 C2 C3 116.9(5) . . ?
C3 C2 P1 123.5(4) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 C17 120.2(4) . . ?
C19 C18 H18 119.9 . . ?
N4 C20 C19 123.2(4) . . ?
N4 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
N6 C25 C24 121.3(5) . . ?
N6 C25 C26 114.8(4) . . ?
C24 C25 C26 123.8(5) . . ?
H26A O26 H26B 109.4 . . ?
H28A O28 H28B 109.3 . . ?
H22A O22 H22B 109.5 . . ?
H21A O21 H21B 109.5 . . ?
H23A O23 H23B 109.6 . . ?
H27A O27 H27B 109.5 . . ?
H25A O25 H25B 109.5 . . ?
P1X O4A H4AA 109.3 . . ?
H27C O27A H27D 109.5 . . ?
Gd01 O19A H19C 109.3 . . ?
Gd01 O19A H19D 107.9 . . ?
H19C O19A H19D 109.4 . . ?
Gd01 O20A H20C 112.6 . . ?
Gd01 O20A H20D 113.1 . . ?
H20C O20A H20D 105.7 . . ?

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
Co02 N1 C1 C2 175.7(3) . . . . ?
Co02 N1 C5 C4 -178.0(4) . . . . ?
Co02 N1 C5 C6 2.0(5) . . . . ?
Co02 N3 C11 C12 -165.3(4) . . . . ?
Co02 N3 C15 C14 167.9(4) . . . . ?
Co02 N3 C15 C16 -8.3(5) . . . . ?
Co02 N4 C16 C15 -4.0(5) . . . . ?
Co02 N4 C16 C17 174.3(4) . . . . ?
Co02 N4 C20 C19 -172.6(4) . . . . ?
Co02 N6 C21 C22 -171.0(3) . . . . ?
Co02 N6 C25 C24 171.1(4) . . . . ?
Co02 N6 C25 C26 -5.1(5) . . . . ?
Co02 N5 C26 C27 171.5(4) . . . . ?
Co02 N5 C26 C25 -6.9(5) . . . . ?
Co02 N5 C30 C29 -171.5(4) . . . . ?
Co02 N2 C10 C9 176.9(4) . . . . ?
Co02 N2 C6 C5 2.2(6) . . . . ?
Co02 N2 C6 C7 -176.9(5) . . . . ?
P1X C9 C8 C7 -161.6(8) . . . . ?
P5 C22 C23 C24 177.4(4) . . . . ?
P3 C12 C13 C14 -176.1(4) . . . . ?
P4 C19 C18 C17 -179.4(4) . . . . ?
P4 C19 C20 N4 177.3(4) . . . . ?
P6 C29 C30 N5 174.9(4) . . . . ?
P6 C29 C28 C27 -178.9(5) . . . . ?
P2 C9 C8 C7 -179.4(6) . . . . ?
O14 P5 C22 C21 -86.4(4) . . . . ?
O14 P5 C22 C23 93.5(4) . . . . ?
O10 P4 O12 Gd01 -19.0(10) . . . 6_566 ?
O10 P4 C19 C18 33.3(4) . . . . ?
O10 P4 C19 C20 -144.4(4) . . . . ?
O11 P4 O12 Gd01 -146.7(9) . . . 6_566 ?
O11 P4 C19 C18 153.2(4) . . . . ?
O11 P4 C19 C20 -24.6(5) . . . . ?
O7 P3 C12 C11 -93.9(4) . . . . ?
O7 P3 C12 C13 81.1(5) . . . . ?
O13 P5 O14 Gd01 -19.6(4) . . . 7_565 ?
O13 P5 C22 C21 156.1(4) . . . . ?
O13 P5 C22 C23 -24.0(5) . . . . ?
O12 P4 C19 C18 -91.8(4) . . . . ?
O12 P4 C19 C20 90.4(4) . . . . ?
O15 P5 O14 Gd01 107.5(3) . . . 7_565 ?
O15 P5 C22 C21 39.1(4) . . . . ?
O15 P5 C22 C23 -141.1(4) . . . . ?
O3 P1 O1 Gd01 140.3(4) . . . . ?
O3 P1 C2 C1 85.7(4) . . . . ?
O3 P1 C2 C3 -93.3(4) . . . . ?
O16 P6 C29 C30 147.9(4) . . . . ?
O16 P6 C29 C28 -36.9(5) . . . . ?
O1 P1 C2 C1 -30.3(4) . . . . ?
O1 P1 C2 C3 150.7(4) . . . . ?
O5 P1X C9 C10 122.2(9) . . . . ?
O5 P1X C9 C8 -82.9(10) . . . . ?
O5 P2 C9 C10 149.1(4) . . . . ?
O5 P2 C9 C8 -31.3(6) . . . . ?
O8 P3 O7 Gd01 -139.9(5) . . . . ?
O8 P3 C12 C11 30.3(5) . . . . ?
O8 P3 C12 C13 -154.7(4) . . . . ?
O2 P1 O1 Gd01 17.1(6) . . . . ?
O2 P1 C2 C1 -158.3(4) . . . . ?
O2 P1 C2 C3 22.7(5) . . . . ?
O18 P6 C29 C30 -86.2(5) . . . . ?
O18 P6 C29 C28 89.1(5) . . . . ?
O17 P6 C29 C30 30.3(5) . . . . ?
O17 P6 C29 C28 -154.4(5) . . . . ?
O2X P6 C29 C30 -17.2(13) . . . . ?
O2X P6 C29 C28 158.1(13) . . . . ?
O4X P6 C29 C30 97.9(16) . . . . ?
O4X P6 C29 C28 -86.8(16) . . . . ?
O3X P6 C29 C30 -130.6(17) . . . . ?
O3X P6 C29 C28 44.7(17) . . . . ?
O9 P3 O7 Gd01 93.1(6) . . . . ?
O9 P3 C12 C11 148.3(4) . . . . ?
O9 P3 C12 C13 -36.7(5) . . . . ?
O4 P2 O5 Gd01 37.8(5) . . . 4 ?
O4 P2 C9 C10 32.0(5) . . . . ?
O4 P2 C9 C8 -148.4(6) . . . . ?
O6 P1X O5 Gd01 158.8(9) . . . 4 ?
O6 P1X C9 C10 -13.9(19) . . . . ?
O6 P1X C9 C8 141.0(11) . . . . ?
O6 P2 O5 Gd01 165.3(4) . . . 4 ?
O6 P2 C9 C10 -82.0(5) . . . . ?
O6 P2 C9 C8 97.6(6) . . . . ?
N1 C1 C2 P1 -177.1(4) . . . . ?
N1 C1 C2 C3 2.0(7) . . . . ?
N1 C5 C4 C3 1.4(8) . . . . ?
N1 C5 C6 N2 -2.8(7) . . . . ?
N1 C5 C6 C7 176.3(6) . . . . ?
N3 C11 C12 P3 172.6(4) . . . . ?
N3 C11 C12 C13 -2.7(8) . . . . ?
N3 C15 C14 C13 -0.1(7) . . . . ?
N3 C15 C16 N4 8.1(6) . . . . ?
N3 C15 C16 C17 -170.1(4) . . . . ?
N6 C21 C22 P5 179.2(3) . . . . ?
N6 C21 C22 C23 -0.6(7) . . . . ?
N5 C26 C27 C28 1.7(9) . . . . ?
N5 C26 C25 N6 8.1(6) . . . . ?
N5 C26 C25 C24 -168.1(5) . . . . ?
N2 C10 C9 P1X 152.6(10) . . . . ?
N2 C10 C9 P2 179.9(4) . . . . ?
N2 C10 C9 C8 0.3(8) . . . . ?
N2 C6 C7 C8 -0.8(10) . . . . ?
C11 N3 C15 C14 -3.5(7) . . . . ?
C11 N3 C15 C16 -179.8(4) . . . . ?
C11 C12 C13 C14 -1.1(8) . . . . ?
C15 N3 C11 C12 5.0(7) . . . . ?
C15 C14 C13 C12 2.4(8) . . . . ?
C1 N1 C5 C4 -1.7(7) . . . . ?
C1 N1 C5 C6 178.2(4) . . . . ?
C14 C15 C16 N4 -168.0(4) . . . . ?
C14 C15 C16 C17 13.8(8) . . . . ?
C21 N6 C25 C24 -4.9(7) . . . . ?
C21 N6 C25 C26 178.8(4) . . . . ?
C21 C22 C23 C24 -2.8(7) . . . . ?
C12 P3 O7 Gd01 -20.2(6) . . . . ?
C22 P5 O14 Gd01 -132.5(3) . . . 7_565 ?
C10 N2 C6 C5 -179.5(4) . . . . ?
C10 N2 C6 C7 1.4(8) . . . . ?
C10 C9 C8 C7 0.2(10) . . . . ?
C26 N5 C30 C29 4.8(7) . . . . ?
C26 C27 C28 C29 2.8(10) . . . . ?
C30 N5 C26 C27 -5.3(7) . . . . ?
C30 N5 C26 C25 176.2(4) . . . . ?
C30 C29 C28 C27 -3.4(9) . . . . ?
C5 N1 C1 C2 0.0(7) . . . . ?
C5 C6 C7 C8 -179.9(6) . . . . ?
C27 C26 C25 N6 -170.3(5) . . . . ?
C27 C26 C25 C24 13.5(8) . . . . ?
C9 P1X O5 Gd01 26(3) . . . 4 ?
C9 P2 O5 Gd01 -74.1(5) . . . 4 ?
C9 C8 C7 C6 0.1(11) . . . . ?
C4 C5 C6 N2 177.2(5) . . . . ?
C4 C5 C6 C7 -3.8(9) . . . . ?
C4 C3 C2 P1 176.8(4) . . . . ?
C4 C3 C2 C1 -2.3(7) . . . . ?
C28 C29 C30 N5 -0.4(8) . . . . ?
C6 N2 C10 C9 -1.1(7) . . . . ?
C6 C5 C4 C3 -178.6(5) . . . . ?
C16 N4 C20 C19 1.6(7) . . . . ?
C16 C15 C14 C13 175.7(5) . . . . ?
C16 C17 C18 C19 2.4(7) . . . . ?
C19 P4 O12 Gd01 99.2(9) . . . 6_566 ?
C23 C24 C25 N6 1.6(8) . . . . ?
C23 C24 C25 C26 177.5(5) . . . . ?
C2 P1 O1 Gd01 -106.7(5) . . . . ?
C2 C3 C4 C5 0.7(9) . . . . ?
C18 C17 C16 N4 -1.3(7) . . . . ?
C18 C17 C16 C15 176.8(4) . . . . ?
C18 C19 C20 N4 -0.5(7) . . . . ?
C20 N4 C16 C15 -179.0(4) . . . . ?
C20 N4 C16 C17 -0.7(7) . . . . ?
C20 C19 C18 C17 -1.6(7) . . . . ?
C25 N6 C21 C22 4.5(7) . . . . ?
C25 C24 C23 C22 2.3(8) . . . . ?
C25 C26 C27 C28 179.9(6) . . . . ?
O4A P1X O5 Gd01 -102(2) . . . 4 ?
O4A P1X C9 C10 -137(2) . . . . ?
O4A P1X C9 C8 18(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound-3b
_database_code_depnum_ccdc_archive 'CCDC 1477304'
_audit_update_record             
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_audit_creation_date             2016-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        Compound-3b
_chemical_formula_moiety         'C30 H27 Co Dy N6 O20 P6, 5(H2 O), 1.5(O)'
_chemical_formula_sum            'C30 H37 Co Dy N6 O26.50 P6'
_chemical_formula_weight         1312.90
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.1186(12)
_cell_length_b                   17.0759(9)
_cell_length_c                   22.9551(14)
_cell_angle_alpha                90
_cell_angle_beta                 116.0600(10)
_cell_angle_gamma                90
_cell_volume                     8845.0(8)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2788
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      23.350
_cell_measurement_theta_min      2.582
_shelx_estimated_absorpt_T_max   0.954
_shelx_estimated_absorpt_T_min   0.556
_exptl_absorpt_coefficient_mu    2.371
_exptl_absorpt_correction_T_max  0.8198
_exptl_absorpt_correction_T_min  0.7169
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.972
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5232
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0795
_diffrn_reflns_av_unetI/netI     0.1377
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26124
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.953
_diffrn_reflns_theta_min         1.495
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6247
_reflns_number_total             10611
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.084
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.166
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.887
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         10611
_refine_ls_number_restraints     99
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0526
_refine_ls_restrained_S_all      4.341
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0387P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1174
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O11-H11
 0.87 with sigma of 0.01
 P4A-H11
 1.945852 with sigma of 0.02
 Dy1-H11
 2.558956 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(P4A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.005
Uanis(O18A) \\sim Ueq, Uanis(O16A) \\sim Ueq, Uanis(O17A) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O18A) \\sim Ueq, Uanis(P6A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.001
Uanis(O30) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O12A) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of
0.0005
Uanis(O10A) \\sim Ueq: with sigma of 0.009 and sigma for terminal atoms of 0.019
Uanis(O20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O19A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O25) \\sim Ueq, Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O40) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(P4A)=Sof(O10A)=Sof(H11)=Sof(O12A)=1-FVAR(1)
 Sof(P4)=Sof(O10)=Sof(O12)=Sof(H12)=FVAR(1)
 Sof(P6A)=Sof(O16A)=Sof(O17A)=Sof(H17A)=Sof(O18A)=1-FVAR(2)
 Sof(P6)=Sof(O16)=Sof(H16)=Sof(O17)=Sof(O18)=FVAR(2)
 Sof(O20A)=Sof(H20C)=Sof(H20D)=1-FVAR(3)
 Sof(O20)=Sof(H20A)=Sof(H20B)=FVAR(3)
 Fixed Sof: O19(0.75) H19A(0.75) H19B(0.75) O19A(0.25) H19C(0.25) H19D(0.25)
 H24A(0.5) H24B(0.5) O25(0.25) H25A(0.25) H25B(0.25) O0AA(0.5) O29(0.25)
 O30(0.25) O40(0.25) H40A(0.25) H40B(0.25) O28(0.5)
5.a Riding coordinates:
 O11(H11), O19A(H19C,H19D), O24(H24A,H24B), O25(H25A,H25B), O40(H40A,H40B),
 O22(H22A,H22B), O27(H27A,H27B), O21(H21A,H21B)
5.b Free rotating group:
 O23(H23A,H23B)
5.c Rotating group:
 O19(H19A,H19B), O20(H20A,H20B), O20A(H20C,H20D)
5.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11A), C13(H13A),
 C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C27(H27),
  C28(H28), C30(H30)
5.e Idealised tetrahedral OH refined as rotating group:
 O2(H2), O6(H6), O12(H12), O13(H13), O16(H16), O17A(H17A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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 0.73783(2) 0.59379(2) 0.96674(2) 0.02089(9) Uani 1 1 d D . . . .
Co1 Co 0.64076(4) 0.72808(4) 0.65679(4) 0.0152(2) Uani 1 1 d . . . . .
P1 P 0.59447(9) 0.69234(10) 0.87457(10) 0.0247(4) Uani 1 1 d . . . . .
P2 P 0.61027(8) 0.53927(10) 0.43821(9) 0.0205(4) Uani 1 1 d . . . . .
P3 P 0.79485(8) 0.52374(11) 0.85713(9) 0.0244(4) Uani 1 1 d . . . . .
P4 P 0.66209(15) 0.92357(16) 0.46657(13) 0.0283(8) Uani 0.832(8) 1 d . . . A 1
P4A P 0.6851(9) 0.9006(10) 0.4616(8) 0.047(5) Uani 0.168(8) 1 d D U . A 2
P5 P 0.76330(8) 0.91903(9) 0.88102(9) 0.0202(4) Uani 1 1 d . . . . .
P6 P 0.4192(2) 0.7629(3) 0.4284(3) 0.0221(9) Uani 0.845(8) 1 d . . . B 1
P6A P 0.4273(13) 0.7449(14) 0.4282(15) 0.016(5) Uani 0.155(8) 1 d . U . B 2
O1 O 0.6550(2) 0.6674(3) 0.9244(2) 0.0309(12) Uani 1 1 d . . . . .
O2 O 0.5443(2) 0.6530(3) 0.8858(2) 0.0252(11) Uani 1 1 d . . . . .
H2 H 0.5508 0.6047 0.8914 0.038 Uiso 1 1 calc GR . . . .
O3 O 0.5859(3) 0.7788(3) 0.8672(3) 0.0404(14) Uani 1 1 d . . . . .
O4 O 0.6670(2) 0.4973(3) 0.4525(2) 0.0285(12) Uani 1 1 d . . . . .
O5 O 0.5539(2) 0.4968(3) 0.3951(2) 0.0307(12) Uani 1 1 d . . . . .
O6 O 0.6140(2) 0.6214(3) 0.4126(3) 0.0336(13) Uani 1 1 d . . . . .
H6 H 0.5834 0.6469 0.4062 0.050 Uiso 1 1 calc GR . . . .
O7 O 0.7531(2) 0.5471(3) 0.8849(2) 0.0321(12) Uani 1 1 d . . . . .
O8 O 0.7762(2) 0.4453(2) 0.8218(2) 0.0277(12) Uani 1 1 d . . . . .
O9 O 0.8592(2) 0.5212(4) 0.9026(3) 0.0532(17) Uani 1 1 d . . . . .
O10 O 0.6371(5) 0.8735(6) 0.4089(5) 0.065(3) Uani 0.832(8) 1 d . . . A 1
O10A O 0.621(3) 0.900(3) 0.418(3) 0.064(17) Uani 0.168(8) 1 d . U . A 2
O11 O 0.7077(2) 0.9817(3) 0.4760(3) 0.0497(17) Uani 1 1 d D . . . .
H11 H 0.7413 0.9818 0.5078 0.075 Uiso 0.168(8) 1 d DR . . A 2
O12 O 0.6105(3) 0.9626(4) 0.4761(4) 0.054(3) Uani 0.832(8) 1 d . . . A 1
H12 H 0.6236 1.0008 0.5016 0.081 Uiso 0.832(8) 1 calc GR . . A 1
O12A O 0.7219(14) 0.8836(17) 0.4286(18) 0.043(8) Uani 0.168(8) 1 d . U . A 2
O13 O 0.7614(2) 1.0093(2) 0.8901(3) 0.0321(13) Uani 1 1 d . . . . .
H13 H 0.7467 1.0188 0.9159 0.048 Uiso 1 1 calc GR . . . .
O14 O 0.7542(2) 0.8752(2) 0.9327(2) 0.0239(11) Uani 1 1 d . . . . .
O15 O 0.8171(2) 0.8962(3) 0.8731(2) 0.0286(11) Uani 1 1 d . . . . .
O16 O 0.4199(3) 0.6725(3) 0.4390(3) 0.0370(19) Uani 0.845(8) 1 d . . . B 1
H16 H 0.3849 0.6561 0.4254 0.056 Uiso 0.845(8) 1 calc GR . . B 1
O16A O 0.4558(13) 0.6872(16) 0.4148(16) 0.024(8) Uani 0.155(8) 1 d . U . B 2
O17 O 0.3618(2) 0.7980(4) 0.4165(3) 0.0354(18) Uani 0.845(8) 1 d . . . B 1
O17A O 0.3683(14) 0.7340(18) 0.4362(17) 0.028(9) Uani 0.155(8) 1 d . U . B 2
H17A H 0.3523 0.6912 0.4194 0.042 Uiso 0.155(8) 1 calc GR . . B 2
O18 O 0.4434(3) 0.7793(4) 0.3798(3) 0.0368(18) Uani 0.845(8) 1 d . . . B 1
O18A O 0.4169(14) 0.8191(18) 0.3874(17) 0.028(8) Uani 0.155(8) 1 d . U . B 2
O19 O 0.7483(4) 0.7097(4) 0.9036(5) 0.045(2) Uani 0.75 1 d . . . C 1
H19A H 0.7319 0.6983 0.8622 0.067 Uiso 0.75 1 d GR . . C 1
H19B H 0.7858 0.7202 0.9162 0.067 Uiso 0.75 1 d GR . . C 1
O19A O 0.7778(11) 0.7130(14) 0.9549(15) 0.054(7) Uani 0.25 1 d . U . C 2
H19C H 0.8187 0.7177 0.9823 0.081 Uiso 0.25 1 d R . . C 2
H19D H 0.7602 0.7562 0.9647 0.081 Uiso 0.25 1 d R . . C 2
O20 O 0.8335(7) 0.6469(13) 1.0150(8) 0.047(4) Uani 0.68(5) 1 d . U . C 1
H20A H 0.8354 0.6901 0.9933 0.071 Uiso 0.68(5) 1 d GR . . C 1
H20B H 0.8618 0.6135 1.0157 0.071 Uiso 0.68(5) 1 d GR . . C 1
O20A O 0.8467(14) 0.618(2) 1.042(3) 0.055(10) Uani 0.32(5) 1 d . U . C 2
H20C H 0.8689 0.5687 1.0577 0.083 Uiso 0.32(5) 1 d GR . . C 2
H20D H 0.8545 0.6482 1.0823 0.083 Uiso 0.32(5) 1 d GR . . C 2
N1 N 0.6041(2) 0.6758(3) 0.7042(3) 0.0125(11) Uani 1 1 d . . . . .
N2 N 0.6197(2) 0.6341(3) 0.6050(3) 0.0133(11) Uani 1 1 d . . . . .
N3 N 0.7169(2) 0.6803(3) 0.7112(3) 0.0190(13) Uani 1 1 d . . . . .
N4 N 0.6836(3) 0.7739(3) 0.6126(3) 0.0209(13) Uani 1 1 d . . . . .
N5 N 0.6537(2) 0.8217(3) 0.7084(3) 0.0141(11) Uani 1 1 d . . . . .
N6 N 0.5668(2) 0.7784(3) 0.6014(3) 0.0155(11) Uani 1 1 d . . . . .
C1 C 0.6020(3) 0.7013(3) 0.7580(3) 0.0178(14) Uani 1 1 d . . . . .
H1 H 0.6110 0.7547 0.7700 0.021 Uiso 1 1 calc R . . . .
C2 C 0.5872(3) 0.6534(3) 0.7968(3) 0.0176(14) Uani 1 1 d . . . . .
C3 C 0.5712(3) 0.5773(4) 0.7768(3) 0.0207(15) Uani 1 1 d . . . . .
H3 H 0.5607 0.5428 0.8025 0.025 Uiso 1 1 calc R . . . .
C4 C 0.5705(3) 0.5511(4) 0.7195(3) 0.0174(14) Uani 1 1 d . . . . .
H4 H 0.5583 0.4992 0.7047 0.021 Uiso 1 1 calc R . . . .
C5 C 0.5876(3) 0.6014(3) 0.6842(3) 0.0121(12) Uani 1 1 d . . . . .
C6 C 0.5916(3) 0.5793(3) 0.6250(3) 0.0127(13) Uani 1 1 d . . . . .
C7 C 0.5703(3) 0.5121(3) 0.5901(3) 0.0171(14) Uani 1 1 d . . . . .
H7 H 0.5517 0.4737 0.6049 0.021 Uiso 1 1 calc R . . . .
C8 C 0.5758(3) 0.4999(3) 0.5339(3) 0.0176(14) Uani 1 1 d . . . . .
H8 H 0.5602 0.4537 0.5093 0.021 Uiso 1 1 calc R . . . .
C9 C 0.6040(3) 0.5547(3) 0.5131(3) 0.0144(13) Uani 1 1 d . . . . .
C10 C 0.6263(3) 0.6202(3) 0.5516(3) 0.0159(14) Uani 1 1 d . . . . .
H10 H 0.6475 0.6574 0.5392 0.019 Uiso 1 1 calc R . . . .
C11 C 0.7291(3) 0.6290(3) 0.7601(3) 0.0176(14) Uani 1 1 d . . . . .
H11A H 0.6983 0.6150 0.7715 0.021 Uiso 1 1 calc R . . . .
C12 C 0.7846(3) 0.5957(4) 0.7944(3) 0.0206(15) Uani 1 1 d . . . . .
C13 C 0.8285(3) 0.6181(4) 0.7774(4) 0.0286(18) Uani 1 1 d . . . . .
H13A H 0.8674 0.5975 0.8005 0.034 Uiso 1 1 calc R . . . .
C14 C 0.8167(3) 0.6699(4) 0.7273(4) 0.034(2) Uani 1 1 d . . . . .
H14 H 0.8472 0.6847 0.7156 0.041 Uiso 1 1 calc R . . . .
C15 C 0.7607(3) 0.7000(4) 0.6943(4) 0.0226(16) Uani 1 1 d . . . . .
C16 C 0.7421(3) 0.7542(4) 0.6396(4) 0.0263(17) Uani 1 1 d . . . . .
C17 C 0.7788(4) 0.7846(5) 0.6142(5) 0.045(2) Uani 1 1 d . . . . .
H17 H 0.8197 0.7716 0.6325 0.054 Uiso 1 1 calc R . . D .
C18 C 0.7538(4) 0.8349(5) 0.5611(5) 0.051(3) Uani 1 1 d . . . E 1
H18 H 0.7782 0.8558 0.5430 0.061 Uiso 1 1 calc R . . E 1
C19 C 0.6955(4) 0.8549(4) 0.5343(4) 0.0320(19) Uani 1 1 d . . . . .
C20 C 0.6616(3) 0.8234(3) 0.5614(3) 0.0235(16) Uani 1 1 d . . . . .
H20 H 0.6208 0.8367 0.5435 0.028 Uiso 1 1 calc R . . . .
C21 C 0.6993(3) 0.8371(3) 0.7660(3) 0.0184(15) Uani 1 1 d . . . . .
H21 H 0.7324 0.8028 0.7813 0.022 Uiso 1 1 calc R . . . .
C22 C 0.7007(3) 0.9006(3) 0.8045(3) 0.0171(13) Uani 1 1 d . . . . .
C23 C 0.6520(3) 0.9489(3) 0.7810(3) 0.0196(15) Uani 1 1 d . . . . .
H23 H 0.6501 0.9914 0.8068 0.024 Uiso 1 1 calc R . . . .
C24 C 0.6066(3) 0.9367(4) 0.7212(3) 0.0215(15) Uani 1 1 d . . . . .
H24 H 0.5740 0.9719 0.7043 0.026 Uiso 1 1 calc R . . . .
C25 C 0.6084(3) 0.8718(3) 0.6851(3) 0.0180(14) Uani 1 1 d . . . . .
C26 C 0.5610(3) 0.8502(4) 0.6223(3) 0.0204(15) Uani 1 1 d . . . . .
C27 C 0.5140(3) 0.8977(4) 0.5846(4) 0.040(2) Uani 1 1 d . . . . .
H27 H 0.5109 0.9488 0.5991 0.048 Uiso 1 1 calc R . . . .
C28 C 0.4719(3) 0.8710(4) 0.5261(4) 0.041(2) Uani 1 1 d . . . . .
H28 H 0.4404 0.9044 0.4992 0.050 Uiso 1 1 calc R . . . .
C29 C 0.4752(3) 0.7955(4) 0.5064(3) 0.0213(15) Uani 1 1 d . . . . .
C30 C 0.5230(3) 0.7520(3) 0.5455(3) 0.0191(15) Uani 1 1 d . . . . .
H30 H 0.5258 0.6999 0.5326 0.023 Uiso 1 1 calc R . . . .
O24 O 0.5000 0.8477(5) 0.7500 0.086(4) Uani 1 2 d S T P . .
H24A H 0.5241 0.8108 0.7508 0.129 Uiso 0.5 1 d R . . . .
H24B H 0.4697 0.8490 0.7121 0.129 Uiso 0.5 1 d R . . . .
O25 O 0.5000 1.0126(13) 0.7500 0.110(8) Uani 0.5 2 d S TU P F 2
H25A H 0.4934 0.9632 0.7399 0.165 Uiso 0.25 1 d R . . F 2
H25B H 0.4954 1.0393 0.7159 0.165 Uiso 0.25 1 d R . . F 2
O0AA O 0.4862(11) 0.3922(8) 0.7273(10) 0.117(8) Uani 0.5 1 d . U . G 2
O29 O 0.5604(11) 0.1084(18) 0.7770(14) 0.076(9) Uani 0.25 1 d . U . H 1
O23 O 0.6696(3) 0.4215(4) 0.7362(4) 0.072(2) Uani 1 1 d . . . . .
H23A H 0.7030 0.4316 0.7696 0.108 Uiso 1 1 d G . . . .
H23B H 0.6612 0.3721 0.7359 0.108 Uiso 1 1 d G . . . .
O30 O 0.5507(16) -0.045(2) 0.830(2) 0.133(13) Uani 0.25 1 d . U . I 1
O40 O 0.9409(15) 0.4559(19) 0.9995(19) 0.128(13) Uani 0.25 1 d . U . J 2
H40A H 0.9186 0.4726 1.0170 0.192 Uiso 0.25 1 d R . . J 2
H40B H 0.9313 0.4800 0.9628 0.192 Uiso 0.25 1 d R . . J 2
O28 O 0.5611(6) 0.1887(10) 0.7955(9) 0.095(5) Uani 0.5 1 d . U . K 2
O22 O 0.5641(3) 0.7491(4) 0.4216(4) 0.084(2) Uani 1 1 d . . . . .
H22A H 0.5271 0.7354 0.4060 0.126 Uiso 1 1 d R . . . .
H22B H 0.5699 0.7755 0.3924 0.126 Uiso 1 1 d R . . . .
O27 O 0.4147(4) 0.6827(5) 0.2679(5) 0.122(3) Uani 1 1 d . . . L 1
H27A H 0.4168 0.6367 0.2528 0.183 Uiso 1 1 d R . . L 1
H27B H 0.4427 0.6873 0.3072 0.183 Uiso 1 1 d R . . L 1
O21 O 0.4917(4) 0.9211(4) 0.3627(5) 0.141(5) Uani 1 1 d . . . . .
H21A H 0.5202 0.8895 0.3864 0.212 Uiso 1 1 d R . . . .
H21B H 0.4596 0.8943 0.3408 0.212 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 O1 2.252(5) . ?
Dy1 O4 2.276(4) 6_566 ?
Dy1 O7 2.225(5) . ?
Dy1 O11 2.384(5) 4_646 ?
Dy1 O14 2.291(5) 7_667 ?
Dy1 O19 2.534(7) . ?
Dy1 O19A 2.34(2) . ?
Dy1 O20 2.342(12) . ?
Dy1 O20A 2.55(4) . ?
Co1 N1 1.925(5) . ?
Co1 N2 1.928(5) . ?
Co1 N3 1.946(6) . ?
Co1 N4 1.939(6) . ?
Co1 N5 1.931(5) . ?
Co1 N6 1.933(5) . ?
P1 O1 1.509(5) . ?
P1 O2 1.547(5) . ?
P1 O3 1.491(5) . ?
P1 C2 1.836(7) . ?
P2 O4 1.496(5) . ?
P2 O5 1.510(5) . ?
P2 O6 1.540(5) . ?
P2 C9 1.812(6) . ?
P3 O7 1.500(5) . ?
P3 O8 1.529(5) . ?
P3 O9 1.490(6) . ?
P3 C12 1.824(7) . ?
P4 O10 1.466(10) . ?
P4 O11 1.457(6) . ?
P4 O12 1.557(8) . ?
P4 C19 1.830(8) . ?
P4A O10A 1.49(6) . ?
P4A O11 1.477(14) . ?
P4A O12A 1.46(4) . ?
P4A C19 1.756(19) . ?
P5 O13 1.559(4) . ?
P5 O14 1.502(5) . ?
P5 O15 1.492(5) . ?
P5 C22 1.797(7) . ?
P6 O16 1.562(7) . ?
P6 O17 1.472(8) . ?
P6 O18 1.511(9) . ?
P6 C29 1.811(8) . ?
P6A O16A 1.33(4) . ?
P6A O17A 1.58(4) . ?
P6A O18A 1.53(4) . ?
P6A C29 1.87(3) . ?
O2 H2 0.8400 . ?
O4 Dy1 2.276(4) 6_565 ?
O6 H6 0.8400 . ?
O11 Dy1 2.384(5) 4_656 ?
O11 H11 0.8400 . ?
O12 H12 0.8400 . ?
O13 H13 0.8400 . ?
O14 Dy1 2.290(5) 7_667 ?
O16 H16 0.8400 . ?
O17A H17A 0.8400 . ?
O19 H19A 0.8750 . ?
O19 H19B 0.8743 . ?
O19A H19C 0.9425 . ?
O19A H19D 0.9382 . ?
O20 H20A 0.9020 . ?
O20 H20B 0.9065 . ?
O20A H20C 0.9879 . ?
O20A H20D 0.9980 . ?
N1 C1 1.334(8) . ?
N1 C5 1.351(7) . ?
N2 C6 1.366(7) . ?
N2 C10 1.329(8) . ?
N3 C11 1.348(8) . ?
N3 C15 1.360(8) . ?
N4 C16 1.363(9) . ?
N4 C20 1.353(8) . ?
N5 C21 1.341(8) . ?
N5 C25 1.333(8) . ?
N6 C26 1.348(7) . ?
N6 C30 1.349(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.375(9) . ?
C2 C3 1.378(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(9) . ?
C4 H4 0.9500 . ?
C4 C5 1.372(8) . ?
C5 C6 1.457(8) . ?
C6 C7 1.367(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.372(9) . ?
C8 H8 0.9500 . ?
C8 C9 1.379(8) . ?
C9 C10 1.383(8) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9500 . ?
C11 C12 1.385(9) . ?
C12 C13 1.376(9) . ?
C13 H13A 0.9500 . ?
C13 C14 1.376(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.371(9) . ?
C15 C16 1.461(10) . ?
C16 C17 1.388(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.396(12) . ?
C18 H18 0.9500 . ?
C18 C19 1.359(11) . ?
C19 C20 1.365(9) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.390(8) . ?
C22 C23 1.373(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.361(9) . ?
C24 H24 0.9500 . ?
C24 C25 1.396(8) . ?
C25 C26 1.458(9) . ?
C26 C27 1.378(9) . ?
C27 H27 0.9500 . ?
C27 C28 1.372(10) . ?
C28 H28 0.9500 . ?
C28 C29 1.381(9) . ?
C29 C30 1.362(9) . ?
C30 H30 0.9500 . ?
O24 H24A 0.8697 . ?
O24 H24B 0.8698 . ?
O25 H25A 0.8699 . ?
O25 H25B 0.8698 . ?
O0AA O0AA 0.97(4) 2_656 ?
O23 H23A 0.8699 . ?
O23 H23B 0.8699 . ?
O40 H40A 0.8702 . ?
O40 H40B 0.8714 . ?
O22 H22A 0.8702 . ?
O22 H22B 0.8699 . ?
O27 H27A 0.8709 . ?
O27 H27B 0.8705 . ?
O21 H21A 0.8700 . ?
O21 H21B 0.8703 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Dy1 O4 78.68(17) . 6_566 ?
O1 Dy1 O11 152.08(19) . 4_646 ?
O1 Dy1 O14 87.78(17) . 7_667 ?
O1 Dy1 O19 68.0(2) . . ?
O1 Dy1 O19A 80.0(7) . . ?
O1 Dy1 O20 123.3(7) . . ?
O1 Dy1 O20A 135.6(8) . . ?
O4 Dy1 O11 75.78(18) 6_566 4_646 ?
O4 Dy1 O14 91.08(17) 6_566 7_667 ?
O4 Dy1 O19 136.2(3) 6_566 . ?
O4 Dy1 O19A 158.0(7) 6_566 . ?
O4 Dy1 O20 155.2(6) 6_566 . ?
O4 Dy1 O20A 138.4(13) 6_566 . ?
O7 Dy1 O1 107.77(18) . . ?
O7 Dy1 O4 92.77(18) . 6_566 ?
O7 Dy1 O11 84.68(19) . 4_646 ?
O7 Dy1 O14 164.43(17) . 7_667 ?
O7 Dy1 O19 72.4(2) . . ?
O7 Dy1 O19A 88.4(7) . . ?
O7 Dy1 O20 90.9(3) . . ?
O7 Dy1 O20A 95.7(10) . . ?
O11 Dy1 O19 139.8(2) 4_646 . ?
O11 Dy1 O20A 64.6(11) 4_646 . ?
O14 Dy1 O11 81.65(18) 7_667 4_646 ?
O14 Dy1 O19 114.3(2) 7_667 . ?
O14 Dy1 O19A 93.7(7) 7_667 . ?
O14 Dy1 O20 79.4(3) 7_667 . ?
O14 Dy1 O20A 71.7(11) 7_667 . ?
O19A Dy1 O11 126.2(7) . 4_646 ?
O19A Dy1 O20A 63.2(14) . . ?
O20 Dy1 O11 80.2(7) . 4_646 ?
O20 Dy1 O19 68.0(6) . . ?
N1 Co1 N2 83.8(2) . . ?
N1 Co1 N3 91.3(2) . . ?
N1 Co1 N4 174.7(2) . . ?
N1 Co1 N5 91.7(2) . . ?
N1 Co1 N6 91.0(2) . . ?
N2 Co1 N3 88.5(2) . . ?
N2 Co1 N4 94.5(2) . . ?
N2 Co1 N5 173.9(2) . . ?
N2 Co1 N6 92.3(2) . . ?
N4 Co1 N3 83.7(2) . . ?
N5 Co1 N3 95.7(2) . . ?
N5 Co1 N4 90.3(2) . . ?
N5 Co1 N6 83.6(2) . . ?
N6 Co1 N3 177.7(2) . . ?
N6 Co1 N4 94.1(2) . . ?
O1 P1 O2 112.1(3) . . ?
O1 P1 C2 105.8(3) . . ?
O2 P1 C2 105.3(3) . . ?
O3 P1 O1 114.4(3) . . ?
O3 P1 O2 111.1(3) . . ?
O3 P1 C2 107.5(3) . . ?
O4 P2 O5 116.2(3) . . ?
O4 P2 O6 107.9(3) . . ?
O4 P2 C9 109.4(3) . . ?
O5 P2 O6 112.6(3) . . ?
O5 P2 C9 104.1(3) . . ?
O6 P2 C9 106.0(3) . . ?
O7 P3 O8 110.4(3) . . ?
O7 P3 C12 105.9(3) . . ?
O8 P3 C12 105.5(3) . . ?
O9 P3 O7 117.0(3) . . ?
O9 P3 O8 109.4(3) . . ?
O9 P3 C12 107.9(3) . . ?
O10 P4 O12 108.9(6) . . ?
O10 P4 C19 104.4(5) . . ?
O11 P4 O10 121.9(6) . . ?
O11 P4 O12 109.6(4) . . ?
O11 P4 C19 105.9(4) . . ?
O12 P4 C19 104.7(4) . . ?
O10A P4A C19 108(3) . . ?
O11 P4A O10A 111(2) . . ?
O11 P4A C19 108.7(10) . . ?
O12A P4A O10A 113(3) . . ?
O12A P4A O11 92.0(15) . . ?
O12A P4A C19 122.8(19) . . ?
O13 P5 C22 103.8(3) . . ?
O14 P5 O13 111.3(3) . . ?
O14 P5 C22 108.2(3) . . ?
O15 P5 O13 110.9(3) . . ?
O15 P5 O14 115.2(3) . . ?
O15 P5 C22 106.6(3) . . ?
O16 P6 C29 101.5(4) . . ?
O17 P6 O16 111.9(5) . . ?
O17 P6 O18 117.7(5) . . ?
O17 P6 C29 109.3(4) . . ?
O18 P6 O16 108.5(5) . . ?
O18 P6 C29 106.5(4) . . ?
O16A P6A O17A 125(2) . . ?
O16A P6A O18A 116(3) . . ?
O16A P6A C29 112(2) . . ?
O17A P6A C29 101(2) . . ?
O18A P6A O17A 105(2) . . ?
O18A P6A C29 93.9(18) . . ?
P1 O1 Dy1 156.5(3) . . ?
P1 O2 H2 109.5 . . ?
P2 O4 Dy1 165.4(3) . 6_565 ?
P2 O6 H6 109.5 . . ?
P3 O7 Dy1 150.0(3) . . ?
Dy1 O11 H11 53.4 4_656 . ?
P4 O11 Dy1 148.4(4) . 4_656 ?
P4A O11 Dy1 161.2(8) . 4_656 ?
P4A O11 H11 109.7 . . ?
P4 O12 H12 109.5 . . ?
P5 O13 H13 109.5 . . ?
P5 O14 Dy1 134.8(3) . 7_667 ?
P6 O16 H16 109.5 . . ?
P6A O17A H17A 109.5 . . ?
Dy1 O19 H19A 109.3 . . ?
Dy1 O19 H19B 109.7 . . ?
H19A O19 H19B 109.2 . . ?
Dy1 O19A H19C 113.2 . . ?
Dy1 O19A H19D 112.7 . . ?
H19C O19A H19D 105.3 . . ?
Dy1 O20 H20A 110.4 . . ?
Dy1 O20 H20B 113.5 . . ?
H20A O20 H20B 107.1 . . ?
Dy1 O20A H20C 112.0 . . ?
Dy1 O20A H20D 115.3 . . ?
H20C O20A H20D 104.7 . . ?
C1 N1 Co1 126.6(4) . . ?
C1 N1 C5 119.3(5) . . ?
C5 N1 Co1 113.4(4) . . ?
C6 N2 Co1 113.9(4) . . ?
C10 N2 Co1 127.2(4) . . ?
C10 N2 C6 118.7(5) . . ?
C11 N3 Co1 127.4(4) . . ?
C11 N3 C15 118.8(6) . . ?
C15 N3 Co1 113.8(5) . . ?
C16 N4 Co1 113.5(5) . . ?
C20 N4 Co1 126.7(5) . . ?
C20 N4 C16 119.8(6) . . ?
C21 N5 Co1 127.4(4) . . ?
C25 N5 Co1 113.7(4) . . ?
C25 N5 C21 118.6(5) . . ?
C26 N6 Co1 113.2(4) . . ?
C26 N6 C30 118.3(6) . . ?
C30 N6 Co1 128.5(4) . . ?
N1 C1 H1 118.7 . . ?
N1 C1 C2 122.6(6) . . ?
C2 C1 H1 118.7 . . ?
C1 C2 P1 118.4(5) . . ?
C1 C2 C3 117.8(6) . . ?
C3 C2 P1 123.7(5) . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.2(6) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.8(6) . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 121.2(6) . . ?
N1 C5 C6 115.0(5) . . ?
C4 C5 C6 123.8(5) . . ?
N2 C6 C5 113.2(5) . . ?
N2 C6 C7 120.3(6) . . ?
C7 C6 C5 126.5(5) . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.2(6) . . ?
C8 C7 H7 119.9 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.2(6) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 P2 120.2(5) . . ?
C8 C9 C10 116.8(6) . . ?
C10 C9 P2 123.0(5) . . ?
N2 C10 C9 123.7(6) . . ?
N2 C10 H10 118.2 . . ?
C9 C10 H10 118.2 . . ?
N3 C11 H11A 118.5 . . ?
N3 C11 C12 122.9(6) . . ?
C12 C11 H11A 118.5 . . ?
C11 C12 P3 118.9(5) . . ?
C13 C12 P3 123.9(5) . . ?
C13 C12 C11 117.2(6) . . ?
C12 C13 H13A 119.7 . . ?
C12 C13 C14 120.7(7) . . ?
C14 C13 H13A 119.7 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.6(7) . . ?
C15 C14 H14 120.2 . . ?
N3 C15 C14 120.8(7) . . ?
N3 C15 C16 114.1(6) . . ?
C14 C15 C16 125.1(6) . . ?
N4 C16 C15 114.9(6) . . ?
N4 C16 C17 119.9(7) . . ?
C17 C16 C15 125.2(7) . . ?
C16 C17 H17 121.0 . . ?
C16 C17 C18 118.1(8) . . ?
C18 C17 H17 121.0 . . ?
C17 C18 H18 118.9 . . ?
C19 C18 C17 122.1(7) . . ?
C19 C18 H18 118.9 . . ?
C18 C19 P4 123.1(6) . . ?
C18 C19 C20 117.2(7) . . ?
C20 C19 P4 119.7(6) . . ?
C20 C19 P4A 138.3(9) . . ?
N4 C20 C19 123.0(7) . . ?
N4 C20 H20 118.5 . . ?
C19 C20 H20 118.5 . . ?
N5 C21 H21 118.3 . . ?
N5 C21 C22 123.5(6) . . ?
C22 C21 H21 118.3 . . ?
C21 C22 P5 121.7(5) . . ?
C23 C22 P5 121.6(5) . . ?
C23 C22 C21 116.7(6) . . ?
C22 C23 H23 119.6 . . ?
C24 C23 C22 120.7(6) . . ?
C24 C23 H23 119.6 . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.3(6) . . ?
C25 C24 H24 120.4 . . ?
N5 C25 C24 121.0(6) . . ?
N5 C25 C26 114.7(5) . . ?
C24 C25 C26 124.2(6) . . ?
N6 C26 C25 114.4(6) . . ?
N6 C26 C27 120.5(6) . . ?
C27 C26 C25 125.1(6) . . ?
C26 C27 H27 120.0 . . ?
C28 C27 C26 119.9(7) . . ?
C28 C27 H27 120.0 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 120.0(7) . . ?
C29 C28 H28 120.0 . . ?
C28 C29 P6 118.6(6) . . ?
C28 C29 P6A 129.7(9) . . ?
C30 C29 P6 124.1(5) . . ?
C30 C29 P6A 112.9(9) . . ?
C30 C29 C28 117.1(6) . . ?
N6 C30 C29 124.0(6) . . ?
N6 C30 H30 118.0 . . ?
C29 C30 H30 118.0 . . ?
H24A O24 H24B 109.5 . . ?
H25A O25 H25B 109.5 . . ?
H23A O23 H23B 109.6 . . ?
H40A O40 H40B 109.3 . . ?
H22A O22 H22B 109.4 . . ?
H27A O27 H27B 109.4 . . ?
H21A O21 H21B 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
O2 H2 O5 0.84 1.74 2.571(7) 171.9 6_566
O12 H12 O9 0.84 2.08 2.732(11) 134.7 4_656
O13 H13 O12A 0.84 1.85 2.42(3) 124.6 6_576
O16 H16 O15 0.84 1.83 2.626(7) 157.9 8_465
O19 H19B O17 0.87 1.93 2.738(10) 152.7 8_566
O20A H20D O3 1.00 1.90 2.68(3) 133.1 7_667

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
Co1 N1 C1 C2 -164.8(5) . . . . ?
Co1 N1 C5 C4 168.4(5) . . . . ?
Co1 N1 C5 C6 -9.4(7) . . . . ?
Co1 N2 C6 C5 -4.3(6) . . . . ?
Co1 N2 C6 C7 175.4(5) . . . . ?
Co1 N2 C10 C9 -172.5(5) . . . . ?
Co1 N3 C11 C12 177.2(4) . . . . ?
Co1 N3 C15 C14 -178.8(5) . . . . ?
Co1 N3 C15 C16 1.1(7) . . . . ?
Co1 N4 C16 C15 2.6(7) . . . . ?
Co1 N4 C16 C17 -178.1(6) . . . . ?
Co1 N4 C20 C19 177.9(5) . . . . ?
Co1 N5 C21 C22 -169.8(4) . . . . ?
Co1 N5 C25 C24 170.5(5) . . . . ?
Co1 N5 C25 C26 -6.0(7) . . . . ?
Co1 N6 C26 C25 -5.9(7) . . . . ?
Co1 N6 C26 C27 172.5(6) . . . . ?
Co1 N6 C30 C29 -172.9(5) . . . . ?
P1 C2 C3 C4 -175.8(5) . . . . ?
P2 C9 C10 N2 176.8(5) . . . . ?
P3 C12 C13 C14 176.7(6) . . . . ?
P4 C19 C20 N4 -178.2(5) . . . . ?
P4A C19 C20 N4 162.1(11) . . . . ?
P5 C22 C23 C24 176.1(5) . . . . ?
P6 C29 C30 N6 175.3(5) . . . . ?
P6A C29 C30 N6 173.8(12) . . . . ?
O1 P1 C2 C1 -94.1(5) . . . . ?
O1 P1 C2 C3 81.7(6) . . . . ?
O2 P1 O1 Dy1 91.2(8) . . . . ?
O2 P1 C2 C1 147.0(5) . . . . ?
O2 P1 C2 C3 -37.1(6) . . . . ?
O3 P1 O1 Dy1 -141.2(7) . . . . ?
O3 P1 C2 C1 28.4(6) . . . . ?
O3 P1 C2 C3 -155.7(6) . . . . ?
O4 P2 C9 C8 -91.1(5) . . . . ?
O4 P2 C9 C10 89.1(6) . . . . ?
O5 P2 O4 Dy1 -20.2(14) . . . 6_565 ?
O5 P2 C9 C8 33.8(6) . . . . ?
O5 P2 C9 C10 -146.0(5) . . . . ?
O6 P2 O4 Dy1 -147.8(12) . . . 6_565 ?
O6 P2 C9 C8 152.7(5) . . . . ?
O6 P2 C9 C10 -27.0(6) . . . . ?
O7 P3 C12 C11 -31.8(6) . . . . ?
O7 P3 C12 C13 150.0(6) . . . . ?
O8 P3 O7 Dy1 135.4(6) . . . . ?
O8 P3 C12 C11 85.3(5) . . . . ?
O8 P3 C12 C13 -92.9(6) . . . . ?
O9 P3 O7 Dy1 9.3(8) . . . . ?
O9 P3 C12 C11 -157.8(5) . . . . ?
O9 P3 C12 C13 23.9(7) . . . . ?
O10 P4 O11 Dy1 165.6(7) . . . 4_656 ?
O10 P4 C19 C18 95.3(9) . . . . ?
O10 P4 C19 C20 -86.7(8) . . . . ?
O10A P4A O11 Dy1 141(3) . . . 4_656 ?
O10A P4A C19 C20 -4(3) . . . . ?
O11 P4 C19 C18 -34.5(9) . . . . ?
O11 P4 C19 C20 143.4(6) . . . . ?
O11 P4A C19 C20 116.6(11) . . . . ?
O12 P4 O11 Dy1 36.7(8) . . . 4_656 ?
O12 P4 C19 C18 -150.3(7) . . . . ?
O12 P4 C19 C20 27.7(7) . . . . ?
O12A P4A O11 Dy1 -103(3) . . . 4_656 ?
O12A P4A C19 C20 -138.1(18) . . . . ?
O13 P5 O14 Dy1 -19.3(5) . . . 7_667 ?
O13 P5 C22 C21 153.2(5) . . . . ?
O13 P5 C22 C23 -26.4(6) . . . . ?
O14 P5 C22 C21 -88.5(5) . . . . ?
O14 P5 C22 C23 91.9(5) . . . . ?
O15 P5 O14 Dy1 108.1(4) . . . 7_667 ?
O15 P5 C22 C21 36.0(6) . . . . ?
O15 P5 C22 C23 -143.6(5) . . . . ?
O16 P6 C29 C28 -154.1(6) . . . . ?
O16 P6 C29 C30 30.4(8) . . . . ?
O16A P6A C29 C28 154.1(19) . . . . ?
O16A P6A C29 C30 -19(3) . . . . ?
O17 P6 C29 C28 -35.8(8) . . . . ?
O17 P6 C29 C30 148.8(6) . . . . ?
O17A P6A C29 C28 -71(2) . . . . ?
O17A P6A C29 C30 115.4(15) . . . . ?
O18 P6 C29 C28 92.4(7) . . . . ?
O18 P6 C29 C30 -83.1(7) . . . . ?
O18A P6A C29 C28 34(2) . . . . ?
O18A P6A C29 C30 -138.9(16) . . . . ?
N1 C1 C2 P1 172.8(5) . . . . ?
N1 C1 C2 C3 -3.4(10) . . . . ?
N1 C5 C6 N2 9.0(8) . . . . ?
N1 C5 C6 C7 -170.6(6) . . . . ?
N2 C6 C7 C8 -1.5(9) . . . . ?
N3 C11 C12 P3 -177.4(5) . . . . ?
N3 C11 C12 C13 1.0(9) . . . . ?
N3 C15 C16 N4 -2.4(9) . . . . ?
N3 C15 C16 C17 178.2(7) . . . . ?
N4 C16 C17 C18 -0.2(12) . . . . ?
N5 C21 C22 P5 -179.4(5) . . . . ?
N5 C21 C22 C23 0.2(9) . . . . ?
N5 C25 C26 N6 7.9(8) . . . . ?
N5 C25 C26 C27 -170.4(7) . . . . ?
N6 C26 C27 C28 1.8(12) . . . . ?
C1 N1 C5 C4 -2.1(9) . . . . ?
C1 N1 C5 C6 -179.9(5) . . . . ?
C1 C2 C3 C4 0.1(10) . . . . ?
C2 P1 O1 Dy1 -23.1(8) . . . . ?
C2 C3 C4 C5 1.9(10) . . . . ?
C3 C4 C5 N1 -1.0(9) . . . . ?
C3 C4 C5 C6 176.6(6) . . . . ?
C4 C5 C6 N2 -168.7(6) . . . . ?
C4 C5 C6 C7 11.7(10) . . . . ?
C5 N1 C1 C2 4.4(9) . . . . ?
C5 C6 C7 C8 178.1(6) . . . . ?
C6 N2 C10 C9 3.0(9) . . . . ?
C6 C7 C8 C9 1.4(10) . . . . ?
C7 C8 C9 P2 -179.1(5) . . . . ?
C7 C8 C9 C10 0.7(9) . . . . ?
C8 C9 C10 N2 -3.0(9) . . . . ?
C9 P2 O4 Dy1 97.3(13) . . . 6_565 ?
C10 N2 C6 C5 179.7(5) . . . . ?
C10 N2 C6 C7 -0.7(9) . . . . ?
C11 N3 C15 C14 -1.7(9) . . . . ?
C11 N3 C15 C16 178.2(6) . . . . ?
C11 C12 C13 C14 -1.5(10) . . . . ?
C12 P3 O7 Dy1 -110.9(6) . . . . ?
C12 C13 C14 C15 0.5(11) . . . . ?
C13 C14 C15 N3 1.1(11) . . . . ?
C13 C14 C15 C16 -178.7(7) . . . . ?
C14 C15 C16 N4 177.4(6) . . . . ?
C14 C15 C16 C17 -1.9(12) . . . . ?
C15 N3 C11 C12 0.6(9) . . . . ?
C15 C16 C17 C18 179.1(8) . . . . ?
C16 N4 C20 C19 0.5(10) . . . . ?
C16 C17 C18 C19 0.6(14) . . . . ?
C17 C18 C19 P4 177.6(7) . . . . ?
C17 C18 C19 C20 -0.4(13) . . . . ?
C18 C19 C20 N4 -0.1(11) . . . . ?
C19 P4 O11 Dy1 -75.6(7) . . . 4_656 ?
C19 P4A O11 Dy1 23(4) . . . 4_656 ?
C20 N4 C16 C15 -179.7(6) . . . . ?
C20 N4 C16 C17 -0.3(10) . . . . ?
C21 N5 C25 C24 -3.6(9) . . . . ?
C21 N5 C25 C26 179.9(5) . . . . ?
C21 C22 C23 C24 -3.5(9) . . . . ?
C22 P5 O14 Dy1 -132.7(4) . . . 7_667 ?
C22 C23 C24 C25 3.4(10) . . . . ?
C23 C24 C25 N5 0.3(10) . . . . ?
C23 C24 C25 C26 176.5(6) . . . . ?
C24 C25 C26 N6 -168.4(6) . . . . ?
C24 C25 C26 C27 13.2(11) . . . . ?
C25 N5 C21 C22 3.4(9) . . . . ?
C25 C26 C27 C28 -180.0(8) . . . . ?
C26 N6 C30 C29 4.7(10) . . . . ?
C26 C27 C28 C29 2.7(13) . . . . ?
C27 C28 C29 P6 -179.2(7) . . . . ?
C27 C28 C29 P6A -176.3(15) . . . . ?
C27 C28 C29 C30 -3.5(12) . . . . ?
C28 C29 C30 N6 -0.3(11) . . . . ?
C30 N6 C26 C25 176.2(6) . . . . ?
C30 N6 C26 C27 -5.4(9) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound-3c
_database_code_depnum_ccdc_archive 'CCDC 1477305'
_audit_update_record             
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_audit_creation_date             2016-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        Compound-3c
_chemical_formula_moiety         'C30 H26 Co N6 O20 P6 Tb, 5.5(H2 O), 0.5(O)'
_chemical_formula_sum            'C30 H37 Co N6 O26 P6 Tb'
_chemical_formula_weight         1301.32
_chemical_melting_point          ?
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'
Co Co 0.3494 0.9721 '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'
Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   25.203(2)
_cell_length_b                   17.0993(14)
_cell_length_c                   22.983(2)
_cell_angle_alpha                90
_cell_angle_beta                 116.064(2)
_cell_angle_gamma                90
_cell_volume                     8897.4(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2635
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      23.340
_cell_measurement_theta_min      2.579
_shelx_estimated_absorpt_T_max   0.895
_shelx_estimated_absorpt_T_min   0.612
_exptl_absorpt_coefficient_mu    2.266
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6613
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.0629 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.8869.
The λ/2 correction factor is 0.00150.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             5192
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_av_unetI/netI     0.1067
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25646
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.955
_diffrn_reflns_theta_min         1.973
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7015
_reflns_number_total             10680
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.001
_refine_diff_density_min         -1.502
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         10680
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0689
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0889P)²+75.5867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1916
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O18A) \\sim Ueq, Uanis(O16A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(N1) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.003
Uanis(O17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O24A) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.05
Uanis(O24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O27) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
3. Others
 Sof(O28A)=Sof(H28C)=Sof(H28D)=1-FVAR(1)
 Sof(O28)=Sof(H28A)=Sof(H28B)=FVAR(1)
 Sof(O18A)=Sof(O16A)=Sof(O17A)=Sof(H17A)=1-FVAR(2)
 Sof(O16)=Sof(H16)=Sof(O17)=Sof(O18)=FVAR(2)
 Fixed Sof: O24(0.5) H24A(0.5) H24B(0.5) H23A(0.5) H23B(0.5) O27(0.25)
 H27A(0.25) H27B(0.25) O26(0.5) O24A(0.25) H24C(0.25) H24D(0.25)
4.a Riding coordinates:
 O24(H24A,H24B), O23(H23A,H23B), O27(H27A,H27B), O21(H21A,H21B), O24A(H24C,
 H24D), O28A(H28C,H28D), O17A(H17A)
4.b Free rotating group:
 O22(H22A,H22B), O28(H28A,H28B), O25(H25A,H25B)
4.c Rotating group:
 O19(H19A,H19B), O20(H20A,H20B)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C27(H27),
  C28(H28), C30(H30)
4.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O8(H8A), O13(H13A), O16(H16)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7291(4) 0.6284(4) 0.7598(4) 0.0171(16) Uani 1 1 d . . . . .
H1 H 0.6983 0.6142 0.7709 0.021 Uiso 1 1 calc R . . . .
C2 C 0.7840(4) 0.5954(4) 0.7941(4) 0.0182(16) Uani 1 1 d . . . . .
C3 C 0.8287(4) 0.6179(5) 0.7772(5) 0.028(2) Uani 1 1 d . . . . .
H3 H 0.8675 0.5978 0.8007 0.033 Uiso 1 1 calc R . . . .
C4 C 0.8166(4) 0.6695(5) 0.7264(5) 0.030(2) Uani 1 1 d . . . . .
H4 H 0.8467 0.6836 0.7141 0.036 Uiso 1 1 calc R . . . .
C5 C 0.7601(4) 0.7004(4) 0.6936(4) 0.0209(17) Uani 1 1 d . . . . .
C6 C 0.7418(4) 0.7545(5) 0.6391(4) 0.0230(18) Uani 1 1 d . . . . .
C7 C 0.7786(5) 0.7864(6) 0.6158(6) 0.042(3) Uani 1 1 d . . . . .
H7 H 0.8197 0.7748 0.6352 0.050 Uiso 1 1 calc R . . . .
C8 C 0.7538(5) 0.8366(7) 0.5625(6) 0.049(3) Uani 1 1 d . . . . .
H8 H 0.7784 0.8576 0.5447 0.059 Uiso 1 1 calc R . . . .
C9 C 0.6956(4) 0.8566(5) 0.5353(4) 0.0266(19) Uani 1 1 d . . . . .
C10 C 0.6616(4) 0.8233(5) 0.5621(4) 0.0238(18) Uani 1 1 d . . . . .
H10 H 0.6207 0.8358 0.5438 0.029 Uiso 1 1 calc R . . . .
C11 C 0.6015(4) 0.7021(4) 0.7577(4) 0.0182(16) Uani 1 1 d . . . . .
H11 H 0.6106 0.7554 0.7694 0.022 Uiso 1 1 calc R . . . .
C12 C 0.5862(4) 0.6546(4) 0.7972(4) 0.0181(16) Uani 1 1 d . . . . .
C13 C 0.5703(4) 0.5781(4) 0.7769(4) 0.0178(16) Uani 1 1 d . . . . .
H13 H 0.5594 0.5438 0.8023 0.021 Uiso 1 1 calc R . . . .
C14 C 0.5701(4) 0.5508(5) 0.7197(4) 0.0182(16) Uani 1 1 d . . . . .
H14 H 0.5583 0.4987 0.7053 0.022 Uiso 1 1 calc R . . . .
C15 C 0.5875(3) 0.6011(4) 0.6844(3) 0.0115(14) Uani 1 1 d . . . . .
C16 C 0.5920(3) 0.5792(4) 0.6252(3) 0.0113(14) Uani 1 1 d . . . . .
C17 C 0.5701(3) 0.5116(4) 0.5908(4) 0.0164(15) Uani 1 1 d . . . . .
H17 H 0.5517 0.4734 0.6058 0.020 Uiso 1 1 calc R . . . .
C18 C 0.5753(3) 0.5000(4) 0.5336(4) 0.0174(16) Uani 1 1 d . . . . .
H18 H 0.5593 0.4542 0.5086 0.021 Uiso 1 1 calc R . . . .
C19 C 0.6036(3) 0.5546(4) 0.5130(4) 0.0160(15) Uani 1 1 d . . . . .
C20 C 0.6262(3) 0.6214(4) 0.5511(4) 0.0149(15) Uani 1 1 d . . . . .
H20 H 0.6468 0.6589 0.5383 0.018 Uiso 1 1 calc R . . . .
C21 C 0.6997(3) 0.8368(4) 0.7659(4) 0.0150(15) Uani 1 1 d . . . . .
H21 H 0.7327 0.8026 0.7812 0.018 Uiso 1 1 calc R . . . .
C22 C 0.7005(3) 0.9003(4) 0.8040(4) 0.0144(14) Uani 1 1 d . . . . .
C23 C 0.6523(3) 0.9498(4) 0.7804(4) 0.0174(16) Uani 1 1 d . . . . .
H23 H 0.6509 0.9930 0.8056 0.021 Uiso 1 1 calc R . . . .
C24 C 0.6066(4) 0.9368(4) 0.7204(4) 0.0194(17) Uani 1 1 d . . . . .
H24 H 0.5739 0.9716 0.7035 0.023 Uiso 1 1 calc R . . . .
C25 C 0.6086(3) 0.8721(4) 0.6848(4) 0.0133(14) Uani 1 1 d . . . . .
C26 C 0.5611(4) 0.8507(5) 0.6222(4) 0.0197(17) Uani 1 1 d . . . . .
C27 C 0.5149(4) 0.8989(5) 0.5849(5) 0.035(2) Uani 1 1 d . . . . .
H27 H 0.5122 0.9501 0.5995 0.042 Uiso 1 1 calc R . . . .
C28 C 0.4725(4) 0.8722(5) 0.5262(5) 0.032(2) Uani 1 1 d . . . . .
H28 H 0.4412 0.9057 0.4992 0.039 Uiso 1 1 calc R . . . .
C29 C 0.4756(4) 0.7961(5) 0.5066(4) 0.0207(17) Uani 1 1 d . . . . .
C30 C 0.5228(4) 0.7522(4) 0.5456(4) 0.0182(16) Uani 1 1 d . . . . .
H30 H 0.5252 0.6999 0.5330 0.022 Uiso 1 1 calc R . . . .
Co1 Co 0.64059(5) 0.72793(5) 0.65663(5) 0.0129(2) Uani 1 1 d . . . . .
N1 N 0.7168(3) 0.6804(4) 0.7109(3) 0.0147(13) Uani 1 1 d . U . . .
N2 N 0.6834(3) 0.7741(4) 0.6125(3) 0.0190(14) Uani 1 1 d . . . . .
N3 N 0.6039(3) 0.6762(3) 0.7040(3) 0.0119(12) Uani 1 1 d . . . . .
N4 N 0.6197(3) 0.6340(3) 0.6048(3) 0.0130(12) Uani 1 1 d . . . . .
N5 N 0.6540(3) 0.8219(3) 0.7082(3) 0.0120(12) Uani 1 1 d . . . . .
N6 N 0.5663(3) 0.7788(4) 0.6011(3) 0.0152(13) Uani 1 1 d . . . . .
O1 O 0.7532(3) 0.5461(4) 0.8847(3) 0.0284(14) Uani 1 1 d . . . . .
O2 O 0.7764(3) 0.4443(3) 0.8215(3) 0.0280(14) Uani 1 1 d . . . . .
O3 O 0.8589(3) 0.5194(5) 0.9020(3) 0.047(2) Uani 1 1 d . . . . .
O4 O 0.7090(3) 0.9811(4) 0.4734(4) 0.0439(18) Uani 1 1 d . . . . .
O5 O 0.6112(4) 0.9633(5) 0.4772(5) 0.064(3) Uani 1 1 d . . . . .
H5 H 0.6085 1.0104 0.4658 0.097 Uiso 1 1 calc GR . . . .
O6 O 0.6374(5) 0.8753(5) 0.4101(4) 0.073(3) Uani 1 1 d . . . . .
O7 O 0.6537(3) 0.6690(4) 0.9248(3) 0.0318(15) Uani 1 1 d . . . . .
O8 O 0.5439(3) 0.6536(4) 0.8856(3) 0.0262(13) Uani 1 1 d . . . . .
H8A H 0.5517 0.6059 0.8938 0.039 Uiso 1 1 calc GR . . . .
O9 O 0.5848(4) 0.7797(4) 0.8666(3) 0.0431(19) Uani 1 1 d . . . . .
O10 O 0.6138(3) 0.6211(4) 0.4128(3) 0.0301(15) Uani 1 1 d . . . . .
O11 O 0.6663(3) 0.4954(4) 0.4526(3) 0.0297(14) Uani 1 1 d . . . . .
O12 O 0.5538(3) 0.4956(4) 0.3955(3) 0.0300(14) Uani 1 1 d . . . . .
O13 O 0.7620(3) 1.0087(3) 0.8906(3) 0.0289(14) Uani 1 1 d . . . . .
H13A H 0.7401 1.0185 0.9087 0.043 Uiso 1 1 calc GR . . . .
O14 O 0.7538(3) 0.8744(4) 0.9323(3) 0.0258(13) Uani 1 1 d . . . . .
O15 O 0.8174(3) 0.8961(4) 0.8735(3) 0.0253(13) Uani 1 1 d . . . . .
O16 O 0.4192(3) 0.6727(4) 0.4380(4) 0.0295(19) Uani 0.873(11) 1 d . . . A 1
H16 H 0.3856 0.6594 0.4338 0.044 Uiso 0.873(11) 1 calc GR . . A 1
O17 O 0.4440(4) 0.7798(5) 0.3799(4) 0.034(2) Uani 0.873(11) 1 d . . . A 1
O18 O 0.3621(3) 0.7985(4) 0.4167(3) 0.032(2) Uani 0.873(11) 1 d . . . A 1
O19 O 0.7494(4) 0.7100(4) 0.9038(5) 0.069(3) Uani 1 1 d . . . . .
H19A H 0.7793 0.7017 0.8930 0.104 Uiso 1 1 d GR . . . .
H19B H 0.7576 0.7540 0.9278 0.104 Uiso 1 1 d GR . . . .
O20 O 0.8369(4) 0.6397(7) 1.0201(5) 0.083(4) Uani 1 1 d . . . . .
H20A H 0.8542 0.6352 0.9943 0.125 Uiso 1 1 d GR . . . .
H20B H 0.8564 0.6113 1.0551 0.125 Uiso 1 1 d GR . . . .
P1 P 0.79454(10) 0.52349(13) 0.85643(10) 0.0217(5) Uani 1 1 d . . . . .
P2 P 0.66283(13) 0.92249(16) 0.46664(14) 0.0393(7) Uani 1 1 d . . . . .
P3 P 0.59373(11) 0.69294(13) 0.87428(11) 0.0245(5) Uani 1 1 d . . . . .
P4 P 0.60960(10) 0.53863(13) 0.43802(10) 0.0199(4) Uani 1 1 d . . . . .
P5 P 0.76381(9) 0.91845(12) 0.88111(10) 0.0182(4) Uani 1 1 d . . . . .
P6 P 0.42044(10) 0.76147(13) 0.42826(11) 0.0244(5) Uani 1 1 d . . . . .
Tb1 Tb 0.73742(2) 0.59513(2) 0.96616(2) 0.02137(13) Uani 1 1 d . . . . .
O22 O 0.5643(5) 0.7493(6) 0.4220(5) 0.078(3) Uani 1 1 d . . . . .
H22A H 0.5304 0.7620 0.3907 0.116 Uiso 1 1 d G . . . .
H22B H 0.5784 0.7086 0.4104 0.116 Uiso 1 1 d G . . . .
O28 O 0.5851(6) 0.3150(8) 0.7297(6) 0.073(5) Uani 0.84(2) 1 d . . . B 2
H28A H 0.5727 0.3233 0.7590 0.109 Uiso 0.84(2) 1 d G . . B 2
H28B H 0.5665 0.3457 0.6969 0.109 Uiso 0.84(2) 1 d G . . B 2
O25 O 0.6698(4) 0.4209(6) 0.7360(5) 0.070(3) Uani 1 1 d . . . . .
H25A H 0.6452 0.3826 0.7303 0.105 Uiso 1 1 d G . . . .
H25B H 0.7053 0.4063 0.7628 0.105 Uiso 1 1 d G . . . .
O24 O 0.5621(10) 0.8084(14) 0.2961(13) 0.093(7) Uani 0.5 1 d . U . C 2
H24A H 0.5685 0.7689 0.3222 0.139 Uiso 0.5 1 d R . . C 2
H24B H 0.5502 0.7913 0.2567 0.139 Uiso 0.5 1 d R . . C 2
O23 O 0.5000 0.8475(8) 0.7500 0.091(6) Uani 1 2 d S T P . .
H23A H 0.5208 0.8824 0.7417 0.137 Uiso 0.5 1 d R . . . .
H23B H 0.5196 0.8052 0.7668 0.137 Uiso 0.5 1 d R . . . .
O27 O 0.5000 0.9933(17) 0.2500 0.080(8) Uani 0.5 2 d S TU P D 2
H27A H 0.5143 0.9566 0.2789 0.119 Uiso 0.25 1 d R . . D 2
H27B H 0.4740 0.9735 0.2138 0.119 Uiso 0.25 1 d R . . D 2
O21 O 0.4938(5) 0.9214(5) 0.3654(7) 0.093(4) Uani 1 1 d . . . . .
H21A H 0.4848 0.8905 0.3324 0.139 Uiso 1 1 d R . . . .
H21B H 0.4731 0.9087 0.3859 0.139 Uiso 1 1 d R . . . .
O26 O 0.5111(17) 0.6059(11) 0.2714(10) 0.090(9) Uani 0.5 1 d . . . E 2
O24A O 0.5619(18) 0.883(3) 0.2736(17) 0.082(13) Uani 0.25 1 d . U . F 1
H24C H 0.5871 0.9064 0.3083 0.123 Uiso 0.25 1 d R . . F 1
H24D H 0.5275 0.8813 0.2740 0.123 Uiso 0.25 1 d R . . F 1
O28A O 0.594(2) 0.636(3) 0.283(2) 0.046(15) Uani 0.16(2) 1 d . . . B 1
H28C H 0.5772 0.6328 0.3096 0.069 Uiso 0.16(2) 1 d R . . B 1
H28D H 0.6014 0.6842 0.2789 0.069 Uiso 0.16(2) 1 d R . . B 1
O18A O 0.419(2) 0.818(3) 0.387(2) 0.029(13) Uani 0.127(11) 1 d . U . A 2
O16A O 0.372(2) 0.731(3) 0.436(2) 0.023(11) Uani 0.127(11) 1 d . U . A 2
O17A O 0.457(2) 0.679(3) 0.413(3) 0.033(13) Uani 0.127(11) 1 d . U . A 2
H17A H 0.4800 0.6943 0.3973 0.050 Uiso 0.127(11) 1 d R . . A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9500 . ?
C1 C2 1.377(11) . ?
C1 N1 1.358(10) . ?
C2 C3 1.396(12) . ?
C2 P1 1.817(8) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.389(12) . ?
C5 C6 1.460(12) . ?
C5 N1 1.358(9) . ?
C6 C7 1.372(12) . ?
C6 N2 1.366(11) . ?
C7 H7 0.9500 . ?
C7 C8 1.397(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.362(15) . ?
C9 C10 1.378(11) . ?
C9 P2 1.816(9) . ?
C10 H10 0.9500 . ?
C10 N2 1.340(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.394(11) . ?
C11 N3 1.337(9) . ?
C12 C13 1.389(10) . ?
C12 P3 1.818(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.392(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.379(10) . ?
C15 C16 1.464(10) . ?
C15 N3 1.363(9) . ?
C16 C17 1.371(10) . ?
C16 N4 1.368(9) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(11) . ?
C18 H18 0.9500 . ?
C18 C19 1.378(11) . ?
C19 C20 1.400(10) . ?
C19 P4 1.814(8) . ?
C20 H20 0.9500 . ?
C20 N4 1.333(9) . ?
C21 H21 0.9500 . ?
C21 C22 1.389(10) . ?
C21 N5 1.344(10) . ?
C22 C23 1.380(11) . ?
C22 P5 1.817(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.371(11) . ?
C24 H24 0.9500 . ?
C24 C25 1.389(10) . ?
C25 C26 1.457(11) . ?
C25 N5 1.340(10) . ?
C26 C27 1.376(13) . ?
C26 N6 1.349(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.381(13) . ?
C28 H28 0.9500 . ?
C28 C29 1.390(12) . ?
C29 C30 1.358(12) . ?
C29 P6 1.825(8) . ?
C30 H30 0.9500 . ?
C30 N6 1.344(10) . ?
Co1 N1 1.950(7) . ?
Co1 N2 1.943(6) . ?
Co1 N3 1.926(6) . ?
Co1 N4 1.930(6) . ?
Co1 N5 1.937(6) . ?
Co1 N6 1.947(7) . ?
O1 P1 1.501(6) . ?
O1 Tb1 2.241(6) . ?
O2 P1 1.537(7) . ?
O3 P1 1.496(7) . ?
O4 P2 1.491(7) . ?
O4 Tb1 2.431(7) 4_656 ?
O5 H5 0.8400 . ?
O5 P2 1.586(9) . ?
O6 P2 1.421(10) . ?
O7 P3 1.503(7) . ?
O7 Tb1 2.279(7) . ?
O8 H8A 0.8400 . ?
O8 P3 1.545(6) . ?
O9 P3 1.499(7) . ?
O10 P4 1.546(6) . ?
O11 P4 1.510(6) . ?
O11 Tb1 2.284(6) 6_565 ?
O12 P4 1.506(7) . ?
O13 H13A 0.8400 . ?
O13 P5 1.562(6) . ?
O14 P5 1.510(6) . ?
O14 Tb1 2.304(6) 7_667 ?
O15 P5 1.488(6) . ?
O16 H16 0.8400 . ?
O16 P6 1.537(7) . ?
O17 P6 1.506(8) . ?
O18 P6 1.514(7) . ?
O19 H19A 0.9024 . ?
O19 H19B 0.9012 . ?
O19 Tb1 2.526(8) . ?
O20 H20A 0.8812 . ?
O20 H20B 0.8800 . ?
O20 Tb1 2.382(8) . ?
P6 O18A 1.33(5) . ?
P6 O16A 1.42(4) . ?
P6 O17A 1.81(5) . ?
Tb1 O4 2.431(7) 4_646 ?
Tb1 O11 2.284(6) 6_566 ?
Tb1 O14 2.304(6) 7_667 ?
O22 H22A 0.8688 . ?
O22 H22B 0.8724 . ?
O28 H28A 0.8708 . ?
O28 H28B 0.8687 . ?
O25 H25A 0.8712 . ?
O25 H25B 0.8710 . ?
O24 H24A 0.8703 . ?
O24 H24B 0.8701 . ?
O23 H23A 0.8697 . ?
O23 H23B 0.8657 . ?
O27 H27A 0.8696 . ?
O27 H27B 0.8700 . ?
O21 H21A 0.8695 . ?
O21 H21B 0.8698 . ?
O26 O26 0.89(5) 2_655 ?
O24A H24C 0.8699 . ?
O24A H24D 0.8706 . ?
O28A H28C 0.8697 . ?
O28A H28D 0.8704 . ?
O17A H17A 0.8395 . ?

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
C2 C1 H1 118.4 . . ?
N1 C1 H1 118.4 . . ?
N1 C1 C2 123.3(7) . . ?
C1 C2 C3 117.3(8) . . ?
C1 C2 P1 119.4(6) . . ?
C3 C2 P1 123.3(6) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 C2 120.2(8) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 H4 120.3 . . ?
C3 C4 C5 119.5(8) . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 124.6(7) . . ?
N1 C5 C4 120.7(8) . . ?
N1 C5 C6 114.7(7) . . ?
C7 C6 C5 125.1(9) . . ?
N2 C6 C5 114.3(7) . . ?
N2 C6 C7 120.6(8) . . ?
C6 C7 H7 121.1 . . ?
C6 C7 C8 117.9(10) . . ?
C8 C7 H7 121.1 . . ?
C7 C8 H8 118.9 . . ?
C9 C8 C7 122.2(9) . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C10 116.6(9) . . ?
C8 C9 P2 122.7(7) . . ?
C10 C9 P2 120.6(7) . . ?
C9 C10 H10 118.4 . . ?
N2 C10 C9 123.1(9) . . ?
N2 C10 H10 118.4 . . ?
C12 C11 H11 118.4 . . ?
N3 C11 H11 118.4 . . ?
N3 C11 C12 123.1(7) . . ?
C11 C12 P3 119.0(6) . . ?
C13 C12 C11 116.8(7) . . ?
C13 C12 P3 124.0(6) . . ?
C12 C13 H13 119.5 . . ?
C12 C13 C14 121.0(7) . . ?
C14 C13 H13 119.5 . . ?
C13 C14 H14 120.8 . . ?
C15 C14 C13 118.4(7) . . ?
C15 C14 H14 120.8 . . ?
C14 C15 C16 124.1(7) . . ?
N3 C15 C14 121.5(7) . . ?
N3 C15 C16 114.3(6) . . ?
C17 C16 C15 125.2(7) . . ?
N4 C16 C15 113.8(6) . . ?
N4 C16 C17 121.0(7) . . ?
C16 C17 H17 120.5 . . ?
C16 C17 C18 119.0(7) . . ?
C18 C17 H17 120.5 . . ?
C17 C18 H18 119.8 . . ?
C19 C18 C17 120.4(7) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 117.8(7) . . ?
C18 C19 P4 119.7(6) . . ?
C20 C19 P4 122.4(6) . . ?
C19 C20 H20 119.0 . . ?
N4 C20 C19 122.1(7) . . ?
N4 C20 H20 119.0 . . ?
C22 C21 H21 118.7 . . ?
N5 C21 H21 118.7 . . ?
N5 C21 C22 122.6(7) . . ?
C21 C22 P5 120.7(6) . . ?
C23 C22 C21 117.7(7) . . ?
C23 C22 P5 121.5(6) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 C22 120.1(7) . . ?
C24 C23 H23 120.0 . . ?
C23 C24 H24 120.4 . . ?
C23 C24 C25 119.3(7) . . ?
C25 C24 H24 120.4 . . ?
C24 C25 C26 123.7(7) . . ?
N5 C25 C24 121.3(7) . . ?
N5 C25 C26 114.9(6) . . ?
C27 C26 C25 124.6(7) . . ?
N6 C26 C25 114.6(7) . . ?
N6 C26 C27 120.7(8) . . ?
C26 C27 H27 120.3 . . ?
C26 C27 C28 119.5(8) . . ?
C28 C27 H27 120.3 . . ?
C27 C28 H28 120.2 . . ?
C27 C28 C29 119.7(8) . . ?
C29 C28 H28 120.2 . . ?
C28 C29 P6 119.7(7) . . ?
C30 C29 C28 117.6(8) . . ?
C30 C29 P6 122.6(6) . . ?
C29 C30 H30 118.3 . . ?
N6 C30 C29 123.5(7) . . ?
N6 C30 H30 118.3 . . ?
N2 Co1 N1 83.5(3) . . ?
N2 Co1 N6 94.1(3) . . ?
N3 Co1 N1 91.7(3) . . ?
N3 Co1 N2 175.1(3) . . ?
N3 Co1 N4 84.1(3) . . ?
N3 Co1 N5 91.9(2) . . ?
N3 Co1 N6 90.7(3) . . ?
N4 Co1 N1 88.4(3) . . ?
N4 Co1 N2 94.6(3) . . ?
N4 Co1 N5 174.5(3) . . ?
N4 Co1 N6 92.6(3) . . ?
N5 Co1 N1 95.5(3) . . ?
N5 Co1 N2 89.7(2) . . ?
N5 Co1 N6 83.6(3) . . ?
N6 Co1 N1 177.4(3) . . ?
C1 N1 C5 119.1(7) . . ?
C1 N1 Co1 127.2(5) . . ?
C5 N1 Co1 113.7(6) . . ?
C6 N2 Co1 113.8(5) . . ?
C10 N2 C6 119.6(7) . . ?
C10 N2 Co1 126.6(6) . . ?
C11 N3 C15 119.1(6) . . ?
C11 N3 Co1 126.7(5) . . ?
C15 N3 Co1 113.4(5) . . ?
C16 N4 Co1 113.6(5) . . ?
C20 N4 C16 119.7(6) . . ?
C20 N4 Co1 126.5(5) . . ?
C21 N5 Co1 127.2(5) . . ?
C25 N5 C21 119.0(6) . . ?
C25 N5 Co1 113.4(5) . . ?
C26 N6 Co1 112.9(5) . . ?
C30 N6 C26 118.8(7) . . ?
C30 N6 Co1 128.2(5) . . ?
P1 O1 Tb1 150.5(4) . . ?
P2 O4 Tb1 144.2(5) . 4_656 ?
P2 O5 H5 109.5 . . ?
P3 O7 Tb1 154.9(4) . . ?
P3 O8 H8A 109.5 . . ?
P4 O11 Tb1 166.3(4) . 6_565 ?
P5 O13 H13A 109.5 . . ?
P5 O14 Tb1 134.6(3) . 7_667 ?
P6 O16 H16 109.5 . . ?
H19A O19 H19B 107.8 . . ?
Tb1 O19 H19A 110.9 . . ?
Tb1 O19 H19B 110.7 . . ?
H20A O20 H20B 108.9 . . ?
Tb1 O20 H20A 109.9 . . ?
Tb1 O20 H20B 109.6 . . ?
O1 P1 C2 106.2(4) . . ?
O1 P1 O2 110.4(4) . . ?
O2 P1 C2 106.1(4) . . ?
O3 P1 C2 108.7(4) . . ?
O3 P1 O1 117.0(4) . . ?
O3 P1 O2 107.9(4) . . ?
O4 P2 C9 106.9(4) . . ?
O4 P2 O5 110.1(5) . . ?
O5 P2 C9 103.3(5) . . ?
O6 P2 C9 107.0(5) . . ?
O6 P2 O4 119.6(6) . . ?
O6 P2 O5 108.6(6) . . ?
O7 P3 C12 107.1(4) . . ?
O7 P3 O8 111.5(4) . . ?
O8 P3 C12 105.3(4) . . ?
O9 P3 C12 107.2(4) . . ?
O9 P3 O7 114.1(4) . . ?
O9 P3 O8 111.2(4) . . ?
O10 P4 C19 105.5(3) . . ?
O11 P4 C19 109.2(4) . . ?
O11 P4 O10 108.4(4) . . ?
O12 P4 C19 104.2(3) . . ?
O12 P4 O10 113.6(4) . . ?
O12 P4 O11 115.4(4) . . ?
O13 P5 C22 103.8(3) . . ?
O14 P5 C22 107.4(3) . . ?
O14 P5 O13 111.0(4) . . ?
O15 P5 C22 107.2(3) . . ?
O15 P5 O13 110.8(4) . . ?
O15 P5 O14 115.8(4) . . ?
O16 P6 C29 103.4(4) . . ?
O17 P6 C29 106.6(4) . . ?
O17 P6 O16 110.7(5) . . ?
O17 P6 O18 116.9(5) . . ?
O18 P6 C29 107.3(4) . . ?
O18 P6 O16 111.0(4) . . ?
O18A P6 C29 104(2) . . ?
O18A P6 O16A 126(3) . . ?
O18A P6 O17A 107(3) . . ?
O16A P6 C29 108.5(18) . . ?
O16A P6 O17A 107(2) . . ?
O17A P6 C29 102.3(17) . . ?
O1 Tb1 O4 85.3(2) . 4_646 ?
O1 Tb1 O7 109.4(2) . . ?
O1 Tb1 O11 92.8(2) . 6_566 ?
O1 Tb1 O14 163.2(2) . 7_667 ?
O1 Tb1 O19 73.0(2) . . ?
O1 Tb1 O20 91.3(3) . . ?
O4 Tb1 O19 140.6(3) 4_646 . ?
O7 Tb1 O4 149.7(3) . 4_646 ?
O7 Tb1 O11 78.0(2) . 6_566 ?
O7 Tb1 O14 87.5(2) . 7_667 ?
O7 Tb1 O19 69.7(3) . . ?
O7 Tb1 O20 127.6(3) . . ?
O11 Tb1 O4 74.9(2) 6_566 4_646 ?
O11 Tb1 O14 90.7(2) 6_566 7_667 ?
O11 Tb1 O19 137.1(3) 6_566 . ?
O11 Tb1 O20 150.6(4) 6_566 . ?
O14 Tb1 O4 79.7(2) 7_667 4_646 ?
O14 Tb1 O19 114.6(3) 7_667 . ?
O14 Tb1 O20 77.8(3) 7_667 . ?
O20 Tb1 O4 76.5(4) . 4_646 ?
O20 Tb1 O19 71.7(4) . . ?
H22A O22 H22B 109.3 . . ?
H28A O28 H28B 109.4 . . ?
H25A O25 H25B 109.4 . . ?
H24A O24 H24B 109.5 . . ?
H23A O23 H23B 112.9 . . ?
H27A O27 H27B 109.5 . . ?
H21A O21 H21B 109.5 . . ?
H24C O24A H24D 109.5 . . ?
H28C O28A H28D 109.5 . . ?
P6 O17A H17A 109.7 . . ?

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
C1 C2 C3 C4 -2.2(12) . . . . ?
C1 C2 P1 O1 -32.1(7) . . . . ?
C1 C2 P1 O2 85.4(7) . . . . ?
C1 C2 P1 O3 -158.8(6) . . . . ?
C2 C1 N1 C5 1.1(11) . . . . ?
C2 C1 N1 Co1 177.3(6) . . . . ?
C2 C3 C4 C5 1.9(14) . . . . ?
C3 C2 P1 O1 149.8(7) . . . . ?
C3 C2 P1 O2 -92.7(8) . . . . ?
C3 C2 P1 O3 23.1(8) . . . . ?
C3 C4 C5 C6 -179.4(8) . . . . ?
C3 C4 C5 N1 -0.1(13) . . . . ?
C4 C5 C6 C7 -4.9(14) . . . . ?
C4 C5 C6 N2 177.0(8) . . . . ?
C4 C5 N1 C1 -1.4(11) . . . . ?
C4 C5 N1 Co1 -178.1(7) . . . . ?
C5 C6 C7 C8 179.2(10) . . . . ?
C5 C6 N2 C10 -179.8(7) . . . . ?
C5 C6 N2 Co1 2.2(9) . . . . ?
C6 C5 N1 C1 177.9(7) . . . . ?
C6 C5 N1 Co1 1.2(9) . . . . ?
C6 C7 C8 C9 2.5(18) . . . . ?
C7 C6 N2 C10 2.0(12) . . . . ?
C7 C6 N2 Co1 -175.9(8) . . . . ?
C7 C8 C9 C10 -1.4(17) . . . . ?
C7 C8 C9 P2 179.3(9) . . . . ?
C8 C9 C10 N2 0.5(13) . . . . ?
C8 C9 P2 O4 -33.5(10) . . . . ?
C8 C9 P2 O5 -149.6(9) . . . . ?
C8 C9 P2 O6 95.8(10) . . . . ?
C9 C10 N2 C6 -0.8(12) . . . . ?
C9 C10 N2 Co1 176.8(6) . . . . ?
C10 C9 P2 O4 147.3(7) . . . . ?
C10 C9 P2 O5 31.1(9) . . . . ?
C10 C9 P2 O6 -83.5(9) . . . . ?
C11 C12 C13 C14 0.3(12) . . . . ?
C11 C12 P3 O7 -93.3(7) . . . . ?
C11 C12 P3 O8 147.9(7) . . . . ?
C11 C12 P3 O9 29.5(8) . . . . ?
C12 C11 N3 C15 3.9(12) . . . . ?
C12 C11 N3 Co1 -165.1(6) . . . . ?
C12 C13 C14 C15 1.5(12) . . . . ?
C13 C12 P3 O7 81.5(8) . . . . ?
C13 C12 P3 O8 -37.3(8) . . . . ?
C13 C12 P3 O9 -155.7(7) . . . . ?
C13 C14 C15 C16 177.0(7) . . . . ?
C13 C14 C15 N3 -0.8(11) . . . . ?
C14 C15 C16 C17 12.3(12) . . . . ?
C14 C15 C16 N4 -169.2(7) . . . . ?
C14 C15 N3 C11 -1.9(11) . . . . ?
C14 C15 N3 Co1 168.5(6) . . . . ?
C15 C16 C17 C18 177.1(7) . . . . ?
C15 C16 N4 C20 -179.3(7) . . . . ?
C15 C16 N4 Co1 -3.7(8) . . . . ?
C16 C15 N3 C11 -179.8(7) . . . . ?
C16 C15 N3 Co1 -9.4(8) . . . . ?
C16 C17 C18 C19 1.9(12) . . . . ?
C17 C16 N4 C20 -0.8(11) . . . . ?
C17 C16 N4 Co1 174.8(6) . . . . ?
C17 C18 C19 C20 -0.4(11) . . . . ?
C17 C18 C19 P4 -179.7(6) . . . . ?
C18 C19 C20 N4 -1.7(12) . . . . ?
C18 C19 P4 O10 152.9(6) . . . . ?
C18 C19 P4 O11 -90.8(7) . . . . ?
C18 C19 P4 O12 33.0(7) . . . . ?
C19 C20 N4 C16 2.3(11) . . . . ?
C19 C20 N4 Co1 -172.7(6) . . . . ?
C20 C19 P4 O10 -26.3(8) . . . . ?
C20 C19 P4 O11 89.9(7) . . . . ?
C20 C19 P4 O12 -146.3(7) . . . . ?
C21 C22 C23 C24 -1.7(11) . . . . ?
C21 C22 P5 O13 153.3(6) . . . . ?
C21 C22 P5 O14 -89.1(7) . . . . ?
C21 C22 P5 O15 36.0(7) . . . . ?
C22 C21 N5 C25 3.2(10) . . . . ?
C22 C21 N5 Co1 -169.0(5) . . . . ?
C22 C23 C24 C25 1.8(12) . . . . ?
C23 C22 P5 O13 -25.0(7) . . . . ?
C23 C22 P5 O14 92.6(7) . . . . ?
C23 C22 P5 O15 -142.3(6) . . . . ?
C23 C24 C25 C26 176.9(7) . . . . ?
C23 C24 C25 N5 0.6(12) . . . . ?
C24 C25 C26 C27 13.9(13) . . . . ?
C24 C25 C26 N6 -168.1(7) . . . . ?
C24 C25 N5 C21 -3.1(11) . . . . ?
C24 C25 N5 Co1 170.2(6) . . . . ?
C25 C26 C27 C28 179.9(9) . . . . ?
C25 C26 N6 C30 176.1(7) . . . . ?
C25 C26 N6 Co1 -6.1(8) . . . . ?
C26 C25 N5 C21 -179.7(6) . . . . ?
C26 C25 N5 Co1 -6.4(8) . . . . ?
C26 C27 C28 C29 2.6(16) . . . . ?
C27 C26 N6 C30 -5.8(12) . . . . ?
C27 C26 N6 Co1 172.0(7) . . . . ?
C27 C28 C29 C30 -3.2(14) . . . . ?
C27 C28 C29 P6 -178.7(8) . . . . ?
C28 C29 C30 N6 -0.7(13) . . . . ?
C28 C29 P6 O16 -153.3(8) . . . . ?
C28 C29 P6 O17 90.0(8) . . . . ?
C28 C29 P6 O18 -36.0(9) . . . . ?
C28 C29 P6 O18A 49(3) . . . . ?
C28 C29 P6 O16A -87(2) . . . . ?
C28 C29 P6 O17A 159.7(19) . . . . ?
C29 C30 N6 C26 5.2(12) . . . . ?
C29 C30 N6 Co1 -172.2(6) . . . . ?
C30 C29 P6 O16 31.4(8) . . . . ?
C30 C29 P6 O17 -85.3(8) . . . . ?
C30 C29 P6 O18 148.8(7) . . . . ?
C30 C29 P6 O18A -126(3) . . . . ?
C30 C29 P6 O16A 97(2) . . . . ?
C30 C29 P6 O17A -15.5(19) . . . . ?
N1 C1 C2 C3 0.7(11) . . . . ?
N1 C1 C2 P1 -177.5(6) . . . . ?
N1 C5 C6 C7 175.8(9) . . . . ?
N1 C5 C6 N2 -2.3(10) . . . . ?
N2 C6 C7 C8 -2.8(15) . . . . ?
N3 C11 C12 C13 -3.1(12) . . . . ?
N3 C11 C12 P3 172.1(6) . . . . ?
N3 C15 C16 C17 -169.8(7) . . . . ?
N3 C15 C16 N4 8.7(9) . . . . ?
N4 C16 C17 C18 -1.3(11) . . . . ?
N5 C21 C22 C23 -0.8(11) . . . . ?
N5 C21 C22 P5 -179.1(5) . . . . ?
N5 C25 C26 C27 -169.7(8) . . . . ?
N5 C25 C26 N6 8.3(10) . . . . ?
N6 C26 C27 C28 2.0(14) . . . . ?
P1 C2 C3 C4 175.9(7) . . . . ?
P2 C9 C10 N2 179.8(6) . . . . ?
P3 C12 C13 C14 -174.6(7) . . . . ?
P4 C19 C20 N4 177.5(6) . . . . ?
P5 C22 C23 C24 176.6(6) . . . . ?
P6 C29 C30 N6 174.7(6) . . . . ?
Tb1 O1 P1 C2 -107.9(8) . . . . ?
Tb1 O1 P1 O2 137.5(7) . . . . ?
Tb1 O1 P1 O3 13.7(10) . . . . ?
Tb1 O4 P2 C9 -73.4(8) 4_656 . . . ?
Tb1 O4 P2 O5 38.1(9) 4_656 . . . ?
Tb1 O4 P2 O6 165.0(7) 4_656 . . . ?
Tb1 O7 P3 C12 -20.5(10) . . . . ?
Tb1 O7 P3 O8 94.2(10) . . . . ?
Tb1 O7 P3 O9 -138.9(9) . . . . ?
Tb1 O11 P4 C19 100.4(16) 6_565 . . . ?
Tb1 O11 P4 O10 -145.1(16) 6_565 . . . ?
Tb1 O11 P4 O12 -16.4(18) 6_565 . . . ?
Tb1 O14 P5 C22 -133.6(5) 7_667 . . . ?
Tb1 O14 P5 O13 -20.8(6) 7_667 . . . ?
Tb1 O14 P5 O15 106.6(5) 7_667 . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound-4
_database_code_depnum_ccdc_archive 'CCDC 1477306'
_audit_update_record             
;
2016-07-09 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_audit_creation_date             2016-07-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        Compound-4
_chemical_formula_moiety         
'C30 H28 Gd N6 Ni O21 P6, Cl, H Na O0.5, 2.5(H2 O), 3(O)'
_chemical_formula_sum            'C30 H34 Cl Gd N6 Na Ni O27 P6'
_chemical_formula_weight         1370.85
_chemical_absolute_configuration syn
_chemical_melting_point          ?
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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   22.6611(11)
_cell_length_b                   16.9747(8)
_cell_length_c                   15.2845(7)
_cell_angle_alpha                90
_cell_angle_beta                 106.794(2)
_cell_angle_gamma                90
_cell_volume                     5628.7(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7418
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      21.553
_cell_measurement_theta_min      2.239
_shelx_estimated_absorpt_T_max   0.915
_shelx_estimated_absorpt_T_min   0.713
_exptl_absorpt_coefficient_mu    1.811
_exptl_absorpt_correction_T_max  0.8992
_exptl_absorpt_correction_T_min  0.7379
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2728
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_unetI/netI     0.1174
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            59575
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.850
_diffrn_reflns_theta_min         1.523
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_reflns_Friedel_coverage         0.933
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                8222
_reflns_number_total             13356
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 
;
 Flack x determined using 2749 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     800
_refine_ls_number_reflns         13356
_refine_ls_number_restraints     115
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0678
_refine_ls_restrained_S_all      0.952
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0973P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1771
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O10A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O4) \\sim Ueq, Uanis(O4A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(O29) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(Cl1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(O5A) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(O17A) \\sim Ueq, Uanis(P6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(P6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O18) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(O17) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.01
Uanis(O5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O28) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.05
Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(P4A)=Sof(O11A)=Sof(H11B)=Sof(O10A)=1-FVAR(1)
 Sof(P4)=Sof(O10)=Sof(O11)=Sof(H11)=FVAR(1)
 Sof(O4)=Sof(P2A)=Sof(O5A)=Sof(H5A)=Sof(O6A)=1-FVAR(2)
 Sof(P2)=Sof(O5)=Sof(O6)=Sof(H2)=Sof(O4A)=FVAR(2)
 Sof(P6A)=Sof(O17A)=Sof(O18A)=Sof(H18B)=1-FVAR(3)
 Sof(P6)=Sof(O17)=Sof(O18)=Sof(H18)=FVAR(3)
 Fixed Sof: O22(0.5) H22A(0.5) H22B(0.5) O27(0.25) H27A(0.25) H27B(0.25)
 O35(0.75) H35A(0.75) H35B(0.75) O30(0.5) O33(0.5) O34(0.5) H34A(0.5) H34B(0.5)
 O36(0.5) H36A(0.5) H36B(0.5) O31(0.5) H31A(0.5) H31B(0.5) O28(0.5) O29(0.5)
4.a Riding coordinates:
 O20(H20A,H20B), O21(H21A,H21B), O27(H27A,H27B), O11A(H11B), O35(H35A,H35B),
 O34(H34A,H34B), O36(H36A,H36B), O31(H31A,H31B), O18A(H18B)
4.b Rotating group:
 O22(H22A,H22B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11A), C13(H13A),
 C14(H14), C17(H17), C18(H18A), C20(H20), C21(H21), C23(H23), C24(H24),
 C27(H27), C28(H28), C30(H30)
4.d Idealised tetrahedral OH refined as rotating group:
 O1(H1), O6(H2), O9(H9), O11(H11), O13(H13), O18(H18), O5A(H5A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
Gd1 Gd 0.69322(4) 0.28863(6) 0.29060(4) 0.0525(3) Uani 1 1 d . . . . .
Ni1 Ni 0.33165(7) 0.36753(11) 0.19365(12) 0.0339(4) Uani 1 1 d . . . . .
P1 P 0.56783(14) 0.3840(2) 0.1183(2) 0.0270(7) Uani 1 1 d . . . . .
P2 P 0.2066(15) 0.5688(18) 0.380(2) 0.032(5) Uani 0.38(5) 1 d . . . A 1
P3 P 0.3437(2) 0.1460(3) -0.0970(3) 0.0509(11) Uani 1 1 d . . . . .
P4 P 0.4142(6) 0.3416(9) 0.5794(8) 0.035(3) Uani 0.64(4) 1 d . . . B 1
P5 P 0.2991(2) 0.5669(3) -0.1230(3) 0.0573(12) Uani 1 1 d . . . . .
P6 P 0.1449(10) 0.2245(16) 0.3290(17) 0.039(5) Uani 0.44(5) 1 d . U . C 1
Cl1 Cl 0.3188(3) 0.6780(5) 0.0969(3) 0.097(2) Uani 1 1 d . U . . .
O1 O 0.5731(4) 0.4371(5) 0.0394(5) 0.034(2) Uani 1 1 d . . . . .
H1 H 0.5808 0.4835 0.0585 0.050 Uiso 1 1 calc GR . . . .
O2 O 0.6271(4) 0.3725(6) 0.1902(6) 0.040(2) Uani 1 1 d . . . . .
O3 O 0.5396(4) 0.3069(5) 0.0747(5) 0.033(2) Uani 1 1 d . . . . .
O4 O 0.1998(14) 0.6733(19) 0.358(2) 0.046(7) Uani 0.62(5) 1 d . U . A 2
O5 O 0.2245(17) 0.553(3) 0.479(2) 0.050(12) Uani 0.38(5) 1 d . U . A 1
O6 O 0.1587(18) 0.514(2) 0.329(4) 0.049(12) Uani 0.38(5) 1 d . . . A 1
H2 H 0.1573 0.4750 0.3616 0.074 Uiso 0.38(5) 1 calc GR . . A 1
O7 O 0.3258(5) 0.2174(8) -0.1526(6) 0.057(3) Uani 1 1 d . . . . .
O8 O 0.3998(6) 0.1029(7) -0.1089(8) 0.066(3) Uani 1 1 d . . . . .
O9 O 0.2917(7) 0.0824(9) -0.1149(8) 0.076(4) Uani 1 1 d . . . . .
H9 H 0.2698 0.0902 -0.0798 0.115 Uiso 1 1 calc GR . . . .
O10 O 0.4269(10) 0.4284(11) 0.5673(12) 0.048(6) Uani 0.64(4) 1 d . . . B 1
O11 O 0.4742(8) 0.3049(15) 0.6470(11) 0.046(7) Uani 0.64(4) 1 d . . . B 1
H11 H 0.4644 0.2672 0.6755 0.069 Uiso 0.64(4) 1 calc GR . . B 1
O12 O 0.3632(5) 0.3245(6) 0.6133(6) 0.048(3) Uani 1 1 d . . . . .
O13 O 0.2696(6) 0.6451(7) -0.1040(8) 0.062(3) Uani 1 1 d . . . . .
H13 H 0.2838 0.6569 -0.0485 0.094 Uiso 1 1 calc GR . . . .
O14 O 0.3670(6) 0.5662(7) -0.0803(8) 0.065(3) Uani 1 1 d . . . . .
O15 O 0.2766(7) 0.5543(9) -0.2231(8) 0.077(4) Uani 1 1 d . . . . .
O16 O 0.2040(7) 0.2132(8) 0.4112(9) 0.080(4) Uani 1 1 d . . . . .
O17 O 0.1167(18) 0.142(2) 0.308(2) 0.062(11) Uani 0.44(5) 1 d . U . C 1
O18 O 0.102(2) 0.288(4) 0.352(3) 0.106(15) Uani 0.44(5) 1 d . U . C 1
H18 H 0.0789 0.2670 0.3788 0.159 Uiso 0.44(5) 1 calc GR . . C 1
O19 O 0.7369(7) 0.4222(9) 0.3207(10) 0.095(5) Uani 1 1 d . . . . .
O20 O 0.7783(5) 0.2931(12) 0.4336(6) 0.084(4) Uani 1 1 d . . . . .
H20A H 0.8055 0.3275 0.4281 0.125 Uiso 1 1 d R . . . .
H20B H 0.7956 0.2469 0.4446 0.125 Uiso 1 1 d R . . . .
O21 O 0.7857(6) 0.2764(13) 0.2468(8) 0.097(5) Uani 1 1 d . U . . .
H21A H 0.8166 0.3216 0.2656 0.146 Uiso 1 1 d R . . . .
H21B H 0.7810 0.2728 0.1780 0.146 Uiso 1 1 d R . . . .
N1 N 0.4152(5) 0.4199(6) 0.1965(7) 0.030(2) Uani 1 1 d . . . . .
N2 N 0.3260(5) 0.4713(7) 0.2623(8) 0.040(3) Uani 1 1 d . . . . .
N3 N 0.3519(5) 0.2599(6) 0.1401(7) 0.034(3) Uani 1 1 d . . . . .
N4 N 0.3731(4) 0.3065(7) 0.3124(6) 0.032(3) Uani 1 1 d . . . . .
N5 N 0.2806(5) 0.4138(8) 0.0697(9) 0.045(3) Uani 1 1 d . . . . .
N6 N 0.2440(5) 0.3273(7) 0.1858(8) 0.039(3) Uani 1 1 d . . . . .
C1 C 0.4584(5) 0.3914(7) 0.1640(8) 0.025(3) Uani 1 1 d . . . . .
H1A H 0.4508 0.3416 0.1345 0.030 Uiso 1 1 calc R . . . .
C2 C 0.5140(5) 0.4275(8) 0.1688(8) 0.028(3) Uani 1 1 d . . . . .
C3 C 0.5229(6) 0.5026(8) 0.2103(10) 0.036(3) Uani 1 1 d . . . . .
H3 H 0.5591 0.5319 0.2130 0.043 Uiso 1 1 calc R . . . .
C4 C 0.4785(6) 0.5336(9) 0.2471(9) 0.038(3) Uani 1 1 d . . . . .
H4 H 0.4850 0.5835 0.2767 0.045 Uiso 1 1 calc R . . . .
C5 C 0.4255(6) 0.4927(7) 0.2409(8) 0.027(3) Uani 1 1 d . . . . .
C6 C 0.3763(6) 0.5191(8) 0.2780(9) 0.034(3) Uani 1 1 d . . . . .
C7 C 0.3802(7) 0.5885(10) 0.3283(11) 0.049(4) Uani 1 1 d . . . . .
H7 H 0.4154 0.6216 0.3389 0.059 Uiso 1 1 calc R . . . .
C8 C 0.3323(8) 0.6080(13) 0.3621(12) 0.063(5) Uani 1 1 d . . . . .
H8 H 0.3346 0.6549 0.3969 0.076 Uiso 1 1 calc R . . . .
C9 C 0.2788(7) 0.5589(11) 0.3459(9) 0.050(4) Uani 1 1 d . . . . .
C10 C 0.2796(7) 0.4902(9) 0.2957(11) 0.045(4) Uani 1 1 d . . . . .
H10 H 0.2454 0.4553 0.2848 0.054 Uiso 1 1 calc R . . . .
C11 C 0.3432(6) 0.2402(8) 0.0519(8) 0.034(3) Uani 1 1 d . . . . .
H11A H 0.3239 0.2781 0.0071 0.040 Uiso 1 1 calc R . . . .
C12 C 0.3595(6) 0.1708(9) 0.0217(9) 0.037(3) Uani 1 1 d . . . . .
C13 C 0.3873(7) 0.1155(10) 0.0893(10) 0.048(4) Uani 1 1 d . . . . .
H13A H 0.4004 0.0662 0.0722 0.057 Uiso 1 1 calc R . . . .
C14 C 0.3959(7) 0.1326(10) 0.1811(11) 0.046(4) Uani 1 1 d . . . . .
H14 H 0.4137 0.0951 0.2273 0.055 Uiso 1 1 calc R . . . .
C15 C 0.3779(5) 0.2054(8) 0.2028(8) 0.031(3) Uani 1 1 d . . . . .
C16 C 0.3867(6) 0.2291(9) 0.2989(9) 0.033(3) Uani 1 1 d . U . . .
C17 C 0.4077(9) 0.1790(11) 0.3722(11) 0.061(5) Uani 1 1 d . . . . .
H17 H 0.4142 0.1248 0.3623 0.073 Uiso 1 1 calc R . . . .
C18 C 0.4194(9) 0.2081(12) 0.4614(11) 0.065(5) Uani 1 1 d . . . . .
H18A H 0.4349 0.1745 0.5126 0.078 Uiso 1 1 calc R . . . .
C19 C 0.4077(6) 0.2882(12) 0.4732(8) 0.046(3) Uani 1 1 d . . . . .
C20 C 0.3838(6) 0.3325(10) 0.3982(9) 0.041(3) Uani 1 1 d . . . . .
H20 H 0.3740 0.3858 0.4068 0.050 Uiso 1 1 calc R . . . .
C21 C 0.3030(8) 0.4661(10) 0.0207(10) 0.051(4) Uani 1 1 d . . . . .
H21 H 0.3436 0.4862 0.0446 0.061 Uiso 1 1 calc R . . . .
C22 C 0.2666(8) 0.4906(12) -0.0647(12) 0.061(5) Uani 1 1 d . . . . .
C23 C 0.2082(8) 0.4571(12) -0.0983(12) 0.061(5) Uani 1 1 d . U . . .
H23 H 0.1835 0.4708 -0.1580 0.073 Uiso 1 1 calc R . . . .
C24 C 0.1861(8) 0.4066(14) -0.0493(12) 0.070(6) Uani 1 1 d . . . . .
H24 H 0.1465 0.3835 -0.0734 0.084 Uiso 1 1 calc R . . . .
C25 C 0.2220(7) 0.3889(11) 0.0371(11) 0.054(4) Uani 1 1 d . . . . .
C26 C 0.2020(7) 0.3395(11) 0.1047(11) 0.054(4) Uani 1 1 d . . . . .
C27 C 0.1398(7) 0.3109(15) 0.0843(11) 0.080(8) Uani 1 1 d . . . . .
H27 H 0.1114 0.3176 0.0254 0.096 Uiso 1 1 calc R . . . .
C28 C 0.1230(7) 0.2730(16) 0.1544(12) 0.080(7) Uani 1 1 d . . . . .
H28 H 0.0814 0.2573 0.1453 0.096 Uiso 1 1 calc R . . . .
C29 C 0.1679(7) 0.2576(12) 0.2402(11) 0.069(6) Uani 1 1 d . . . . .
C30 C 0.2267(6) 0.2885(13) 0.2494(9) 0.049(3) Uani 1 1 d . . . . .
H30 H 0.2569 0.2809 0.3066 0.058 Uiso 1 1 calc R . . . .
O22 O -0.0402(9) 0.2466(15) 0.1650(18) 0.065(7) Uani 0.5 1 d . . . D 1
H22A H -0.0120 0.2097 0.2333 0.097 Uiso 0.5 1 d GR . . D 1
H22B H -0.0292 0.2021 0.1094 0.097 Uiso 0.5 1 d GR . . D 1
Na23 Na 0.9792(4) 0.4198(5) 0.1524(7) 0.100(3) Uani 1 1 d . . . . .
O27 O 0.5000 0.4976(16) 0.5000 0.071(10) Uani 0.5 2 d S T P E 2
H27A H 0.5134 0.4581 0.4749 0.106 Uiso 0.25 1 d R . . E 2
H27B H 0.4625 0.4883 0.5009 0.106 Uiso 0.25 1 d R . . E 2
P4A P 0.4277(10) 0.3103(18) 0.5960(13) 0.035(5) Uani 0.36(4) 1 d . . . B 2
O11A O 0.475(2) 0.251(4) 0.659(3) 0.081(16) Uani 0.36(4) 1 d . U . B 2
H11B H 0.4562 0.2093 0.6648 0.122 Uiso 0.36(4) 1 d R . . B 2
O10A O 0.4631(18) 0.389(2) 0.599(3) 0.061(13) Uani 0.36(4) 1 d . U . B 2
P2A P 0.2196(9) 0.5943(15) 0.3889(12) 0.039(4) Uani 0.62(5) 1 d . . . A 2
O5A O 0.2436(12) 0.5938(17) 0.4972(14) 0.047(7) Uani 0.62(5) 1 d . U . A 2
H5A H 0.2530 0.6398 0.5162 0.071 Uiso 0.62(5) 1 calc GR . . A 2
O6A O 0.1734(14) 0.531(2) 0.369(2) 0.063(8) Uani 0.62(5) 1 d . U . A 2
O4A O 0.186(2) 0.650(3) 0.352(3) 0.036(10) Uani 0.38(5) 1 d . U . A 1
O32 O 0.5182(7) 0.6688(11) 0.4610(12) 0.109(6) Uani 1 1 d . . . . .
O35 O 0.5695(9) 0.2144(10) 0.2362(11) 0.078(5) Uani 0.75 1 d . . . F 1
H35A H 0.5696 0.2465 0.1919 0.117 Uiso 0.75 1 d R . . F 1
H35B H 0.5634 0.1665 0.2152 0.117 Uiso 0.75 1 d R . . F 1
O30 O 0.9099(9) 0.289(3) 0.3346(17) 0.101(10) Uani 0.5 1 d . . . G 2
O33 O 0.4687(13) 0.6750(19) -0.006(2) 0.080(9) Uani 0.5 1 d . . . H 1
O34 O 0.4467(11) 0.6398(17) 0.040(2) 0.081(9) Uani 0.5 1 d . . . I 2
H34A H 0.4073 0.6395 0.0328 0.122 Uiso 0.5 1 d R . . I 2
H34B H 0.4579 0.5942 0.0235 0.122 Uiso 0.5 1 d R . . I 2
O36 O 0.1182(13) 0.4794(16) 0.2020(18) 0.076(8) Uani 0.5 1 d . . . J 2
H36A H 0.1416 0.4984 0.1711 0.115 Uiso 0.5 1 d R . . J 2
H36B H 0.1377 0.4806 0.2600 0.115 Uiso 0.5 1 d R . . J 2
O31 O 0.8435(10) 0.4332(18) 0.491(2) 0.089(10) Uani 0.5 1 d . U . K 2
H31A H 0.8475 0.4722 0.4559 0.134 Uiso 0.5 1 d R . . K 2
H31B H 0.8181 0.4465 0.5214 0.134 Uiso 0.5 1 d R . . K 2
O28 O 0.8955(17) 0.4608(14) 0.3512(18) 0.091(9) Uani 0.5 1 d . U . L 1
P6A P 0.1539(13) 0.197(2) 0.3348(17) 0.069(6) Uani 0.56(5) 1 d . U . C 2
O17A O 0.1441(18) 0.116(2) 0.2995(18) 0.074(10) Uani 0.56(5) 1 d . U . C 2
O18A O 0.0879(13) 0.233(3) 0.3361(19) 0.090(16) Uani 0.56(5) 1 d . . . C 2
H18B H 0.0724 0.2041 0.3684 0.135 Uiso 0.56(5) 1 d R . . C 2
O29 O 0.988(2) 0.506(2) 0.458(2) 0.131(14) Uani 0.5 1 d . U . M 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O2 2.301(9) . ?
Gd1 O4 2.20(3) 3_545 ?
Gd1 O7 2.360(11) 2_655 ?
Gd1 O12 2.290(9) 2_656 ?
Gd1 O19 2.463(15) . ?
Gd1 O20 2.463(10) . ?
Gd1 O21 2.386(11) . ?
Gd1 O4A 2.55(4) 3_545 ?
Ni1 N1 2.080(10) . ?
Ni1 N2 2.074(12) . ?
Ni1 N3 2.106(11) . ?
Ni1 N4 2.065(10) . ?
Ni1 N5 2.068(12) . ?
Ni1 N6 2.071(11) . ?
P1 O1 1.539(9) . ?
P1 O2 1.482(9) . ?
P1 O3 1.523(9) . ?
P1 C2 1.781(13) . ?
P2 O5 1.47(4) . ?
P2 O6 1.47(4) . ?
P2 C9 1.86(3) . ?
P2 O4A 1.48(5) . ?
P3 O7 1.468(13) . ?
P3 O8 1.524(13) . ?
P3 O9 1.563(13) . ?
P3 C12 1.795(13) . ?
P4 O10 1.52(2) . ?
P4 O11 1.58(2) . ?
P4 O12 1.427(14) . ?
P4 C19 1.828(16) . ?
P5 O13 1.552(12) . ?
P5 O14 1.488(14) . ?
P5 O15 1.482(13) . ?
P5 C22 1.84(2) . ?
P6 O16 1.56(3) . ?
P6 O17 1.53(4) . ?
P6 O18 1.56(6) . ?
P6 C29 1.69(3) . ?
O1 H1 0.8400 . ?
O4 Gd1 2.20(3) 3_455 ?
O4 P2A 1.45(3) . ?
O6 H2 0.8400 . ?
O7 Gd1 2.360(11) 2_655 ?
O9 H9 0.8400 . ?
O11 H11 0.8400 . ?
O12 Gd1 2.290(9) 2_656 ?
O12 P4A 1.58(2) . ?
O13 H13 0.8400 . ?
O16 P6A 1.40(3) . ?
O18 H18 0.8400 . ?
O20 H20A 0.8705 . ?
O20 H20B 0.8703 . ?
O21 H21A 1.0241 . ?
O21 H21B 1.0281 . ?
N1 C1 1.312(15) . ?
N1 C5 1.396(16) . ?
N2 C6 1.363(18) . ?
N2 C10 1.334(18) . ?
N3 C11 1.347(16) . ?
N3 C15 1.339(17) . ?
N4 C16 1.379(18) . ?
N4 C20 1.337(16) . ?
N5 C21 1.352(19) . ?
N5 C25 1.34(2) . ?
N6 C26 1.344(19) . ?
N6 C30 1.325(18) . ?
C1 H1A 0.9500 . ?
C1 C2 1.384(16) . ?
C2 C3 1.412(19) . ?
C3 H3 0.9500 . ?
C3 C4 1.391(19) . ?
C4 H4 0.9500 . ?
C4 C5 1.366(18) . ?
C5 C6 1.460(18) . ?
C6 C7 1.40(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.37(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.43(3) . ?
C9 C10 1.40(2) . ?
C9 P2A 1.76(2) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9500 . ?
C11 C12 1.35(2) . ?
C12 C13 1.40(2) . ?
C13 H13A 0.9500 . ?
C13 C14 1.39(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.37(2) . ?
C15 C16 1.479(17) . ?
C16 C17 1.38(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.40(2) . ?
C18 H18A 0.9500 . ?
C18 C19 1.41(3) . ?
C19 C20 1.35(2) . ?
C19 P4A 1.84(2) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.39(2) . ?
C22 C23 1.39(3) . ?
C23 H23 0.9500 . ?
C23 C24 1.33(3) . ?
C24 H24 0.9500 . ?
C24 C25 1.37(2) . ?
C25 C26 1.50(2) . ?
C26 C27 1.44(2) . ?
C27 H27 0.9500 . ?
C27 C28 1.40(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.43(2) . ?
C29 C30 1.40(2) . ?
C29 P6A 1.87(3) . ?
C30 H30 0.9500 . ?
O22 H22A 1.2266 . ?
O22 H22B 1.2152 . ?
O22 Na23 2.99(3) 1_455 ?
Na23 O22 2.99(3) 1_655 ?
O27 H27A 0.8702 . ?
O27 H27B 0.8698 . ?
P4A O11A 1.57(5) . ?
P4A O10A 1.55(4) . ?
O11A H11B 0.8401 . ?
P2A O5A 1.59(3) . ?
P2A O6A 1.47(3) . ?
O5A H5A 0.8400 . ?
O4A Gd1 2.55(4) 3_455 ?
O32 O32 1.63(3) 2_656 ?
O35 H35A 0.8706 . ?
O35 H35B 0.8698 . ?
O33 O33 1.38(6) 2_655 ?
O34 H34A 0.8702 . ?
O34 H34B 0.8702 . ?
O36 H36A 0.8691 . ?
O36 H36B 0.8686 . ?
O31 H31A 0.8697 . ?
O31 H31B 0.8701 . ?
P6A O17A 1.48(4) . ?
P6A O18A 1.62(4) . ?
O18A H18B 0.8401 . ?
O29 O29 1.25(7) 2_756 ?

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 Gd1 O7 78.8(3) . 2_655 ?
O2 Gd1 O19 72.8(4) . . ?
O2 Gd1 O20 139.9(5) . . ?
O2 Gd1 O21 108.8(5) . . ?
O2 Gd1 O4A 135.7(10) . 3_545 ?
O4 Gd1 O2 143.8(8) 3_545 . ?
O4 Gd1 O7 86.2(8) 3_545 2_655 ?
O4 Gd1 O12 84.9(8) 3_545 2_656 ?
O4 Gd1 O19 139.7(9) 3_545 . ?
O4 Gd1 O20 71.4(10) 3_545 . ?
O4 Gd1 O21 96.2(9) 3_545 . ?
O7 Gd1 O19 126.7(5) 2_655 . ?
O7 Gd1 O20 134.6(5) 2_655 . ?
O7 Gd1 O21 69.7(5) 2_655 . ?
O7 Gd1 O4A 80.8(11) 2_655 3_545 ?
O12 Gd1 O2 83.5(3) 2_656 . ?
O12 Gd1 O7 135.8(4) 2_656 2_655 ?
O12 Gd1 O19 84.5(5) 2_656 . ?
O12 Gd1 O20 82.0(4) 2_656 . ?
O12 Gd1 O21 154.3(4) 2_656 . ?
O12 Gd1 O4A 84.5(11) 2_656 3_545 ?
O19 Gd1 O20 68.7(5) . . ?
O19 Gd1 O4A 147.6(11) . 3_545 ?
O20 Gd1 O4A 79.6(11) . 3_545 ?
O21 Gd1 O19 78.1(7) . . ?
O21 Gd1 O20 74.1(4) . . ?
O21 Gd1 O4A 100.2(12) . 3_545 ?
N1 Ni1 N3 94.6(4) . . ?
N2 Ni1 N1 79.3(4) . . ?
N2 Ni1 N3 170.4(4) . . ?
N4 Ni1 N1 90.9(4) . . ?
N4 Ni1 N2 93.4(4) . . ?
N4 Ni1 N3 79.2(4) . . ?
N4 Ni1 N5 170.9(5) . . ?
N4 Ni1 N6 94.0(4) . . ?
N5 Ni1 N1 97.0(5) . . ?
N5 Ni1 N2 92.4(5) . . ?
N5 Ni1 N3 95.8(5) . . ?
N5 Ni1 N6 78.4(5) . . ?
N6 Ni1 N1 173.7(5) . . ?
N6 Ni1 N2 96.4(5) . . ?
N6 Ni1 N3 90.3(4) . . ?
O1 P1 C2 108.3(6) . . ?
O2 P1 O1 113.5(5) . . ?
O2 P1 O3 112.9(5) . . ?
O2 P1 C2 108.7(5) . . ?
O3 P1 O1 106.2(5) . . ?
O3 P1 C2 107.0(6) . . ?
O5 P2 O6 112(3) . . ?
O5 P2 C9 105(2) . . ?
O5 P2 O4A 116(3) . . ?
O6 P2 C9 112(2) . . ?
O6 P2 O4A 108(3) . . ?
O4A P2 C9 103(2) . . ?
O7 P3 O8 115.3(7) . . ?
O7 P3 O9 113.7(8) . . ?
O7 P3 C12 109.5(7) . . ?
O8 P3 O9 105.0(8) . . ?
O8 P3 C12 107.6(7) . . ?
O9 P3 C12 105.1(6) . . ?
O10 P4 O11 107.7(12) . . ?
O10 P4 C19 109.9(11) . . ?
O11 P4 C19 102.6(11) . . ?
O12 P4 O10 116.3(11) . . ?
O12 P4 O11 108.6(11) . . ?
O12 P4 C19 110.8(9) . . ?
O13 P5 C22 104.8(8) . . ?
O14 P5 O13 111.8(8) . . ?
O14 P5 C22 106.9(7) . . ?
O15 P5 O13 106.2(7) . . ?
O15 P5 O14 117.1(8) . . ?
O15 P5 C22 109.4(9) . . ?
O16 P6 C29 107.2(14) . . ?
O17 P6 O16 105(2) . . ?
O17 P6 O18 116(3) . . ?
O17 P6 C29 110(2) . . ?
O18 P6 O16 110(2) . . ?
O18 P6 C29 108(2) . . ?
P1 O1 H1 109.5 . . ?
P1 O2 Gd1 148.3(6) . . ?
P2A O4 Gd1 162(2) . 3_455 ?
P2 O6 H2 109.5 . . ?
P3 O7 Gd1 152.8(7) . 2_655 ?
P3 O9 H9 109.5 . . ?
P4 O11 H11 109.5 . . ?
P4 O12 Gd1 161.4(9) . 2_656 ?
P4A O12 Gd1 141.5(12) . 2_656 ?
P5 O13 H13 109.5 . . ?
P6 O18 H18 109.5 . . ?
Gd1 O20 H20A 109.2 . . ?
Gd1 O20 H20B 109.6 . . ?
H20A O20 H20B 109.4 . . ?
Gd1 O21 H21A 116.2 . . ?
Gd1 O21 H21B 117.0 . . ?
H21A O21 H21B 101.0 . . ?
C1 N1 Ni1 127.5(8) . . ?
C1 N1 C5 118.1(10) . . ?
C5 N1 Ni1 114.4(8) . . ?
C6 N2 Ni1 115.1(9) . . ?
C10 N2 Ni1 124.6(11) . . ?
C10 N2 C6 120.1(13) . . ?
C11 N3 Ni1 128.2(9) . . ?
C15 N3 Ni1 114.9(8) . . ?
C15 N3 C11 116.8(12) . . ?
C16 N4 Ni1 114.2(8) . . ?
C20 N4 Ni1 127.2(11) . . ?
C20 N4 C16 118.5(12) . . ?
C21 N5 Ni1 123.8(10) . . ?
C25 N5 Ni1 116.8(11) . . ?
C25 N5 C21 119.3(14) . . ?
C26 N6 Ni1 114.5(9) . . ?
C30 N6 Ni1 127.2(9) . . ?
C30 N6 C26 118.2(12) . . ?
N1 C1 H1A 117.1 . . ?
N1 C1 C2 125.8(11) . . ?
C2 C1 H1A 117.1 . . ?
C1 C2 P1 121.4(10) . . ?
C1 C2 C3 115.6(11) . . ?
C3 C2 P1 122.8(10) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 C2 119.8(12) . . ?
C4 C3 H3 120.1 . . ?
C3 C4 H4 119.9 . . ?
C5 C4 C3 120.2(12) . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C6 114.9(11) . . ?
C4 C5 N1 120.4(11) . . ?
C4 C5 C6 124.8(12) . . ?
N2 C6 C5 116.3(12) . . ?
N2 C6 C7 121.1(13) . . ?
C7 C6 C5 122.6(13) . . ?
C6 C7 H7 120.7 . . ?
C8 C7 C6 118.6(16) . . ?
C8 C7 H7 120.7 . . ?
C7 C8 H8 119.4 . . ?
C7 C8 C9 121.2(17) . . ?
C9 C8 H8 119.4 . . ?
C8 C9 P2 131.8(17) . . ?
C8 C9 P2A 115.7(16) . . ?
C10 C9 P2 112.4(16) . . ?
C10 C9 C8 115.8(14) . . ?
C10 C9 P2A 128.4(17) . . ?
N2 C10 C9 123.1(15) . . ?
N2 C10 H10 118.4 . . ?
C9 C10 H10 118.4 . . ?
N3 C11 H11A 117.2 . . ?
N3 C11 C12 125.6(13) . . ?
C12 C11 H11A 117.2 . . ?
C11 C12 P3 123.6(11) . . ?
C11 C12 C13 116.1(12) . . ?
C13 C12 P3 120.2(11) . . ?
C12 C13 H13A 119.8 . . ?
C14 C13 C12 120.3(15) . . ?
C14 C13 H13A 119.8 . . ?
C13 C14 H14 121.1 . . ?
C15 C14 C13 117.9(15) . . ?
C15 C14 H14 121.1 . . ?
N3 C15 C14 123.2(12) . . ?
N3 C15 C16 115.3(12) . . ?
C14 C15 C16 121.4(13) . . ?
N4 C16 C15 115.9(12) . . ?
C17 C16 N4 120.4(12) . . ?
C17 C16 C15 123.7(13) . . ?
C16 C17 H17 120.1 . . ?
C16 C17 C18 119.9(16) . . ?
C18 C17 H17 120.1 . . ?
C17 C18 H18A 120.8 . . ?
C17 C18 C19 118.4(16) . . ?
C19 C18 H18A 120.8 . . ?
C18 C19 P4 128.6(14) . . ?
C18 C19 P4A 109.2(16) . . ?
C20 C19 P4 112.8(15) . . ?
C20 C19 C18 118.3(13) . . ?
C20 C19 P4A 132.5(18) . . ?
N4 C20 C19 124.3(15) . . ?
N4 C20 H20 117.8 . . ?
C19 C20 H20 117.8 . . ?
N5 C21 H21 120.0 . . ?
N5 C21 C22 120.0(17) . . ?
C22 C21 H21 120.0 . . ?
C21 C22 P5 116.9(15) . . ?
C21 C22 C23 117.8(17) . . ?
C23 C22 P5 125.3(13) . . ?
C22 C23 H23 119.1 . . ?
C24 C23 C22 121.9(15) . . ?
C24 C23 H23 119.1 . . ?
C23 C24 H24 121.0 . . ?
C23 C24 C25 118.0(17) . . ?
C25 C24 H24 121.0 . . ?
N5 C25 C24 122.5(17) . . ?
N5 C25 C26 112.5(13) . . ?
C24 C25 C26 124.9(15) . . ?
N6 C26 C25 116.6(13) . . ?
N6 C26 C27 122.5(14) . . ?
C27 C26 C25 120.8(14) . . ?
C26 C27 H27 121.4 . . ?
C28 C27 C26 117.2(14) . . ?
C28 C27 H27 121.4 . . ?
C27 C28 H28 119.8 . . ?
C27 C28 C29 120.5(13) . . ?
C29 C28 H28 119.8 . . ?
C28 C29 P6 119.6(14) . . ?
C28 C29 P6A 124.9(14) . . ?
C30 C29 P6 123.4(14) . . ?
C30 C29 C28 115.4(15) . . ?
C30 C29 P6A 119.7(15) . . ?
N6 C30 C29 126.0(13) . . ?
N6 C30 H30 117.0 . . ?
C29 C30 H30 117.0 . . ?
H22A O22 H22B 96.8 . . ?
Na23 O22 H22A 120.4 1_455 . ?
Na23 O22 H22B 120.2 1_455 . ?
H27A O27 H27B 109.5 . . ?
O12 P4A C19 103.5(12) . . ?
O11A P4A O12 119(2) . . ?
O11A P4A C19 115(2) . . ?
O10A P4A O12 111.2(19) . . ?
O10A P4A C19 100.3(18) . . ?
O10A P4A O11A 106(3) . . ?
P4A O11A H11B 109.6 . . ?
O4 P2A C9 113.1(16) . . ?
O4 P2A O5A 109.0(16) . . ?
O4 P2A O6A 118(2) . . ?
O5A P2A C9 108.6(13) . . ?
O6A P2A C9 104.3(18) . . ?
O6A P2A O5A 102.7(18) . . ?
P2A O5A H5A 109.5 . . ?
P2 O4A Gd1 157(3) . 3_455 ?
H35A O35 H35B 109.5 . . ?
H34A O34 H34B 109.5 . . ?
H36A O36 H36B 109.6 . . ?
H31A O31 H31B 109.5 . . ?
O16 P6A C29 105.3(15) . . ?
O16 P6A O17A 119(2) . . ?
O16 P6A O18A 117(2) . . ?
O17A P6A C29 105.7(19) . . ?
O17A P6A O18A 108(2) . . ?
O18A P6A C29 99.9(18) . . ?
P6A O18A H18B 109.8 . . ?

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
O1 H1 O14 0.84 1.80 2.557(13) 148.5 2_655
O9 H9 Cl1 0.84 2.45 3.062(18) 130.1 4_545
O13 H13 Cl1 0.84 2.16 3.001(13) 175.4 .
O20 H20A O31 0.87 2.10 2.80(3) 137.6 .
O21 H21B Cl1 1.03 2.34 3.097(15) 129.6 3_545
O27 H27A O10A 0.87 1.82 2.67(4) 167.8 2_656
O5A H5A O16 0.84 1.76 2.55(4) 156.1 4_556
O35 H35A O2 0.87 2.51 3.15(2) 131.4 .
O35 H35A O3 0.87 2.00 2.838(18) 159.9 .
O35 H35B O8 0.87 2.30 2.94(2) 130.5 2_655
O36 H36B O6A 0.87 1.84 2.65(4) 153.7 .
O31 H31B O6A 0.87 2.17 2.82(4) 131.6 2_656
O18A H18B O32 0.84 2.21 3.01(3) 159.9 3_445

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
Gd1 O4 P2A C9 -2(7) 3_455 . . . ?
Gd1 O4 P2A O5A 119(6) 3_455 . . . ?
Gd1 O4 P2A O6A -125(6) 3_455 . . . ?
Gd1 O12 P4A C19 131.2(13) 2_656 . . . ?
Gd1 O12 P4A O11A 2(3) 2_656 . . . ?
Gd1 O12 P4A O10A -122(2) 2_656 . . . ?
Ni1 N1 C1 C2 -178.7(9) . . . . ?
Ni1 N1 C5 C4 -179.6(10) . . . . ?
Ni1 N1 C5 C6 0.4(13) . . . . ?
Ni1 N2 C6 C5 2.8(14) . . . . ?
Ni1 N2 C6 C7 -176.1(11) . . . . ?
Ni1 N2 C10 C9 176.5(10) . . . . ?
Ni1 N3 C11 C12 177.1(9) . . . . ?
Ni1 N3 C15 C14 -178.1(10) . . . . ?
Ni1 N3 C15 C16 1.3(14) . . . . ?
Ni1 N4 C16 C15 8.2(14) . . . . ?
Ni1 N4 C16 C17 -172.4(12) . . . . ?
Ni1 N4 C20 C19 175.8(10) . . . . ?
Ni1 N5 C21 C22 176.1(12) . . . . ?
Ni1 N5 C25 C24 -171.1(15) . . . . ?
Ni1 N5 C25 C26 8.0(18) . . . . ?
Ni1 N6 C26 C25 -7.7(19) . . . . ?
Ni1 N6 C26 C27 175.6(15) . . . . ?
Ni1 N6 C30 C29 -175.6(15) . . . . ?
P1 C2 C3 C4 179.0(11) . . . . ?
P2 C9 C10 N2 178.6(15) . . . . ?
P3 C12 C13 C14 -175.7(11) . . . . ?
P4 C19 C20 N4 -178.3(11) . . . . ?
P5 C22 C23 C24 -174.9(16) . . . . ?
P6 C29 C30 N6 -167.7(19) . . . . ?
O1 P1 O2 Gd1 -139.0(10) . . . . ?
O1 P1 C2 C1 114.1(10) . . . . ?
O1 P1 C2 C3 -61.4(12) . . . . ?
O2 P1 C2 C1 -122.2(10) . . . . ?
O2 P1 C2 C3 62.3(12) . . . . ?
O3 P1 O2 Gd1 -18.1(12) . . . . ?
O3 P1 C2 C1 0.0(11) . . . . ?
O3 P1 C2 C3 -175.5(10) . . . . ?
O5 P2 C9 C8 -72(3) . . . . ?
O5 P2 C9 C10 107(2) . . . . ?
O5 P2 O4A Gd1 108(7) . . . 3_455 ?
O6 P2 C9 C8 166(3) . . . . ?
O6 P2 C9 C10 -14(3) . . . . ?
O6 P2 O4A Gd1 -125(6) . . . 3_455 ?
O7 P3 C12 C11 14.2(13) . . . . ?
O7 P3 C12 C13 -169.2(11) . . . . ?
O8 P3 O7 Gd1 44.3(16) . . . 2_655 ?
O8 P3 C12 C11 140.2(11) . . . . ?
O8 P3 C12 C13 -43.2(13) . . . . ?
O9 P3 O7 Gd1 -77.1(16) . . . 2_655 ?
O9 P3 C12 C11 -108.2(13) . . . . ?
O9 P3 C12 C13 68.3(14) . . . . ?
O10 P4 O12 Gd1 -105(3) . . . 2_656 ?
O10 P4 C19 C18 153.4(17) . . . . ?
O10 P4 C19 C20 -32.2(15) . . . . ?
O11 P4 O12 Gd1 16(3) . . . 2_656 ?
O11 P4 C19 C18 39.0(19) . . . . ?
O11 P4 C19 C20 -146.6(12) . . . . ?
O12 P4 C19 C18 -76.7(19) . . . . ?
O12 P4 C19 C20 97.7(15) . . . . ?
O13 P5 C22 C21 -99.0(14) . . . . ?
O13 P5 C22 C23 79.4(18) . . . . ?
O14 P5 C22 C21 19.8(16) . . . . ?
O14 P5 C22 C23 -161.8(16) . . . . ?
O15 P5 C22 C21 147.5(13) . . . . ?
O15 P5 C22 C23 -34.1(19) . . . . ?
O16 P6 C29 C28 179.7(19) . . . . ?
O16 P6 C29 C30 -16(3) . . . . ?
O17 P6 C29 C28 66(3) . . . . ?
O17 P6 C29 C30 -130(2) . . . . ?
O18 P6 C29 C28 -61(3) . . . . ?
O18 P6 C29 C30 103(3) . . . . ?
N1 C1 C2 P1 -177.9(10) . . . . ?
N1 C1 C2 C3 -2.1(18) . . . . ?
N1 C5 C6 N2 -2.1(16) . . . . ?
N1 C5 C6 C7 176.8(13) . . . . ?
N2 C6 C7 C8 0(2) . . . . ?
N3 C11 C12 P3 177.2(10) . . . . ?
N3 C11 C12 C13 0.5(19) . . . . ?
N3 C15 C16 N4 -6.3(17) . . . . ?
N3 C15 C16 C17 174.3(14) . . . . ?
N4 C16 C17 C18 -5(3) . . . . ?
N5 C21 C22 P5 176.1(12) . . . . ?
N5 C21 C22 C23 -2(2) . . . . ?
N5 C25 C26 N6 0(2) . . . . ?
N5 C25 C26 C27 176.6(17) . . . . ?
N6 C26 C27 C28 3(3) . . . . ?
C1 N1 C5 C4 2.1(18) . . . . ?
C1 N1 C5 C6 -177.9(11) . . . . ?
C1 C2 C3 C4 3.3(19) . . . . ?
C2 P1 O2 Gd1 100.5(11) . . . . ?
C2 C3 C4 C5 -2(2) . . . . ?
C3 C4 C5 N1 -1(2) . . . . ?
C3 C4 C5 C6 179.2(13) . . . . ?
C4 C5 C6 N2 177.9(13) . . . . ?
C4 C5 C6 C7 -3(2) . . . . ?
C5 N1 C1 C2 -0.6(18) . . . . ?
C5 C6 C7 C8 -178.7(15) . . . . ?
C6 N2 C10 C9 1(2) . . . . ?
C6 C7 C8 C9 -1(3) . . . . ?
C7 C8 C9 P2 -179.1(18) . . . . ?
C7 C8 C9 C10 1(2) . . . . ?
C7 C8 C9 P2A -177.0(15) . . . . ?
C8 C9 C10 N2 -2(2) . . . . ?
C8 C9 P2A O4 54(2) . . . . ?
C8 C9 P2A O5A -67.0(17) . . . . ?
C8 C9 P2A O6A -175.9(18) . . . . ?
C9 P2 O4A Gd1 -7(8) . . . 3_455 ?
C10 N2 C6 C5 178.5(12) . . . . ?
C10 N2 C6 C7 0(2) . . . . ?
C10 C9 P2A O4 -123.8(18) . . . . ?
C10 C9 P2A O5A 115.0(16) . . . . ?
C10 C9 P2A O6A 6(2) . . . . ?
C11 N3 C15 C14 0.7(18) . . . . ?
C11 N3 C15 C16 -180.0(11) . . . . ?
C11 C12 C13 C14 1(2) . . . . ?
C12 P3 O7 Gd1 165.8(13) . . . 2_655 ?
C12 C13 C14 C15 -2(2) . . . . ?
C13 C14 C15 N3 1(2) . . . . ?
C13 C14 C15 C16 -178.5(13) . . . . ?
C14 C15 C16 N4 173.0(12) . . . . ?
C14 C15 C16 C17 -6(2) . . . . ?
C15 N3 C11 C12 -1.4(18) . . . . ?
C15 C16 C17 C18 174.8(16) . . . . ?
C16 N4 C20 C19 0.5(19) . . . . ?
C16 C17 C18 C19 2(3) . . . . ?
C17 C18 C19 P4 176.3(14) . . . . ?
C17 C18 C19 C20 2(3) . . . . ?
C17 C18 C19 P4A -179.5(16) . . . . ?
C18 C19 C20 N4 -3(2) . . . . ?
C18 C19 P4A O12 -109.8(18) . . . . ?
C18 C19 P4A O11A 22(3) . . . . ?
C18 C19 P4A O10A 135(2) . . . . ?
C19 P4 O12 Gd1 128(2) . . . 2_656 ?
C20 N4 C16 C15 -175.9(11) . . . . ?
C20 N4 C16 C17 3.5(19) . . . . ?
C20 C19 P4A O12 68(2) . . . . ?
C20 C19 P4A O11A -160(3) . . . . ?
C20 C19 P4A O10A -47(2) . . . . ?
C21 N5 C25 C24 8(3) . . . . ?
C21 N5 C25 C26 -172.6(14) . . . . ?
C21 C22 C23 C24 4(3) . . . . ?
C22 C23 C24 C25 1(3) . . . . ?
C23 C24 C25 N5 -7(3) . . . . ?
C23 C24 C25 C26 173.8(18) . . . . ?
C24 C25 C26 N6 179.0(18) . . . . ?
C24 C25 C26 C27 -4(3) . . . . ?
C25 N5 C21 C22 -3(2) . . . . ?
C25 C26 C27 C28 -173(2) . . . . ?
C26 N6 C30 C29 1(3) . . . . ?
C26 C27 C28 C29 -5(3) . . . . ?
C27 C28 C29 P6 171(2) . . . . ?
C27 C28 C29 C30 5(3) . . . . ?
C27 C28 C29 P6A -173(2) . . . . ?
C28 C29 C30 N6 -2(3) . . . . ?
C28 C29 P6A O16 -166(2) . . . . ?
C28 C29 P6A O17A 67(3) . . . . ?
C28 C29 P6A O18A -45(3) . . . . ?
C30 N6 C26 C25 175.5(16) . . . . ?
C30 N6 C26 C27 -1(3) . . . . ?
C30 C29 P6A O16 16(3) . . . . ?
C30 C29 P6A O17A -111(2) . . . . ?
C30 C29 P6A O18A 137(2) . . . . ?
P4A C19 C20 N4 178.7(13) . . . . ?
P2A C9 C10 N2 176.3(14) . . . . ?
O4A P2 C9 C8 50(3) . . . . ?
O4A P2 C9 C10 -130(2) . . . . ?
P6A C29 C30 N6 175.2(19) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Compound-SI1
_database_code_depnum_ccdc_archive 'CCDC 1477307'
_audit_update_record             
;
2016-04-29 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_audit_creation_date             2016-04-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H10 N2 O6 P2'
_chemical_formula_sum            'C10 H10 N2 O6 P2'
_chemical_formula_weight         316.14
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_H-M_alt        'P b c n'
_space_group_name_Hall           '-P 2n 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   13.6133(9)
_cell_length_b                   13.0066(8)
_cell_length_c                   14.3436(9)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2539.7(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.019
_cell_measurement_theta_min      2.590
_shelx_estimated_absorpt_T_max   0.837
_shelx_estimated_absorpt_T_min   0.756
_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_T_max  1.0447
_exptl_absorpt_correction_T_min  0.6474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.5
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0738
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28368
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.019
_diffrn_reflns_theta_min         2.166
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2763
_reflns_number_total             3074
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3074
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0424P)²+1.6550P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0879
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Riding coordinates:
 O4(H4), O1(H1), O2(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1B), C4(H4A), C8(H8), C3(H3), C7(H7), C10(H10)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
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
P2 P 0.33152(3) 0.64877(3) 0.37054(2) 0.01326(10) Uani 1 1 d . . . . .
P1 P 0.61318(3) -0.10707(3) 0.36591(2) 0.01426(10) Uani 1 1 d . . . . .
O6 O 0.23089(7) 0.62661(8) 0.40975(7) 0.0187(2) Uani 1 1 d . . . . .
O5 O 0.33392(8) 0.68897(8) 0.27167(7) 0.0210(2) Uani 1 1 d . . . . .
O3 O 0.53637(8) -0.16561(8) 0.41657(7) 0.0213(2) Uani 1 1 d . . . . .
O4 O 0.38614(8) 0.72172(8) 0.43933(7) 0.0198(2) Uani 1 1 d . . . . .
H4 H 0.4366 0.7557 0.4212 0.030 Uiso 1 1 d R . . . .
O1 O 0.71575(7) -0.11131(8) 0.41421(7) 0.0204(2) Uani 1 1 d . . . . .
H1 H 0.7177 -0.1190 0.4758 0.031 Uiso 1 1 d R . . . .
O2 O 0.63082(9) -0.13194(8) 0.26335(7) 0.0232(2) Uani 1 1 d . . . . .
H2 H 0.6432 -0.2042 0.2469 0.035 Uiso 1 1 d R . . . .
N1 N 0.45978(9) 0.15715(9) 0.37126(8) 0.0154(2) Uani 1 1 d . . . . .
N2 N 0.38690(10) 0.34322(10) 0.36323(10) 0.0233(3) Uani 1 1 d . . . . .
C1 C 0.48410(10) 0.05755(11) 0.37289(9) 0.0159(3) Uani 1 1 d . . . . .
H1B H 0.4343 0.0069 0.3797 0.019 Uiso 1 1 calc R . . . .
C4 C 0.62448(10) 0.20840(11) 0.35347(10) 0.0181(3) Uani 1 1 d . . . . .
H4A H 0.6726 0.2607 0.3462 0.022 Uiso 1 1 calc R . . . .
C5 C 0.52586(10) 0.23394(11) 0.36363(9) 0.0147(3) Uani 1 1 d . . . . .
C9 C 0.39712(10) 0.52827(11) 0.37038(9) 0.0154(3) Uani 1 1 d . . . . .
C2 C 0.58149(10) 0.02777(11) 0.36466(9) 0.0143(3) Uani 1 1 d . . . . .
C8 C 0.49954(11) 0.52256(11) 0.37228(10) 0.0190(3) Uani 1 1 d . . . . .
H8 H 0.5379 0.5835 0.3748 0.023 Uiso 1 1 calc R . . . .
C6 C 0.48548(10) 0.33951(11) 0.36583(9) 0.0155(3) Uani 1 1 d . . . . .
C3 C 0.65171(11) 0.10539(11) 0.35405(10) 0.0184(3) Uani 1 1 d . . . . .
H3 H 0.7190 0.0875 0.3471 0.022 Uiso 1 1 calc R . . . .
C7 C 0.54485(11) 0.42657(12) 0.37040(10) 0.0188(3) Uani 1 1 d . . . . .
H7 H 0.6144 0.4206 0.3722 0.023 Uiso 1 1 calc R . . . .
C10 C 0.34480(11) 0.43613(12) 0.36564(11) 0.0229(3) Uani 1 1 d . . . . .
H10 H 0.2751 0.4396 0.3640 0.028 Uiso 1 1 calc R . . . .
H1A H 0.3925(18) 0.1710(19) 0.3800(15) 0.042(6) 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
P2 O6 1.5086(10) . ?
P2 O5 1.5118(10) . ?
P2 O4 1.5578(10) . ?
P2 C9 1.8039(14) . ?
P1 O3 1.4836(11) . ?
P1 O1 1.5598(10) . ?
P1 O2 1.5253(11) . ?
P1 C2 1.8061(14) . ?
O4 H4 0.8576 . ?
O1 H1 0.8900 . ?
O2 H2 0.9835 . ?
N1 C1 1.3373(18) . ?
N1 C5 1.3486(18) . ?
N1 H1A 0.94(2) . ?
N2 C6 1.3433(19) . ?
N2 C10 1.338(2) . ?
C1 H1B 0.9500 . ?
C1 C2 1.3863(19) . ?
C4 H4A 0.9500 . ?
C4 C5 1.3907(19) . ?
C4 C3 1.390(2) . ?
C5 C6 1.4795(18) . ?
C9 C8 1.3966(19) . ?
C9 C10 1.396(2) . ?
C2 C3 1.399(2) . ?
C8 H8 0.9500 . ?
C8 C7 1.393(2) . ?
C6 C7 1.393(2) . ?
C3 H3 0.9500 . ?
C7 H7 0.9500 . ?
C10 H10 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
O6 P2 O5 115.81(6) . . ?
O6 P2 O4 108.29(6) . . ?
O6 P2 C9 106.50(6) . . ?
O5 P2 O4 111.91(6) . . ?
O5 P2 C9 106.77(6) . . ?
O4 P2 C9 107.09(6) . . ?
O3 P1 O1 113.28(6) . . ?
O3 P1 O2 118.33(6) . . ?
O3 P1 C2 109.57(6) . . ?
O1 P1 C2 104.63(6) . . ?
O2 P1 O1 106.26(6) . . ?
O2 P1 C2 103.53(6) . . ?
P2 O4 H4 120.3 . . ?
P1 O1 H1 118.2 . . ?
P1 O2 H2 117.5 . . ?
C1 N1 C5 123.62(13) . . ?
C1 N1 H1A 115.1(15) . . ?
C5 N1 H1A 121.2(15) . . ?
C10 N2 C6 117.37(13) . . ?
N1 C1 H1B 119.8 . . ?
N1 C1 C2 120.39(13) . . ?
C2 C1 H1B 119.8 . . ?
C5 C4 H4A 120.4 . . ?
C3 C4 H4A 120.4 . . ?
C3 C4 C5 119.14(13) . . ?
N1 C5 C4 118.40(13) . . ?
N1 C5 C6 115.96(12) . . ?
C4 C5 C6 125.63(13) . . ?
C8 C9 P2 122.71(11) . . ?
C10 C9 P2 119.57(11) . . ?
C10 C9 C8 117.70(13) . . ?
C1 C2 P1 119.93(11) . . ?
C1 C2 C3 117.46(13) . . ?
C3 C2 P1 122.60(11) . . ?
C9 C8 H8 120.3 . . ?
C7 C8 C9 119.30(13) . . ?
C7 C8 H8 120.3 . . ?
N2 C6 C5 113.82(13) . . ?
N2 C6 C7 123.49(14) . . ?
C7 C6 C5 122.68(13) . . ?
C4 C3 C2 120.94(13) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C8 C7 H7 120.9 . . ?
C6 C7 C8 118.21(13) . . ?
C6 C7 H7 120.9 . . ?
N2 C10 C9 123.93(14) . . ?
N2 C10 H10 118.0 . . ?
C9 C10 H10 118.0 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O2 H2 O5 0.98 1.45 2.4308(15) 175.9 3_645

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
P2 C9 C8 C7 -178.91(10) . . . . ?
P2 C9 C10 N2 178.59(12) . . . . ?
P1 C2 C3 C4 -179.97(11) . . . . ?
O6 P2 C9 C8 -155.77(12) . . . . ?
O6 P2 C9 C10 26.02(13) . . . . ?
O5 P2 C9 C8 79.93(13) . . . . ?
O5 P2 C9 C10 -98.28(12) . . . . ?
O3 P1 C2 C1 -25.12(13) . . . . ?
O3 P1 C2 C3 155.97(11) . . . . ?
O4 P2 C9 C8 -40.09(13) . . . . ?
O4 P2 C9 C10 141.70(11) . . . . ?
O1 P1 C2 C1 -146.87(11) . . . . ?
O1 P1 C2 C3 34.22(13) . . . . ?
O2 P1 C2 C1 102.01(11) . . . . ?
O2 P1 C2 C3 -76.91(12) . . . . ?
N1 C1 C2 P1 -179.44(10) . . . . ?
N1 C1 C2 C3 -0.47(19) . . . . ?
N1 C5 C6 N2 -8.05(18) . . . . ?
N1 C5 C6 C7 171.80(13) . . . . ?
N2 C6 C7 C8 -0.1(2) . . . . ?
C1 N1 C5 C4 2.4(2) . . . . ?
C1 N1 C5 C6 -178.26(12) . . . . ?
C1 C2 C3 C4 1.1(2) . . . . ?
C4 C5 C6 N2 171.19(14) . . . . ?
C4 C5 C6 C7 -9.0(2) . . . . ?
C5 N1 C1 C2 -1.3(2) . . . . ?
C5 C4 C3 C2 0.0(2) . . . . ?
C5 C6 C7 C8 -179.90(13) . . . . ?
C9 C8 C7 C6 0.6(2) . . . . ?
C8 C9 C10 N2 0.3(2) . . . . ?
C6 N2 C10 C9 0.2(2) . . . . ?
C3 C4 C5 N1 -1.7(2) . . . . ?
C3 C4 C5 C6 179.06(13) . . . . ?
C10 N2 C6 C5 179.54(13) . . . . ?
C10 N2 C6 C7 -0.3(2) . . . . ?
C10 C9 C8 C7 -0.7(2) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
