# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 793553'
_audit_update_record             
;
2017-04-12 deposited with the CCDC.
2017-04-20 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT417_shelx               
;
PROBLEM: Short Inter D-H..H-D       H12F   ..  H13A    ..       1.85 Ang.
RESPONSE: The remaining CheckCif 417_ALERT_2_A is due to disorder in one of the water ligands. Modlling this disorder is not sensible.
;
# Added during the CSD deposition process: Wednesday 12 April 2017 08:43 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C13 H21 Ca N O8, H2 O'
_chemical_formula_sum            'C13 H23 Ca N O9'
_chemical_formula_weight         377.40

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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   6.2649(10)
_cell_length_b                   8.2062(10)
_cell_length_c                   33.649(6)
_cell_angle_alpha                96.66(2)
_cell_angle_beta                 94.77(2)
_cell_angle_gamma                92.07(2)
_cell_volume                     1710.5(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6602
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      25.86

_exptl_crystal_description       Needle
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_F_000             800
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.413
_shelx_estimated_absorpt_T_min   0.790
_shelx_estimated_absorpt_T_max   0.980
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker Smart Apex'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            6606
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         0.612
_diffrn_reflns_theta_max         25.865
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6606
_reflns_number_gt                5135
_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 Smart'
_computing_cell_refinement       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0665P)²+0.0282P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6606
_refine_ls_number_parameters     493
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1316
_refine_ls_wR_factor_gt          0.1191
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.10354(8) 0.75878(6) 0.56589(2) 0.01585(15) Uani 1 1 d . . . . .
O1 O 0.1790(3) 0.9876(3) 0.63041(7) 0.0326(5) Uani 1 1 d D . . . .
O3 O -0.2412(3) 0.8437(2) 0.58430(6) 0.0269(5) Uani 1 1 d . . . . .
O4 O 0.0993(3) 0.4636(2) 0.56180(6) 0.0242(4) Uani 1 1 d . . . . .
O5 O 0.2035(5) 0.2541(3) 0.59296(7) 0.0504(7) Uani 1 1 d . . . . .
O6 O -0.5583(3) 0.7312(3) 0.59441(7) 0.0401(6) Uani 1 1 d . . . . .
O7 O 0.3047(3) 0.6849(2) 0.50424(6) 0.0309(5) Uani 1 1 d . . . . .
O8 O 0.1475(3) 1.0044(2) 0.53449(6) 0.0264(5) Uani 1 1 d . . . . .
H8C H 0.026964 1.010746 0.514300 0.06(2) Uiso 0.5 1 calc R . P . .
H8B H 0.281871 1.002426 0.521507 0.11(4) Uiso 0.5 1 calc R . P . .
H8A H 0.151629 1.100357 0.554850 0.076(14) Uiso 1 1 calc R . . . .
O9 O -0.1863(3) 0.6637(2) 0.51144(6) 0.0281(5) Uani 1 1 d . . . . .
N1 N -0.0223(3) 0.6363(3) 0.62841(7) 0.0197(5) Uani 1 1 d . . . . .
C1 C 0.2958(5) 0.9457(3) 0.66385(9) 0.0252(7) Uani 1 1 d . . . . .
C2 C 0.2065(5) 0.8181(3) 0.68166(8) 0.0223(6) Uani 1 1 d . . . . .
C3 C 0.3210(5) 0.7666(4) 0.71477(9) 0.0297(7) Uani 1 1 d . . . . .
H3 H 0.261888 0.678760 0.727029 0.036 Uiso 1 1 calc R U . . .
C4 C 0.5181(5) 0.8385(4) 0.73060(9) 0.0338(8) Uani 1 1 d . . . . .
C5 C 0.5966(5) 0.9676(4) 0.71258(10) 0.0348(8) Uani 1 1 d . . . . .
H5 H 0.729350 1.020692 0.723531 0.042 Uiso 1 1 calc R U . . .
C6 C 0.4917(5) 1.0243(4) 0.67918(10) 0.0319(7) Uani 1 1 d . . . . .
C7 C 0.5887(6) 1.1629(4) 0.66050(14) 0.0557(11) Uani 1 1 d . . . . .
H7C H 0.488085 1.251546 0.659979 0.084 Uiso 1 1 calc R U . . .
H7D H 0.619195 1.123966 0.632995 0.084 Uiso 1 1 calc R U . . .
H7E H 0.722246 1.204127 0.676274 0.084 Uiso 1 1 calc R U . . .
C8 C 0.6407(7) 0.7795(5) 0.76613(11) 0.0573(11) Uani 1 1 d . . . . .
H8F H 0.572586 0.676666 0.772018 0.086 Uiso 1 1 calc R U . . .
H8D H 0.640745 0.862638 0.789527 0.086 Uiso 1 1 calc R U . . .
H8E H 0.788692 0.760792 0.760006 0.086 Uiso 1 1 calc R U . . .
C9 C -0.0122(5) 0.7454(4) 0.66684(8) 0.0241(6) Uani 1 1 d . . . . .
H9D H -0.065721 0.682209 0.687597 0.029 Uiso 1 1 calc R U . . .
H9F H -0.109842 0.836019 0.663517 0.029 Uiso 1 1 calc R U . . .
C19 C -0.2506(4) 0.5971(4) 0.61533(9) 0.0278(7) Uani 1 1 d . . . . .
H19A H -0.326162 0.571889 0.638743 0.033 Uiso 1 1 calc R U . . .
H19B H -0.262964 0.497653 0.595427 0.033 Uiso 1 1 calc R U . . .
C20 C -0.3590(5) 0.7365(4) 0.59678(8) 0.0262(7) Uani 1 1 d . . . . .
C21 C 0.0924(5) 0.4866(3) 0.63269(8) 0.0230(6) Uani 1 1 d . . . . .
H21A H 0.007750 0.413965 0.647629 0.028 Uiso 1 1 calc R U . . .
H21B H 0.231370 0.515596 0.648632 0.028 Uiso 1 1 calc R U . . .
C22 C 0.1330(5) 0.3944(3) 0.59267(8) 0.0238(6) Uani 1 1 d . . . . .
Ca2 Ca 0.78347(8) 1.31114(6) 0.93554(2) 0.01576(15) Uani 1 1 d . . . . .
O2 O 0.8113(3) 1.0933(2) 0.87366(6) 0.0266(5) Uani 1 1 d D . . . .
O10 O 0.9008(3) 1.8287(2) 0.91149(6) 0.0244(4) Uani 1 1 d . . . . .
O11 O 0.8041(3) 1.6149(2) 0.94181(5) 0.0233(4) Uani 1 1 d . . . . .
O12 O 0.6881(3) 1.4048(3) 1.00273(6) 0.0310(5) Uani 1 1 d . . . . .
H12A H 0.696286 1.313802 1.019184 0.047 Uiso 0.5 1 calc R U P . .
H12B H 0.541669 1.443229 1.001141 0.047 Uiso 0.5 1 calc R U P . .
H12F H 0.787795 1.494975 1.014925 0.047 Uiso 1 1 calc R U . . .
O13 O 1.0926(3) 1.2393(3) 0.97930(6) 0.0344(5) Uani 1 1 d . . . . .
H13A H 1.109374 1.316941 1.003891 0.052 Uiso 0.5 1 calc R U P . .
H13B H 1.222833 1.244599 0.965164 0.052 Uiso 1 1 calc R U . . .
H13F H 1.068548 1.127745 0.986234 0.052 Uiso 0.5 1 calc R U P . .
O14 O 0.6851(3) 1.0470(2) 0.95855(6) 0.0240(5) Uani 1 1 d . . . . .
H14F H 0.536984 1.013616 0.948401 0.012(13) Uiso 0.5 1 calc R . P . .
H14A H 0.697759 1.058743 0.987982 0.07(3) Uiso 0.5 1 calc R . P . .
H14B H 0.781470 0.963425 0.948447 0.082(15) Uiso 1 1 calc R . . . .
O15 O 0.0929(3) 1.3837(3) 0.90532(6) 0.0292(5) Uani 1 1 d . . . . .
O16 O 0.4006(3) 1.2794(3) 0.92512(6) 0.0281(5) Uani 1 1 d . . . . .
N2 N 0.6198(3) 1.4452(3) 0.87353(6) 0.0167(5) Uani 1 1 d . . . . .
C10 C 1.0494(5) 1.2436(4) 0.77118(9) 0.0270(7) Uani 1 1 d . . . . .
C11 C 1.1351(6) 1.3006(5) 0.73429(10) 0.0429(9) Uani 1 1 d . . . . .
H11A H 1.117859 1.210963 0.712192 0.064 Uiso 1 1 calc R U . . .
H11B H 1.287516 1.333499 0.740113 0.064 Uiso 1 1 calc R U . . .
H11C H 1.055755 1.394554 0.726619 0.064 Uiso 1 1 calc R U . . .
C12 C 1.1904(6) 0.9352(4) 0.84406(12) 0.0447(9) Uani 1 1 d . . . . .
H12C H 1.095549 0.836824 0.842945 0.067 Uiso 1 1 calc R U . . .
H12D H 1.234234 0.976569 0.872164 0.067 Uiso 1 1 calc R U . . .
H12E H 1.317693 0.907438 0.830057 0.067 Uiso 1 1 calc R U . . .
C13 C 1.0728(5) 1.0658(3) 0.82404(9) 0.0268(7) Uani 1 1 d . . . . .
C14 C 1.1447(5) 1.1189(4) 0.78976(9) 0.0270(7) Uani 1 1 d . . . . .
H14 H 1.263522 1.068241 0.778539 0.032 Uiso 1 1 calc R U . . .
C15 C 0.8730(5) 1.3117(4) 0.78742(8) 0.0248(6) Uani 1 1 d . . . . .
H15 H 0.805195 1.396796 0.775003 0.030 Uiso 1 1 calc R U . . .
C16 C 0.7909(4) 1.2602(3) 0.82128(8) 0.0211(6) Uani 1 1 d . . . . .
C17 C 0.8946(4) 1.1373(3) 0.83956(8) 0.0214(6) Uani 1 1 d . . . . .
C18 C 0.5914(4) 1.3310(3) 0.83606(8) 0.0217(6) Uani 1 1 d . . . . .
H18A H 0.521591 1.389437 0.814719 0.026 Uiso 1 1 calc R U . . .
H18B H 0.492026 1.239142 0.840197 0.026 Uiso 1 1 calc R U . . .
C23 C 0.7546(4) 1.5900(3) 0.86995(8) 0.0178(6) Uani 1 1 d . . . . .
H23A H 0.674355 1.663126 0.853296 0.021 Uiso 1 1 calc R U . . .
H23B H 0.882858 1.556290 0.856328 0.021 Uiso 1 1 calc R U . . .
C24 C 0.8250(4) 1.6835(3) 0.91122(8) 0.0174(6) Uani 1 1 d . . . . .
C25 C 0.4056(4) 1.4947(3) 0.88373(9) 0.0216(6) Uani 1 1 d . . . . .
H25A H 0.317157 1.508011 0.858630 0.026 Uiso 1 1 calc R U . . .
H25B H 0.420314 1.602832 0.900366 0.026 Uiso 1 1 calc R U . . .
C26 C 0.2905(4) 1.3750(3) 0.90596(8) 0.0199(6) Uani 1 1 d . . . . .
O17 O 0.2941(3) 0.8716(3) 0.95762(7) 0.0314(5) Uani 1 1 d D . . . .
O0AA O 0.6424(9) 1.1571(7) 0.56062(16) 0.0472(19) Uani 0.499(7) 1 d D . P A 2
O1AA O 0.6147(7) 1.0348(6) 0.53109(14) 0.0312(15) Uani 0.501(7) 1 d D . P A 1
H0AA H 0.662(8) 1.043(3) 0.5582(7) 0.12(2) Uiso 1 1 d D . . . .
H17A H 0.172(4) 0.867(5) 0.9412(10) 0.072(14) Uiso 1 1 d D . . . .
H9B H -0.300388 0.742620 0.511992 0.16(3) Uiso 1 1 d . . . . .
H9A H -0.126410 0.656950 0.485286 0.089(16) Uiso 1 1 d . . . . .
H7A H 0.276197 0.764462 0.485065 0.074(14) Uiso 1 1 d . . . . .
H7B H 0.256559 0.574533 0.491568 0.081(14) Uiso 1 1 d . . . . .
H1 H 0.211(6) 1.090(3) 0.6259(11) 0.059(12) Uiso 1 1 d D . . . .
H2 H 0.851(6) 0.994(3) 0.8784(11) 0.056(12) Uiso 1 1 d D . . . .
H17B H 0.244(10) 0.895(10) 0.9823(9) 0.07(3) Uiso 0.5 1 d D . P B 2
H0AB H 0.513(6) 1.170(8) 0.572(2) 0.05(2) Uiso 0.499(7) 1 d D . P A 2
H17C H 0.394(9) 0.926(13) 0.945(2) 0.13(5) Uiso 0.5 1 d D . P C 1
H1AB H 0.483(7) 0.984(10) 0.525(2) 0.08(3) Uiso 0.501(7) 1 d D . P A 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
Ca1 O6 2.282(2) 1_655 ?
Ca1 O8 2.399(2) . ?
Ca1 O3 2.401(2) . ?
Ca1 O4 2.410(2) . ?
Ca1 O9 2.505(2) . ?
Ca1 O7 2.541(2) . ?
Ca1 N1 2.601(2) . ?
Ca1 O1 2.698(2) . ?
Ca1 C20 3.165(3) . ?
Ca1 C19 3.219(3) . ?
Ca1 C22 3.229(3) . ?
O1 C1 1.375(3) . ?
O3 C20 1.259(4) . ?
O4 C22 1.247(3) . ?
O5 C22 1.249(4) . ?
O6 C20 1.244(3) . ?
N1 C21 1.461(4) . ?
N1 C19 1.473(4) . ?
N1 C9 1.481(4) . ?
C1 C2 1.388(4) . ?
C1 C6 1.396(4) . ?
C2 C3 1.390(4) . ?
C2 C9 1.496(4) . ?
C3 C4 1.386(5) . ?
C4 C5 1.376(5) . ?
C4 C8 1.504(4) . ?
C5 C6 1.390(4) . ?
C6 C7 1.496(5) . ?
C19 C20 1.520(4) . ?
C21 C22 1.512(4) . ?
Ca2 O15 2.352(2) 1_655 ?
Ca2 O16 2.396(2) . ?
Ca2 O12 2.432(2) . ?
Ca2 O14 2.459(2) . ?
Ca2 O13 2.465(2) . ?
Ca2 O11 2.4748(19) . ?
Ca2 O2 2.604(2) . ?
Ca2 N2 2.622(2) . ?
O2 C17 1.378(3) . ?
O10 C24 1.266(3) . ?
O11 C24 1.243(3) . ?
O15 C26 1.241(3) . ?
O16 C26 1.261(3) . ?
N2 C23 1.455(3) . ?
N2 C25 1.472(3) . ?
N2 C18 1.475(3) . ?
C10 C15 1.381(4) . ?
C10 C14 1.387(4) . ?
C10 C11 1.509(4) . ?
C12 C13 1.513(4) . ?
C13 C14 1.383(4) . ?
C13 C17 1.392(4) . ?
C15 C16 1.391(4) . ?
C16 C17 1.394(4) . ?
C16 C18 1.495(4) . ?
C23 C24 1.529(4) . ?
C25 C26 1.501(4) . ?

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 Ca1 O8 101.88(8) 1_655 . ?
O6 Ca1 O3 140.17(8) 1_655 . ?
O8 Ca1 O3 89.57(7) . . ?
O6 Ca1 O4 81.24(8) 1_655 . ?
O8 Ca1 O4 149.52(7) . . ?
O3 Ca1 O4 107.54(7) . . ?
O6 Ca1 O9 148.57(8) 1_655 . ?
O8 Ca1 O9 87.92(7) . . ?
O3 Ca1 O9 68.58(7) . . ?
O4 Ca1 O9 75.82(7) . . ?
O6 Ca1 O7 78.55(8) 1_655 . ?
O8 Ca1 O7 72.84(7) . . ?
O3 Ca1 O7 140.90(7) . . ?
O4 Ca1 O7 78.23(7) . . ?
O9 Ca1 O7 75.97(7) . . ?
O6 Ca1 N1 85.12(8) 1_655 . ?
O8 Ca1 N1 145.29(7) . . ?
O3 Ca1 N1 65.73(7) . . ?
O4 Ca1 N1 64.82(7) . . ?
O9 Ca1 N1 103.78(7) . . ?
O7 Ca1 N1 141.45(7) . . ?
O6 Ca1 O1 71.56(8) 1_655 . ?
O8 Ca1 O1 78.57(7) . . ?
O3 Ca1 O1 73.67(7) . . ?
O4 Ca1 O1 129.86(7) . . ?
O9 Ca1 O1 139.88(7) . . ?
O7 Ca1 O1 132.84(7) . . ?
N1 Ca1 O1 71.47(7) . . ?
O6 Ca1 C20 133.97(8) 1_655 . ?
O8 Ca1 C20 109.99(8) . . ?
O3 Ca1 C20 20.92(8) . . ?
O4 Ca1 C20 87.14(8) . . ?
O9 Ca1 C20 66.37(7) . . ?
O7 Ca1 C20 141.93(7) . . ?
N1 Ca1 C20 50.06(7) . . ?
O1 Ca1 C20 82.98(7) . . ?
O6 Ca1 C19 111.10(8) 1_655 . ?
O8 Ca1 C19 137.05(8) . . ?
O3 Ca1 C19 47.49(8) . . ?
O4 Ca1 C19 65.04(8) . . ?
O9 Ca1 C19 78.21(7) . . ?
O7 Ca1 C19 139.16(8) . . ?
N1 Ca1 C19 26.72(7) . . ?
O1 Ca1 C19 86.37(8) . . ?
C20 Ca1 C19 27.54(8) . . ?
O6 Ca1 C22 71.43(9) 1_655 . ?
O8 Ca1 C22 165.30(8) . . ?
O3 Ca1 C22 103.95(8) . . ?
O4 Ca1 C22 19.40(7) . . ?
O9 Ca1 C22 91.66(7) . . ?
O7 Ca1 C22 92.80(7) . . ?
N1 Ca1 C22 48.75(7) . . ?
O1 Ca1 C22 110.46(7) . . ?
C20 Ca1 C22 83.16(8) . . ?
C19 Ca1 C22 56.86(8) . . ?
C1 O1 Ca1 118.41(17) . . ?
C20 O3 Ca1 116.17(18) . . ?
C22 O4 Ca1 120.66(17) . . ?
C20 O6 Ca1 156.5(2) . 1_455 ?
C21 N1 C19 110.8(2) . . ?
C21 N1 C9 111.6(2) . . ?
C19 N1 C9 107.4(2) . . ?
C21 N1 Ca1 107.81(16) . . ?
C19 N1 Ca1 100.73(16) . . ?
C9 N1 Ca1 117.92(16) . . ?
O1 C1 C2 115.5(2) . . ?
O1 C1 C6 123.0(3) . . ?
C2 C1 C6 121.5(3) . . ?
C1 C2 C3 118.1(3) . . ?
C1 C2 C9 120.5(2) . . ?
C3 C2 C9 121.4(3) . . ?
C4 C3 C2 122.6(3) . . ?
C5 C4 C3 117.1(3) . . ?
C5 C4 C8 121.2(3) . . ?
C3 C4 C8 121.7(3) . . ?
C4 C5 C6 123.3(3) . . ?
C5 C6 C1 117.4(3) . . ?
C5 C6 C7 120.6(3) . . ?
C1 C6 C7 122.0(3) . . ?
N1 C9 C2 114.8(2) . . ?
N1 C19 C20 112.7(2) . . ?
N1 C19 Ca1 52.55(13) . . ?
C20 C19 Ca1 74.25(15) . . ?
O6 C20 O3 125.9(3) . . ?
O6 C20 C19 116.3(3) . . ?
O3 C20 C19 117.8(2) . . ?
O6 C20 Ca1 157.0(2) . . ?
O3 C20 Ca1 42.91(13) . . ?
C19 C20 Ca1 78.21(15) . . ?
N1 C21 C22 112.6(2) . . ?
O4 C22 O5 124.2(3) . . ?
O4 C22 C21 118.5(2) . . ?
O5 C22 C21 117.2(2) . . ?
O4 C22 Ca1 39.94(13) . . ?
O5 C22 Ca1 155.8(2) . . ?
C21 C22 Ca1 81.25(15) . . ?
O15 Ca2 O16 143.54(7) 1_655 . ?
O15 Ca2 O12 128.01(8) 1_655 . ?
O16 Ca2 O12 79.77(8) . . ?
O15 Ca2 O14 128.40(7) 1_655 . ?
O16 Ca2 O14 73.75(7) . . ?
O12 Ca2 O14 79.63(7) . . ?
O15 Ca2 O13 73.35(7) 1_655 . ?
O16 Ca2 O13 142.28(7) . . ?
O12 Ca2 O13 76.65(8) . . ?
O14 Ca2 O13 73.35(7) . . ?
O15 Ca2 O11 74.06(8) 1_655 . ?
O16 Ca2 O11 96.42(7) . . ?
O12 Ca2 O11 73.80(7) . . ?
O14 Ca2 O11 152.97(7) . . ?
O13 Ca2 O11 104.64(8) . . ?
O15 Ca2 O2 72.94(7) 1_655 . ?
O16 Ca2 O2 89.28(8) . . ?
O12 Ca2 O2 154.40(7) . . ?
O14 Ca2 O2 75.09(7) . . ?
O13 Ca2 O2 99.58(7) . . ?
O11 Ca2 O2 130.84(7) . . ?
O15 Ca2 N2 78.23(7) 1_655 . ?
O16 Ca2 N2 66.28(7) . . ?
O12 Ca2 N2 120.33(7) . . ?
O14 Ca2 N2 129.35(7) . . ?
O13 Ca2 N2 151.41(7) . . ?
O11 Ca2 N2 63.71(7) . . ?
O2 Ca2 N2 74.61(7) . . ?
C17 O2 Ca2 120.50(16) . . ?
C24 O11 Ca2 118.78(17) . . ?
C26 O15 Ca2 145.48(19) . 1_455 ?
C26 O16 Ca2 122.02(17) . . ?
C23 N2 C25 109.8(2) . . ?
C23 N2 C18 112.7(2) . . ?
C25 N2 C18 107.6(2) . . ?
C23 N2 Ca2 107.41(15) . . ?
C25 N2 Ca2 105.42(16) . . ?
C18 N2 Ca2 113.61(16) . . ?
C15 C10 C14 117.6(3) . . ?
C15 C10 C11 121.6(3) . . ?
C14 C10 C11 120.8(3) . . ?
C14 C13 C17 118.5(3) . . ?
C14 C13 C12 119.8(3) . . ?
C17 C13 C12 121.8(3) . . ?
C13 C14 C10 122.3(3) . . ?
C10 C15 C16 122.4(3) . . ?
C15 C16 C17 118.1(3) . . ?
C15 C16 C18 120.1(3) . . ?
C17 C16 C18 121.7(2) . . ?
O2 C17 C13 122.8(3) . . ?
O2 C17 C16 116.1(2) . . ?
C13 C17 C16 121.1(3) . . ?
N2 C18 C16 116.2(2) . . ?
N2 C23 C24 111.1(2) . . ?
O11 C24 O10 124.5(3) . . ?
O11 C24 C23 119.3(2) . . ?
O10 C24 C23 116.3(2) . . ?
N2 C25 C26 113.9(2) . . ?
O15 C26 O16 125.1(3) . . ?
O15 C26 C25 116.5(2) . . ?
O16 C26 C25 118.3(2) . . ?

_refine_diff_density_max         0.433
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.119


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: H2O/MeOH 1:1 (v/v)'
