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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_CPO-71-Cu
_database_code_depnum_ccdc_archive 'CCDC 1483001'
_audit_update_record             
;
2016-06-01 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT220_CPO-71-Cu           
;
PROBLEM: Non-Solvent Resd 1   C   Ueq(max)/Ueq(min) Range        8.8 Ratio
RESPONSE: This is related to the somewhat large thermal ellipsoids of the coordinated solvent molecule. 
;
_vrf_PLAT934_CPO-71-Cu           
;
PROBLEM: Number of (Iobs-Icalc)/SigmaW &gt; 10 Outliers ....          2 Check
RESPONSE: These are low angle reflections that seem to be influenced by the beamstop. Removing the reflections from the refinement does not noticably influence the final result. 
;
# Added during the CSD deposition process: Wednesday 01 June 2016 10:29 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        CPO-71-Cu
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H19 Cu N O7'
_chemical_formula_sum            'C19 H19 Cu N O7'
_chemical_formula_weight         436.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   18.0477(7)
_cell_length_b                   10.3801(4)
_cell_length_c                   23.4227(9)
_cell_angle_alpha                90
_cell_angle_beta                 96.7430(10)
_cell_angle_gamma                90
_cell_volume                     4357.6(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      27.43

_exptl_crystal_description       needle
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             1800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.136
_exptl_absorpt_coefficient_mu    1.039
_shelx_estimated_absorpt_T_min   0.775
_shelx_estimated_absorpt_T_max   0.872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6460
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      105(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker PHOTON CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34274
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.267
_diffrn_reflns_theta_max         27.507
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             5023
_reflns_number_gt                4065
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 (Bruker, 2007)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          SQUEEZE
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0295P)²+9.3159P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5023
_refine_ls_number_parameters     257
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0405
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0792
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.041 0.250 216 48 ' '
2 0.000 -0.041 0.750 216 48 ' '
3 0.500 0.459 0.750 216 48 ' '
4 0.500 0.541 0.250 216 48 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

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 0.16557(15) 0.5838(2) 0.23465(10) 0.0231(6) Uani 1 1 d . . . . .
C1C C 0.07860(16) 0.0163(3) 0.42863(14) 0.0399(8) Uani 1 1 d . . . . .
H1C H 0.1243 -0.0300 0.4344 0.048 Uiso 1 1 calc R U . . .
C2 C 0.09842(15) 0.5155(3) 0.22971(11) 0.0282(6) Uani 1 1 d . . . . .
H2 H 0.0801 0.4845 0.2636 0.034 Uiso 1 1 calc R U . . .
C2C C -0.05434(18) 0.0148(5) 0.4030(2) 0.0768(14) Uani 1 1 d . . . . .
H2CA H -0.0784 -0.0057 0.3643 0.115 Uiso 1 1 calc R U . . .
H2CB H -0.0469 0.1082 0.4065 0.115 Uiso 1 1 calc R U . . .
H2CC H -0.0861 -0.0143 0.4316 0.115 Uiso 1 1 calc R U . . .
C3 C 0.05775(14) 0.4918(3) 0.17691(10) 0.0237(6) Uani 1 1 d . . . . .
H3 H 0.0126 0.4441 0.1749 0.028 Uiso 1 1 calc R U . . .
C3C C 0.0175(3) -0.1874(3) 0.4039(2) 0.106(2) Uani 1 1 d . . . . .
H3CA H -0.0130 -0.2082 0.3677 0.158 Uiso 1 1 calc R U . . .
H3CB H -0.0033 -0.2301 0.4358 0.158 Uiso 1 1 calc R U . . .
H3CC H 0.0687 -0.2173 0.4023 0.158 Uiso 1 1 calc R U . . .
C4 C 0.08256(13) 0.5373(2) 0.12695(10) 0.0159(5) Uani 1 1 d . . . . .
C5 C 0.15191(12) 0.6010(2) 0.13043(10) 0.0146(5) Uani 1 1 d . . . . .
C6 C 0.19191(13) 0.6226(2) 0.18415(10) 0.0176(5) Uani 1 1 d . . . . .
H6 H 0.2387 0.6653 0.1862 0.021 Uiso 1 1 calc R U . . .
C7 C 0.20621(15) 0.6126(3) 0.29244(10) 0.0259(6) Uani 1 1 d . . . . .
C8 C 0.20500(13) 0.5258(2) 0.33750(10) 0.0188(5) Uani 1 1 d . . . . .
H8 H 0.1794 0.4463 0.3306 0.023 Uiso 1 1 calc R U . . .
C9 C 0.24006(13) 0.5514(2) 0.39250(10) 0.0170(5) Uani 1 1 d . . . . .
C10 C 0.27602(15) 0.6704(2) 0.40359(10) 0.0240(6) Uani 1 1 d . . . . .
C11 C 0.27792(19) 0.7570(3) 0.35845(12) 0.0404(8) Uani 1 1 d . . . . .
H11 H 0.3024 0.8375 0.3652 0.048 Uiso 1 1 calc R U . . .
C12 C 0.24465(19) 0.7272(3) 0.30396(12) 0.0419(8) Uani 1 1 d . . . . .
H12 H 0.2482 0.7867 0.2736 0.050 Uiso 1 1 calc R U . . .
C13 C 0.18594(12) 0.6467(2) 0.07874(9) 0.0120(4) Uani 1 1 d . . . . .
C14 C -0.02640(14) 0.4554(3) 0.07101(11) 0.0242(6) Uani 1 1 d . . . . .
H14A H -0.0489 0.4511 0.0309 0.036 Uiso 1 1 calc R U . . .
H14B H -0.0594 0.5036 0.0937 0.036 Uiso 1 1 calc R U . . .
H14C H -0.0194 0.3680 0.0865 0.036 Uiso 1 1 calc R U . . .
C15 C 0.24040(12) 0.4459(2) 0.43626(9) 0.0129(5) Uani 1 1 d . . . . .
C16 C 0.33525(19) 0.8202(3) 0.47083(12) 0.0389(8) Uani 1 1 d . . . . .
H16A H 0.3489 0.8292 0.5124 0.058 Uiso 1 1 calc R U . . .
H16B H 0.2973 0.8845 0.4576 0.058 Uiso 1 1 calc R U . . .
H16C H 0.3795 0.8334 0.4510 0.058 Uiso 1 1 calc R U . . .
N1C N 0.01768(14) -0.0502(2) 0.41269(11) 0.0391(6) Uani 1 1 d . . . . .
O1 O 0.25567(8) 0.63396(16) 0.08085(7) 0.0178(4) Uani 1 1 d . . . . .
O1C O 0.08160(9) 0.13273(16) 0.43672(7) 0.0221(4) Uani 1 1 d . . . . .
O2 O 0.14412(9) 0.69773(15) 0.03824(6) 0.0167(3) Uani 1 1 d . . . . .
O3 O 0.04471(8) 0.51929(16) 0.07392(7) 0.0175(4) Uani 1 1 d . . . . .
O4 O 0.18496(8) 0.37146(15) 0.43091(7) 0.0166(3) Uani 1 1 d . . . . .
O5 O 0.29621(9) 0.43638(15) 0.47347(7) 0.0193(4) Uani 1 1 d . . . . .
O6 O 0.30608(11) 0.69405(16) 0.45841(7) 0.0261(4) Uani 1 1 d . . . . .
Cu1 Cu 0.18508(2) 0.21262(2) 0.47519(2) 0.00978(8) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C6 1.385(3) . ?
C1 C2 1.397(4) . ?
C1 C7 1.492(3) . ?
C1C O1C 1.223(3) . ?
C1C N1C 1.315(3) . ?
C1C H1C 0.9500 . ?
C2 C3 1.384(3) . ?
C2 H2 0.9500 . ?
C2C N1C 1.458(5) . ?
C2C H2CA 0.9800 . ?
C2C H2CB 0.9800 . ?
C2C H2CC 0.9800 . ?
C3 C4 1.384(3) . ?
C3 H3 0.9500 . ?
C3C N1C 1.439(4) . ?
C3C H3CA 0.9800 . ?
C3C H3CB 0.9800 . ?
C3C H3CC 0.9800 . ?
C4 O3 1.358(3) . ?
C4 C5 1.409(3) . ?
C5 C6 1.393(3) . ?
C5 C13 1.498(3) . ?
C6 H6 0.9500 . ?
C7 C12 1.388(4) . ?
C7 C8 1.390(3) . ?
C8 C9 1.393(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.405(3) . ?
C9 C15 1.500(3) . ?
C10 O6 1.356(3) . ?
C10 C11 1.391(4) . ?
C11 C12 1.380(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 O2 1.258(3) . ?
C13 O1 1.261(3) . ?
C14 O3 1.439(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 O5 1.256(3) . ?
C15 O4 1.259(3) . ?
C16 O6 1.429(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1 Cu1 1.9654(15) 4 ?
O1C Cu1 2.1430(16) . ?
O2 Cu1 1.9621(15) 6_565 ?
O4 Cu1 1.9477(15) . ?
O5 Cu1 1.9639(16) 7_556 ?
Cu1 O2 1.9620(15) 6_566 ?
Cu1 O5 1.9639(16) 7_556 ?
Cu1 O1 1.9655(15) 4_545 ?
Cu1 Cu1 2.6086(5) 7_556 ?

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
C6 C1 C2 117.3(2) . . ?
C6 C1 C7 122.3(2) . . ?
C2 C1 C7 120.4(2) . . ?
O1C C1C N1C 125.7(3) . . ?
O1C C1C H1C 117.2 . . ?
N1C C1C H1C 117.2 . . ?
C3 C2 C1 121.9(2) . . ?
C3 C2 H2 119.1 . . ?
C1 C2 H2 119.1 . . ?
N1C C2C H2CA 109.5 . . ?
N1C C2C H2CB 109.5 . . ?
H2CA C2C H2CB 109.5 . . ?
N1C C2C H2CC 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
C2 C3 C4 120.3(2) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
N1C C3C H3CA 109.5 . . ?
N1C C3C H3CB 109.5 . . ?
H3CA C3C H3CB 109.5 . . ?
N1C C3C H3CC 109.5 . . ?
H3CA C3C H3CC 109.5 . . ?
H3CB C3C H3CC 109.5 . . ?
O3 C4 C3 123.2(2) . . ?
O3 C4 C5 117.7(2) . . ?
C3 C4 C5 119.0(2) . . ?
C6 C5 C4 119.4(2) . . ?
C6 C5 C13 117.4(2) . . ?
C4 C5 C13 123.2(2) . . ?
C1 C6 C5 122.1(2) . . ?
C1 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C12 C7 C8 117.4(2) . . ?
C12 C7 C1 122.0(2) . . ?
C8 C7 C1 120.6(2) . . ?
C7 C8 C9 122.2(2) . . ?
C7 C8 H8 118.9 . . ?
C9 C8 H8 118.9 . . ?
C8 C9 C10 119.3(2) . . ?
C8 C9 C15 117.2(2) . . ?
C10 C9 C15 123.4(2) . . ?
O6 C10 C11 124.1(2) . . ?
O6 C10 C9 117.3(2) . . ?
C11 C10 C9 118.6(2) . . ?
C12 C11 C10 120.8(2) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C7 121.7(2) . . ?
C11 C12 H12 119.2 . . ?
C7 C12 H12 119.2 . . ?
O2 C13 O1 125.6(2) . . ?
O2 C13 C5 118.46(19) . . ?
O1 C13 C5 115.91(19) . . ?
O3 C14 H14A 109.5 . . ?
O3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O5 C15 O4 125.7(2) . . ?
O5 C15 C9 118.1(2) . . ?
O4 C15 C9 116.2(2) . . ?
O6 C16 H16A 109.5 . . ?
O6 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O6 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C1C N1C C3C 123.2(3) . . ?
C1C N1C C2C 120.1(3) . . ?
C3C N1C C2C 116.7(3) . . ?
C13 O1 Cu1 123.29(14) . 4 ?
C1C O1C Cu1 117.90(17) . . ?
C13 O2 Cu1 121.44(14) . 6_565 ?
C4 O3 C14 117.17(18) . . ?
C15 O4 Cu1 121.04(14) . . ?
C15 O5 Cu1 123.59(15) . 7_556 ?
C10 O6 C16 117.09(19) . . ?
O4 Cu1 O2 91.28(7) . 6_566 ?
O4 Cu1 O5 169.13(7) . 7_556 ?
O2 Cu1 O5 88.03(7) 6_566 7_556 ?
O4 Cu1 O1 87.86(7) . 4_545 ?
O2 Cu1 O1 169.22(6) 6_566 4_545 ?
O5 Cu1 O1 90.79(7) 7_556 4_545 ?
O4 Cu1 O1C 99.05(6) . . ?
O2 Cu1 O1C 96.51(7) 6_566 . ?
O5 Cu1 O1C 91.80(7) 7_556 . ?
O1 Cu1 O1C 94.24(6) 4_545 . ?
O4 Cu1 Cu1 86.00(5) . 7_556 ?
O2 Cu1 Cu1 85.51(5) 6_566 7_556 ?
O5 Cu1 Cu1 83.14(5) 7_556 7_556 ?
O1 Cu1 Cu1 83.71(5) 4_545 7_556 ?
O1C Cu1 Cu1 174.50(5) . 7_556 ?

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
C6 C1 C2 C3 -2.7(4) . . . . ?
C7 C1 C2 C3 177.3(3) . . . . ?
C1 C2 C3 C4 -0.9(4) . . . . ?
C2 C3 C4 O3 -178.8(2) . . . . ?
C2 C3 C4 C5 3.9(4) . . . . ?
O3 C4 C5 C6 179.2(2) . . . . ?
C3 C4 C5 C6 -3.4(3) . . . . ?
O3 C4 C5 C13 -1.2(3) . . . . ?
C3 C4 C5 C13 176.2(2) . . . . ?
C2 C1 C6 C5 3.2(4) . . . . ?
C7 C1 C6 C5 -176.8(2) . . . . ?
C4 C5 C6 C1 -0.2(4) . . . . ?
C13 C5 C6 C1 -179.8(2) . . . . ?
C6 C1 C7 C12 35.9(4) . . . . ?
C2 C1 C7 C12 -144.0(3) . . . . ?
C6 C1 C7 C8 -145.9(3) . . . . ?
C2 C1 C7 C8 34.1(4) . . . . ?
C12 C7 C8 C9 0.6(4) . . . . ?
C1 C7 C8 C9 -177.7(2) . . . . ?
C7 C8 C9 C10 2.0(4) . . . . ?
C7 C8 C9 C15 -175.0(2) . . . . ?
C8 C9 C10 O6 176.7(2) . . . . ?
C15 C9 C10 O6 -6.6(4) . . . . ?
C8 C9 C10 C11 -2.5(4) . . . . ?
C15 C9 C10 C11 174.2(3) . . . . ?
O6 C10 C11 C12 -178.6(3) . . . . ?
C9 C10 C11 C12 0.5(5) . . . . ?
C10 C11 C12 C7 2.1(6) . . . . ?
C8 C7 C12 C11 -2.6(5) . . . . ?
C1 C7 C12 C11 175.6(3) . . . . ?
C6 C5 C13 O2 -139.7(2) . . . . ?
C4 C5 C13 O2 40.7(3) . . . . ?
C6 C5 C13 O1 38.0(3) . . . . ?
C4 C5 C13 O1 -141.6(2) . . . . ?
C8 C9 C15 O5 146.2(2) . . . . ?
C10 C9 C15 O5 -30.7(3) . . . . ?
C8 C9 C15 O4 -31.5(3) . . . . ?
C10 C9 C15 O4 151.7(2) . . . . ?
O1C C1C N1C C3C -179.9(4) . . . . ?
O1C C1C N1C C2C 0.1(5) . . . . ?
O2 C13 O1 Cu1 8.3(3) . . . 4 ?
C5 C13 O1 Cu1 -169.25(14) . . . 4 ?
N1C C1C O1C Cu1 170.5(3) . . . . ?
O1 C13 O2 Cu1 -8.3(3) . . . 6_565 ?
C5 C13 O2 Cu1 169.19(14) . . . 6_565 ?
C3 C4 O3 C14 3.3(3) . . . . ?
C5 C4 O3 C14 -179.4(2) . . . . ?
O5 C15 O4 Cu1 -8.6(3) . . . . ?
C9 C15 O4 Cu1 168.86(14) . . . . ?
O4 C15 O5 Cu1 9.0(3) . . . 7_556 ?
C9 C15 O5 Cu1 -168.39(15) . . . 7_556 ?
C11 C10 O6 C16 5.9(4) . . . . ?
C9 C10 O6 C16 -173.3(3) . . . . ?

_refine_diff_density_max         0.594
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.077

_shelxl_version_number           2014/6

_exptl_crystal_recrystallization_method 'solvothermal synthesis'
####################################################################### 
# 
# 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_cpo-72-la
_database_code_depnum_ccdc_archive 'CCDC 1483002'
_audit_update_record             
;
2016-07-01 deposited with the CCDC.
2016-07-25 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT230_cpo-72-la           
;
PROBLEM: Hirshfeld Test Diff for    O1C    --  C1C     ..        9.5 s.u.
RESPONSE: The difference in the termal ellipsoids is likely due to a slighty increased rotational freedom of the non-oxygen atoms of the coordinated solvent. 
;
_vrf_PLAT417_cpo-72-la           
;
PROBLEM: Short Inter D-H..H-D       H3CD   ..  H4CB    ..       2.07 Ang.
RESPONSE: These short contacts stem from limitations when locating the exact position of hydrogen atoms in water molecules. The positions are in our opinion satisfactory accurate to ignore this warning. 
;
_vrf_PLAT971_cpo-72-la           
;
PROBLEM: Check Calcd Residual Density  0.99A From     La2       2.67 eA-3
RESPONSE: This residual density in the structure is likely due to the combination of a very heavy and relativelty light atoms in the same structure.
;
# Added during the CSD deposition process: Friday 01 July 2016 01:27 PM
# end Validation Reply Form

_audit_creation_date             2016-06-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_chemical_name_common            ?
_chemical_name_systematic        CPO-72-La
_chemical_formula_moiety         '4(H2 O), C3 H7 N O, C51 H49 La2 N O22'
_chemical_formula_sum            'C54 H64 La2 N2 O27'
_chemical_formula_weight         1450.89
_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'
La La -0.2871 2.4523 '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'

_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                   13.4844(5)
_cell_length_b                   14.1740(6)
_cell_length_c                   15.6448(6)
_cell_angle_alpha                90.4630(10)
_cell_angle_beta                 105.8700(10)
_cell_angle_gamma                99.8160(10)
_cell_volume                     2829.36(19)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.43
_shelx_estimated_absorpt_T_max   0.720
_shelx_estimated_absorpt_T_min   0.382
_exptl_absorpt_coefficient_mu    1.582
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1464
_exptl_crystal_recrystallization_method 'Solvothermal synthesis'
_exptl_crystal_size_max          0.753
_exptl_crystal_size_mid          0.302
_exptl_crystal_size_min          0.222
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            90197
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.349
_diffrn_reflns_theta_min         2.169
_diffrn_ambient_temperature      105.06
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker PHOTON CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                11880
_reflns_number_total             14080
_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       'Bruker APEX2 (Bruker, 2007)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         2.989
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         14080
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.102
_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)+(0.0268P)²+5.2737P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0683
_refine_ls_wR_factor_ref         0.0720
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3C-H3CD = O3C-H3CE
 0.87 with sigma of 0.02
 O4W-H4WA = O4W-H4WB
 0.87 with sigma of 0.02
 H3CD-H3CE
 1.38 with sigma of 0.04
 H4WA-H4WB
 1.38 with sigma of 0.04
 N1S-C3S \\sim N1S-C2S \\sim N2S-C5S \\sim N2S-C6S
 with sigma of 0.02
 La1-H3CD \\sim La1-H3CE
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C4S, N2S, C5S, C6S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1S, C1S, N1S, C3S, C2S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: C1S(0.75) H1S(0.75) C2S(0.75) H2SA(0.75) H2SB(0.75) H2SC(0.75)
 C3S(0.75) H3SA(0.75) H3SB(0.75) H3SC(0.75) N1S(0.75) C4S(0.25) H4S(0.25)
 C6S(0.25) H6SA(0.25) H6SB(0.25) H6SC(0.25) N2S(0.25) C5S(0.25) H5SA(0.25)
 H5SB(0.25) H5SC(0.25)
5.a Free rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
5.b Rotating group:
 O2C(H2CD,H2CE), O4C(H4CA,H4CB)
5.c Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C1C(H1C), C2(H2), C5(H5), C6(H6), C10(H10), C13(H13), C14(H14),
 C18(H18), C21(H21), C22(H22), C26(H26), C29(H29), C30(H30), C34(H34), C37(H37),
  C38(H38), C42(H42), C45(H45), C46(H46), C4S(H4S)
5.d Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C2C(H2CA,H2CB,H2CC), C3C(H3CA,H3CB,
 H3CC), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C32(H32A,
 H32B,H32C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C6S(H6SA,H6SB,H6SC),
 C5S(H5SA,H5SB,H5SC)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
O1W O 0.99638(19) 0.18384(16) 0.60901(15) 0.0301(5) Uani 1 1 d . . . . .
H1WA H 1.0101 0.2078 0.5617 0.045 Uiso 1 1 d G . . . .
H1WB H 1.0467 0.2074 0.6559 0.045 Uiso 1 1 d G . . . .
O2W O 0.1367(2) 0.21330(19) -0.2231(2) 0.0519(8) Uani 1 1 d . . . . .
H2WA H 0.1468 0.1554 -0.2104 0.078 Uiso 1 1 d G . . . .
H2WB H 0.0947 0.2301 -0.1947 0.078 Uiso 1 1 d G . . . .
O3W O 0.8733(2) 0.26484(18) 0.70198(19) 0.0424(6) Uani 1 1 d . . . . .
H3WA H 0.8599 0.3222 0.6919 0.064 Uiso 1 1 d G . . . .
H3WB H 0.9131 0.2513 0.6699 0.064 Uiso 1 1 d G . . . .
O4W O 0.01075(19) 0.29667(17) -0.13134(15) 0.0298(5) Uani 1 1 d D . . . .
H4WA H -0.002(3) 0.274(3) -0.0845(16) 0.045 Uiso 1 1 d DR . . . .
H4WB H -0.041(2) 0.279(3) -0.1758(17) 0.045 Uiso 1 1 d DR . . . .
C1S C 0.3326(4) 0.6327(4) 0.1535(3) 0.0341(11) Uani 0.75 1 d . U P A 1
H1S H 0.2630 0.6369 0.1535 0.041 Uiso 0.75 1 calc R . P A 1
C2S C 0.3914(4) 0.7681(4) 0.2610(4) 0.0339(12) Uani 0.75 1 d D U P A 1
H2SA H 0.3161 0.7613 0.2544 0.051 Uiso 0.75 1 calc GR . P A 1
H2SB H 0.4184 0.8328 0.2465 0.051 Uiso 0.75 1 calc GR . P A 1
H2SC H 0.4279 0.7572 0.3225 0.051 Uiso 0.75 1 calc GR . P A 1
C3S C 0.5185(3) 0.6982(3) 0.2041(4) 0.0368(11) Uani 0.75 1 d D U P A 1
H3SA H 0.5564 0.6816 0.2633 0.055 Uiso 0.75 1 calc GR . P A 1
H3SB H 0.5507 0.7621 0.1919 0.055 Uiso 0.75 1 calc GR . P A 1
H3SC H 0.5216 0.6510 0.1592 0.055 Uiso 0.75 1 calc GR . P A 1
N1S N 0.4092(3) 0.6980(3) 0.2010(3) 0.0293(10) Uani 0.75 1 d D U P A 1
O1S O 0.3463(2) 0.5615(2) 0.10566(17) 0.0420(6) Uani 1 1 d . U . . .
C1C C 0.8242(3) -0.0043(3) 0.4272(2) 0.0358(8) Uani 1 1 d . . . . .
H1C H 0.8864 -0.0234 0.4619 0.043 Uiso 1 1 calc R . . . .
C2C C 0.6406(3) -0.0499(3) 0.3528(3) 0.0544(12) Uani 1 1 d . . . . .
H2CA H 0.6146 -0.0989 0.3035 0.082 Uiso 1 1 calc GR . . . .
H2CB H 0.6534 0.0134 0.3292 0.082 Uiso 1 1 calc GR . . . .
H2CC H 0.5882 -0.0512 0.3858 0.082 Uiso 1 1 calc GR . . . .
C3C C 0.7348(3) -0.1640(3) 0.4437(3) 0.0505(11) Uani 1 1 d . . . . .
H3CA H 0.7204 -0.2111 0.3938 0.076 Uiso 1 1 calc GR . . . .
H3CB H 0.6804 -0.1783 0.4747 0.076 Uiso 1 1 calc GR . . . .
H3CC H 0.8033 -0.1668 0.4852 0.076 Uiso 1 1 calc GR . . . .
N1C N 0.7354(2) -0.06902(19) 0.41069(19) 0.0293(6) Uani 1 1 d . . . . .
O1C O 0.83239(16) 0.07611(15) 0.40206(14) 0.0254(5) Uani 1 1 d . . . . .
O2C O 1.03115(16) 0.01142(14) 0.37785(14) 0.0229(4) Uani 1 1 d . . . . .
H2CD H 1.0917 0.0133 0.3639 0.034 Uiso 1 1 d GR . . . .
H2CE H 0.9928 -0.0474 0.3624 0.034 Uiso 1 1 d GR . . . .
O3C O 0.15433(15) 0.45374(16) 0.07368(13) 0.0214(4) Uani 1 1 d D . . . .
H3CD H 0.122(2) 0.473(2) 0.0239(14) 0.032 Uiso 1 1 d DR . . . .
H3CE H 0.2159(16) 0.486(2) 0.0840(18) 0.032 Uiso 1 1 d DR . . . .
O4C O -0.04413(14) 0.51209(14) 0.10145(13) 0.0179(4) Uani 1 1 d . . . . .
H4CA H -0.0128 0.5735 0.1227 0.027 Uiso 1 1 d GR . . . .
H4CB H -0.1104 0.5023 0.1085 0.027 Uiso 1 1 d GR . . . .
C1 C 0.36840(19) 0.40301(18) 0.55022(17) 0.0119(5) Uani 1 1 d . . . . .
C2 C 0.28063(19) 0.36305(19) 0.48004(17) 0.0131(5) Uani 1 1 d . . . . .
H2 H 0.2912 0.3354 0.4284 0.016 Uiso 1 1 calc R . . . .
C3 C 0.17896(19) 0.36279(18) 0.48404(17) 0.0117(5) Uani 1 1 d . . . . .
C4 C 0.16163(19) 0.40821(19) 0.55672(18) 0.0138(5) Uani 1 1 d . . . . .
C5 C 0.2471(2) 0.4525(2) 0.62469(18) 0.0184(6) Uani 1 1 d . . . . .
H5 H 0.2365 0.4857 0.6735 0.022 Uiso 1 1 calc R . . . .
C6 C 0.3484(2) 0.4482(2) 0.62154(18) 0.0173(6) Uani 1 1 d . . . . .
H6 H 0.4058 0.4771 0.6697 0.021 Uiso 1 1 calc R . . . .
C7 C 0.08895(19) 0.30371(19) 0.41527(17) 0.0122(5) Uani 1 1 d . . . . .
C8 C 0.0410(2) 0.4625(2) 0.6236(2) 0.0230(6) Uani 1 1 d . . . . .
H8A H 0.0736 0.5297 0.6228 0.034 Uiso 1 1 calc GR . . . .
H8B H 0.0714 0.4377 0.6814 0.034 Uiso 1 1 calc GR . . . .
H8C H -0.0346 0.4580 0.6138 0.034 Uiso 1 1 calc GR . . . .
C9 C 0.47706(19) 0.39414(19) 0.54999(17) 0.0127(5) Uani 1 1 d . . . . .
C10 C 0.56563(19) 0.44296(19) 0.61422(17) 0.0125(5) Uani 1 1 d . . . . .
H10 H 0.5557 0.4843 0.6580 0.015 Uiso 1 1 calc R . . . .
C11 C 0.66765(19) 0.43360(18) 0.61678(17) 0.0121(5) Uani 1 1 d . . . . .
C12 C 0.68338(19) 0.37602(19) 0.54974(17) 0.0139(5) Uani 1 1 d . . . . .
C13 C 0.5963(2) 0.3273(2) 0.48513(18) 0.0171(6) Uani 1 1 d . . . . .
H13 H 0.6060 0.2878 0.4398 0.020 Uiso 1 1 calc R . . . .
C14 C 0.4957(2) 0.3358(2) 0.48596(18) 0.0173(6) Uani 1 1 d . . . . .
H14 H 0.4378 0.3008 0.4417 0.021 Uiso 1 1 calc R . . . .
C15 C 0.75542(19) 0.48837(19) 0.69074(17) 0.0126(5) Uani 1 1 d . . . . .
C16 C 0.7981(2) 0.3178(2) 0.47780(19) 0.0210(6) Uani 1 1 d . . . . .
H16A H 0.7630 0.3419 0.4210 0.031 Uiso 1 1 calc GR . . . .
H16B H 0.7681 0.2501 0.4799 0.031 Uiso 1 1 calc GR . . . .
H16C H 0.8732 0.3242 0.4834 0.031 Uiso 1 1 calc GR . . . .
C17 C 0.63296(19) 0.10428(19) -0.05345(17) 0.0133(5) Uani 1 1 d . . . . .
C18 C 0.7203(2) 0.15848(19) 0.00763(17) 0.0151(5) Uani 1 1 d . . . . .
H18 H 0.7100 0.1980 0.0526 0.018 Uiso 1 1 calc R . . . .
C19 C 0.82201(19) 0.15612(19) 0.00441(17) 0.0135(5) Uani 1 1 d . . . . .
C20 C 0.8390(2) 0.09675(19) -0.05981(17) 0.0143(5) Uani 1 1 d . . . . .
C21 C 0.7534(2) 0.0403(2) -0.11979(18) 0.0171(6) Uani 1 1 d . . . . .
H21 H 0.7638 -0.0012 -0.1633 0.020 Uiso 1 1 calc R . . . .
C22 C 0.6526(2) 0.0447(2) -0.11581(18) 0.0173(6) Uani 1 1 d . . . . .
H22 H 0.5949 0.0057 -0.1572 0.021 Uiso 1 1 calc R . . . .
C23 C 0.91134(19) 0.22147(19) 0.06791(17) 0.0140(5) Uani 1 1 d . . . . .
C24 C 0.9596(2) 0.0349(2) -0.1218(2) 0.0236(6) Uani 1 1 d . . . . .
H24A H 0.9257 0.0519 -0.1821 0.035 Uiso 1 1 calc GR . . . .
H24B H 0.9307 -0.0315 -0.1135 0.035 Uiso 1 1 calc GR . . . .
H24C H 1.0352 0.0415 -0.1137 0.035 Uiso 1 1 calc GR . . . .
C25 C 0.52422(19) 0.11119(19) -0.05234(17) 0.0131(5) Uani 1 1 d . . . . .
C26 C 0.4368(2) 0.05158(19) -0.10818(17) 0.0137(5) Uani 1 1 d . . . . .
H26 H 0.4477 0.0042 -0.1462 0.016 Uiso 1 1 calc R . . . .
C27 C 0.33423(19) 0.05865(19) -0.11053(17) 0.0135(5) Uani 1 1 d . . . . .
C28 C 0.3173(2) 0.1248(2) -0.05071(18) 0.0152(5) Uani 1 1 d . . . . .
C29 C 0.4034(2) 0.1840(2) 0.00592(19) 0.0200(6) Uani 1 1 d . . . . .
H29 H 0.3930 0.2293 0.0462 0.024 Uiso 1 1 calc R . . . .
C30 C 0.5048(2) 0.1777(2) 0.00446(19) 0.0199(6) Uani 1 1 d . . . . .
H30 H 0.5622 0.2197 0.0432 0.024 Uiso 1 1 calc R . . . .
C31 C 0.2473(2) -0.00705(19) -0.17650(18) 0.0147(5) Uani 1 1 d . . . . .
C32 C 0.2020(2) 0.1834(2) 0.01991(18) 0.0186(6) Uani 1 1 d . . . . .
H32A H 0.2275 0.2513 0.0135 0.028 Uiso 1 1 calc GR . . . .
H32B H 0.2411 0.1642 0.0776 0.028 Uiso 1 1 calc GR . . . .
H32C H 0.1273 0.1739 0.0164 0.028 Uiso 1 1 calc GR . . . .
C33 C 0.46167(19) 0.22815(19) 0.26028(17) 0.0131(5) Uani 1 1 d . . . . .
C34 C 0.35690(19) 0.23577(19) 0.24726(17) 0.0131(5) Uani 1 1 d . . . . .
H34 H 0.3327 0.2887 0.2167 0.016 Uiso 1 1 calc R . . . .
C35 C 0.28575(19) 0.16998(19) 0.27666(17) 0.0129(5) Uani 1 1 d . . . . .
C36 C 0.3214(2) 0.0936(2) 0.32513(18) 0.0157(5) Uani 1 1 d . . . . .
C37 C 0.4266(2) 0.0854(2) 0.34008(19) 0.0191(6) Uani 1 1 d . . . . .
H37 H 0.4522 0.0343 0.3730 0.023 Uiso 1 1 calc R . . . .
C38 C 0.4941(2) 0.1506(2) 0.30756(19) 0.0181(6) Uani 1 1 d . . . . .
H38 H 0.5647 0.1424 0.3178 0.022 Uiso 1 1 calc R . . . .
C39 C 0.17341(19) 0.18531(19) 0.24894(17) 0.0134(5) Uani 1 1 d . . . . .
C40 C 0.2863(3) -0.0540(2) 0.3938(3) 0.0349(8) Uani 1 1 d . . . . .
H40A H 0.2283 -0.0948 0.4096 0.052 Uiso 1 1 calc GR . . . .
H40B H 0.3446 -0.0349 0.4476 0.052 Uiso 1 1 calc GR . . . .
H40C H 0.3097 -0.0897 0.3514 0.052 Uiso 1 1 calc GR . . . .
C41 C 0.53321(19) 0.29919(19) 0.22526(17) 0.0130(5) Uani 1 1 d . . . . .
C42 C 0.63781(19) 0.29120(19) 0.23882(17) 0.0125(5) Uani 1 1 d . . . . .
H42 H 0.6620 0.2387 0.2703 0.015 Uiso 1 1 calc R . . . .
C43 C 0.70882(19) 0.35611(19) 0.20870(17) 0.0130(5) Uani 1 1 d . . . . .
C44 C 0.67259(19) 0.43248(19) 0.15910(17) 0.0139(5) Uani 1 1 d . . . . .
C45 C 0.5675(2) 0.4408(2) 0.14361(18) 0.0164(5) Uani 1 1 d . . . . .
H45 H 0.5419 0.4913 0.1098 0.020 Uiso 1 1 calc R . . . .
C46 C 0.5000(2) 0.37622(19) 0.17701(18) 0.0152(5) Uani 1 1 d . . . . .
H46 H 0.4293 0.3845 0.1669 0.018 Uiso 1 1 calc R . . . .
C47 C 0.82087(19) 0.34129(18) 0.23557(17) 0.0117(5) Uani 1 1 d . . . . .
C48 C 0.7071(2) 0.5779(2) 0.0870(2) 0.0260(7) Uani 1 1 d . . . . .
H48A H 0.7655 0.6188 0.0718 0.039 Uiso 1 1 calc GR . . . .
H48B H 0.6805 0.6146 0.1265 0.039 Uiso 1 1 calc GR . . . .
H48C H 0.6509 0.5559 0.0325 0.039 Uiso 1 1 calc GR . . . .
O1 O 0.07485(13) 0.31910(14) 0.33368(12) 0.0144(4) Uani 1 1 d . . . . .
O2 O 0.03292(14) 0.23585(13) 0.44121(12) 0.0139(4) Uani 1 1 d . . . . .
O3 O 0.05970(14) 0.40715(14) 0.55442(13) 0.0183(4) Uani 1 1 d . . . . .
O4 O 0.73934(13) 0.56031(13) 0.72888(12) 0.0152(4) Uani 1 1 d . . . . .
O5 O 0.84373(14) 0.46092(14) 0.71485(13) 0.0170(4) Uani 1 1 d . . . . .
O6 O 0.78351(14) 0.37234(14) 0.54970(12) 0.0170(4) Uani 1 1 d . . . . .
O7 O 0.92551(14) 0.21254(14) 0.15087(12) 0.0155(4) Uani 1 1 d . . . . .
O8 O 0.96621(14) 0.28651(14) 0.03821(12) 0.0177(4) Uani 1 1 d . . . . .
O9 O 0.94097(14) 0.09770(14) -0.05795(13) 0.0187(4) Uani 1 1 d . . . . .
O10 O 0.26527(14) -0.08484(14) -0.20306(14) 0.0218(4) Uani 1 1 d . . . . .
O11 O 0.15803(14) 0.01735(14) -0.20587(13) 0.0181(4) Uani 1 1 d . . . . .
O12 O 0.21698(14) 0.12632(14) -0.05011(13) 0.0187(4) Uani 1 1 d . . . . .
O13 O 0.15284(13) 0.24648(13) 0.19275(12) 0.0136(4) Uani 1 1 d . . . . .
O14 O 0.10781(14) 0.13568(14) 0.28214(13) 0.0174(4) Uani 1 1 d . . . . .
O15 O 0.25196(15) 0.02947(14) 0.35448(14) 0.0206(4) Uani 1 1 d . . . . .
O16 O 0.84208(13) 0.27881(13) 0.29139(12) 0.0134(4) Uani 1 1 d . . . . .
O17 O 0.88718(14) 0.39057(14) 0.20330(13) 0.0159(4) Uani 1 1 d . . . . .
O18 O 0.74277(14) 0.49679(14) 0.13114(13) 0.0183(4) Uani 1 1 d . . . . .
La1 La 0.06673(2) 0.38433(2) 0.18678(2) 0.00987(4) Uani 1 1 d D . . . .
La2 La 0.92799(2) 0.14185(2) 0.29462(2) 0.01111(4) Uani 1 1 d . . . . .
C4S C 0.4040(9) 0.6100(9) 0.1591(9) 0.026(3) Uani 0.25 1 d . U P A 2
H4S H 0.4750 0.6027 0.1824 0.032 Uiso 0.25 1 calc R . P A 2
C6S C 0.2515(10) 0.6844(10) 0.1480(10) 0.036(3) Uani 0.25 1 d D U P A 2
H6SA H 0.2299 0.6553 0.0872 0.053 Uiso 0.25 1 calc GR . P A 2
H6SB H 0.2408 0.7511 0.1464 0.053 Uiso 0.25 1 calc GR . P A 2
H6SC H 0.2095 0.6484 0.1832 0.053 Uiso 0.25 1 calc GR . P A 2
N2S N 0.3618(11) 0.6818(12) 0.1883(10) 0.034(3) Uani 0.25 1 d D U P A 2
C5S C 0.4332(17) 0.7520(15) 0.2587(15) 0.060(6) Uani 0.25 1 d D U P A 2
H5SA H 0.5038 0.7364 0.2741 0.090 Uiso 0.25 1 calc GR . P A 2
H5SB H 0.4075 0.7492 0.3117 0.090 Uiso 0.25 1 calc GR . P A 2
H5SC H 0.4354 0.8167 0.2369 0.090 Uiso 0.25 1 calc GR . 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
O1W H1WA 0.8700 . ?
O1W H1WB 0.8693 . ?
O2W H2WA 0.8701 . ?
O2W H2WB 0.8700 . ?
O3W H3WA 0.8690 . ?
O3W H3WB 0.8704 . ?
O4W H4WA 0.855(18) . ?
O4W H4WB 0.840(18) . ?
C1S H1S 0.9500 . ?
C1S N1S 1.311(7) . ?
C1S O1S 1.319(6) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
C2S N1S 1.453(6) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 0.9800 . ?
C3S N1S 1.461(6) . ?
O1S C4S 1.108(13) . ?
C1C H1C 0.9500 . ?
C1C N1C 1.340(4) . ?
C1C O1C 1.206(4) . ?
C2C H2CA 0.9800 . ?
C2C H2CB 0.9800 . ?
C2C H2CC 0.9800 . ?
C2C N1C 1.421(4) . ?
C3C H3CA 0.9800 . ?
C3C H3CB 0.9800 . ?
C3C H3CC 0.9800 . ?
C3C N1C 1.445(4) . ?
O1C La2 2.481(2) . ?
O2C H2CD 0.8968 . ?
O2C H2CE 0.8962 . ?
O2C La2 2.641(2) . ?
O3C H3CD 0.856(17) . ?
O3C H3CE 0.847(17) . ?
O3C La1 2.5038(19) . ?
O4C H4CA 0.9166 . ?
O4C H4CB 0.9180 . ?
O4C La1 2.6770(19) . ?
C1 C2 1.406(3) . ?
C1 C6 1.393(4) . ?
C1 C9 1.493(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.389(3) . ?
C3 C4 1.395(4) . ?
C3 C7 1.502(3) . ?
C4 C5 1.388(4) . ?
C4 O3 1.363(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(4) . ?
C6 H6 0.9500 . ?
C7 O1 1.264(3) . ?
C7 O2 1.260(3) . ?
C7 La2 3.087(2) 1_455 ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 O3 1.433(3) . ?
C9 C10 1.402(3) . ?
C9 C14 1.395(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.394(3) . ?
C11 C12 1.406(4) . ?
C11 C15 1.505(3) . ?
C12 C13 1.393(4) . ?
C12 O6 1.360(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.385(4) . ?
C14 H14 0.9500 . ?
C15 O4 1.257(3) . ?
C15 O5 1.275(3) . ?
C15 La1 2.938(2) 2_666 ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 O6 1.435(3) . ?
C17 C18 1.398(3) . ?
C17 C22 1.392(4) . ?
C17 C25 1.491(4) . ?
C18 H18 0.9500 . ?
C18 C19 1.391(4) . ?
C19 C20 1.396(4) . ?
C19 C23 1.499(3) . ?
C20 C21 1.391(4) . ?
C20 O9 1.365(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.390(4) . ?
C22 H22 0.9500 . ?
C23 O7 1.270(3) . ?
C23 O8 1.255(3) . ?
C23 La1 3.054(3) 1_655 ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 O9 1.433(3) . ?
C25 C26 1.397(3) . ?
C25 C30 1.394(4) . ?
C26 H26 0.9500 . ?
C26 C27 1.394(4) . ?
C27 C28 1.409(4) . ?
C27 C31 1.502(3) . ?
C28 C29 1.389(4) . ?
C28 O12 1.358(3) . ?
C29 H29 0.9500 . ?
C29 C30 1.391(4) . ?
C30 H30 0.9500 . ?
C31 O10 1.259(3) . ?
C31 O11 1.274(3) . ?
C31 La2 2.944(2) 2_655 ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C32 O12 1.434(3) . ?
C33 C34 1.394(3) . ?
C33 C38 1.394(4) . ?
C33 C41 1.487(4) . ?
C34 H34 0.9500 . ?
C34 C35 1.395(4) . ?
C35 C36 1.404(4) . ?
C35 C39 1.512(3) . ?
C36 C37 1.399(4) . ?
C36 O15 1.366(3) . ?
C37 H37 0.9500 . ?
C37 C38 1.384(4) . ?
C38 H38 0.9500 . ?
C39 O13 1.250(3) . ?
C39 O14 1.262(3) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C40 O15 1.427(4) . ?
C41 C42 1.392(3) . ?
C41 C46 1.399(4) . ?
C42 H42 0.9500 . ?
C42 C43 1.393(4) . ?
C43 C44 1.414(4) . ?
C43 C47 1.505(3) . ?
C44 C45 1.397(4) . ?
C44 O18 1.362(3) . ?
C45 H45 0.9500 . ?
C45 C46 1.386(4) . ?
C46 H46 0.9500 . ?
C47 O16 1.261(3) . ?
C47 O17 1.258(3) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C48 O18 1.432(3) . ?
O1 La1 2.4659(18) . ?
O1 La2 2.8676(18) 1_455 ?
O2 La2 2.5632(18) 1_455 ?
O4 La1 2.5674(17) 2_666 ?
O5 La1 2.5813(18) 2_666 ?
O7 La1 2.7718(18) 1_655 ?
O7 La2 2.4636(19) . ?
O8 La1 2.5974(18) 1_655 ?
O10 La2 2.5919(18) 2_655 ?
O11 La2 2.5576(18) 2_655 ?
O13 La1 2.4273(18) . ?
O14 La2 2.5012(18) 1_455 ?
O16 La2 2.4186(18) . ?
O17 La1 2.5202(17) 1_655 ?
La1 C15 2.938(2) 2_666 ?
La1 C23 3.054(3) 1_455 ?
La1 O4 2.5674(17) 2_666 ?
La1 O5 2.5813(18) 2_666 ?
La1 O7 2.7719(18) 1_455 ?
La1 O8 2.5974(18) 1_455 ?
La1 O17 2.5203(17) 1_455 ?
La1 La2 4.2174(2) 1_455 ?
La2 C7 3.087(2) 1_655 ?
La2 C31 2.944(2) 2_655 ?
La2 O1 2.8677(18) 1_655 ?
La2 O2 2.5632(18) 1_655 ?
La2 O10 2.5918(18) 2_655 ?
La2 O11 2.5575(19) 2_655 ?
La2 O14 2.5013(18) 1_655 ?
La2 La1 4.2174(2) 1_655 ?
C4S H4S 0.9500 . ?
C4S N2S 1.379(19) . ?
C6S H6SA 0.9800 . ?
C6S H6SB 0.9800 . ?
C6S H6SC 0.9800 . ?
C6S N2S 1.455(13) . ?
N2S C5S 1.486(14) . ?
C5S H5SA 0.9800 . ?
C5S H5SB 0.9800 . ?
C5S H5SC 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
H1WA O1W H1WB 109.6 . . ?
H2WA O2W H2WB 109.5 . . ?
H3WA O3W H3WB 109.6 . . ?
H4WA O4W H4WB 110(3) . . ?
N1S C1S H1S 118.1 . . ?
N1S C1S O1S 123.9(4) . . ?
O1S C1S H1S 118.1 . . ?
H2SA C2S H2SB 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
N1S C2S H2SA 109.5 . . ?
N1S C2S H2SB 109.5 . . ?
N1S C2S H2SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 109.5 . . ?
N1S C3S H3SA 109.5 . . ?
N1S C3S H3SB 109.5 . . ?
N1S C3S H3SC 109.5 . . ?
C1S N1S C2S 121.8(5) . . ?
C1S N1S C3S 122.0(4) . . ?
C2S N1S C3S 115.9(4) . . ?
N1C C1C H1C 117.0 . . ?
O1C C1C H1C 117.0 . . ?
O1C C1C N1C 125.9(3) . . ?
H2CA C2C H2CB 109.5 . . ?
H2CA C2C H2CC 109.5 . . ?
H2CB C2C H2CC 109.5 . . ?
N1C C2C H2CA 109.5 . . ?
N1C C2C H2CB 109.5 . . ?
N1C C2C H2CC 109.5 . . ?
H3CA C3C H3CB 109.5 . . ?
H3CA C3C H3CC 109.5 . . ?
H3CB C3C H3CC 109.5 . . ?
N1C C3C H3CA 109.5 . . ?
N1C C3C H3CB 109.5 . . ?
N1C C3C H3CC 109.5 . . ?
C1C N1C C2C 121.0(3) . . ?
C1C N1C C3C 121.3(3) . . ?
C2C N1C C3C 117.5(3) . . ?
C1C O1C La2 127.1(2) . . ?
H2CD O2C H2CE 108.2 . . ?
La2 O2C H2CD 110.8 . . ?
La2 O2C H2CE 110.4 . . ?
H3CD O3C H3CE 104(3) . . ?
La1 O3C H3CD 123.9(18) . . ?
La1 O3C H3CE 126.6(19) . . ?
H4CA O4C H4CB 107.4 . . ?
La1 O4C H4CA 111.2 . . ?
La1 O4C H4CB 111.3 . . ?
C2 C1 C9 121.8(2) . . ?
C6 C1 C2 116.5(2) . . ?
C6 C1 C9 121.7(2) . . ?
C1 C2 H2 119.1 . . ?
C3 C2 C1 121.9(2) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 C4 120.0(2) . . ?
C2 C3 C7 119.3(2) . . ?
C4 C3 C7 120.3(2) . . ?
C5 C4 C3 119.0(2) . . ?
O3 C4 C3 116.4(2) . . ?
O3 C4 C5 124.5(2) . . ?
C4 C5 H5 119.9 . . ?
C4 C5 C6 120.1(2) . . ?
C6 C5 H5 119.9 . . ?
C1 C6 H6 118.9 . . ?
C5 C6 C1 122.2(2) . . ?
C5 C6 H6 118.9 . . ?
C3 C7 La2 166.24(18) . 1_455 ?
O1 C7 C3 120.1(2) . . ?
O1 C7 La2 68.16(13) . 1_455 ?
O2 C7 C3 117.9(2) . . ?
O2 C7 O1 121.8(2) . . ?
O2 C7 La2 54.23(12) . 1_455 ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
C10 C9 C1 122.1(2) . . ?
C14 C9 C1 121.5(2) . . ?
C14 C9 C10 116.4(2) . . ?
C9 C10 H10 118.5 . . ?
C11 C10 C9 123.0(2) . . ?
C11 C10 H10 118.5 . . ?
C10 C11 C12 118.8(2) . . ?
C10 C11 C15 117.5(2) . . ?
C12 C11 C15 123.6(2) . . ?
C13 C12 C11 118.8(2) . . ?
O6 C12 C11 118.3(2) . . ?
O6 C12 C13 122.9(2) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 C12 120.9(2) . . ?
C14 C13 H13 119.5 . . ?
C9 C14 H14 119.1 . . ?
C13 C14 C9 121.9(2) . . ?
C13 C14 H14 119.1 . . ?
C11 C15 La1 170.88(18) . 2_666 ?
O4 C15 C11 118.8(2) . . ?
O4 C15 O5 121.0(2) . . ?
O4 C15 La1 60.63(13) . 2_666 ?
O5 C15 C11 120.3(2) . . ?
O5 C15 La1 61.31(13) . 2_666 ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O6 C16 H16A 109.5 . . ?
O6 C16 H16B 109.5 . . ?
O6 C16 H16C 109.5 . . ?
C18 C17 C25 121.4(2) . . ?
C22 C17 C18 116.7(2) . . ?
C22 C17 C25 121.8(2) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 C17 121.9(2) . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C20 120.0(2) . . ?
C18 C19 C23 118.8(2) . . ?
C20 C19 C23 121.1(2) . . ?
C21 C20 C19 119.2(2) . . ?
O9 C20 C19 116.4(2) . . ?
O9 C20 C21 124.4(2) . . ?
C20 C21 H21 120.1 . . ?
C22 C21 C20 119.7(2) . . ?
C22 C21 H21 120.1 . . ?
C17 C22 H22 118.8 . . ?
C21 C22 C17 122.5(2) . . ?
C21 C22 H22 118.8 . . ?
C19 C23 La1 168.83(18) . 1_655 ?
O7 C23 C19 118.6(2) . . ?
O7 C23 La1 65.17(13) . 1_655 ?
O8 C23 C19 119.5(2) . . ?
O8 C23 O7 121.8(2) . . ?
O8 C23 La1 57.17(13) . 1_655 ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O9 C24 H24A 109.5 . . ?
O9 C24 H24B 109.5 . . ?
O9 C24 H24C 109.5 . . ?
C26 C25 C17 121.7(2) . . ?
C30 C25 C17 121.6(2) . . ?
C30 C25 C26 116.7(2) . . ?
C25 C26 H26 118.6 . . ?
C27 C26 C25 122.9(2) . . ?
C27 C26 H26 118.6 . . ?
C26 C27 C28 119.0(2) . . ?
C26 C27 C31 117.4(2) . . ?
C28 C27 C31 123.6(2) . . ?
C29 C28 C27 118.7(2) . . ?
O12 C28 C27 118.1(2) . . ?
O12 C28 C29 123.2(2) . . ?
C28 C29 H29 119.5 . . ?
C28 C29 C30 120.9(3) . . ?
C30 C29 H29 119.5 . . ?
C25 C30 H30 119.2 . . ?
C29 C30 C25 121.7(2) . . ?
C29 C30 H30 119.2 . . ?
C27 C31 La2 175.77(18) . 2_655 ?
O10 C31 C27 118.9(2) . . ?
O10 C31 O11 121.2(2) . . ?
O10 C31 La2 61.52(13) . 2_655 ?
O11 C31 C27 119.9(2) . . ?
O11 C31 La2 60.01(13) . 2_655 ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O12 C32 H32A 109.5 . . ?
O12 C32 H32B 109.5 . . ?
O12 C32 H32C 109.5 . . ?
C34 C33 C38 116.0(2) . . ?
C34 C33 C41 121.2(2) . . ?
C38 C33 C41 122.9(2) . . ?
C33 C34 H34 118.2 . . ?
C33 C34 C35 123.6(3) . . ?
C35 C34 H34 118.2 . . ?
C34 C35 C36 118.9(2) . . ?
C34 C35 C39 115.8(2) . . ?
C36 C35 C39 125.2(2) . . ?
C37 C36 C35 118.4(2) . . ?
O15 C36 C35 118.9(2) . . ?
O15 C36 C37 122.7(3) . . ?
C36 C37 H37 119.5 . . ?
C38 C37 C36 121.0(3) . . ?
C38 C37 H37 119.5 . . ?
C33 C38 H38 118.9 . . ?
C37 C38 C33 122.1(2) . . ?
C37 C38 H38 118.9 . . ?
O13 C39 C35 116.1(2) . . ?
O13 C39 O14 125.0(2) . . ?
O14 C39 C35 118.8(2) . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O15 C40 H40A 109.5 . . ?
O15 C40 H40B 109.5 . . ?
O15 C40 H40C 109.5 . . ?
C42 C41 C33 120.8(2) . . ?
C42 C41 C46 116.6(2) . . ?
C46 C41 C33 122.6(2) . . ?
C41 C42 H42 118.3 . . ?
C41 C42 C43 123.4(2) . . ?
C43 C42 H42 118.3 . . ?
C42 C43 C44 118.6(2) . . ?
C42 C43 C47 116.4(2) . . ?
C44 C43 C47 124.9(2) . . ?
C45 C44 C43 118.7(2) . . ?
O18 C44 C43 118.4(2) . . ?
O18 C44 C45 122.8(2) . . ?
C44 C45 H45 119.6 . . ?
C46 C45 C44 120.8(3) . . ?
C46 C45 H45 119.6 . . ?
C41 C46 H46 119.1 . . ?
C45 C46 C41 121.7(2) . . ?
C45 C46 H46 119.1 . . ?
O16 C47 C43 116.1(2) . . ?
O17 C47 C43 120.0(2) . . ?
O17 C47 O16 123.9(2) . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
O18 C48 H48A 109.5 . . ?
O18 C48 H48B 109.5 . . ?
O18 C48 H48C 109.5 . . ?
C7 O1 La1 167.67(17) . . ?
C7 O1 La2 87.68(15) . 1_455 ?
La1 O1 La2 104.26(6) . 1_455 ?
C7 O2 La2 102.26(15) . 1_455 ?
C4 O3 C8 116.9(2) . . ?
C15 O4 La1 94.12(14) . 2_666 ?
C15 O5 La1 93.00(15) . 2_666 ?
C12 O6 C16 117.5(2) . . ?
C23 O7 La1 90.27(15) . 1_655 ?
C23 O7 La2 161.63(18) . . ?
La2 O7 La1 107.18(6) . 1_655 ?
C23 O8 La1 98.87(15) . 1_655 ?
C20 O9 C24 117.0(2) . . ?
C31 O10 La2 93.20(15) . 2_655 ?
C31 O11 La2 94.43(15) . 2_655 ?
C28 O12 C32 117.3(2) . . ?
C39 O13 La1 133.56(16) . . ?
C39 O14 La2 136.77(17) . 1_455 ?
C36 O15 C40 118.0(2) . . ?
C47 O16 La2 133.44(16) . . ?
C47 O17 La1 138.05(17) . 1_655 ?
C44 O18 C48 118.0(2) . . ?
O3C La1 O4C 72.57(6) . . ?
O3C La1 C15 82.16(7) . 2_666 ?
O3C La1 C23 98.05(7) . 1_455 ?
O3C La1 O4 74.02(6) . 2_666 ?
O3C La1 O5 87.13(7) . 2_666 ?
O3C La1 O7 121.36(6) . 1_455 ?
O3C La1 O8 74.41(6) . 1_455 ?
O3C La1 O17 130.50(6) . 1_455 ?
O3C La1 La2 149.34(5) . 1_455 ?
O4C La1 C15 101.04(7) . 2_666 ?
O4C La1 C23 90.21(7) . 1_455 ?
O4C La1 O7 103.94(6) . 1_455 ?
O4C La1 La2 122.30(4) . 1_455 ?
C15 La1 C23 168.21(7) 2_666 1_455 ?
C15 La1 La2 116.72(5) 2_666 1_455 ?
C23 La1 La2 58.41(5) 1_455 1_455 ?
O1 La1 O3C 151.00(6) . . ?
O1 La1 O4C 129.96(6) . . ?
O1 La1 C15 75.95(6) . 2_666 ?
O1 La1 C23 99.59(7) . 1_455 ?
O1 La1 O4 78.12(6) . 2_666 ?
O1 La1 O5 81.36(6) . 2_666 ?
O1 La1 O7 75.15(6) . 1_455 ?
O1 La1 O8 122.77(6) . 1_455 ?
O1 La1 O17 77.19(6) . 1_455 ?
O1 La1 La2 41.23(4) . 1_455 ?
O4 La1 O4C 119.40(6) 2_666 . ?
O4 La1 C15 25.25(6) 2_666 2_666 ?
O4 La1 C23 143.62(6) 2_666 1_455 ?
O4 La1 O5 50.67(6) 2_666 2_666 ?
O4 La1 O7 136.63(6) 2_666 1_455 ?
O4 La1 O8 135.04(6) 2_666 1_455 ?
O4 La1 La2 112.17(4) 2_666 1_455 ?
O5 La1 O4C 78.57(6) 2_666 . ?
O5 La1 C15 25.68(6) 2_666 2_666 ?
O5 La1 C23 165.68(6) 2_666 1_455 ?
O5 La1 O7 151.10(6) 2_666 1_455 ?
O5 La1 O8 154.80(6) 2_666 1_455 ?
O5 La1 La2 120.66(4) 2_666 1_455 ?
O7 La1 C15 149.86(6) 1_455 2_666 ?
O7 La1 C23 24.57(6) 1_455 1_455 ?
O7 La1 La2 33.92(4) 1_455 1_455 ?
O8 La1 O4C 79.58(6) 1_455 . ?
O8 La1 C15 155.28(6) 1_455 2_666 ?
O8 La1 C23 23.96(6) 1_455 1_455 ?
O8 La1 O7 48.40(6) 1_455 1_455 ?
O8 La1 La2 81.95(4) 1_455 1_455 ?
O13 La1 O3C 90.13(7) . . ?
O13 La1 O4C 153.50(6) . . ?
O13 La1 C15 96.12(7) . 2_666 ?
O13 La1 C23 72.09(6) . 1_455 ?
O13 La1 O1 73.77(6) . . ?
O13 La1 O4 72.47(6) . 2_666 ?
O13 La1 O5 121.44(6) . 2_666 ?
O13 La1 O7 67.62(6) . 1_455 ?
O13 La1 O8 76.44(6) . 1_455 ?
O13 La1 O17 128.40(6) . 1_455 ?
O13 La1 La2 65.17(4) . 1_455 ?
O17 La1 O4C 59.51(6) 1_455 . ?
O17 La1 C15 116.89(7) 1_455 2_666 ?
O17 La1 C23 71.91(6) 1_455 1_455 ?
O17 La1 O4 139.91(6) 1_455 2_666 ?
O17 La1 O5 94.56(6) 1_455 2_666 ?
O17 La1 O7 64.18(6) 1_455 1_455 ?
O17 La1 O8 85.02(6) 1_455 1_455 ?
O17 La1 La2 64.79(4) 1_455 1_455 ?
O1C La2 O2C 74.17(7) . . ?
O1C La2 C7 99.49(7) . 1_655 ?
O1C La2 C31 79.16(7) . 2_655 ?
O1C La2 O1 121.56(6) . 1_655 ?
O1C La2 O2 76.69(6) . 1_655 ?
O1C La2 O10 73.69(7) . 2_655 ?
O1C La2 O11 84.14(7) . 2_655 ?
O1C La2 O14 132.47(7) . 1_655 ?
O1C La2 La1 148.39(5) . 1_655 ?
O2C La2 C7 90.78(7) . 1_655 ?
O2C La2 C31 96.77(7) . 2_655 ?
O2C La2 O1 105.47(6) . 1_655 ?
O2C La2 La1 124.20(4) . 1_655 ?
C7 La2 La1 58.65(5) 1_655 1_655 ?
C31 La2 C7 171.60(7) 2_655 1_655 ?
C31 La2 La1 118.88(5) 2_655 1_655 ?
O1 La2 C7 24.16(6) 1_655 1_655 ?
O1 La2 C31 152.82(6) 1_655 2_655 ?
O1 La2 La1 34.52(4) 1_655 1_655 ?
O2 La2 O2C 79.22(6) 1_655 . ?
O2 La2 C7 23.50(6) 1_655 1_655 ?
O2 La2 C31 155.70(6) 1_655 2_655 ?
O2 La2 O1 47.53(5) 1_655 1_655 ?
O2 La2 O10 139.39(6) 1_655 2_655 ?
O2 La2 La1 81.83(4) 1_655 1_655 ?
O7 La2 O1C 149.44(7) . . ?
O7 La2 O2C 130.81(6) . . ?
O7 La2 C7 97.54(6) . 1_655 ?
O7 La2 C31 80.29(7) . 2_655 ?
O7 La2 O1 73.41(6) . 1_655 ?
O7 La2 O2 120.53(6) . 1_655 ?
O7 La2 O10 78.06(6) . 2_655 ?
O7 La2 O11 87.00(6) . 2_655 ?
O7 La2 O14 77.39(6) . 1_655 ?
O7 La2 La1 38.90(4) . 1_655 ?
O10 La2 O2C 117.55(6) 2_655 . ?
O10 La2 C7 146.37(6) 2_655 1_655 ?
O10 La2 C31 25.28(7) 2_655 2_655 ?
O10 La2 O1 136.97(6) 2_655 1_655 ?
O10 La2 La1 110.86(5) 2_655 1_655 ?
O11 La2 O2C 73.98(6) 2_655 . ?
O11 La2 C7 162.84(6) 2_655 1_655 ?
O11 La2 C31 25.56(7) 2_655 2_655 ?
O11 La2 O1 153.62(6) 2_655 1_655 ?
O11 La2 O2 150.44(6) 2_655 1_655 ?
O11 La2 O10 50.76(6) 2_655 2_655 ?
O11 La2 La1 123.80(4) 2_655 1_655 ?
O14 La2 O2C 60.28(6) 1_655 . ?
O14 La2 C7 69.95(6) 1_655 1_655 ?
O14 La2 C31 117.10(7) 1_655 2_655 ?
O14 La2 O1 63.87(6) 1_655 1_655 ?
O14 La2 O2 81.97(6) 1_655 1_655 ?
O14 La2 O10 138.63(6) 1_655 2_655 ?
O14 La2 O11 95.15(6) 1_655 2_655 ?
O14 La2 La1 65.38(4) 1_655 1_655 ?
O16 La2 O1C 86.85(7) . . ?
O16 La2 O2C 152.81(6) . . ?
O16 La2 C7 73.04(6) . 1_655 ?
O16 La2 C31 98.58(7) . 2_655 ?
O16 La2 O1 67.94(5) . 1_655 ?
O16 La2 O2 77.55(6) . 1_655 ?
O16 La2 O7 74.13(6) . . ?
O16 La2 O10 73.71(6) . 2_655 ?
O16 La2 O11 124.05(6) . 2_655 ?
O16 La2 O14 129.08(6) . 1_655 ?
O16 La2 La1 65.87(4) . 1_655 ?
O1S C4S H4S 123.6 . . ?
O1S C4S N2S 112.9(11) . . ?
N2S C4S H4S 123.6 . . ?
H6SA C6S H6SB 109.5 . . ?
H6SA C6S H6SC 109.5 . . ?
H6SB C6S H6SC 109.5 . . ?
N2S C6S H6SA 109.5 . . ?
N2S C6S H6SB 109.5 . . ?
N2S C6S H6SC 109.5 . . ?
C4S N2S C6S 118.3(13) . . ?
C4S N2S C5S 117.2(13) . . ?
C6S N2S C5S 124.5(15) . . ?
N2S C5S H5SA 109.5 . . ?
N2S C5S H5SB 109.5 . . ?
N2S C5S H5SC 109.5 . . ?
H5SA C5S H5SB 109.5 . . ?
H5SA C5S H5SC 109.5 . . ?
H5SB C5S H5SC 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O2 0.87 2.02 2.880(3) 168.4 1_655
O1W H1WB O2W 0.87 1.94 2.765(4) 157.5 1_656
O2W H2WA O11 0.87 1.99 2.848(3) 169.2 .
O2W H2WB O4W 0.87 2.03 2.886(4) 168.4 .
O3W H3WA O5 0.87 2.05 2.887(3) 160.3 .
O3W H3WB O1W 0.87 2.00 2.851(4) 164.0 .
O4W H4WA O8 0.855(18) 2.09(2) 2.875(3) 153(4) 1_455
O4W H4WB O3W 0.840(18) 1.93(2) 2.737(4) 160(4) 1_454
O2C H2CD O15 0.90 2.18 3.066(3) 169.6 1_655
O2C H2CE O1W 0.90 2.01 2.746(3) 138.6 2_756
O3C H3CD O4C 0.856(17) 1.986(18) 2.827(3) 167(3) 2_565
O3C H3CE O1S 0.847(17) 1.841(17) 2.687(3) 177(3) .
O4C H4CA O4W 0.92 1.84 2.686(3) 152.7 2_565
O4C H4CB O18 0.92 2.09 3.007(3) 173.2 1_455

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
O1S C1S N1S C2S -172.3(5) . . . . ?
O1S C1S N1S C3S 0.9(8) . . . . ?
O1S C4S N2S C6S 1(2) . . . . ?
O1S C4S N2S C5S -178.8(16) . . . . ?
N1C C1C O1C La2 -113.8(4) . . . . ?
O1C C1C N1C C2C 5.8(6) . . . . ?
O1C C1C N1C C3C 179.5(4) . . . . ?
C1 C2 C3 C4 4.0(4) . . . . ?
C1 C2 C3 C7 -168.8(2) . . . . ?
C1 C9 C10 C11 178.1(2) . . . . ?
C1 C9 C14 C13 179.8(3) . . . . ?
C2 C1 C6 C5 1.2(4) . . . . ?
C2 C1 C9 C10 172.4(2) . . . . ?
C2 C1 C9 C14 -8.2(4) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C2 C3 C4 O3 178.2(2) . . . . ?
C2 C3 C7 O1 -59.3(3) . . . . ?
C2 C3 C7 O2 116.6(3) . . . . ?
C2 C3 C7 La2 64.8(8) . . . 1_455 ?
C3 C4 C5 C6 -2.4(4) . . . . ?
C3 C4 O3 C8 -173.2(2) . . . . ?
C3 C7 O1 La1 -26.7(9) . . . . ?
C3 C7 O1 La2 167.8(2) . . . 1_455 ?
C3 C7 O2 La2 -166.67(18) . . . 1_455 ?
C4 C3 C7 O1 127.8(3) . . . . ?
C4 C3 C7 O2 -56.2(3) . . . . ?
C4 C3 C7 La2 -108.1(7) . . . 1_455 ?
C4 C5 C6 C1 2.1(4) . . . . ?
C5 C4 O3 C8 5.4(4) . . . . ?
C6 C1 C2 C3 -4.2(4) . . . . ?
C6 C1 C9 C10 -10.0(4) . . . . ?
C6 C1 C9 C14 169.4(3) . . . . ?
C7 C3 C4 C5 172.2(3) . . . . ?
C7 C3 C4 O3 -9.1(4) . . . . ?
C9 C1 C2 C3 173.5(2) . . . . ?
C9 C1 C6 C5 -176.5(3) . . . . ?
C9 C10 C11 C12 2.9(4) . . . . ?
C9 C10 C11 C15 -178.5(2) . . . . ?
C10 C9 C14 C13 -0.8(4) . . . . ?
C10 C11 C12 C13 -2.5(4) . . . . ?
C10 C11 C12 O6 175.9(2) . . . . ?
C10 C11 C15 O4 -21.8(4) . . . . ?
C10 C11 C15 O5 157.1(2) . . . . ?
C11 C12 C13 C14 0.6(4) . . . . ?
C11 C12 O6 C16 -176.4(2) . . . . ?
C11 C15 O4 La1 -169.6(2) . . . 2_666 ?
C11 C15 O5 La1 169.7(2) . . . 2_666 ?
C12 C11 C15 O4 156.6(3) . . . . ?
C12 C11 C15 O5 -24.5(4) . . . . ?
C12 C13 C14 C9 1.1(4) . . . . ?
C13 C12 O6 C16 1.9(4) . . . . ?
C14 C9 C10 C11 -1.3(4) . . . . ?
C15 C11 C12 C13 179.1(2) . . . . ?
C15 C11 C12 O6 -2.5(4) . . . . ?
C17 C18 C19 C20 -1.5(4) . . . . ?
C17 C18 C19 C23 175.6(2) . . . . ?
C17 C25 C26 C27 -177.8(3) . . . . ?
C17 C25 C30 C29 -179.7(3) . . . . ?
C18 C17 C22 C21 -1.7(4) . . . . ?
C18 C17 C25 C26 -174.6(3) . . . . ?
C18 C17 C25 C30 5.5(4) . . . . ?
C18 C19 C20 C21 -0.2(4) . . . . ?
C18 C19 C20 O9 -179.3(2) . . . . ?
C18 C19 C23 O7 61.0(4) . . . . ?
C18 C19 C23 O8 -115.1(3) . . . . ?
C18 C19 C23 La1 -45.8(10) . . . 1_655 ?
C19 C20 C21 C22 0.9(4) . . . . ?
C19 C20 O9 C24 178.2(2) . . . . ?
C19 C23 O7 La1 -168.2(2) . . . 1_655 ?
C19 C23 O7 La2 29.7(7) . . . . ?
C19 C23 O8 La1 167.5(2) . . . 1_655 ?
C20 C19 C23 O7 -121.9(3) . . . . ?
C20 C19 C23 O8 62.0(4) . . . . ?
C20 C19 C23 La1 131.3(8) . . . 1_655 ?
C20 C21 C22 C17 0.0(4) . . . . ?
C21 C20 O9 C24 -0.8(4) . . . . ?
C22 C17 C18 C19 2.4(4) . . . . ?
C22 C17 C25 C26 6.3(4) . . . . ?
C22 C17 C25 C30 -173.6(3) . . . . ?
C23 C19 C20 C21 -177.3(3) . . . . ?
C23 C19 C20 O9 3.6(4) . . . . ?
C25 C17 C18 C19 -176.8(3) . . . . ?
C25 C17 C22 C21 177.5(3) . . . . ?
C25 C26 C27 C28 -3.7(4) . . . . ?
C25 C26 C27 C31 177.4(2) . . . . ?
C26 C25 C30 C29 0.4(4) . . . . ?
C26 C27 C28 C29 2.9(4) . . . . ?
C26 C27 C28 O12 -175.8(2) . . . . ?
C26 C27 C31 O10 24.8(4) . . . . ?
C26 C27 C31 O11 -153.8(3) . . . . ?
C27 C28 C29 C30 -0.6(4) . . . . ?
C27 C28 O12 C32 170.8(2) . . . . ?
C27 C31 O10 La2 175.2(2) . . . 2_655 ?
C27 C31 O11 La2 -175.1(2) . . . 2_655 ?
C28 C27 C31 O10 -154.0(3) . . . . ?
C28 C27 C31 O11 27.4(4) . . . . ?
C28 C29 C30 C25 -1.1(5) . . . . ?
C29 C28 O12 C32 -7.9(4) . . . . ?
C30 C25 C26 C27 2.0(4) . . . . ?
C31 C27 C28 C29 -178.3(3) . . . . ?
C31 C27 C28 O12 2.9(4) . . . . ?
C33 C34 C35 C36 2.6(4) . . . . ?
C33 C34 C35 C39 -174.6(2) . . . . ?
C33 C41 C42 C43 -179.1(2) . . . . ?
C33 C41 C46 C45 -178.9(2) . . . . ?
C34 C33 C38 C37 -0.3(4) . . . . ?
C34 C33 C41 C42 179.8(2) . . . . ?
C34 C33 C41 C46 -0.7(4) . . . . ?
C34 C35 C36 C37 -1.5(4) . . . . ?
C34 C35 C36 O15 179.6(2) . . . . ?
C34 C35 C39 O13 9.6(3) . . . . ?
C34 C35 C39 O14 -171.5(2) . . . . ?
C35 C36 C37 C38 -0.3(4) . . . . ?
C35 C36 O15 C40 172.4(3) . . . . ?
C35 C39 O13 La1 -128.6(2) . . . . ?
C35 C39 O14 La2 164.39(17) . . . 1_455 ?
C36 C35 C39 O13 -167.3(2) . . . . ?
C36 C35 C39 O14 11.6(4) . . . . ?
C36 C37 C38 C33 1.3(4) . . . . ?
C37 C36 O15 C40 -6.5(4) . . . . ?
C38 C33 C34 C35 -1.6(4) . . . . ?
C38 C33 C41 C42 -0.2(4) . . . . ?
C38 C33 C41 C46 179.3(3) . . . . ?
C39 C35 C36 C37 175.4(2) . . . . ?
C39 C35 C36 O15 -3.6(4) . . . . ?
C41 C33 C34 C35 178.3(2) . . . . ?
C41 C33 C38 C37 179.7(3) . . . . ?
C41 C42 C43 C44 -2.2(4) . . . . ?
C41 C42 C43 C47 175.2(2) . . . . ?
C42 C41 C46 C45 0.6(4) . . . . ?
C42 C43 C44 C45 1.1(4) . . . . ?
C42 C43 C44 O18 178.8(2) . . . . ?
C42 C43 C47 O16 -8.2(3) . . . . ?
C42 C43 C47 O17 172.5(2) . . . . ?
C43 C44 C45 C46 0.8(4) . . . . ?
C43 C44 O18 C48 -175.2(2) . . . . ?
C43 C47 O16 La2 128.4(2) . . . . ?
C43 C47 O17 La1 -162.53(17) . . . 1_655 ?
C44 C43 C47 O16 169.0(2) . . . . ?
C44 C43 C47 O17 -10.3(4) . . . . ?
C44 C45 C46 C41 -1.7(4) . . . . ?
C45 C44 O18 C48 2.4(4) . . . . ?
C46 C41 C42 C43 1.3(4) . . . . ?
C47 C43 C44 C45 -176.0(2) . . . . ?
C47 C43 C44 O18 1.7(4) . . . . ?
O1 C7 O2 La2 9.2(3) . . . 1_455 ?
O2 C7 O1 La1 157.5(6) . . . . ?
O2 C7 O1 La2 -8.0(2) . . . 1_455 ?
O3 C4 C5 C6 179.0(3) . . . . ?
O4 C15 O5 La1 -11.5(3) . . . 2_666 ?
O5 C15 O4 La1 11.5(3) . . . 2_666 ?
O6 C12 C13 C14 -177.7(3) . . . . ?
O7 C23 O8 La1 -8.5(3) . . . 1_655 ?
O8 C23 O7 La1 7.8(3) . . . 1_655 ?
O8 C23 O7 La2 -154.3(4) . . . . ?
O9 C20 C21 C22 179.9(3) . . . . ?
O10 C31 O11 La2 6.3(3) . . . 2_655 ?
O11 C31 O10 La2 -6.2(3) . . . 2_655 ?
O12 C28 C29 C30 178.1(3) . . . . ?
O13 C39 O14 La2 -16.8(4) . . . 1_455 ?
O14 C39 O13 La1 52.6(4) . . . . ?
O15 C36 C37 C38 178.5(3) . . . . ?
O16 C47 O17 La1 18.2(4) . . . 1_655 ?
O17 C47 O16 La2 -52.4(3) . . . . ?
O18 C44 C45 C46 -176.9(2) . . . . ?
La1 C23 O7 La2 -162.1(5) 1_655 . . . ?
La2 C7 O1 La1 165.5(8) 1_455 . . . ?

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