# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_CaSyr_I_E512a
_database_code_depnum_ccdc_archive 'CCDC 2214086'
loop_
_audit_author_name
_audit_author_address
'Oriol Vallcorba'
;ALBA Synchrotron Light Source
Spain
;
_audit_update_record             
;
2022-10-19 deposited with the CCDC.	2023-03-01 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT420_CaSyr_I_E512a       
;
PROBLEM: D-H Bond Without Acceptor  O11      --H11A     .     Please Check
RESPONSE: These H-bonds are between H2O molecules coordinated to Ca atoms and the solvent molecules, which are masked. This is why the acceptor is missing
;
_vrf_PLAT420_CaSyr_I_E512a_2     
;
PROBLEM: D-H Bond Without Acceptor  O11      --H11B     .     Please Check
RESPONSE: These H-bonds are between H2O molecules coordinated to Ca atoms and the solvent molecules, which are masked. This is why the acceptor is missing
;
_vrf_PLAT420_CaSyr_I_E512a_3     
;
PROBLEM: D-H Bond Without Acceptor  O12      --H12B     .     Please Check
RESPONSE: These H-bonds are between H2O molecules coordinated to Ca atoms and the solvent molecules, which are masked. This is why the acceptor is missing
;
# Added during the CSD deposition process: Wednesday 19 October 2022 04:50 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 H20 Ca2 O12, 2(H2 O1), 2(C3 H7 N1 O1)'
_chemical_formula_sum            'C24 H38 Ca2 N2 O16'
_chemical_formula_weight         690.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0024 0.0017 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2105 0.3233 '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 0.0046 0.0035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0086 0.0064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   30.963(2)
_cell_length_b                   30.963(2)
_cell_length_c                   16.9530(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     14075(2)
_cell_formula_units_Z            18
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24167
_cell_measurement_theta_min      1.350
_cell_measurement_theta_max      34.464

_exptl_crystal_description       prism
_exptl_crystal_colour            white
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_F_000             6552
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.469
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_absorpt_special_details   'from ABSORB.cbf scaled to 1'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_source                   'XALOC beamline, ALBA-CELLS, Barcelona'
_diffrn_measurement_device_type  'CCD Pilatus 6M-Dectris'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean 5.814
_diffrn_reflns_number            83456
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.458
_diffrn_reflns_theta_max         30.427
_diffrn_reflns_theta_full        25.950
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8717
_reflns_number_gt                7990
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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       ?
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'PLATON (Spek 2009)'
_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)+(0.0484P)²+30.7293P] 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         8717
_refine_ls_number_parameters     295
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.1018
_refine_ls_wR_factor_gt          0.1001
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.061
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca2 Ca 0.49268(2) 0.48202(2) 0.65220(2) 0.01302(6) Uani 1 1 d . . . . .
Ca1 Ca 0.35633(2) 0.15983(2) 0.52905(2) 0.01385(6) Uani 1 1 d . . . . .
O1 O 0.37716(4) 0.15116(4) 0.65425(6) 0.01969(19) Uani 1 1 d . . . . .
O3 O 0.41249(4) 0.01862(4) 0.86718(6) 0.01874(19) Uani 1 1 d . . . . .
O4 O 0.46571(4) 0.01500(4) 0.74798(6) 0.01814(18) Uani 1 1 d . . . . .
O8 O 0.37182(4) 0.27258(3) 0.30937(6) 0.0198(2) Uani 1 1 d . . . . .
O6 O 0.48323(4) 0.44056(4) 0.53793(6) 0.02014(19) Uani 1 1 d . . . . .
O7 O 0.50136(4) 0.44902(3) 0.40962(6) 0.01966(19) Uani 1 1 d . . . . .
O9 O 0.36871(4) 0.21587(3) 0.42825(6) 0.01946(19) Uani 1 1 d . . . . .
O2 O 0.38056(4) 0.16304(4) 0.78384(6) 0.0228(2) Uani 1 1 d . . . . .
O5 O 0.48771(4) 0.07175(4) 0.62008(6) 0.0232(2) Uani 1 1 d . . . . .
O10 O 0.40597(4) 0.25085(4) 0.56981(6) 0.0242(2) Uani 1 1 d . . . . .
O12 O 0.49418(4) 0.41694(4) 0.72560(7) 0.0270(2) Uani 1 1 d . . . . .
H12A H 0.4995 0.4252 0.7741 0.040 Uiso 1 1 d R U . . .
H12B H 0.5191 0.4143 0.7113 0.040 Uiso 1 1 d R U . . .
O11 O 0.43793(4) 0.17371(5) 0.49603(7) 0.0290(2) Uani 1 1 d . . . . .
H11A H 0.4658 0.1915 0.5222 0.043 Uiso 1 1 d R U . . .
H11B H 0.4463 0.1619 0.4555 0.043 Uiso 1 1 d R U . . .
C4 C 0.41955(5) 0.04974(5) 0.80381(7) 0.0144(2) Uani 1 1 d . . . . .
C6 C 0.45857(5) 0.07722(5) 0.67659(7) 0.0163(2) Uani 1 1 d . . . . .
C11 C 0.44687(5) 0.36815(4) 0.45939(8) 0.0153(2) Uani 1 1 d . . . . .
C7 C 0.43945(5) 0.10906(5) 0.66994(8) 0.0168(2) Uani 1 1 d . . . . .
H7 H 0.4457 0.1286 0.6251 0.020 Uiso 1 1 calc R U . . .
C3 C 0.40063(5) 0.08196(5) 0.79883(7) 0.0151(2) Uani 1 1 d . . . . .
H3 H 0.3816 0.0838 0.8398 0.018 Uiso 1 1 calc R U . . .
C12 C 0.42498(5) 0.34848(4) 0.38622(7) 0.0158(2) Uani 1 1 d . . . . .
H12 H 0.4292 0.3695 0.3441 0.019 Uiso 1 1 calc R U . . .
C2 C 0.41049(5) 0.11152(5) 0.73160(7) 0.0148(2) Uani 1 1 d . . . . .
C1 C 0.38781(5) 0.14405(5) 0.72248(8) 0.0153(2) Uani 1 1 d . . . . .
C13 C 0.39686(5) 0.29704(5) 0.37753(7) 0.0157(2) Uani 1 1 d . . . . .
C5 C 0.44862(5) 0.04599(5) 0.74307(7) 0.0146(2) Uani 1 1 d . . . . .
C14 C 0.39213(5) 0.26417(4) 0.43900(7) 0.0161(2) Uani 1 1 d . . . . .
C10 C 0.47904(5) 0.42303(4) 0.47020(8) 0.0152(2) Uani 1 1 d . . . . .
C16 C 0.44019(5) 0.33689(5) 0.52334(8) 0.0175(2) Uani 1 1 d . . . . .
H16 H 0.4534 0.3503 0.5725 0.021 Uiso 1 1 calc R U . . .
C15 C 0.41366(5) 0.28564(5) 0.51250(8) 0.0177(2) Uani 1 1 d . . . . .
C17 C 0.36933(7) 0.30336(5) 0.24833(9) 0.0294(3) Uani 1 1 d . . . . .
H17A H 0.3512 0.2829 0.2041 0.044 Uiso 1 1 calc R U . . .
H17B H 0.4025 0.3275 0.2321 0.044 Uiso 1 1 calc R U . . .
H17C H 0.3526 0.3202 0.2680 0.044 Uiso 1 1 calc R U . . .
C8 C 0.37560(6) 0.01356(6) 0.92353(9) 0.0261(3) Uani 1 1 d . . . . .
H8A H 0.3445 0.0032 0.8970 0.039 Uiso 1 1 calc R U . . .
H8B H 0.3864 0.0450 0.9490 0.039 Uiso 1 1 calc R U . . .
H8C H 0.3712 -0.0109 0.9623 0.039 Uiso 1 1 calc R U . . .
C18 C 0.43196(7) 0.26975(6) 0.64267(9) 0.0306(3) Uani 1 1 d . . . . .
H18A H 0.4240 0.2425 0.6780 0.046 Uiso 1 1 calc R U . . .
H18B H 0.4221 0.2918 0.6660 0.046 Uiso 1 1 calc R U . . .
H18C H 0.4672 0.2877 0.6330 0.046 Uiso 1 1 calc R U . . .
C9 C 0.50481(8) 0.10687(8) 0.55655(11) 0.0405(5) Uani 1 1 d . . . . .
H9A H 0.5267 0.1397 0.5768 0.061 Uiso 1 1 calc R U . . .
H9B H 0.4768 0.1063 0.5313 0.061 Uiso 1 1 calc R U . . .
H9C H 0.5224 0.0982 0.5190 0.061 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca2 O6 2.2606(10) . ?
Ca2 O7 2.3017(10) 10_666 ?
Ca2 O9 2.3032(10) 5 ?
Ca2 O4 2.3433(10) 3_665 ?
Ca2 O12 2.3884(11) . ?
Ca2 O5 2.5547(10) 3_665 ?
Ca2 O8 2.6486(10) 5 ?
Ca2 Ca1 3.7990(4) 5 ?
Ca1 O1 2.2731(10) . ?
Ca1 O4 2.3082(10) 8_544 ?
Ca1 O9 2.3265(10) . ?
Ca1 O2 2.3786(11) 13_556 ?
Ca1 O11 2.4075(12) . ?
Ca1 O10 2.5397(10) . ?
Ca1 O3 2.6755(10) 8_544 ?
Ca1 C14 3.2273(13) . ?
Ca1 Ca2 3.7989(4) 9_554 ?
O1 C1 1.2520(16) . ?
O3 C4 1.3855(15) . ?
O3 C8 1.4364(16) . ?
O3 Ca1 2.6752(10) 6 ?
O4 C5 1.3096(14) . ?
O4 Ca1 2.3080(10) 6 ?
O4 Ca2 2.3435(9) 2_655 ?
O8 C13 1.3866(15) . ?
O8 C17 1.4348(16) . ?
O8 Ca2 2.6485(10) 9_554 ?
O6 C10 1.2489(16) . ?
O7 C10 1.2743(16) . ?
O7 Ca2 2.3018(10) 10_666 ?
O9 C14 1.3082(14) . ?
O9 Ca2 2.3031(10) 9_554 ?
O2 C1 1.2688(16) . ?
O2 Ca1 2.3786(11) 13_556 ?
O5 C6 1.3831(15) . ?
O5 C9 1.4307(18) . ?
O5 Ca2 2.5548(10) 2_655 ?
O10 C15 1.3801(15) . ?
O10 C18 1.4301(17) . ?
O12 H12A 0.8518 . ?
O12 H12B 0.8512 . ?
O11 H11A 0.8776 . ?
O11 H11B 0.8753 . ?
C4 C3 1.3892(16) . ?
C4 C5 1.4102(17) . ?
C6 C7 1.3852(17) . ?
C6 C5 1.4149(17) . ?
C11 C16 1.3983(18) . ?
C11 C12 1.3986(17) . ?
C11 C10 1.4901(16) . ?
C7 C2 1.4041(17) . ?
C7 H7 0.9300 . ?
C3 C2 1.3967(17) . ?
C3 H3 0.9300 . ?
C12 C13 1.3893(16) . ?
C12 H12 0.9300 . ?
C2 C1 1.4964(16) . ?
C13 C14 1.4121(17) . ?
C14 C15 1.4128(17) . ?
C16 C15 1.3866(17) . ?
C16 H16 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?

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 Ca2 O7 93.68(4) . 10_666 ?
O6 Ca2 O9 143.62(4) . 5 ?
O7 Ca2 O9 95.79(4) 10_666 5 ?
O6 Ca2 O4 145.65(4) . 3_665 ?
O7 Ca2 O4 89.40(4) 10_666 3_665 ?
O9 Ca2 O4 69.58(3) 5 3_665 ?
O6 Ca2 O12 91.09(4) . . ?
O7 Ca2 O12 173.48(4) 10_666 . ?
O9 Ca2 O12 82.92(4) 5 . ?
O4 Ca2 O12 84.16(4) 3_665 . ?
O6 Ca2 O5 80.26(3) . 3_665 ?
O7 Ca2 O5 90.12(4) 10_666 3_665 ?
O9 Ca2 O5 134.61(3) 5 3_665 ?
O4 Ca2 O5 65.52(3) 3_665 3_665 ?
O12 Ca2 O5 86.30(4) . 3_665 ?
O6 Ca2 O8 80.52(3) . 5 ?
O7 Ca2 O8 92.47(4) 10_666 5 ?
O9 Ca2 O8 64.07(3) 5 5 ?
O4 Ca2 O8 133.57(3) 3_665 5 ?
O12 Ca2 O8 92.70(4) . 5 ?
O5 Ca2 O8 160.73(3) 3_665 5 ?
O6 Ca2 Ca1 169.11(3) . 5 ?
O7 Ca2 Ca1 97.21(3) 10_666 5 ?
O9 Ca2 Ca1 35.06(2) 5 5 ?
O4 Ca2 Ca1 34.94(2) 3_665 5 ?
O12 Ca2 Ca1 78.05(3) . 5 ?
O5 Ca2 Ca1 99.56(2) 3_665 5 ?
O8 Ca2 Ca1 99.05(2) 5 5 ?
O1 Ca1 O4 144.22(4) . 8_544 ?
O1 Ca1 O9 145.42(4) . . ?
O4 Ca1 O9 69.79(3) 8_544 . ?
O1 Ca1 O2 102.29(4) . 13_556 ?
O4 Ca1 O2 87.70(4) 8_544 13_556 ?
O9 Ca1 O2 80.01(4) . 13_556 ?
O1 Ca1 O11 84.47(4) . . ?
O4 Ca1 O11 95.55(4) 8_544 . ?
O9 Ca1 O11 85.94(4) . . ?
O2 Ca1 O11 163.50(4) 13_556 . ?
O1 Ca1 O10 80.04(3) . . ?
O4 Ca1 O10 135.56(3) 8_544 . ?
O9 Ca1 O10 65.77(3) . . ?
O2 Ca1 O10 84.05(4) 13_556 . ?
O11 Ca1 O10 82.32(4) . . ?
O1 Ca1 O3 80.67(3) . 8_544 ?
O4 Ca1 O3 63.61(3) 8_544 8_544 ?
O9 Ca1 O3 133.20(3) . 8_544 ?
O2 Ca1 O3 101.79(4) 13_556 8_544 ?
O11 Ca1 O3 94.11(4) . 8_544 ?
O10 Ca1 O3 160.63(3) . 8_544 ?
O1 Ca1 C14 125.75(4) . . ?
O4 Ca1 C14 89.70(3) 8_544 . ?
O9 Ca1 C14 19.93(3) . . ?
O2 Ca1 C14 79.19(4) 13_556 . ?
O11 Ca1 C14 84.65(4) . . ?
O10 Ca1 C14 45.85(3) . . ?
O3 Ca1 C14 153.10(3) 8_544 . ?
O1 Ca1 Ca2 179.31(3) . 9_554 ?
O4 Ca1 Ca2 35.56(2) 8_544 9_554 ?
O9 Ca1 Ca2 34.66(2) . 9_554 ?
O2 Ca1 Ca2 78.40(3) 13_556 9_554 ?
O11 Ca1 Ca2 94.89(3) . 9_554 ?
O10 Ca1 Ca2 100.13(2) . 9_554 ?
O3 Ca1 Ca2 99.14(2) 8_544 9_554 ?
C14 Ca1 Ca2 54.38(2) . 9_554 ?
C1 O1 Ca1 177.05(9) . . ?
C4 O3 C8 115.58(10) . . ?
C4 O3 Ca1 113.59(7) . 6 ?
C8 O3 Ca1 130.82(8) . 6 ?
C5 O4 Ca1 125.15(8) . 6 ?
C5 O4 Ca2 122.80(8) . 2_655 ?
Ca1 O4 Ca2 109.51(4) 6 2_655 ?
C13 O8 C17 116.05(10) . . ?
C13 O8 Ca2 114.90(7) . 9_554 ?
C17 O8 Ca2 128.22(8) . 9_554 ?
C10 O6 Ca2 172.11(9) . . ?
C10 O7 Ca2 136.00(9) . 10_666 ?
C14 O9 Ca2 126.09(8) . 9_554 ?
C14 O9 Ca1 122.74(8) . . ?
Ca2 O9 Ca1 110.29(4) 9_554 . ?
C1 O2 Ca1 124.62(9) . 13_556 ?
C6 O5 C9 116.41(11) . . ?
C6 O5 Ca2 116.50(7) . 2_655 ?
C9 O5 Ca2 126.13(8) . 2_655 ?
C15 O10 C18 116.51(11) . . ?
C15 O10 Ca1 116.56(8) . . ?
C18 O10 Ca1 126.42(8) . . ?
Ca2 O12 H12A 109.5 . . ?
Ca2 O12 H12B 109.5 . . ?
H12A O12 H12B 104.7 . . ?
Ca1 O11 H11A 127.6 . . ?
Ca1 O11 H11B 127.7 . . ?
H11A O11 H11B 104.7 . . ?
O3 C4 C3 124.75(11) . . ?
O3 C4 C5 113.21(10) . . ?
C3 C4 C5 122.04(11) . . ?
O5 C6 C7 124.59(11) . . ?
O5 C6 C5 113.61(11) . . ?
C7 C6 C5 121.79(11) . . ?
C16 C11 C12 120.96(11) . . ?
C16 C11 C10 118.51(11) . . ?
C12 C11 C10 120.51(11) . . ?
C6 C7 C2 119.33(12) . . ?
C6 C7 H7 120.3 . . ?
C2 C7 H7 120.3 . . ?
C4 C3 C2 119.19(11) . . ?
C4 C3 H3 120.4 . . ?
C2 C3 H3 120.4 . . ?
C13 C12 C11 118.87(11) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C3 C2 C7 120.55(11) . . ?
C3 C2 C1 120.20(11) . . ?
C7 C2 C1 119.15(11) . . ?
O1 C1 O2 123.57(11) . . ?
O1 C1 C2 117.84(11) . . ?
O2 C1 C2 118.58(11) . . ?
O8 C13 C12 124.99(11) . . ?
O8 C13 C14 113.15(10) . . ?
C12 C13 C14 121.85(11) . . ?
O4 C5 C4 121.49(11) . . ?
O4 C5 C6 121.44(11) . . ?
C4 C5 C6 117.07(11) . . ?
O9 C14 C13 121.30(11) . . ?
O9 C14 C15 121.48(11) . . ?
C13 C14 C15 117.21(11) . . ?
O9 C14 Ca1 37.33(6) . . ?
C13 C14 Ca1 158.50(9) . . ?
C15 C14 Ca1 84.20(7) . . ?
O6 C10 O7 124.12(12) . . ?
O6 C10 C11 118.27(11) . . ?
O7 C10 C11 117.60(11) . . ?
C15 C16 C11 119.17(12) . . ?
C15 C16 H16 120.4 . . ?
C11 C16 H16 120.4 . . ?
O10 C15 C16 124.91(12) . . ?
O10 C15 C14 113.38(11) . . ?
C16 C15 C14 121.70(12) . . ?
O8 C17 H17A 109.5 . . ?
O8 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O8 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 C8 H8A 109.5 . . ?
O3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O10 C18 H18A 109.5 . . ?
O10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
O10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O5 C9 H9A 109.5 . . ?
O5 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
O5 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 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
C8 O3 C4 C3 11.83(19) . . . . ?
Ca1 O3 C4 C3 -168.80(10) 6 . . . ?
C8 O3 C4 C5 -168.41(12) . . . . ?
Ca1 O3 C4 C5 10.96(13) 6 . . . ?
C9 O5 C6 C7 9.6(2) . . . . ?
Ca2 O5 C6 C7 179.06(11) 2_655 . . . ?
C9 O5 C6 C5 -171.75(15) . . . . ?
Ca2 O5 C6 C5 -2.24(15) 2_655 . . . ?
O5 C6 C7 C2 -179.70(13) . . . . ?
C5 C6 C7 C2 1.7(2) . . . . ?
O3 C4 C3 C2 179.92(12) . . . . ?
C5 C4 C3 C2 0.18(19) . . . . ?
C16 C11 C12 C13 -0.9(2) . . . . ?
C10 C11 C12 C13 177.44(12) . . . . ?
C4 C3 C2 C7 -0.45(19) . . . . ?
C4 C3 C2 C1 176.03(12) . . . . ?
C6 C7 C2 C3 -0.5(2) . . . . ?
C6 C7 C2 C1 -176.99(12) . . . . ?
Ca1 O2 C1 O1 37.73(18) 13_556 . . . ?
Ca1 O2 C1 C2 -142.53(9) 13_556 . . . ?
C3 C2 C1 O1 -147.38(13) . . . . ?
C7 C2 C1 O1 29.14(18) . . . . ?
C3 C2 C1 O2 32.85(18) . . . . ?
C7 C2 C1 O2 -150.62(13) . . . . ?
C17 O8 C13 C12 -9.5(2) . . . . ?
Ca2 O8 C13 C12 -179.98(11) 9_554 . . . ?
C17 O8 C13 C14 171.82(13) . . . . ?
Ca2 O8 C13 C14 1.34(14) 9_554 . . . ?
C11 C12 C13 O8 177.83(12) . . . . ?
C11 C12 C13 C14 -3.6(2) . . . . ?
Ca1 O4 C5 C4 -16.32(17) 6 . . . ?
Ca2 O4 C5 C4 -176.34(9) 2_655 . . . ?
Ca1 O4 C5 C6 163.62(9) 6 . . . ?
Ca2 O4 C5 C6 3.60(17) 2_655 . . . ?
O3 C4 C5 O4 1.15(18) . . . . ?
C3 C4 C5 O4 -179.09(12) . . . . ?
O3 C4 C5 C6 -178.79(11) . . . . ?
C3 C4 C5 C6 0.97(19) . . . . ?
O5 C6 C5 O4 -0.61(19) . . . . ?
C7 C6 C5 O4 178.12(13) . . . . ?
O5 C6 C5 C4 179.33(11) . . . . ?
C7 C6 C5 C4 -1.93(19) . . . . ?
Ca2 O9 C14 C13 -8.63(19) 9_554 . . . ?
Ca1 O9 C14 C13 -176.81(10) . . . . ?
Ca2 O9 C14 C15 171.25(10) 9_554 . . . ?
Ca1 O9 C14 C15 3.07(18) . . . . ?
Ca2 O9 C14 Ca1 168.18(15) 9_554 . . . ?
O8 C13 C14 O9 3.94(19) . . . . ?
C12 C13 C14 O9 -174.78(13) . . . . ?
O8 C13 C14 C15 -175.95(12) . . . . ?
C12 C13 C14 C15 5.3(2) . . . . ?
O8 C13 C14 Ca1 -1.3(3) . . . . ?
C12 C13 C14 Ca1 179.93(19) . . . . ?
Ca2 O7 C10 O6 -54.9(2) 10_666 . . . ?
Ca2 O7 C10 C11 126.54(11) 10_666 . . . ?
C16 C11 C10 O6 -26.78(18) . . . . ?
C12 C11 C10 O6 154.81(13) . . . . ?
C16 C11 C10 O7 151.87(13) . . . . ?
C12 C11 C10 O7 -26.54(18) . . . . ?
C12 C11 C16 C15 3.5(2) . . . . ?
C10 C11 C16 C15 -174.92(12) . . . . ?
C18 O10 C15 C16 -6.9(2) . . . . ?
Ca1 O10 C15 C16 -179.32(11) . . . . ?
C18 O10 C15 C14 172.27(14) . . . . ?
Ca1 O10 C15 C14 -0.10(15) . . . . ?
C11 C16 C15 O10 177.54(13) . . . . ?
C11 C16 C15 C14 -1.6(2) . . . . ?
O9 C14 C15 O10 -1.8(2) . . . . ?
C13 C14 C15 O10 178.09(12) . . . . ?
Ca1 C14 C15 O10 0.07(11) . . . . ?
O9 C14 C15 C16 177.44(13) . . . . ?
C13 C14 C15 C16 -2.7(2) . . . . ?
Ca1 C14 C15 C16 179.32(13) . . . . ?

_refine_diff_density_max         0.451
_refine_diff_density_min         -0.494
_refine_diff_density_rms         0.068



