# Supplementary Information (SI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2025

####################################################################### 
# 
# 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_fmf2
_database_code_depnum_ccdc_archive 'CCDC 2421320'
loop_
_audit_author_name
_audit_author_address
'Jerome Marrot'
;Institut Lavoisier de Versailles
France
;
_audit_update_record             
;
2025-03-18 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
_audit_creation_date             2025-03-04
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7181)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C46 H40 Ca N2 O10'
_chemical_formula_sum            'C46 H40 Ca N2 O10'
_chemical_formula_weight         820.88
_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 0.0037 0.0018 '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 0.2370 0.3270 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0071 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0122 0.0066 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   18.6216(6)
_cell_length_b                   35.2831(8)
_cell_length_c                   10.5028(3)
_cell_angle_alpha                90
_cell_angle_beta                 120.910(3)
_cell_angle_gamma                90
_cell_volume                     5920.6(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7647
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.29
_cell_measurement_theta_min      1.91
_shelx_estimated_absorpt_T_max   0.998
_shelx_estimated_absorpt_T_min   0.997
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.921
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.2119
_diffrn_reflns_av_unetI/netI     0.1908
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29282
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.950
_diffrn_reflns_theta_max         27.667
_diffrn_reflns_theta_min         2.369
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.799
_diffrn_measurement_device_type  'PROXIMA 2A - Synchrotron SOLEIL'
_diffrn_measurement_method       ?
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7293
_diffrn_source                   synchrotron
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2551
_reflns_number_total             5127

# start Validation Reply Form
_vrf_PLAT029_fmf2                
;
PROBLEM: diffrn_measured_fraction_theta_full value Low
RESPONSE: The diffractometer was single axis (synchrotron)
;
# end Validation Reply Form

_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'XDS package'
_computing_data_collection       'XDS package'
_computing_data_reduction        'XDS package'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1423
_refine_ls_R_factor_gt           0.1034
_refine_ls_restrained_S_all      0.952
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1439P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2659
_refine_ls_wR_factor_ref         0.2924
_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
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C5(H5), C6(H6), C8(H8), C11(H11), C12(H12), C14(H14),
 C15(H15), C20(H20)
2.b Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.250000 0.250000 0.500000 0.0844(5) Uani 1 2 d S . P . .
O1 O 0.30370(19) 0.19420(7) 0.4634(3) 0.0883(10) Uani 1 1 d . . . . .
O2 O 0.2531(2) 0.16667(8) 0.2427(4) 0.0856(9) Uani 1 1 d . . . . .
O3 O 0.35577(19) -0.25757(7) 0.2458(4) 0.0823(9) Uani 1 1 d . . . . .
O4 O 0.3087(2) -0.27429(8) 0.3958(4) 0.0931(10) Uani 1 1 d . . . . .
O5 O 0.1858(3) 0.21253(9) 0.5911(4) 0.1025(11) Uani 1 1 d . . . . .
C1 C 0.3774(3) -0.21543(11) 0.4359(5) 0.0712(11) Uani 1 1 d . . . . .
C2 C 0.3554(3) -0.20450(11) 0.5394(5) 0.0832(13) Uani 1 1 d . . . . .
H2A H 0.320280 -0.220272 0.557653 0.100 Uiso 1 1 calc R U . . .
C3 C 0.3847(3) -0.17092(10) 0.6146(5) 0.0759(12) Uani 1 1 d . . . . .
H3 H 0.369446 -0.163682 0.684590 0.091 Uiso 1 1 calc R U . . .
C4 C 0.4359(2) -0.14742(9) 0.5908(4) 0.0599(10) Uani 1 1 d . . . . .
C5 C 0.4566(2) -0.15830(9) 0.4872(4) 0.0607(10) Uani 1 1 d . . . . .
H5 H 0.491672 -0.142572 0.468752 0.073 Uiso 1 1 calc R U . . .
C6 C 0.4266(2) -0.19181(10) 0.4105(4) 0.0653(10) Uani 1 1 d . . . . .
H6 H 0.440532 -0.198612 0.338257 0.078 Uiso 1 1 calc R U . . .
C7 C 0.4670(2) -0.11078(9) 0.6717(4) 0.0555(10) Uani 1 1 d . . . . .
C8 C 0.4349(2) -0.07704(9) 0.6038(3) 0.0555(10) Uani 1 1 d . . . . .
H8 H 0.389513 -0.077245 0.504121 0.067 Uiso 1 1 calc R U . . .
C9 C 0.4656(2) -0.04184(8) 0.6736(3) 0.0502(9) Uani 1 1 d . . . . .
C10 C 0.4191(2) 0.06266(9) 0.5999(4) 0.0577(10) Uani 1 1 d . . . . .
C11 C 0.4032(2) 0.09119(9) 0.6750(4) 0.0664(10) Uani 1 1 d . . . . .
H11 H 0.419920 0.087570 0.776214 0.080 Uiso 1 1 calc R U . . .
C12 C 0.3638(2) 0.12425(10) 0.6052(5) 0.0680(11) Uani 1 1 d . . . . .
H12 H 0.356162 0.143630 0.659950 0.082 Uiso 1 1 calc R U . . .
C13 C 0.3347(2) 0.12981(9) 0.4545(4) 0.0643(10) Uani 1 1 d . . . . .
C14 C 0.3469(2) 0.10099(9) 0.3782(4) 0.0636(10) Uani 1 1 d . . . . .
H14 H 0.325624 0.103704 0.274874 0.076 Uiso 1 1 calc R U . . .
C15 C 0.3895(2) 0.06828(9) 0.4498(4) 0.0576(10) Uani 1 1 d . . . . .
H15 H 0.398724 0.049324 0.395534 0.069 Uiso 1 1 calc R U . . .
C16 C 0.2945(3) 0.16649(11) 0.3852(6) 0.0759(12) Uani 1 1 d . . . . .
C17 C 0.3458(3) -0.25161(11) 0.3532(6) 0.0778(13) Uani 1 1 d . . . . .
C18 C 0.1423(3) 0.20536(15) 0.6487(7) 0.0971(15) Uani 1 1 d . . . . .
N19 N 0.1542(3) 0.17222(14) 0.7189(5) 0.1099(14) Uani 1 1 d . . . . .
C20 C 0.4329(2) -0.00674(9) 0.6070(4) 0.0555(10) Uani 1 1 d . . . . .
H20 H 0.386471 -0.006575 0.508234 0.067 Uiso 1 1 calc R U . . .
C21 C 0.4637(2) 0.02737(9) 0.6755(4) 0.0545(9) Uani 1 1 d . . . . .
C22 C 0.2104(4) 0.14452(16) 0.7184(8) 0.137(2) Uani 1 1 d . . . . .
H22A H 0.211143 0.146607 0.626062 0.205 Uiso 1 1 calc R U . . .
H22B H 0.191674 0.119090 0.725781 0.205 Uiso 1 1 calc R U . . .
H22C H 0.266886 0.148928 0.803188 0.205 Uiso 1 1 calc R U . . .
C23 C 0.1168(7) 0.1610(2) 0.8021(11) 0.210(5) Uani 1 1 d . . . . .
H23A H 0.153424 0.168210 0.906283 0.316 Uiso 1 1 calc R U . . .
H23B H 0.108754 0.133459 0.795095 0.316 Uiso 1 1 calc R U . . .
H23C H 0.062488 0.173593 0.762187 0.316 Uiso 1 1 calc R U . . .
C24 C 0.0832(5) 0.23189(19) 0.6517(13) 0.204(4) Uani 1 1 d . . . . .
H24A H 0.110939 0.245988 0.745361 0.306 Uiso 1 1 calc R U . . .
H24B H 0.035464 0.217884 0.643131 0.306 Uiso 1 1 calc R U . . .
H24C H 0.063453 0.249642 0.568513 0.306 Uiso 1 1 calc R U . . .
H2 H 0.235(3) 0.1967(18) 0.202(6) 0.140(18) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.328(3) . ?
Ca1 O1 2.328(3) 7_556 ?
Ca1 O3 2.322(3) 6_556 ?
Ca1 O3 2.322(3) 4 ?
Ca1 O5 2.295(4) 7_556 ?
Ca1 O5 2.295(4) . ?
Ca1 C17 3.186(5) 4 ?
Ca1 C17 3.186(5) 6_556 ?
O1 C16 1.231(5) . ?
O2 C16 1.284(5) . ?
O2 H2 1.13(6) . ?
O3 C17 1.252(5) . ?
O4 C17 1.279(5) . ?
O5 C18 1.261(6) . ?
C1 C2 1.399(6) . ?
C1 C6 1.362(5) . ?
C1 C17 1.485(5) . ?
C2 H2A 0.9500 . ?
C2 C3 1.372(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.379(6) . ?
C4 C5 1.383(5) . ?
C4 C7 1.491(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.377(5) . ?
C6 H6 0.9500 . ?
C7 C7 1.462(7) 2_656 ?
C7 C8 1.358(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.406(4) . ?
C9 C9 1.451(6) 2_656 ?
C9 C20 1.399(4) . ?
C10 C11 1.402(5) . ?
C10 C15 1.391(5) . ?
C10 C21 1.481(5) . ?
C11 H11 0.9500 . ?
C11 C12 1.373(5) . ?
C12 H12 0.9500 . ?
C12 C13 1.398(5) . ?
C13 C14 1.384(5) . ?
C13 C16 1.485(5) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(5) . ?
C15 H15 0.9500 . ?
C18 N19 1.338(7) . ?
C18 C24 1.457(8) . ?
N19 C22 1.434(7) . ?
N19 C23 1.425(8) . ?
C20 H20 0.9500 . ?
C20 C21 1.368(4) . ?
C21 C21 1.450(6) 2_656 ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 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
O1 Ca1 O1 180.00(7) 7_556 . ?
O1 Ca1 C17 79.85(11) 7_556 6_556 ?
O1 Ca1 C17 100.14(11) . 6_556 ?
O1 Ca1 C17 100.15(11) 7_556 4 ?
O1 Ca1 C17 79.86(11) . 4 ?
O3 Ca1 O1 95.15(10) 6_556 . ?
O3 Ca1 O1 84.84(10) 6_556 7_556 ?
O3 Ca1 O1 95.16(10) 4 7_556 ?
O3 Ca1 O1 84.85(10) 4 . ?
O3 Ca1 O3 180.0 6_556 4 ?
O3 Ca1 C17 160.82(11) 6_556 4 ?
O3 Ca1 C17 19.18(11) 4 4 ?
O3 Ca1 C17 19.18(11) 6_556 6_556 ?
O3 Ca1 C17 160.82(11) 4 6_556 ?
O5 Ca1 O1 93.35(11) 7_556 . ?
O5 Ca1 O1 86.65(11) 7_556 7_556 ?
O5 Ca1 O1 93.35(11) . 7_556 ?
O5 Ca1 O1 86.65(11) . . ?
O5 Ca1 O3 85.92(12) 7_556 4 ?
O5 Ca1 O3 94.08(12) . 4 ?
O5 Ca1 O3 85.92(12) . 6_556 ?
O5 Ca1 O3 94.08(12) 7_556 6_556 ?
O5 Ca1 O5 180.0 . 7_556 ?
O5 Ca1 C17 67.95(13) . 6_556 ?
O5 Ca1 C17 112.05(13) 7_556 6_556 ?
O5 Ca1 C17 112.05(13) . 4 ?
O5 Ca1 C17 67.96(13) 7_556 4 ?
C17 Ca1 C17 180.0 6_556 4 ?
C16 O1 Ca1 149.0(3) . . ?
C16 O2 H2 110(3) . . ?
C17 O3 Ca1 123.3(3) . 4_545 ?
C18 O5 Ca1 156.4(3) . . ?
C2 C1 C17 120.4(4) . . ?
C6 C1 C2 118.6(3) . . ?
C6 C1 C17 121.0(4) . . ?
C1 C2 H2A 120.1 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2A 120.1 . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.6(4) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 118.2(3) . . ?
C3 C4 C7 121.4(4) . . ?
C5 C4 C7 120.4(3) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 C4 120.4(4) . . ?
C6 C5 H5 119.8 . . ?
C1 C6 C5 121.5(4) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
C7 C7 C4 119.79(18) 2_656 . ?
C8 C7 C4 121.6(3) . . ?
C8 C7 C7 118.64(19) . 2_656 ?
C7 C8 H8 118.3 . . ?
C7 C8 C9 123.3(3) . . ?
C9 C8 H8 118.3 . . ?
C8 C9 C9 117.91(17) . 2_656 ?
C20 C9 C8 124.5(3) . . ?
C20 C9 C9 117.60(18) . 2_656 ?
C11 C10 C21 121.6(3) . . ?
C15 C10 C11 117.4(3) . . ?
C15 C10 C21 121.0(3) . . ?
C10 C11 H11 119.4 . . ?
C12 C11 C10 121.3(4) . . ?
C12 C11 H11 119.4 . . ?
C11 C12 H12 119.5 . . ?
C11 C12 C13 120.9(3) . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C16 118.8(4) . . ?
C14 C13 C12 118.0(3) . . ?
C14 C13 C16 123.3(4) . . ?
C13 C14 H14 119.4 . . ?
C13 C14 C15 121.1(4) . . ?
C15 C14 H14 119.4 . . ?
C10 C15 H15 119.4 . . ?
C14 C15 C10 121.2(3) . . ?
C14 C15 H15 119.4 . . ?
O1 C16 O2 124.6(3) . . ?
O1 C16 C13 120.2(4) . . ?
O2 C16 C13 115.1(4) . . ?
O3 C17 Ca1 37.5(2) . 4_545 ?
O3 C17 O4 124.5(4) . . ?
O3 C17 C1 118.3(4) . . ?
O4 C17 Ca1 109.8(3) . 4_545 ?
O4 C17 C1 117.2(4) . . ?
C1 C17 Ca1 118.9(3) . 4_545 ?
O5 C18 N19 118.3(5) . . ?
O5 C18 C24 124.0(6) . . ?
N19 C18 C24 117.6(7) . . ?
C18 N19 C22 120.5(5) . . ?
C18 N19 C23 125.9(6) . . ?
C23 N19 C22 113.6(6) . . ?
C9 C20 H20 118.0 . . ?
C21 C20 C9 124.0(3) . . ?
C21 C20 H20 118.0 . . ?
C20 C21 C10 119.3(3) . . ?
C20 C21 C21 118.30(18) . 2_656 ?
C21 C21 C10 122.26(18) 2_656 . ?
N19 C22 H22A 109.5 . . ?
N19 C22 H22B 109.5 . . ?
N19 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N19 C23 H23A 109.5 . . ?
N19 C23 H23B 109.5 . . ?
N19 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C24 H24A 109.5 . . ?
C18 C24 H24B 109.5 . . ?
C18 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 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
Ca1 O1 C16 O2 34.1(9) . . . . ?
Ca1 O1 C16 C13 -147.8(4) . . . . ?
Ca1 O3 C17 O4 77.2(5) 4_545 . . . ?
Ca1 O3 C17 C1 -101.5(4) 4_545 . . . ?
Ca1 O5 C18 N19 -156.8(6) . . . . ?
Ca1 O5 C18 C24 19.3(13) . . . . ?
O5 C18 N19 C22 -4.7(8) . . . . ?
O5 C18 N19 C23 173.5(7) . . . . ?
C1 C2 C3 C4 -0.1(7) . . . . ?
C2 C1 C6 C5 1.9(6) . . . . ?
C2 C1 C17 Ca1 126.0(4) . . . 4_545 ?
C2 C1 C17 O3 168.9(4) . . . . ?
C2 C1 C17 O4 -9.8(6) . . . . ?
C2 C3 C4 C5 0.7(6) . . . . ?
C2 C3 C4 C7 179.4(4) . . . . ?
C3 C4 C5 C6 -0.1(5) . . . . ?
C3 C4 C7 C7 74.2(6) . . . 2_656 ?
C3 C4 C7 C8 -105.3(5) . . . . ?
C4 C5 C6 C1 -1.2(6) . . . . ?
C4 C7 C8 C9 -176.4(4) . . . . ?
C5 C4 C7 C7 -107.1(5) . . . 2_656 ?
C5 C4 C7 C8 73.4(5) . . . . ?
C6 C1 C2 C3 -1.2(7) . . . . ?
C6 C1 C17 Ca1 -52.5(5) . . . 4_545 ?
C6 C1 C17 O3 -9.5(6) . . . . ?
C6 C1 C17 O4 171.8(4) . . . . ?
C7 C4 C5 C6 -178.8(3) . . . . ?
C7 C7 C8 C9 4.2(7) 2_656 . . . ?
C7 C8 C9 C9 -0.6(7) . . . 2_656 ?
C7 C8 C9 C20 -179.0(4) . . . . ?
C8 C9 C20 C21 -179.3(4) . . . . ?
C9 C9 C20 C21 2.3(6) 2_656 . . . ?
C9 C20 C21 C10 -174.1(4) . . . . ?
C9 C20 C21 C21 2.0(7) . . . 2_656 ?
C10 C11 C12 C13 3.1(6) . . . . ?
C11 C10 C15 C14 0.8(5) . . . . ?
C11 C10 C21 C20 134.2(4) . . . . ?
C11 C10 C21 C21 -41.7(6) . . . 2_656 ?
C11 C12 C13 C14 0.0(6) . . . . ?
C11 C12 C13 C16 -178.4(4) . . . . ?
C12 C13 C14 C15 -2.6(6) . . . . ?
C12 C13 C16 O1 16.6(6) . . . . ?
C12 C13 C16 O2 -165.1(4) . . . . ?
C13 C14 C15 C10 2.2(6) . . . . ?
C14 C13 C16 O1 -161.7(4) . . . . ?
C14 C13 C16 O2 16.6(6) . . . . ?
C15 C10 C11 C12 -3.4(5) . . . . ?
C15 C10 C21 C20 -44.1(5) . . . . ?
C15 C10 C21 C21 140.0(4) . . . 2_656 ?
C16 C13 C14 C15 175.8(4) . . . . ?
C17 C1 C2 C3 -179.7(4) . . . . ?
C17 C1 C6 C5 -179.7(4) . . . . ?
C21 C10 C11 C12 178.2(4) . . . . ?
C21 C10 C15 C14 179.2(3) . . . . ?
C24 C18 N19 C22 179.0(6) . . . . ?
C24 C18 N19 C23 -2.8(10) . . . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.619 1175.1 255.5 ?
2 0.500 0.500 -0.344 1175.1 255.5 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

_olex2_submission_special_instructions 'No special instructions were received'
_Olex_squeeze_details            
'P. van der Sluis and A. L. Spek, Acta Cryst. (1990). A46, 194-201'
####################################################################### 
# 
# 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_bwx1ca
_database_code_depnum_ccdc_archive 'CCDC 2421321'
loop_
_audit_author_name
_audit_author_address
'LIU JIE'
;University of Warwick 
United Kingdom
;
_audit_update_record             
;
2025-03-03 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
_audit_creation_date             2025-03-03
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.02.27 svn.r83f5de26 for OlexSys, GUI svn.r7172)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C114 H74 Ca5 O32, 2(H2 O), 9.8(O)'
_chemical_formula_sum            'C114 H78 Ca5 O43.80'
_chemical_formula_weight         2348.96
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H20 O4 Ca'
_chemical_oxdiff_usercomment     'C20 H20 O4 Ca colourless block bwx13'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   11.0429(4)
_cell_length_b                   14.6332(5)
_cell_length_c                   18.2349(4)
_cell_angle_alpha                99.017(2)
_cell_angle_beta                 91.928(2)
_cell_angle_gamma                99.224(3)
_cell_volume                     2867.36(16)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    15898
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      78.3730
_cell_measurement_theta_min      3.0770
_shelx_estimated_absorpt_T_max   0.946
_shelx_estimated_absorpt_T_min   0.605
_exptl_absorpt_coefficient_mu    2.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.84a (Rigaku Oxford Diffraction, 2023)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1212
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_exptl_crystal_size_rad          0.400
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            81559
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        65.089
_diffrn_reflns_theta_max         65.089
_diffrn_reflns_theta_min         3.102
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00  25.00   0.50    5.00    --  -47.37  96.00  41.00  208
  2  ω     -7.00  79.00   0.50    5.00    --   47.37 -96.00 -67.00  172
  3  ω   -163.00 -84.00   0.50   20.00    --  -91.75 -96.00 -67.00  158
  4  ω    -79.00 -19.00   0.50   20.00    --  -91.75  96.00  41.00  120
  5  ω    106.00 178.00   0.50   20.00    --  113.25  96.00  41.00  144
  6  ω     42.00 105.00   0.50   20.00    --  113.25 -96.00 -67.00  126
  7  ω    -14.00  29.00   0.50    5.00    --   18.00  96.00 146.64   86
  8  ω    -16.00  18.00   0.50    5.00    --   18.00 101.00  -6.65   68
  9  ω     -3.00  27.00   0.50    5.00    --   30.00  98.00-116.77   60
 10  ω      7.00  34.00   0.50    5.00    --   38.00  94.00  -1.52   54
 11  ω     14.00  43.00   0.50    5.00    --   42.00  88.00-139.66   58
 12  ω     14.00  43.00   0.50    5.00    --   42.00  88.00 108.05   58
 13  ω     14.00  43.00   0.50    5.00    --   42.00  89.00 -95.53   58
 14  ω     17.00  43.00   0.50    5.00    --   46.00  90.00 120.98   52
 15  ω     17.00  43.00   0.50    5.00    --   46.00  90.00-145.41   52
 16  ω   -120.00 -35.00   0.50    5.00    --  -47.37 -37.00 -60.00  170
 17  ω   -122.00 -35.00   0.50    5.00    --  -47.37 -19.00  60.00  174
 18  ω   -119.00 -25.00   0.50    5.00    --  -47.37 -77.00 -60.00  188
 19  ω   -122.00 -35.00   0.50    5.00    --  -47.37 -19.00 150.00  174
 20  ω   -122.00 -35.00   0.50    5.00    --  -47.37 -19.00   0.00  174
 21  ω    -24.00  62.00   0.50    5.00    --   47.37 -57.00 -60.00  172
 22  ω     25.00 120.00   0.50    5.00    --   47.37  77.00  60.00  190
 23  ω     32.00 126.00   0.50    5.00    --   54.00  76.00 -66.74  188
 24  ω     35.00 131.00   0.50    5.00    --   58.00  77.00-139.74  192
 25  ω     37.00  67.00   0.50    5.00    --   58.00  72.00 129.16   60
 26  ω     36.00  61.00   0.50    5.00    --   58.00  77.00   4.40   50
 27  ω     35.00  61.00   0.50    5.00    --   58.00  77.00  71.79   52
 28  ω    103.00 129.00   0.50    5.00    --   62.00  72.00  27.62   52
 29  ω     39.00  65.00   0.50    5.00    --   62.00  77.00 161.25   52
 30  ω     40.00  66.00   0.50    5.00    --   62.00  75.00 134.96   52
 31  ω     41.00  67.00   0.50    5.00    --   62.00  72.00  27.62   52
 32  ω     41.00  69.00   0.50    5.00    --   62.00  73.00  39.82   56
 33  ω     39.00  66.00   0.50    5.00    --   62.00  77.00 -26.23   54
 34  ω     44.00  69.00   0.50    5.00    --   66.00  77.00-101.72   50
 35  ω     45.00  70.00   0.50    5.00    --   66.00  76.00 -58.88   50
 36  ω     43.00  80.00   0.50    5.00    --   66.00  77.00-112.31   74
 37  ω    111.00 138.00   0.50    5.00    --   66.00  77.00-101.72   54
 38  ω     44.00  80.00   0.50    5.00    --   66.00  76.00 133.34   72
 39  ω    -78.00 -51.00   0.50   20.00    --  -70.00 -67.00-111.59   54
 40  ω     49.00  80.00   0.50    5.00    --   70.00  75.00-150.46   62
 41  ω    -76.00 -50.00   0.50   20.00    --  -70.00 -69.00  -1.55   52
 42  ω     47.00  73.00   0.50    5.00    --   70.00  77.00 166.10   52
 43  ω     48.00  73.00   0.50    5.00    --   70.00  77.00  55.36   50
 44  ω     47.00  74.00   0.50    5.00    --   70.00  77.00-171.69   54
 45  ω     49.00  75.00   0.50    5.00    --   70.00  74.00  84.96   52
 46  ω    -79.00 -53.00   0.50   20.00    --  -74.00 -73.00 -40.00   52
 47  ω   -145.00-110.00   0.50   20.00    --  -74.00 -73.00 -57.69   70
 48  ω    -79.00 -53.00   0.50   20.00    --  -74.00 -73.00 -57.69   52
 49  ω    -81.00 -55.00   0.50   20.00    --  -78.00 -77.00 -56.70   52
 50  ω    -81.00 -56.00   0.50   20.00    --  -78.00 -74.00 176.45   50
 51  ω   -140.00-115.00   0.50   20.00    --  -78.00 -74.00 176.45   50
 52  ω    -81.00 -55.00   0.50   20.00    --  -78.00 -77.00  -9.66   52
 53  ω    -83.00 -57.00   0.50   20.00    --  -78.00 -72.00  21.97   52
 54  ω    -84.00 -57.00   0.50   20.00    --  -78.00 -73.00-138.50   54
 55  ω    -81.00 -55.00   0.50   20.00    --  -78.00 -76.00  98.37   52
 56  ω    -88.00 -62.00   0.50   20.00    --  -82.00 -71.00  50.73   52
 57  ω    -86.00 -60.00   0.50   20.00    --  -82.00 -74.00-113.33   52
 58  ω    -90.00 -63.00   0.50   20.00    --  -82.00 -71.00 130.43   54
 59  ω    -86.00 -61.00   0.50   20.00    --  -82.00 -72.00 -66.45   50
 60  ω    -94.00 -62.00   0.50   20.00    --  -82.00 -69.00 -96.27   64
 61  ω    -88.00 -61.00   0.50   20.00    --  -82.00 -73.00 -74.44   54
 62  ω   -154.00-126.00   0.50   20.00    --  -82.00 -73.00 -74.44   56
 63  ω    -93.00 -66.00   0.50   20.00    --  -86.00 -70.00-101.04   54
 64  ω    -94.00 -68.00   0.50   20.00    --  -90.00 -74.00 132.57   52
 65  ω    -94.00 -69.00   0.50   20.00    --  -91.75 -77.00-150.00   50
 66  ω    -94.00 -69.00   0.50   20.00    --  -91.75 -76.00  43.23   50
 67  ω   -162.00-120.00   0.50   20.00    --  -91.75 -76.00  43.23   84
 68  ω    -94.00 -69.00   0.50   20.00    --  -91.75 -77.00  60.00   50
 69  ω    -99.00 -72.00   0.50   20.00    --  -91.75 -71.00-140.09   54
 70  ω   -163.00-114.00   0.50   20.00    --  -91.75 -77.00  60.00   98
 71  ω    -94.00 -69.00   0.50   20.00    --  -91.75 -77.00-120.00   50
 72  ω   -100.00 -73.00   0.50   20.00    --  -91.75 -66.00  68.69   54
 73  ω    -97.00 -71.00   0.50   20.00    --  -91.75 -71.00-172.71   52
 74  ω   -157.00-131.00   0.50   20.00    --  -91.75 -71.00-140.09   52
 75  ω   -162.00-137.00   0.50   20.00    --  -91.75 -71.00-172.71   50
 76  ω    -97.00 -70.00   0.50   20.00    --  -91.75 -77.00 -90.00   54
 77  ω    -99.00 -72.00   0.50   20.00    --  -91.75 -71.00  -1.73   54
 78  ω    -97.00 -71.00   0.50   20.00    --  -91.75 -73.00-178.78   52
 79  ω   -145.00-119.00   0.50   20.00    --  -91.75 -73.00-178.78   52
 80  ω    -95.00 -69.00   0.50   20.00    --  -91.75 -77.00  30.00   52
 81  ω    -96.00 -70.00   0.50   20.00    --  -91.75 -74.00  -7.31   52
 82  ω   -162.00-136.00   0.50   20.00    --  -91.75 -74.00  -7.31   52
 83  ω    -97.00 -70.00   0.50   20.00    --  -91.75 -75.00 168.39   54
 84  ω    -96.00 -70.00   0.50   20.00    --  -91.75 -74.00-148.67   52
 85  ω    -95.00 -70.00   0.50   20.00    --  -91.75 -75.00  10.88   50
 86  ω    -96.00 -70.00   0.50   20.00    --  -91.75 -74.00 154.64   52
 87  ω   -162.00-135.00   0.50   20.00    --  -91.75 -75.00  10.88   54
 88  ω   -100.00 -74.00   0.50   20.00    --  -91.75 -75.00 -36.09   52
 89  ω    -94.00 -69.00   0.50   20.00    --  -91.75 -77.00 -60.00   50
 90  ω    -96.00 -70.00   0.50   20.00    --  -91.75 -77.00 120.00   52
 91  ω    -95.00 -69.00   0.50   20.00    --  -91.75 -77.00  90.00   52
 92  ω   -162.00-125.00   0.50   20.00    --  -91.75 -75.00 -36.09   74
 93  ω    -96.00 -70.00   0.50   20.00    --  -91.75 -75.00 -20.02   52
 94  ω   -157.00-131.00   0.50   20.00    --  -91.75 -77.00 -60.00   52
 95  ω    -97.00 -71.00   0.50   20.00    --  -91.75 -72.00-109.70   52
 96  ω   -163.00-132.00   0.50   20.00    --  -91.75 -72.00-109.70   62
 97  ω    -97.00 -71.00   0.50   20.00    --  -91.75 -71.00  86.62   52
 98  ω    -97.00 -71.00   0.50   20.00    --  -91.75 -73.00  62.06   52
 99  ω   -108.00 -74.00   0.50   20.00    --  -91.75 -65.00  90.54   68
100  ω    116.00 178.00   0.50   20.00    --  113.25 125.00  60.00  124
101  ω     81.00 109.00   0.50   20.00    --  113.25-125.00-150.00   56
102  ω    150.00 177.00   0.50   20.00    --  113.25  77.00 -60.00   54
103  ω     43.00  78.00   0.50   20.00    --  113.25-125.00-150.00   70
104  ω     91.00 148.00   0.50   20.00    --  113.25  77.00 -60.00  114
105  ω     70.00 105.00   0.50   20.00    --  113.25 -94.00 150.00   70
106  ω    102.00 161.00   0.50   20.00    --  113.25  61.00 120.00  118
107  ω     99.00 177.00   0.50   20.00    --  113.25  61.00-180.00  156
108  ω     97.00 153.00   0.50   20.00    --  113.25  61.00 150.00  112
109  ω     42.00 106.00   0.50   20.00    --  113.25 -94.00   0.00  128
110  ω     42.00  68.00   0.50   20.00    --  113.25 -94.00 150.00   52
111  ω     42.00  96.00   0.50   20.00    --  113.25-125.00 -90.00  108
112  ω     43.00  88.00   0.50   20.00    --  113.25-125.00  60.00   90
113  ω     73.00 111.00   0.50   20.00    --  113.25-125.00-180.00   76
114  ω     42.00  69.00   0.50   20.00    --  113.25-125.00-180.00   54
115  ω     91.00 128.00   0.50   20.00    --  113.25  77.00  90.00   74
116  ω     99.00 171.00   0.50   20.00    --  113.25  61.00 -60.00  144
117  ω    146.00 176.00   0.50   20.00    --  113.25  77.00  30.00   60
118  ω     43.00 105.00   0.50   20.00    --  113.25 -94.00 -30.00  124
119  ω     96.00 138.00   0.50   20.00    --  113.25  77.00  30.00   84
120  ω     92.00 136.00   0.50   20.00    --  113.25  77.00-150.00   88
121  ω     91.00 119.00   0.50   20.00    --  113.25  77.00 -30.00   56
122  ω     73.00 106.00   0.50   20.00    --  113.25 -94.00-120.00   66
123  ω    153.00 178.00   0.50   20.00    --  113.25  77.00-120.00   50
124  ω    142.00 173.00   0.50   20.00    --  113.25  77.00 150.00   62
125  ω     42.00  72.00   0.50   20.00    --  113.25 -61.00-180.00   60
126  ω     43.00 106.00   0.50   20.00    --  113.25 -94.00 -90.00  126
127  ω     92.00 140.00   0.50   20.00    --  113.25  77.00-120.00   96
128  ω     43.00  72.00   0.50   20.00    --  113.25 -61.00  30.00   58
129  ω    105.00 133.00   0.50   20.00    --  113.25  61.00  60.00   56
130  ω     97.00 167.00   0.50   20.00    --  113.25  61.00-120.00  140
131  ω     98.00 171.00   0.50   20.00    --  113.25  61.00  90.00  146
132  ω     92.00 118.00   0.50   20.00    --  113.25  77.00 150.00   52
133  ω     98.00 176.00   0.50   20.00    --  113.25  61.00 -30.00  156
134  ω    135.00 170.00   0.50   20.00    --  113.25  61.00-150.00   70
135  ω    123.00 176.00   0.50   20.00    --  113.25  77.00  60.00  106
136  ω    100.00 131.00   0.50   20.00    --  113.25  61.00-150.00   62
137  ω     43.00 106.00   0.50   20.00    --  113.25 -94.00  90.00  126
138  ω     91.00 118.00   0.50   20.00    --  113.25  77.00  60.00   54
139  ω     47.00 105.00   0.50   20.00    --  113.25 -94.00-150.00  116
140  ω     91.00 133.00   0.50   20.00    --  113.25  77.00-180.00   84
141  ω     97.00 144.00   0.50   20.00    --  113.25  61.00 -90.00   94
142  ω    151.00 178.00   0.50   20.00    --  113.25  77.00   0.00   54
143  ω     91.00 140.00   0.50   20.00    --  113.25  77.00   0.00   98
144  ω     83.00 110.00   0.50   20.00    --  113.25-125.00  90.00   54
145  ω     42.00  68.00   0.50   20.00    --  113.25-125.00  90.00   52
146  ω     93.00 174.00   0.50   20.00    --  113.25  77.00 120.00  162
147  ω     97.00 168.00   0.50   20.00    --  113.25  61.00  30.00  142
148  ω     42.00  55.00   0.50   20.00    --  113.25-125.00 150.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7870
_reflns_number_total             9740
_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       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.84a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.973
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         9740
_refine_ls_number_restraints     44
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0749
_refine_ls_restrained_S_all      1.050
_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)+(0.1494P)²+3.9564P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2173
_refine_ls_wR_factor_ref         0.2319
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 Ca3-O2 \\sim Ca3-O20 \\sim Ca1-O22
 with sigma of 0.002
 O15-C13 \\sim O18-C57
 with sigma of 0.002
 O6-C13 \\sim O12-C57
 with sigma of 0.002
 Ca3-O15 \\sim Ca3-O15A
 with sigma of 0.02
 O15-C13 \\sim O15A-C13
 with sigma of 0.02
 O8-C1 \\sim O18-C57
 with sigma of 0.02
3. Rigid bond restraints
 O2, O20
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O15, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
O2 \\sim O20: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 2A
O20 \\sim O2: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
O15 \\sim O6: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004 within 2A
O25 \\sim O11 \\sim O24 \\sim O26 \\sim O27: within 2A with sigma of 0.002 and
sigma for terminal atoms of 0.004 within 2A
O15A \\sim O15 \\sim O6: within 2A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 2A
Uanis(O25) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O26) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O25) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27)
\\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 O15, O6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O15, O15A
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Others
 Sof(O15A)=1-FVAR(1)
 Sof(O15)=FVAR(1)
 Fixed Sof: O17(0.65) O9(0.5) O19(0.8) O5(0.35) O21(0.5) O11(0.5) O24(0.5)
 O25(0.5) O26(0.1) O27(0.5)
7.a Free rotating group:
 O3(H3A,H3B)
7.b Rotating group:
 O20(H20A,H20B), O22(H22A,H22B), O2(H2A,H2B)
7.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C26(H26), C30(H30), C34(H34), C38(H38), C40(H40),
 C46(H46), C48(H48), C52(H52), C29(H29), C31(H31), C33(H33), C17(H17), C35(H35),
  C9(H9), C19(H19), C39(H39), C41(H41), C21(H21), C43(H43), C11(H11), C45(H45),
 C23(H23), C47(H47), C49(H49), C25(H25), C51(H51), C53(H53), C55(H55)
7.d Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_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
Ca2 Ca 0.500000 0.500000 0.000000 0.0321(3) Uani 1 2 d S . P . .
Ca1 Ca 1.38280(7) 0.06600(6) 1.05421(4) 0.0324(2) Uani 1 1 d D . . . .
Ca3 Ca 0.50477(8) 0.32956(6) 0.11836(4) 0.0351(2) Uani 1 1 d D . . . .
O1 O 1.3659(3) 0.20970(19) 1.01594(14) 0.0347(6) Uani 1 1 d . . . . .
O4 O 1.5455(3) 0.0886(2) 0.96513(15) 0.0369(6) Uani 1 1 d . . . . .
O6 O 0.5084(3) 0.5187(2) 0.13229(14) 0.0403(7) Uani 1 1 d D . . . .
O8 O 1.3835(3) 0.36062(19) 1.01256(15) 0.0387(7) Uani 1 1 d D . . . .
O10 O 0.5753(3) 0.0691(2) 0.12325(15) 0.0415(7) Uani 1 1 d . . . . .
O12 O 1.3037(3) 0.0088(2) 0.16551(16) 0.0408(7) Uani 1 1 d D . . . .
O14 O 0.4987(3) 0.1943(2) 0.16812(16) 0.0417(7) Uani 1 1 d . . . . .
O16 O 0.6495(3) 0.4101(2) 1.01196(16) 0.0448(7) Uani 1 1 d . . . . .
O18 O 1.2128(3) 0.1153(2) 0.12302(15) 0.0416(7) Uani 1 1 d D . . . .
O20 O 0.2959(2) 0.3111(2) 0.15798(17) 0.0495(8) Uani 1 1 d D . . . .
H20A H 0.274861 0.255112 0.169129 0.074 Uiso 1 1 d R U . . .
H20B H 0.293268 0.348866 0.199709 0.074 Uiso 1 1 d R U . . .
O22 O 1.2367(3) -0.0287(2) 0.96020(16) 0.0475(8) Uani 1 1 d D . . . .
H22A H 1.204427 0.007998 0.934776 0.071 Uiso 1 1 d R U . . .
H22B H 1.175010 -0.056927 0.981183 0.071 Uiso 1 1 d R U . . .
O23 O 0.6456(3) 0.2660(2) 1.03230(18) 0.0502(8) Uani 1 1 d . . . . .
O3 O 1.5434(3) 0.1187(2) 0.81521(18) 0.0483(8) Uani 1 1 d G . . . .
H3A H 1.602866 0.087213 0.804679 0.072 Uiso 1 1 d G U . . .
H3B H 1.514629 0.099692 0.855076 0.072 Uiso 1 1 d G U . . .
O13 O 0.1986(4) 1.4136(3) 0.2864(2) 0.0659(10) Uani 1 1 d . . . . .
O7 O 0.1178(5) 1.4601(3) 0.3933(2) 0.0790(13) Uani 1 1 d . . . . .
H7 H 0.084836 1.493013 0.367322 0.118 Uiso 1 1 calc R U . . .
C1 C 1.3409(4) 0.2755(3) 0.9857(2) 0.0332(9) Uani 1 1 d D . . . .
C4 C 0.5248(4) 0.7563(3) 0.3713(2) 0.0369(9) Uani 1 1 d . . . . .
C6 C 1.1083(4) 0.2237(3) 0.7857(2) 0.0372(9) Uani 1 1 d . . . . .
C8 C 0.8507(4) 0.2587(3) 0.7909(2) 0.0379(9) Uani 1 1 d . . . . .
C10 C 0.9804(4) 0.1329(3) 0.4459(2) 0.0386(9) Uani 1 1 d . . . . .
C12 C 0.5286(4) 0.8405(3) 0.4300(2) 0.0375(9) Uani 1 1 d . . . . .
C14 C 0.8556(4) 0.2059(3) 0.8489(2) 0.0373(9) Uani 1 1 d . . . . .
H14 H 0.897488 0.153578 0.842813 0.045 Uiso 1 1 calc R U . . .
C16 C 1.2315(4) 0.1674(3) 0.8747(2) 0.0375(9) Uani 1 1 d . . . . .
H16 H 1.263878 0.117229 0.891205 0.045 Uiso 1 1 calc R U . . .
C18 C 0.4825(4) 0.9998(3) 0.4621(2) 0.0391(9) Uani 1 1 d . . . . .
C20 C 1.0008(4) 0.1659(3) 0.5814(2) 0.0384(9) Uani 1 1 d . . . . .
C22 C 0.6758(4) 0.3294(3) 0.9943(2) 0.0372(9) Uani 1 1 d . . . . .
C24 C 0.8811(4) 0.1914(3) 0.5836(2) 0.0420(10) Uani 1 1 d . . . . .
C26 C 1.1166(4) 0.0442(3) 0.3645(2) 0.0403(10) Uani 1 1 d . . . . .
H26 H 1.126154 0.007373 0.402213 0.048 Uiso 1 1 calc R U . . .
C28 C 1.2584(4) 0.2575(3) 0.9160(2) 0.0348(9) Uani 1 1 d . . . . .
C30 C 1.0451(4) 0.1357(3) 0.5123(2) 0.0398(10) Uani 1 1 d . . . . .
H30 H 1.123167 0.116212 0.511158 0.048 Uiso 1 1 calc R U . . .
C32 C 1.1640(4) 0.0815(3) 0.2436(2) 0.0391(10) Uani 1 1 d . . . . .
C34 C 0.5575(4) 0.6904(3) 0.2446(2) 0.0366(9) Uani 1 1 d . . . . .
H34 H 0.583404 0.699314 0.196749 0.044 Uiso 1 1 calc R U . . .
C36 C 0.7415(4) 0.3073(3) 0.9249(2) 0.0374(9) Uani 1 1 d . . . . .
C38 C 1.0701(4) 0.1756(3) 0.6497(2) 0.0395(10) Uani 1 1 d . . . . .
H38 H 1.149768 0.158855 0.649044 0.047 Uiso 1 1 calc R U . . .
C40 C 1.1365(4) 0.3143(3) 0.8280(2) 0.0403(10) Uani 1 1 d . . . . .
H40 H 1.103473 0.364554 0.812109 0.048 Uiso 1 1 calc R U . . .
C42 C 0.5669(4) 0.1355(3) 0.1754(2) 0.0386(9) Uani 1 1 d . . . . .
C44 C 0.4330(4) 1.1586(3) 0.4931(2) 0.0377(9) Uani 1 1 d . . . . .
C46 C 0.8361(4) 0.2219(3) 0.6537(2) 0.0403(10) Uani 1 1 d . . . . .
H46 H 0.755573 0.236845 0.655316 0.048 Uiso 1 1 calc R U . . .
C48 C 0.5654(4) 0.7672(3) 0.3013(2) 0.0363(9) Uani 1 1 d . . . . .
H48 H 0.599113 0.827975 0.291971 0.044 Uiso 1 1 calc R U . . .
C50 C 1.0414(4) 0.1131(3) 0.3752(2) 0.0395(10) Uani 1 1 d . . . . .
C52 C 1.1571(4) 0.1511(3) 0.8094(2) 0.0383(9) Uani 1 1 d . . . . .
H52 H 1.139646 0.089820 0.780857 0.046 Uiso 1 1 calc R U . . .
C54 C 1.0273(4) 0.2081(3) 0.7166(2) 0.0383(9) Uani 1 1 d . . . . .
C56 C 0.7801(4) 0.1500(3) 0.3793(2) 0.0403(10) Uani 1 1 d . . . . .
C57 C 1.2308(4) 0.0669(3) 0.1741(2) 0.0388(10) Uani 1 1 d D . . . .
C29 C 0.4403(4) 1.0788(3) 0.4424(2) 0.0417(10) Uani 1 1 d . . . . .
H29 H 0.415636 1.077529 0.391750 0.050 Uiso 1 1 calc R U . . .
C15 C 0.3804(4) 1.2342(3) 0.4645(2) 0.0413(10) Uani 1 1 d . . . . .
C31 C 1.0314(4) 0.1671(3) 0.3188(2) 0.0405(10) Uani 1 1 d . . . . .
H31 H 0.982790 0.215433 0.325396 0.049 Uiso 1 1 calc R U . . .
C2 C 0.9047(4) 0.2305(3) 0.7188(2) 0.0391(9) Uani 1 1 d . . . . .
O15 O 0.494(3) 0.4378(4) 0.2271(5) 0.064(4) Uani 0.59(5) 1 d D U P A 1
C33 C 0.7512(4) 0.0662(3) 0.3294(2) 0.0416(10) Uani 1 1 d . . . . .
H33 H 0.779552 0.011659 0.340565 0.050 Uiso 1 1 calc R U . . .
C17 C 1.0908(4) 0.1513(3) 0.2542(2) 0.0410(10) Uani 1 1 d . . . . .
H17 H 1.082015 0.188126 0.216501 0.049 Uiso 1 1 calc R U . . .
C35 C 0.7364(4) 0.2285(3) 0.3628(2) 0.0435(10) Uani 1 1 d . . . . .
H35 H 0.754378 0.285767 0.396765 0.052 Uiso 1 1 calc R U . . .
C9 C 0.8005(4) 0.2289(3) 0.9144(2) 0.0381(9) Uani 1 1 d . . . . .
H9 H 0.802688 0.191581 0.952436 0.046 Uiso 1 1 calc R U . . .
C37 C 0.8579(4) 0.1562(3) 0.4479(2) 0.0421(10) Uani 1 1 d . . . . .
C19 C 0.4739(4) 0.6669(3) 0.3831(2) 0.0432(10) Uani 1 1 d . . . . .
H19 H 0.442495 0.658653 0.429941 0.052 Uiso 1 1 calc R U . . .
C39 C 0.6814(4) 0.0612(3) 0.2636(2) 0.0391(9) Uani 1 1 d . . . . .
H39 H 0.662023 0.003645 0.230013 0.047 Uiso 1 1 calc R U . . .
C5 C 0.6405(4) 0.1406(3) 0.2475(2) 0.0378(9) Uani 1 1 d . . . . .
C41 C 0.8125(4) 0.1839(3) 0.5152(2) 0.0415(10) Uani 1 1 d . . . . .
H41 H 0.731786 0.198682 0.516064 0.050 Uiso 1 1 calc R U . . .
C21 C 1.2111(4) 0.3307(3) 0.8919(2) 0.0406(10) Uani 1 1 d . . . . .
H21 H 1.230548 0.392302 0.919730 0.049 Uiso 1 1 calc R U . . .
C43 C 1.1770(4) 0.0294(3) 0.2997(2) 0.0399(10) Uani 1 1 d . . . . .
H43 H 1.228135 -0.017322 0.293482 0.048 Uiso 1 1 calc R U . . .
C11 C 0.4893(4) 0.9177(3) 0.4102(2) 0.0397(10) Uani 1 1 d . . . . .
H11 H 0.465496 0.916379 0.359471 0.048 Uiso 1 1 calc R U . . .
C45 C 0.7387(4) 0.3611(3) 0.8692(2) 0.0432(10) Uani 1 1 d . . . . .
H45 H 0.700583 0.415308 0.876530 0.052 Uiso 1 1 calc R U . . .
C23 C 0.2944(4) 1.2826(3) 0.5019(3) 0.0438(10) Uani 1 1 d . . . . .
H23 H 0.276785 1.274071 0.551264 0.053 Uiso 1 1 calc R U . . .
C47 C 0.4685(5) 0.5898(3) 0.3275(2) 0.0481(11) Uani 1 1 d . . . . .
H47 H 0.435173 0.528956 0.336848 0.058 Uiso 1 1 calc R U . . .
C3 C 0.5120(5) 0.6011(3) 0.2577(2) 0.0430(10) Uani 1 1 d . . . . .
C49 C 0.7916(4) 0.3360(3) 0.8020(2) 0.0443(10) Uani 1 1 d . . . . .
H49 H 0.786976 0.372343 0.763438 0.053 Uiso 1 1 calc R U . . .
C25 C 0.6662(4) 0.2245(3) 0.2969(2) 0.0427(10) Uani 1 1 d . . . . .
H25 H 0.636448 0.278628 0.286089 0.051 Uiso 1 1 calc R U . . .
C51 C 0.4075(5) 1.2529(3) 0.3932(2) 0.0454(11) Uani 1 1 d . . . . .
H51 H 0.468318 1.223438 0.367808 0.054 Uiso 1 1 calc R U . . .
C13 C 0.5136(5) 0.5148(3) 0.2006(2) 0.0518(12) Uani 1 1 d D . . . .
C53 C 0.3497(5) 1.3119(4) 0.3592(3) 0.0488(11) Uani 1 1 d . . . . .
H53 H 0.370646 1.322971 0.310913 0.059 Uiso 1 1 calc R U . . .
C27 C 0.2604(5) 1.3558(4) 0.3948(3) 0.0502(11) Uani 1 1 d . . . . .
C55 C 0.2351(5) 1.3423(3) 0.4677(3) 0.0498(11) Uani 1 1 d . . . . .
H55 H 0.177014 1.374375 0.493605 0.060 Uiso 1 1 calc R U . . .
C7 C 0.1903(5) 1.4130(4) 0.3528(3) 0.0615(14) Uani 1 1 d . . . . .
O2 O 0.7112(3) 0.3695(5) 0.1766(3) 0.124(2) Uani 1 1 d D . . . .
H2A H 0.749335 0.321208 0.167379 0.186 Uiso 1 1 d R U . . .
H2B H 0.754699 0.412916 0.155746 0.186 Uiso 1 1 d R U . . .
O17 O 0.9996(7) 0.1282(5) 0.0418(4) 0.087(2) Uani 0.65 1 d . . P . .
O9 O 0.9785(7) 0.5479(6) 0.3205(6) 0.086(3) Uani 0.5 1 d . . P . .
O19 O 0.7345(8) 0.4792(6) 0.3300(5) 0.131(3) Uani 0.8 1 d . . P . .
O5 O 0.9813(9) 0.0052(9) 0.0742(6) 0.064(3) Uani 0.35 1 d . . P . .
O21 O 1.0772(12) 0.3233(9) 0.0655(7) 0.111(4) Uani 0.5 1 d . . P . .
O11 O 0.9500(17) 0.4430(15) 0.1339(11) 0.182(5) Uani 0.5 1 d . U P . .
O24 O 0.8595(18) 0.4457(12) 0.4513(9) 0.157(6) Uani 0.5 1 d . . P . .
O25 O 0.9307(17) 0.3268(15) 0.1193(12) 0.183(5) Uani 0.5 1 d . U P . .
O26 O 0.500000 0.500000 0.500000 0.16(2) Uani 0.2 2 d S U P . .
O27 O 0.906(2) 0.5276(14) 0.0201(12) 0.195(8) Uani 0.5 1 d . U P . .
O15A O 0.554(3) 0.4450(9) 0.2219(9) 0.053(6) Uani 0.41(5) 1 d D U P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca2 Ca3 3.5501(8) 2_665 ?
Ca2 Ca3 3.5501(8) . ?
Ca2 O6 2.382(2) . ?
Ca2 O6 2.382(2) 2_665 ?
Ca2 O8 2.279(3) 2_766 ?
Ca2 O8 2.279(3) 1_454 ?
Ca2 O16 2.295(3) 1_554 ?
Ca2 O16 2.295(3) 2_666 ?
Ca1 Ca1 3.8846(16) 2_857 ?
Ca1 Ca3 3.8563(11) 1_656 ?
Ca1 O1 2.349(3) . ?
Ca1 O4 2.480(3) . ?
Ca1 O4 2.493(3) 2_857 ?
Ca1 O10 2.424(3) 1_656 ?
Ca1 O12 2.450(3) 1_556 ?
Ca1 O14 2.703(3) 1_656 ?
Ca1 O18 2.435(3) 1_556 ?
Ca1 O22 2.411(2) . ?
Ca1 C42 2.895(4) 1_656 ?
Ca1 C57 2.800(4) 1_556 ?
Ca3 O1 2.614(3) 1_454 ?
Ca3 O6 2.733(3) . ?
Ca3 O8 2.453(3) 1_454 ?
Ca3 O14 2.296(3) . ?
Ca3 O16 2.833(3) 1_554 ?
Ca3 O20 2.427(2) . ?
Ca3 O23 2.432(3) 1_554 ?
Ca3 C1 2.898(4) 1_454 ?
Ca3 O15 2.354(9) . ?
Ca3 C13 2.870(5) . ?
Ca3 O2 2.425(3) . ?
Ca3 O15A 2.314(10) . ?
O1 C1 1.245(5) . ?
O6 C13 1.257(4) . ?
O8 C1 1.272(5) . ?
O10 C42 1.265(5) . ?
O12 C57 1.257(4) . ?
O14 C42 1.250(5) . ?
O16 C22 1.257(5) . ?
O18 C57 1.284(4) . ?
O20 H20A 0.8719 . ?
O20 H20B 0.8718 . ?
O22 H22A 0.8709 . ?
O22 H22B 0.8711 . ?
O23 C22 1.252(5) . ?
O3 H3A 0.8700 . ?
O3 H3B 0.8703 . ?
O13 C7 1.218(7) . ?
O7 H7 0.8400 . ?
O7 C7 1.311(7) . ?
C1 C28 1.502(6) . ?
C4 C12 1.493(6) . ?
C4 C48 1.392(6) . ?
C4 C19 1.391(6) . ?
C6 C40 1.408(6) . ?
C6 C52 1.384(6) . ?
C6 C54 1.486(6) . ?
C8 C14 1.410(6) . ?
C8 C2 1.488(6) . ?
C8 C49 1.386(6) . ?
C10 C30 1.377(6) . ?
C10 C50 1.485(6) . ?
C10 C37 1.447(6) . ?
C12 C44 1.449(6) 2_676 ?
C12 C11 1.366(6) . ?
C14 H14 0.9500 . ?
C14 C9 1.377(6) . ?
C16 H16 0.9500 . ?
C16 C28 1.393(6) . ?
C16 C52 1.391(6) . ?
C18 C18 1.423(8) 2_676 ?
C18 C29 1.405(7) . ?
C18 C11 1.422(6) . ?
C20 C24 1.429(6) . ?
C20 C30 1.400(6) . ?
C20 C38 1.416(6) . ?
C22 C36 1.496(6) . ?
C24 C46 1.420(6) . ?
C24 C41 1.418(6) . ?
C26 H26 0.9500 . ?
C26 C50 1.401(7) . ?
C26 C43 1.381(6) . ?
C28 C21 1.387(6) . ?
C30 H30 0.9500 . ?
C32 C57 1.492(6) . ?
C32 C17 1.394(6) . ?
C32 C43 1.386(6) . ?
C34 H34 0.9500 . ?
C34 C48 1.391(6) . ?
C34 C3 1.382(6) . ?
C36 C9 1.399(6) . ?
C36 C45 1.382(6) . ?
C38 H38 0.9500 . ?
C38 C54 1.366(6) . ?
C40 H40 0.9500 . ?
C40 C21 1.371(6) . ?
C42 C5 1.507(6) . ?
C44 C29 1.386(6) . ?
C44 C15 1.482(7) . ?
C46 H46 0.9500 . ?
C46 C2 1.364(6) . ?
C48 H48 0.9500 . ?
C50 C31 1.403(6) . ?
C52 H52 0.9500 . ?
C54 C2 1.443(6) . ?
C56 C33 1.392(6) . ?
C56 C35 1.385(7) . ?
C56 C37 1.476(6) . ?
C29 H29 0.9500 . ?
C15 C23 1.405(7) . ?
C15 C51 1.402(6) . ?
C31 H31 0.9500 . ?
C31 C17 1.373(6) . ?
O15 C13 1.284(5) . ?
C33 H33 0.9500 . ?
C33 C39 1.390(6) . ?
C17 H17 0.9500 . ?
C35 H35 0.9500 . ?
C35 C25 1.395(6) . ?
C9 H9 0.9500 . ?
C37 C41 1.368(6) . ?
C19 H19 0.9500 . ?
C19 C47 1.386(6) . ?
C39 H39 0.9500 . ?
C39 C5 1.381(6) . ?
C5 C25 1.388(6) . ?
C41 H41 0.9500 . ?
C21 H21 0.9500 . ?
C43 H43 0.9500 . ?
C11 H11 0.9500 . ?
C45 H45 0.9500 . ?
C45 C49 1.398(6) . ?
C23 H23 0.9500 . ?
C23 C55 1.381(7) . ?
C47 H47 0.9500 . ?
C47 C3 1.400(6) . ?
C3 C13 1.509(6) . ?
C49 H49 0.9500 . ?
C25 H25 0.9500 . ?
C51 H51 0.9500 . ?
C51 C53 1.362(7) . ?
C13 O15A 1.286(11) . ?
C53 H53 0.9500 . ?
C53 C27 1.387(7) . ?
C27 C55 1.405(7) . ?
C27 C7 1.501(8) . ?
C55 H55 0.9500 . ?
O2 H2A 0.8768 . ?
O2 H2B 0.8768 . ?

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
Ca3 Ca2 Ca3 180.0 . 2_665 ?
O6 Ca2 Ca3 50.27(7) 2_665 2_665 ?
O6 Ca2 Ca3 129.73(7) . 2_665 ?
O6 Ca2 Ca3 50.28(7) . . ?
O6 Ca2 Ca3 129.73(7) 2_665 . ?
O6 Ca2 O6 180.0 2_665 . ?
O8 Ca2 Ca3 136.71(7) 1_454 2_665 ?
O8 Ca2 Ca3 136.71(7) 2_766 . ?
O8 Ca2 Ca3 43.29(7) 1_454 . ?
O8 Ca2 Ca3 43.29(7) 2_766 2_665 ?
O8 Ca2 O6 98.77(10) 1_454 2_665 ?
O8 Ca2 O6 81.23(10) 1_454 . ?
O8 Ca2 O6 81.23(10) 2_766 2_665 ?
O8 Ca2 O6 98.77(10) 2_766 . ?
O8 Ca2 O8 180.0 2_766 1_454 ?
O8 Ca2 O16 79.07(11) 1_454 1_554 ?
O8 Ca2 O16 100.93(11) 1_454 2_666 ?
O8 Ca2 O16 79.07(11) 2_766 2_666 ?
O8 Ca2 O16 100.93(11) 2_766 1_554 ?
O16 Ca2 Ca3 52.85(8) 2_666 2_665 ?
O16 Ca2 Ca3 127.15(8) 1_554 2_665 ?
O16 Ca2 Ca3 127.16(8) 2_666 . ?
O16 Ca2 Ca3 52.84(8) 1_554 . ?
O16 Ca2 O6 83.48(10) 2_666 2_665 ?
O16 Ca2 O6 96.52(10) 1_554 2_665 ?
O16 Ca2 O6 83.48(10) 1_554 . ?
O16 Ca2 O6 96.52(10) 2_666 . ?
O16 Ca2 O16 180.00(14) 2_666 1_554 ?
Ca3 Ca1 Ca1 113.29(3) 1_656 2_857 ?
O1 Ca1 Ca1 113.28(8) . 2_857 ?
O1 Ca1 Ca3 41.57(7) . 1_656 ?
O1 Ca1 O4 75.05(10) . . ?
O1 Ca1 O4 150.72(10) . 2_857 ?
O1 Ca1 O10 113.24(11) . 1_656 ?
O1 Ca1 O12 127.60(10) . 1_556 ?
O1 Ca1 O14 76.82(9) . 1_656 ?
O1 Ca1 O18 77.12(10) . 1_556 ?
O1 Ca1 O22 95.57(11) . . ?
O1 Ca1 C42 98.40(11) . 1_656 ?
O1 Ca1 C57 101.96(11) . 1_556 ?
O4 Ca1 Ca1 38.51(7) 2_857 2_857 ?
O4 Ca1 Ca1 38.75(7) . 2_857 ?
O4 Ca1 Ca3 140.90(7) 2_857 1_656 ?
O4 Ca1 Ca3 80.74(7) . 1_656 ?
O4 Ca1 O4 77.26(11) . 2_857 ?
O4 Ca1 O14 96.41(10) . 1_656 ?
O4 Ca1 O14 115.88(9) 2_857 1_656 ?
O4 Ca1 C42 90.44(11) 2_857 1_656 ?
O4 Ca1 C42 89.05(11) . 1_656 ?
O4 Ca1 C57 107.01(11) 2_857 1_556 ?
O4 Ca1 C57 168.75(12) . 1_556 ?
O10 Ca1 Ca1 64.92(7) 1_656 2_857 ?
O10 Ca1 Ca3 75.90(8) 1_656 1_656 ?
O10 Ca1 O4 74.08(10) 1_656 . ?
O10 Ca1 O4 67.19(10) 1_656 2_857 ?
O10 Ca1 O12 80.36(10) 1_656 1_556 ?
O10 Ca1 O14 50.32(10) 1_656 1_656 ?
O10 Ca1 O18 118.01(10) 1_656 1_556 ?
O10 Ca1 C42 25.62(11) 1_656 1_656 ?
O10 Ca1 C57 97.71(11) 1_656 1_556 ?
O12 Ca1 Ca1 117.96(7) 1_556 2_857 ?
O12 Ca1 Ca3 104.97(7) 1_556 1_656 ?
O12 Ca1 O4 81.68(9) 1_556 2_857 ?
O12 Ca1 O4 151.64(10) 1_556 . ?
O12 Ca1 O14 75.92(10) 1_556 1_656 ?
O12 Ca1 C42 72.22(11) 1_556 1_656 ?
O12 Ca1 C57 26.64(9) 1_556 1_556 ?
O14 Ca1 Ca1 110.57(7) 1_656 2_857 ?
O14 Ca1 Ca3 35.80(6) 1_656 1_656 ?
O14 Ca1 C42 25.51(11) 1_656 1_656 ?
O14 Ca1 C57 72.34(11) 1_656 1_556 ?
O18 Ca1 Ca1 167.81(9) 1_556 2_857 ?
O18 Ca1 Ca3 78.62(8) 1_556 1_656 ?
O18 Ca1 O4 130.05(10) 1_556 2_857 ?
O18 Ca1 O4 152.18(10) 1_556 . ?
O18 Ca1 O12 53.68(9) 1_556 1_556 ?
O18 Ca1 O14 77.28(10) 1_556 1_656 ?
O18 Ca1 C42 95.17(11) 1_556 1_656 ?
O18 Ca1 C57 27.26(10) 1_556 1_556 ?
O22 Ca1 Ca1 83.51(8) . 2_857 ?
O22 Ca1 Ca3 136.95(9) . 1_656 ?
O22 Ca1 O4 93.22(11) . . ?
O22 Ca1 O4 76.58(11) . 2_857 ?
O22 Ca1 O10 143.35(11) . 1_656 ?
O22 Ca1 O12 100.19(11) . 1_556 ?
O22 Ca1 O14 165.69(11) . 1_656 ?
O22 Ca1 O18 89.28(11) . 1_556 ?
O22 Ca1 C42 165.96(13) . 1_656 ?
O22 Ca1 C57 97.90(12) . 1_556 ?
C42 Ca1 Ca1 89.68(9) 1_656 2_857 ?
C42 Ca1 Ca3 57.09(9) 1_656 1_656 ?
C57 Ca1 Ca1 144.47(9) 1_556 2_857 ?
C57 Ca1 Ca3 89.87(9) 1_556 1_656 ?
C57 Ca1 C42 80.60(12) 1_556 1_656 ?
O1 Ca3 O6 122.16(9) 1_454 . ?
O1 Ca3 O16 92.65(9) 1_454 1_554 ?
O1 Ca3 C1 25.44(10) 1_454 1_454 ?
O1 Ca3 C13 139.70(12) 1_454 . ?
O6 Ca3 O16 68.02(9) . 1_554 ?
O6 Ca3 C1 97.02(10) . 1_454 ?
O6 Ca3 C13 25.77(8) . . ?
O8 Ca3 O1 51.25(9) 1_454 1_454 ?
O8 Ca3 O6 71.40(9) 1_454 . ?
O8 Ca3 O16 66.38(9) 1_454 1_554 ?
O8 Ca3 C1 25.82(10) 1_454 1_454 ?
O8 Ca3 C13 93.52(11) 1_454 . ?
O14 Ca3 O1 79.56(10) . 1_454 ?
O14 Ca3 O6 151.68(10) . . ?
O14 Ca3 O8 129.82(10) . 1_454 ?
O14 Ca3 O16 133.81(10) . 1_554 ?
O14 Ca3 O20 80.23(11) . . ?
O14 Ca3 O23 86.01(11) . 1_554 ?
O14 Ca3 C1 104.62(11) . 1_454 ?
O14 Ca3 O15 100.11(19) . . ?
O14 Ca3 C13 125.96(11) . . ?
O14 Ca3 O2 84.22(18) . . ?
O14 Ca3 O15A 102.4(4) . . ?
O16 Ca3 C1 78.55(10) 1_554 1_454 ?
O16 Ca3 C13 88.61(11) 1_554 . ?
O20 Ca3 O1 72.02(10) . 1_454 ?
O20 Ca3 O6 89.27(11) . . ?
O20 Ca3 O8 76.08(11) . 1_454 ?
O20 Ca3 O16 140.52(10) . 1_554 ?
O20 Ca3 O23 145.55(12) . 1_554 ?
O20 Ca3 C1 72.51(11) . 1_454 ?
O20 Ca3 C13 81.71(14) . . ?
O23 Ca3 O1 74.51(11) 1_554 1_454 ?
O23 Ca3 O6 115.73(10) 1_554 . ?
O23 Ca3 O8 89.32(11) 1_554 1_454 ?
O23 Ca3 O16 48.43(10) 1_554 1_554 ?
O23 Ca3 C1 80.80(12) 1_554 1_454 ?
O23 Ca3 C13 130.91(14) 1_554 . ?
O15 Ca3 O1 141.9(7) . 1_454 ?
O15 Ca3 O6 51.59(16) . . ?
O15 Ca3 O8 112.2(5) . 1_454 ?
O15 Ca3 O16 112.5(4) . 1_554 ?
O15 Ca3 O20 70.5(7) . . ?
O15 Ca3 O23 143.5(7) . 1_554 ?
O15 Ca3 C1 130.6(7) . 1_454 ?
O15 Ca3 C13 26.14(13) . . ?
O15 Ca3 O2 73.6(8) . . ?
C13 Ca3 C1 117.47(13) . 1_454 ?
O2 Ca3 O1 142.9(2) . 1_454 ?
O2 Ca3 O6 86.0(2) . . ?
O2 Ca3 O8 140.32(17) . 1_454 ?
O2 Ca3 O16 75.11(16) . 1_554 ?
O2 Ca3 O20 137.35(17) . . ?
O2 Ca3 O23 71.28(19) . 1_554 ?
O2 Ca3 C1 150.13(17) . 1_454 ?
O2 Ca3 C13 75.9(2) . . ?
O15A Ca3 O6 50.4(3) . . ?
O15A Ca3 O20 86.8(10) . . ?
O15A Ca3 C13 26.0(3) . . ?
O15A Ca3 O2 58.3(9) . . ?
Ca1 O1 Ca3 101.82(10) . 1_656 ?
C1 O1 Ca1 168.0(3) . . ?
C1 O1 Ca3 90.1(2) . 1_656 ?
Ca1 O4 Ca1 102.74(11) . 2_857 ?
Ca2 O6 Ca3 87.63(9) . . ?
C13 O6 Ca2 170.9(3) . . ?
C13 O6 Ca3 83.2(3) . . ?
Ca2 O8 Ca3 97.15(10) 1_656 1_656 ?
C1 O8 Ca2 149.4(3) . 1_656 ?
C1 O8 Ca3 97.0(2) . 1_656 ?
C42 O10 Ca1 98.5(3) . 1_454 ?
C57 O12 Ca1 92.4(2) . 1_554 ?
Ca3 O14 Ca1 100.66(10) . 1_454 ?
C42 O14 Ca1 85.9(2) . 1_454 ?
C42 O14 Ca3 138.3(3) . . ?
Ca2 O16 Ca3 86.95(10) 1_556 1_556 ?
C22 O16 Ca2 143.7(3) . 1_556 ?
C22 O16 Ca3 84.9(3) . 1_556 ?
C57 O18 Ca1 92.4(2) . 1_554 ?
Ca3 O20 H20A 109.7 . . ?
Ca3 O20 H20B 109.3 . . ?
H20A O20 H20B 104.4 . . ?
Ca1 O22 H22A 109.0 . . ?
Ca1 O22 H22B 109.8 . . ?
H22A O22 H22B 104.4 . . ?
C22 O23 Ca3 104.1(3) . 1_556 ?
H3A O3 H3B 104.4 . . ?
C7 O7 H7 109.5 . . ?
O1 C1 Ca3 64.4(2) . 1_656 ?
O1 C1 O8 121.6(4) . . ?
O1 C1 C28 121.2(4) . . ?
O8 C1 Ca3 57.1(2) . 1_656 ?
O8 C1 C28 117.3(4) . . ?
C28 C1 Ca3 174.4(3) . 1_656 ?
C48 C4 C12 119.8(4) . . ?
C19 C4 C12 121.6(4) . . ?
C19 C4 C48 118.4(4) . . ?
C40 C6 C54 119.3(4) . . ?
C52 C6 C40 119.2(4) . . ?
C52 C6 C54 121.5(4) . . ?
C14 C8 C2 120.8(4) . . ?
C49 C8 C14 118.3(4) . . ?
C49 C8 C2 120.9(4) . . ?
C30 C10 C50 119.2(4) . . ?
C30 C10 C37 118.5(4) . . ?
C37 C10 C50 122.2(4) . . ?
C44 C12 C4 122.4(4) 2_676 . ?
C11 C12 C4 118.1(4) . . ?
C11 C12 C44 119.4(4) . 2_676 ?
C8 C14 H14 119.5 . . ?
C9 C14 C8 121.0(4) . . ?
C9 C14 H14 119.5 . . ?
C28 C16 H16 120.1 . . ?
C52 C16 H16 120.1 . . ?
C52 C16 C28 119.8(4) . . ?
C29 C18 C18 118.9(5) . 2_676 ?
C29 C18 C11 123.4(4) . . ?
C11 C18 C18 117.7(5) . 2_676 ?
C30 C20 C24 118.8(4) . . ?
C30 C20 C38 123.3(4) . . ?
C38 C20 C24 117.9(4) . . ?
O16 C22 Ca3 70.4(2) . 1_556 ?
O16 C22 C36 119.3(4) . . ?
O23 C22 Ca3 51.9(2) . 1_556 ?
O23 C22 O16 121.6(4) . . ?
O23 C22 C36 119.0(4) . . ?
C36 C22 Ca3 166.1(3) . 1_556 ?
C46 C24 C20 118.8(4) . . ?
C41 C24 C20 118.1(4) . . ?
C41 C24 C46 123.2(4) . . ?
C50 C26 H26 119.8 . . ?
C43 C26 H26 119.8 . . ?
C43 C26 C50 120.5(4) . . ?
C16 C28 C1 119.8(4) . . ?
C21 C28 C1 120.1(4) . . ?
C21 C28 C16 120.1(4) . . ?
C10 C30 C20 122.8(4) . . ?
C10 C30 H30 118.6 . . ?
C20 C30 H30 118.6 . . ?
C17 C32 C57 120.0(4) . . ?
C43 C32 C57 121.1(4) . . ?
C43 C32 C17 118.8(4) . . ?
C48 C34 H34 119.8 . . ?
C3 C34 H34 119.8 . . ?
C3 C34 C48 120.3(4) . . ?
C9 C36 C22 120.1(4) . . ?
C45 C36 C22 120.3(4) . . ?
C45 C36 C9 119.5(4) . . ?
C20 C38 H38 118.6 . . ?
C54 C38 C20 122.7(4) . . ?
C54 C38 H38 118.6 . . ?
C6 C40 H40 119.7 . . ?
C21 C40 C6 120.5(4) . . ?
C21 C40 H40 119.7 . . ?
O10 C42 Ca1 55.9(2) . 1_454 ?
O10 C42 C5 117.8(4) . . ?
O14 C42 Ca1 68.6(2) . 1_454 ?
O14 C42 O10 121.5(4) . . ?
O14 C42 C5 120.8(4) . . ?
C5 C42 Ca1 159.7(3) . 1_454 ?
C12 C44 C15 125.4(4) 2_676 . ?
C29 C44 C12 117.6(4) . 2_676 ?
C29 C44 C15 116.9(4) . . ?
C24 C46 H46 118.9 . . ?
C2 C46 C24 122.2(4) . . ?
C2 C46 H46 118.9 . . ?
C4 C48 H48 119.5 . . ?
C34 C48 C4 120.9(4) . . ?
C34 C48 H48 119.5 . . ?
C26 C50 C10 121.2(4) . . ?
C26 C50 C31 118.0(4) . . ?
C31 C50 C10 120.7(4) . . ?
C6 C52 C16 120.3(4) . . ?
C6 C52 H52 119.9 . . ?
C16 C52 H52 119.9 . . ?
C38 C54 C6 120.1(4) . . ?
C38 C54 C2 119.2(4) . . ?
C2 C54 C6 120.6(4) . . ?
C33 C56 C37 120.9(4) . . ?
C35 C56 C33 118.8(4) . . ?
C35 C56 C37 120.3(4) . . ?
O12 C57 Ca1 60.9(2) . 1_554 ?
O12 C57 O18 120.5(4) . . ?
O12 C57 C32 121.0(4) . . ?
O18 C57 Ca1 60.3(2) . 1_554 ?
O18 C57 C32 118.5(3) . . ?
C32 C57 Ca1 170.6(3) . 1_554 ?
C18 C29 H29 118.4 . . ?
C44 C29 C18 123.3(4) . . ?
C44 C29 H29 118.4 . . ?
C23 C15 C44 123.5(4) . . ?
C51 C15 C44 118.9(4) . . ?
C51 C15 C23 117.3(4) . . ?
C50 C31 H31 119.5 . . ?
C17 C31 C50 121.1(4) . . ?
C17 C31 H31 119.5 . . ?
C46 C2 C8 119.8(4) . . ?
C46 C2 C54 119.1(4) . . ?
C54 C2 C8 121.0(4) . . ?
C13 O15 Ca3 100.0(5) . . ?
C56 C33 H33 119.6 . . ?
C39 C33 C56 120.9(4) . . ?
C39 C33 H33 119.6 . . ?
C32 C17 H17 119.7 . . ?
C31 C17 C32 120.6(4) . . ?
C31 C17 H17 119.7 . . ?
C56 C35 H35 119.5 . . ?
C56 C35 C25 120.9(4) . . ?
C25 C35 H35 119.5 . . ?
C14 C9 C36 120.1(4) . . ?
C14 C9 H9 120.0 . . ?
C36 C9 H9 120.0 . . ?
C10 C37 C56 121.8(4) . . ?
C41 C37 C10 119.2(4) . . ?
C41 C37 C56 119.0(4) . . ?
C4 C19 H19 119.6 . . ?
C47 C19 C4 120.9(4) . . ?
C47 C19 H19 119.6 . . ?
C33 C39 H39 120.3 . . ?
C5 C39 C33 119.5(4) . . ?
C5 C39 H39 120.3 . . ?
C39 C5 C42 119.4(4) . . ?
C39 C5 C25 120.6(4) . . ?
C25 C5 C42 120.0(4) . . ?
C24 C41 H41 118.7 . . ?
C37 C41 C24 122.5(4) . . ?
C37 C41 H41 118.7 . . ?
C28 C21 H21 120.0 . . ?
C40 C21 C28 120.0(4) . . ?
C40 C21 H21 120.0 . . ?
C26 C43 C32 121.0(4) . . ?
C26 C43 H43 119.5 . . ?
C32 C43 H43 119.5 . . ?
C12 C11 C18 123.1(4) . . ?
C12 C11 H11 118.5 . . ?
C18 C11 H11 118.5 . . ?
C36 C45 H45 119.8 . . ?
C36 C45 C49 120.3(4) . . ?
C49 C45 H45 119.8 . . ?
C15 C23 H23 119.6 . . ?
C55 C23 C15 120.8(4) . . ?
C55 C23 H23 119.6 . . ?
C19 C47 H47 119.9 . . ?
C19 C47 C3 120.2(4) . . ?
C3 C47 H47 119.9 . . ?
C34 C3 C47 119.1(4) . . ?
C34 C3 C13 122.2(4) . . ?
C47 C3 C13 118.7(4) . . ?
C8 C49 C45 120.8(4) . . ?
C8 C49 H49 119.6 . . ?
C45 C49 H49 119.6 . . ?
C35 C25 H25 120.4 . . ?
C5 C25 C35 119.2(4) . . ?
C5 C25 H25 120.4 . . ?
C15 C51 H51 118.9 . . ?
C53 C51 C15 122.2(5) . . ?
C53 C51 H51 118.9 . . ?
O6 C13 Ca3 71.0(2) . . ?
O6 C13 O15 123.6(6) . . ?
O6 C13 C3 120.9(4) . . ?
O6 C13 O15A 118.2(10) . . ?
O15 C13 Ca3 53.9(4) . . ?
O15 C13 C3 113.8(5) . . ?
C3 C13 Ca3 167.7(3) . . ?
O15A C13 Ca3 52.1(5) . . ?
O15A C13 C3 118.1(6) . . ?
C51 C53 H53 119.8 . . ?
C51 C53 C27 120.3(5) . . ?
C27 C53 H53 119.8 . . ?
C53 C27 C55 119.0(5) . . ?
C53 C27 C7 118.7(5) . . ?
C55 C27 C7 122.3(5) . . ?
C23 C55 C27 120.3(5) . . ?
C23 C55 H55 119.8 . . ?
C27 C55 H55 119.8 . . ?
O13 C7 O7 123.2(5) . . ?
O13 C7 C27 122.5(5) . . ?
O7 C7 C27 114.2(5) . . ?
Ca3 O2 H2A 109.8 . . ?
Ca3 O2 H2B 110.0 . . ?
H2A O2 H2B 104.2 . . ?
C13 O15A Ca3 101.9(6) . . ?

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
Ca2 O8 C1 Ca3 117.0(5) 1_656 . . 1_656 ?
Ca2 O8 C1 O1 118.2(5) 1_656 . . . ?
Ca2 O8 C1 C28 -62.0(7) 1_656 . . . ?
Ca2 O16 C22 Ca3 -77.7(4) 1_556 . . 1_556 ?
Ca2 O16 C22 O23 -86.8(6) 1_556 . . . ?
Ca2 O16 C22 C36 91.4(6) 1_556 . . . ?
Ca1 O1 C1 Ca3 174.3(13) . . . 1_656 ?
Ca1 O1 C1 O8 173.2(10) . . . . ?
Ca1 O1 C1 C28 -6.5(15) . . . . ?
Ca1 O10 C42 O14 -21.6(4) 1_454 . . . ?
Ca1 O10 C42 C5 157.4(3) 1_454 . . . ?
Ca1 O12 C57 O18 10.3(4) 1_554 . . . ?
Ca1 O12 C57 C32 -169.4(4) 1_554 . . . ?
Ca1 O14 C42 O10 19.2(4) 1_454 . . . ?
Ca1 O14 C42 C5 -159.9(4) 1_454 . . . ?
Ca1 O18 C57 O12 -10.4(4) 1_554 . . . ?
Ca1 O18 C57 C32 169.3(3) 1_554 . . . ?
Ca1 C42 C5 C39 45.9(10) 1_454 . . . ?
Ca1 C42 C5 C25 -133.9(8) 1_454 . . . ?
Ca3 O1 C1 O8 -1.1(4) 1_656 . . . ?
Ca3 O1 C1 C28 179.2(3) 1_656 . . . ?
Ca3 O6 C13 O15 -11.9(17) . . . . ?
Ca3 O6 C13 C3 -176.6(5) . . . . ?
Ca3 O6 C13 O15A 22.7(18) . . . . ?
Ca3 O8 C1 O1 1.1(4) 1_656 . . . ?
Ca3 O8 C1 C28 -179.1(3) 1_656 . . . ?
Ca3 O14 C42 Ca1 -101.4(4) . . . 1_454 ?
Ca3 O14 C42 O10 -82.2(6) . . . . ?
Ca3 O14 C42 C5 98.7(5) . . . . ?
Ca3 O16 C22 O23 -9.1(4) 1_556 . . . ?
Ca3 O16 C22 C36 169.1(4) 1_556 . . . ?
Ca3 O23 C22 O16 10.9(5) 1_556 . . . ?
Ca3 O23 C22 C36 -167.4(3) 1_556 . . . ?
Ca3 C22 C36 C9 -65.0(14) 1_556 . . . ?
Ca3 C22 C36 C45 111.4(12) 1_556 . . . ?
Ca3 O15 C13 O6 13.9(19) . . . . ?
Ca3 O15 C13 C3 179.6(5) . . . . ?
O1 C1 C28 C16 -14.7(6) . . . . ?
O1 C1 C28 C21 166.6(4) . . . . ?
O6 C13 O15A Ca3 -27(2) . . . . ?
O8 C1 C28 C16 165.5(4) . . . . ?
O8 C1 C28 C21 -13.2(6) . . . . ?
O10 C42 C5 C39 -20.5(6) . . . . ?
O10 C42 C5 C25 159.7(4) . . . . ?
O14 C42 C5 C39 158.6(4) . . . . ?
O14 C42 C5 C25 -21.3(6) . . . . ?
O16 C22 C36 C9 162.7(4) . . . . ?
O16 C22 C36 C45 -20.9(6) . . . . ?
O23 C22 C36 C9 -19.1(6) . . . . ?
O23 C22 C36 C45 157.4(4) . . . . ?
C1 C28 C21 C40 179.6(4) . . . . ?
C4 C12 C11 C18 176.4(4) . . . . ?
C4 C19 C47 C3 -1.4(8) . . . . ?
C6 C40 C21 C28 -0.8(7) . . . . ?
C6 C54 C2 C8 -7.5(7) . . . . ?
C6 C54 C2 C46 175.2(4) . . . . ?
C8 C14 C9 C36 -1.8(6) . . . . ?
C10 C50 C31 C17 177.9(4) . . . . ?
C10 C37 C41 C24 0.4(7) . . . . ?
C12 C4 C48 C34 -177.0(4) . . . . ?
C12 C4 C19 C47 178.5(4) . . . . ?
C12 C44 C29 C18 0.2(7) 2_676 . . . ?
C12 C44 C15 C23 -41.0(7) 2_676 . . . ?
C12 C44 C15 C51 145.6(5) 2_676 . . . ?
C14 C8 C2 C46 128.8(5) . . . . ?
C14 C8 C2 C54 -48.5(6) . . . . ?
C14 C8 C49 C45 0.3(7) . . . . ?
C16 C28 C21 C40 0.9(7) . . . . ?
C18 C18 C29 C44 1.2(8) 2_676 . . . ?
C18 C18 C11 C12 -0.5(8) 2_676 . . . ?
C20 C24 C46 C2 2.1(7) . . . . ?
C20 C24 C41 C37 -2.0(7) . . . . ?
C20 C38 C54 C6 -175.2(4) . . . . ?
C20 C38 C54 C2 2.3(7) . . . . ?
C22 C36 C9 C14 176.6(4) . . . . ?
C22 C36 C45 C49 -174.8(4) . . . . ?
C24 C20 C30 C10 2.7(7) . . . . ?
C24 C20 C38 C54 -0.1(7) . . . . ?
C24 C46 C2 C8 -177.2(4) . . . . ?
C24 C46 C2 C54 0.1(7) . . . . ?
C26 C50 C31 C17 1.7(7) . . . . ?
C28 C16 C52 C6 -0.9(6) . . . . ?
C30 C10 C50 C26 41.6(6) . . . . ?
C30 C10 C50 C31 -134.4(5) . . . . ?
C30 C10 C37 C56 -176.7(4) . . . . ?
C30 C10 C37 C41 2.7(7) . . . . ?
C30 C20 C24 C46 179.9(4) . . . . ?
C30 C20 C24 C41 0.5(7) . . . . ?
C30 C20 C38 C54 177.8(4) . . . . ?
C34 C3 C13 Ca3 166.6(15) . . . . ?
C34 C3 C13 O6 -28.9(8) . . . . ?
C34 C3 C13 O15 165.0(15) . . . . ?
C34 C3 C13 O15A 132(2) . . . . ?
C36 C45 C49 C8 -1.9(7) . . . . ?
C38 C20 C24 C46 -2.1(7) . . . . ?
C38 C20 C24 C41 178.5(4) . . . . ?
C38 C20 C30 C10 -175.2(4) . . . . ?
C38 C54 C2 C8 175.0(4) . . . . ?
C38 C54 C2 C46 -2.3(7) . . . . ?
C40 C6 C52 C16 1.0(6) . . . . ?
C40 C6 C54 C38 119.6(5) . . . . ?
C40 C6 C54 C2 -57.9(6) . . . . ?
C42 C5 C25 C35 -178.9(4) . . . . ?
C44 C12 C11 C18 -0.8(7) 2_676 . . . ?
C44 C15 C23 C55 -170.4(4) . . . . ?
C44 C15 C51 C53 170.8(4) . . . . ?
C46 C24 C41 C37 178.6(5) . . . . ?
C48 C4 C12 C44 -138.6(4) . . . 2_676 ?
C48 C4 C12 C11 44.2(6) . . . . ?
C48 C4 C19 C47 2.7(7) . . . . ?
C48 C34 C3 C47 3.1(7) . . . . ?
C48 C34 C3 C13 -173.6(4) . . . . ?
C50 C10 C30 C20 171.2(4) . . . . ?
C50 C10 C37 C56 7.9(7) . . . . ?
C50 C10 C37 C41 -172.7(4) . . . . ?
C50 C26 C43 C32 -0.5(7) . . . . ?
C50 C31 C17 C32 -0.8(7) . . . . ?
C52 C6 C40 C21 -0.1(7) . . . . ?
C52 C6 C54 C38 -60.2(6) . . . . ?
C52 C6 C54 C2 122.4(5) . . . . ?
C52 C16 C28 C1 -178.7(4) . . . . ?
C52 C16 C28 C21 0.0(6) . . . . ?
C54 C6 C40 C21 -179.9(4) . . . . ?
C54 C6 C52 C16 -179.3(4) . . . . ?
C56 C33 C39 C5 0.1(7) . . . . ?
C56 C35 C25 C5 -0.1(7) . . . . ?
C56 C37 C41 C24 179.8(4) . . . . ?
C57 C32 C17 C31 -178.3(4) . . . . ?
C57 C32 C43 C26 178.9(4) . . . . ?
C29 C18 C11 C12 -179.0(4) . . . . ?
C29 C44 C15 C23 135.8(5) . . . . ?
C29 C44 C15 C51 -37.7(6) . . . . ?
C15 C44 C29 C18 -176.8(4) . . . . ?
C15 C23 C55 C27 -0.2(7) . . . . ?
C15 C51 C53 C27 -0.1(8) . . . . ?
C2 C8 C14 C9 -176.8(4) . . . . ?
C2 C8 C49 C45 178.6(4) . . . . ?
C33 C56 C35 C25 -1.0(7) . . . . ?
C33 C56 C37 C10 57.1(6) . . . . ?
C33 C56 C37 C41 -122.3(5) . . . . ?
C33 C39 C5 C42 178.9(4) . . . . ?
C33 C39 C5 C25 -1.3(7) . . . . ?
C17 C32 C57 O12 175.2(4) . . . . ?
C17 C32 C57 O18 -4.5(6) . . . . ?
C17 C32 C43 C26 1.5(7) . . . . ?
C35 C56 C33 C39 1.0(7) . . . . ?
C35 C56 C37 C10 -121.7(5) . . . . ?
C35 C56 C37 C41 58.9(6) . . . . ?
C9 C36 C45 C49 1.7(7) . . . . ?
C37 C10 C30 C20 -4.3(7) . . . . ?
C37 C10 C50 C26 -143.0(5) . . . . ?
C37 C10 C50 C31 41.0(6) . . . . ?
C37 C56 C33 C39 -177.8(4) . . . . ?
C37 C56 C35 C25 177.8(4) . . . . ?
C19 C4 C12 C44 45.6(6) . . . 2_676 ?
C19 C4 C12 C11 -131.5(5) . . . . ?
C19 C4 C48 C34 -1.1(6) . . . . ?
C19 C47 C3 C34 -1.5(7) . . . . ?
C19 C47 C3 C13 175.3(5) . . . . ?
C39 C5 C25 C35 1.3(7) . . . . ?
C41 C24 C46 C2 -178.6(5) . . . . ?
C43 C26 C50 C10 -177.2(4) . . . . ?
C43 C26 C50 C31 -1.1(7) . . . . ?
C43 C32 C57 O12 -2.2(7) . . . . ?
C43 C32 C57 O18 178.1(4) . . . . ?
C43 C32 C17 C31 -0.8(7) . . . . ?
C11 C18 C29 C44 179.6(4) . . . . ?
C45 C36 C9 C14 0.2(6) . . . . ?
C23 C15 C51 C53 -3.1(7) . . . . ?
C47 C3 C13 Ca3 -10(2) . . . . ?
C47 C3 C13 O6 154.4(5) . . . . ?
C47 C3 C13 O15 -11.7(16) . . . . ?
C47 C3 C13 O15A -45(2) . . . . ?
C3 C34 C48 C4 -1.8(7) . . . . ?
C3 C13 O15A Ca3 171.2(6) . . . . ?
C49 C8 C14 C9 1.6(6) . . . . ?
C49 C8 C2 C46 -49.6(6) . . . . ?
C49 C8 C2 C54 133.2(5) . . . . ?
C51 C15 C23 C55 3.2(7) . . . . ?
C51 C53 C27 C55 3.2(8) . . . . ?
C51 C53 C27 C7 -174.2(5) . . . . ?
C53 C27 C55 C23 -3.0(8) . . . . ?
C53 C27 C7 O13 8.7(9) . . . . ?
C53 C27 C7 O7 -172.9(5) . . . . ?
C55 C27 C7 O13 -168.7(5) . . . . ?
C55 C27 C7 O7 9.8(8) . . . . ?
C7 C27 C55 C23 174.3(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.774
_oxdiff_exptl_absorpt_empirical_full_min 0.648
####################################################################### 
# 
# 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_hl61_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2421323'
loop_
_audit_author_name
_audit_author_address
'Jerome Marrot'
;Institut Lavoisier de Versailles
France
;
_audit_update_record             
;
2025-03-18 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
_audit_creation_date             2024-12-18
_audit_creation_method           
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C2 H6 O S), C38 H24 O8'
_chemical_formula_sum            'C42 H36 O10 S2'
_chemical_formula_weight         764.83
_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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   6.8684(2)
_cell_length_b                   13.8322(4)
_cell_length_c                   14.4683(5)
_cell_angle_alpha                105.538(2)
_cell_angle_beta                 95.126(2)
_cell_angle_gamma                101.433(2)
_cell_volume                     1283.19(7)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9927
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      29.95
_cell_measurement_theta_min      2.45
_shelx_estimated_absorpt_T_max   0.991
_shelx_estimated_absorpt_T_min   0.957
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_T_max  0.7383
_exptl_absorpt_correction_T_min  0.6777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1226 before and 0.0843 after correction.
The Ratio of minimum to maximum transmission is 0.9179.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.990
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            72848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.037
_diffrn_reflns_theta_min         1.815
_diffrn_ambient_temperature      292.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5700
_reflns_number_total             7485
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         7485
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0724
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1404P)²+0.3677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2456
_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) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C6(H6), C7(H7), C9(H9), C11(H11), C14(H14), C15(H15),
 C17(H17), C18(H18)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1), O4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.37497(15) 0.38821(5) 0.75345(6) 0.0885(3) Uani 1 1 d . . . . .
O1 O 1.3717(4) 0.8403(2) 0.10764(15) 0.1077(9) Uani 1 1 d . . . . .
H1 H 1.382739 0.795826 0.059198 0.162 Uiso 1 1 calc R U . . .
O2 O 1.1997(4) 0.8977(2) 0.00694(15) 0.1096(9) Uani 1 1 d . . . . .
O3 O -0.5059(2) 0.54774(13) 0.62177(14) 0.0696(4) Uani 1 1 d . . . . .
O4 O -0.2596(3) 0.46470(13) 0.62274(18) 0.0817(6) Uani 1 1 d . . . . .
H4 H -0.350153 0.418439 0.627277 0.123 Uiso 1 1 calc R U . . .
O5 O 0.4961(3) 0.33467(14) 0.68285(19) 0.0921(7) Uani 1 1 d . . . . .
C1 C 1.2357(4) 0.8851(2) 0.08623(15) 0.0623(5) Uani 1 1 d . . . . .
C2 C 1.1207(3) 0.92140(16) 0.16637(13) 0.0483(4) Uani 1 1 d . . . . .
C3 C 0.9715(3) 0.97221(19) 0.15233(14) 0.0580(5) Uani 1 1 d . . . . .
H3 H 0.945065 0.985298 0.093240 0.070 Uiso 1 1 calc R U . . .
C4 C 0.8612(3) 1.00378(16) 0.22566(14) 0.0518(4) Uani 1 1 d . . . . .
H4A H 0.762333 1.038616 0.215459 0.062 Uiso 1 1 calc R U . . .
C5 C 0.8958(2) 0.98426(12) 0.31385(11) 0.0372(3) Uani 1 1 d . . . . .
C6 C 1.0470(3) 0.93398(16) 0.32804(13) 0.0484(4) Uani 1 1 d . . . . .
H6 H 1.073447 0.921022 0.387189 0.058 Uiso 1 1 calc R U . . .
C7 C 1.1590(3) 0.90287(18) 0.25517(13) 0.0530(4) Uani 1 1 d . . . . .
H7 H 1.260123 0.869505 0.265785 0.064 Uiso 1 1 calc R U . . .
C8 C 0.7673(2) 1.01090(12) 0.39003(11) 0.0357(3) Uani 1 1 d . . . . .
C9 C 0.6424(2) 0.93105(12) 0.41097(12) 0.0381(3) Uani 1 1 d . . . . .
H9 H 0.648356 0.863592 0.380472 0.046 Uiso 1 1 calc R U . . .
C10 C 0.5050(2) 0.94873(11) 0.47763(11) 0.0349(3) Uani 1 1 d . . . . .
C11 C 0.3730(2) 0.86646(12) 0.49758(12) 0.0377(3) Uani 1 1 d . . . . .
H11 H 0.378110 0.798862 0.467083 0.045 Uiso 1 1 calc R U . . .
C12 C 0.2371(2) 0.88471(12) 0.56138(11) 0.0360(3) Uani 1 1 d . . . . .
C13 C 0.0912(2) 0.79580(12) 0.57393(12) 0.0378(3) Uani 1 1 d . . . . .
C14 C -0.1127(2) 0.79427(14) 0.56895(14) 0.0456(4) Uani 1 1 d . . . . .
H14 H -0.158144 0.850296 0.559143 0.055 Uiso 1 1 calc R U . . .
C15 C -0.2486(2) 0.71052(15) 0.57840(15) 0.0491(4) Uani 1 1 d . . . . .
H15 H -0.384633 0.710310 0.573581 0.059 Uiso 1 1 calc R U . . .
C16 C -0.1845(2) 0.62678(13) 0.59497(14) 0.0454(4) Uani 1 1 d . . . . .
C17 C 0.0170(3) 0.62584(14) 0.59693(17) 0.0536(5) Uani 1 1 d . . . . .
H17 H 0.061516 0.569127 0.605524 0.064 Uiso 1 1 calc R U . . .
C18 C 0.1522(2) 0.70921(14) 0.58613(16) 0.0503(4) Uani 1 1 d . . . . .
H18 H 0.286965 0.707390 0.587029 0.060 Uiso 1 1 calc R U . . .
C19 C -0.3343(3) 0.54281(15) 0.61339(16) 0.0540(4) Uani 1 1 d . . . . .
C20 C 0.1400(6) 0.3652(4) 0.6881(3) 0.1145(13) Uani 1 1 d . . . . .
H20A H 0.148222 0.399942 0.638827 0.172 Uiso 1 1 calc R U . . .
H20B H 0.050280 0.390512 0.730779 0.172 Uiso 1 1 calc R U . . .
H20C H 0.090566 0.292413 0.658214 0.172 Uiso 1 1 calc R U . . .
C21 C 0.3139(8) 0.3065(3) 0.8291(3) 0.1160(13) Uani 1 1 d . . . . .
H21A H 0.240958 0.239237 0.789604 0.174 Uiso 1 1 calc R U . . .
H21B H 0.232593 0.335476 0.874759 0.174 Uiso 1 1 calc R U . . .
H21C H 0.435322 0.300863 0.863509 0.174 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
S1 O5 1.508(2) . ?
S1 C20 1.721(4) . ?
S1 C21 1.792(3) . ?
O1 H1 0.8200 . ?
O1 C1 1.277(3) . ?
O2 C1 1.217(3) . ?
O3 C19 1.209(2) . ?
O4 H4 0.8200 . ?
O4 C19 1.317(3) . ?
C1 C2 1.494(2) . ?
C2 C3 1.382(3) . ?
C2 C7 1.389(3) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(3) . ?
C4 H4A 0.9300 . ?
C4 C5 1.383(2) . ?
C5 C6 1.389(2) . ?
C5 C8 1.4881(19) . ?
C6 H6 0.9300 . ?
C6 C7 1.386(2) . ?
C7 H7 0.9300 . ?
C8 C9 1.378(2) . ?
C8 C12 1.434(2) 2_676 ?
C9 H9 0.9300 . ?
C9 C10 1.417(2) . ?
C10 C10 1.411(3) 2_676 ?
C10 C11 1.419(2) . ?
C11 H11 0.9300 . ?
C11 C12 1.382(2) . ?
C12 C13 1.488(2) . ?
C13 C14 1.392(2) . ?
C13 C18 1.393(2) . ?
C14 H14 0.9300 . ?
C14 C15 1.382(2) . ?
C15 H15 0.9300 . ?
C15 C16 1.387(2) . ?
C16 C17 1.385(2) . ?
C16 C19 1.490(2) . ?
C17 H17 0.9300 . ?
C17 C18 1.384(2) . ?
C18 H18 0.9300 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 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
O5 S1 C20 105.13(18) . . ?
O5 S1 C21 105.38(17) . . ?
C20 S1 C21 98.5(2) . . ?
C1 O1 H1 109.5 . . ?
C19 O4 H4 109.5 . . ?
O1 C1 C2 114.94(18) . . ?
O2 C1 O1 123.5(2) . . ?
O2 C1 C2 121.5(2) . . ?
C3 C2 C1 120.27(17) . . ?
C3 C2 C7 119.10(16) . . ?
C7 C2 C1 120.62(17) . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.44(16) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4A 119.5 . . ?
C5 C4 C3 120.99(16) . . ?
C5 C4 H4A 119.5 . . ?
C4 C5 C6 118.43(15) . . ?
C4 C5 C8 121.11(14) . . ?
C6 C5 C8 120.37(14) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 C5 120.86(15) . . ?
C7 C6 H6 119.6 . . ?
C2 C7 H7 119.9 . . ?
C6 C7 C2 120.18(16) . . ?
C6 C7 H7 119.9 . . ?
C9 C8 C5 117.87(14) . . ?
C9 C8 C12 119.43(13) . 2_676 ?
C12 C8 C5 122.64(13) 2_676 . ?
C8 C9 H9 119.0 . . ?
C8 C9 C10 121.91(14) . . ?
C10 C9 H9 119.0 . . ?
C9 C10 C11 121.95(14) . . ?
C10 C10 C9 118.58(16) 2_676 . ?
C10 C10 C11 119.42(16) 2_676 . ?
C10 C11 H11 119.3 . . ?
C12 C11 C10 121.37(14) . . ?
C12 C11 H11 119.3 . . ?
C8 C12 C13 121.45(13) 2_676 . ?
C11 C12 C8 119.20(13) . 2_676 ?
C11 C12 C13 119.26(14) . . ?
C14 C13 C12 120.95(14) . . ?
C14 C13 C18 117.74(14) . . ?
C18 C13 C12 121.24(13) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.83(15) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.6 . . ?
C14 C15 C16 120.80(15) . . ?
C16 C15 H15 119.6 . . ?
C15 C16 C19 118.64(16) . . ?
C17 C16 C15 118.91(15) . . ?
C17 C16 C19 122.42(17) . . ?
C16 C17 H17 120.0 . . ?
C18 C17 C16 120.06(16) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 H18 119.2 . . ?
C17 C18 C13 121.55(15) . . ?
C17 C18 H18 119.2 . . ?
O3 C19 O4 123.55(17) . . ?
O3 C19 C16 122.98(18) . . ?
O4 C19 C16 113.44(16) . . ?
S1 C20 H20A 109.5 . . ?
S1 C20 H20B 109.5 . . ?
S1 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
S1 C21 H21A 109.5 . . ?
S1 C21 H21B 109.5 . . ?
S1 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 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
O1 C1 C2 C3 179.1(3) . . . . ?
O1 C1 C2 C7 -2.2(4) . . . . ?
O2 C1 C2 C3 -1.1(4) . . . . ?
O2 C1 C2 C7 177.6(3) . . . . ?
C1 C2 C3 C4 178.4(2) . . . . ?
C1 C2 C7 C6 -177.9(2) . . . . ?
C2 C3 C4 C5 -0.8(3) . . . . ?
C3 C2 C7 C6 0.8(3) . . . . ?
C3 C4 C5 C6 1.3(3) . . . . ?
C3 C4 C5 C8 -175.29(18) . . . . ?
C4 C5 C6 C7 -0.8(3) . . . . ?
C4 C5 C8 C9 111.02(19) . . . . ?
C4 C5 C8 C12 -66.2(2) . . . 2_676 ?
C5 C6 C7 C2 -0.2(3) . . . . ?
C5 C8 C9 C10 -175.71(14) . . . . ?
C6 C5 C8 C9 -65.5(2) . . . . ?
C6 C5 C8 C12 117.25(18) . . . 2_676 ?
C7 C2 C3 C4 -0.3(3) . . . . ?
C8 C5 C6 C7 175.81(18) . . . . ?
C8 C9 C10 C10 1.0(3) . . . 2_676 ?
C8 C9 C10 C11 178.53(15) . . . . ?
C8 C12 C13 C14 45.8(2) 2_676 . . . ?
C8 C12 C13 C18 -137.43(18) 2_676 . . . ?
C9 C10 C11 C12 -178.76(15) . . . . ?
C10 C10 C11 C12 -1.2(3) 2_676 . . . ?
C10 C11 C12 C8 -1.4(2) . . . 2_676 ?
C10 C11 C12 C13 175.22(14) . . . . ?
C11 C12 C13 C14 -130.68(17) . . . . ?
C11 C12 C13 C18 46.0(2) . . . . ?
C12 C8 C9 C10 1.6(2) 2_676 . . . ?
C12 C13 C14 C15 178.49(17) . . . . ?
C12 C13 C18 C17 -179.39(18) . . . . ?
C13 C14 C15 C16 1.3(3) . . . . ?
C14 C13 C18 C17 -2.6(3) . . . . ?
C14 C15 C16 C17 -3.3(3) . . . . ?
C14 C15 C16 C19 174.61(19) . . . . ?
C15 C16 C17 C18 2.4(3) . . . . ?
C15 C16 C19 O3 -5.7(3) . . . . ?
C15 C16 C19 O4 176.4(2) . . . . ?
C16 C17 C18 C13 0.5(3) . . . . ?
C17 C16 C19 O3 172.1(2) . . . . ?
C17 C16 C19 O4 -5.7(3) . . . . ?
C18 C13 C14 C15 1.7(3) . . . . ?
C19 C16 C17 C18 -175.4(2) . . . . ?

loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_platon_squeeze_void_content
1 0.007 0.500 0.000 435 118 ' '
_platon_squeeze_void_probe_radius 1.20

_olex2_submission_special_instructions 'No special instructions were received'
_Platon_squeeze_details          'Spek, A. L. (2015). Acta Cryst. C71, 9-18'
####################################################################### 
# 
# 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_bwx2new_sq
_database_code_depnum_ccdc_archive 'CCDC 2421322'
loop_
_audit_author_name
_audit_author_address
'Guy Clarkson'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2025-03-14 deposited with the CCDC.	2025-03-31 downloaded from the CCDC.
;
# start Validation Reply Form                                                   
_vrf_PLAT430_bwx2new_sq          
;                                                                               
PROBLEM: Short Inter D...A Contact  O126..O202                                  
RESPONSE: This is from the close contact of carboxyl oxygen O202 with the       
carbonyl oxygen O126 of a neighbouring disordered benzoic acid ligand.          
The phenyl group (C119 to C124) of this disordered component forms a pi pi inter
with a phenyl group of a neighbouring ring (C314 to C319,                       
centroid centroid distance is 3.58 Angstroms) at the expense of the close       
contact flagged up in the B alert                                               
;
_vrf_PLAT934_bwx2new_sq          
;                                                                               
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers                          
RESPONSE: These outliers are    probably associated with the weak quality of 
the data and refinement statistics due in part to the large amount of 
disordered solvent in the structure          
;
# end Validation Reply Form                                                     
_audit_creation_date             2025-03-14
_audit_creation_method           
;                                                                               
Olex2 1.5                                                                       
(compiled 2025.03.06 svn.red2d20d0 for OlexSys, GUI svn.r7188)                  
;
_shelx_SHELXL_version_number     2019/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C114 H62 Ca5 O29, 0.5[]'
_chemical_formula_sum            'C114 H62 Ca5 O29'
_chemical_formula_weight         2096.03
_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 0.0181 0.0091 '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 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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                   18.6030(6)
_cell_length_b                   19.2334(7)
_cell_length_c                   20.9801(7)
_cell_angle_alpha                66.031(4)
_cell_angle_beta                 67.392(3)
_cell_angle_gamma                85.309(3)
_cell_volume                     6307.5(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12154
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.6360
_cell_measurement_theta_min      2.4710
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.890
_exptl_absorpt_coefficient_mu    2.397
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86368
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;                                                                               
 CrysAlisPro 1.171.41.94a (Rigaku Oxford Diffraction, 2021) Empirical           
 absorption correction using spherical harmonics, implemented in                
 SCALE3 ABSPACK scaling algorithm.                                              
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.104
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2156
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1301
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            121764
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.112
_diffrn_reflns_theta_min         2.734
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;                                                                               
List of Runs (angles in degrees, time in seconds):                              
                                                                                
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames      
#--------------------------------------------------------------------------      
  1  ω     35.00 122.00   0.50   20.00    --   47.75  32.00 -96.00  174        
  2  ω    -26.00  36.00   0.50   20.00    --   47.75 -32.00 104.00  124        
  3  ω   -165.00 -79.00   0.50   80.00    --  -91.75 -32.00 104.00  172        
  4  ω    100.00 178.00   0.50   80.00    --  113.25  32.00 -96.00  156        
  5  ω    -23.00  28.00   0.50   20.00    --  -47.75  19.00  60.00  102        
  6  ω    -23.00  28.00   0.50   20.00    --  -47.75  19.00-180.00  102        
  7  ω   -119.00 -73.00   0.50   20.00    --  -47.75-125.00-180.00   92        
  8  ω   -119.00 -73.00   0.50   20.00    --  -47.75-125.00  60.00   92        
  9  ω    -36.00  27.00   0.50   20.00    --  -47.75  32.00 -96.00  126        
 10  ω   -121.00 -35.00   0.50   20.00    --  -47.75 -32.00 104.00  172        
 11  ω   -119.00 -73.00   0.50   20.00    --  -47.75-125.00-150.00   92        
 12  ω    -23.00  28.00   0.50   20.00    --  -47.75  19.00 -60.00  102        
 13  ω     34.00  96.00   0.50   20.00    --   47.75-125.00 -30.00  124        
 14  ω    -24.00  71.00   0.50   20.00    --   47.75 -77.00  90.00  190        
 15  ω    -72.00 -19.00   0.50   80.00    --  -91.75  61.00 -60.00  106        
 16  ω    -50.00 -20.00   0.50   80.00    --  -91.75  45.00-120.00   60        
 17  ω    -85.00 -19.00   0.50   80.00    --  -91.75 125.00 -30.00  132        
 18  ω     42.00 106.00   0.50   80.00    --  113.25 -97.00 -40.62  128        
 19  ω    100.00 178.00   0.50   80.00    --  113.25  15.00  60.00  156        
 20  ω    101.00 178.00   0.50   80.00    --  113.25  45.00 -60.00  154        
 21  ω     42.00  72.00   0.50   80.00    --  113.25 -61.00-180.00   60        
 22  ω    101.00 178.00   0.50   80.00    --  113.25  45.00  60.00  154        
 23  ω     91.00 178.00   0.50   80.00    --  113.25  77.00-180.00  174        
 24  ω     42.00  72.00   0.50   80.00    --  113.25 -61.00  30.00   60        
 25  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00 150.00  128        
 26  ω    101.00 178.00   0.50   80.00    --  113.25  30.00   0.00  154        
 27  ω     95.00 178.00   0.50   80.00    --  113.25 125.00-120.00  166        
 28  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00-120.00  128        
 29  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00 -90.00  128        
 30  ω     42.00  72.00   0.50   80.00    --  113.25 -61.00 -30.00   60        
 31  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00   0.00  128        
 32  ω     42.00  72.00   0.50   80.00    --  113.25 -61.00 -90.00   60        
 33  ω     42.00 136.00   0.50   80.00    --  113.25 -77.00-180.00  188        
 34  ω    101.00 178.00   0.50   80.00    --  113.25  30.00-120.00  154        
 35  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00 -30.00  128        
 36  ω     42.00 111.00   0.50   80.00    --  113.25-125.00 150.00  138        
 37  ω    101.00 178.00   0.50   80.00    --  113.25  45.00 150.00  154        
 38  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00  30.00  128        
 39  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00  60.00  128        
 40  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00  90.00  128        
 41  ω    101.00 178.00   0.50   80.00    --  113.25  45.00 -90.00  154        
 42  ω     42.00  72.00   0.50   80.00    --  113.25 -61.00   0.00   60        
 43  ω     42.00 136.00   0.50   80.00    --  113.25 -77.00-180.00  188        
 44  ω     42.00 106.00   0.50   80.00    --  113.25 -94.00 120.00  128        
 45  ω     42.00 107.00   0.50   80.00    --  113.25-105.00-174.24  130        
 46  ω    101.00 168.00   0.50   80.00    --  113.25  45.00   0.00  134        
 47  ω    104.00 176.00   0.50   80.00    --  113.25  45.00 -30.00  144        
 48  ω     79.00 106.00   0.50   80.00    --  113.25 -97.00-169.81   54        
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13438
_reflns_number_total             24708
_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.                                                           
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.884
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.090
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         24708
_refine_ls_number_restraints     172
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0902
_refine_ls_restrained_S_all      1.012
_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)+(0.1935P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2623
_refine_ls_wR_factor_ref         0.3028
_refine_special_details          SQUEEZE
_olex2_refinement_description    
;     
The asymmetric unit contains two complete ligands and two half ligands 
that sit on inversion centres and 5 calcium ions.
I think that works out OK considering charge balance. Based on this I 
believe that the coordinated oxygens O1, O2, O3A, O3B and O5 are waters. 
Hydrogens were located on water O3B where they form hydrogen bonds with 
the oxygens of neighbouring ligands. 
No hydrogens were located on the other coordinated waters which must be 
interacting with diffuse solvent in the voids in the structure.

Two of the terminal benzoic acid legs were modelled as disordered over 
two closely related positions.
The occupancy of benzoic acid leg C119 to O125 and its associated 
component C1 to O8 were linked to a free variable which refined to 62:38
The occupancy of benzoic acid leg C314 to O321 and its associated component 
C14 to O21 were linked to a free variable which refined close to 50:50 but 
was then fixed at this value for the remainder of the refinement. 
Several DFIX and SIMU restraints were used to give the disordered components 
reasonably bond lengths and thermal parameters.
Electron density in the voids were initially modelled as up to 15 partially 
occupied water molecules with no major improvement in the refinement R values.
The refinement was eventually completed using the Squeeze algorithm in Platon.
See Squeeze details at the end of the file.
                                                                          
1. Fixed Uiso                                                                   
 At 1.2 times of:                                                               
  All C(H) groups                                                               
 At 1.5 times of:                                                               
  All O(H,H) groups                                                             
2. Restrained distances                                                         
 C222-C225                                                                      
 1.3 with sigma of 0.008                                                        
 C122-C125                                                                      
 1.3 with sigma of 0.008                                                        
 C1-C7 = C17-C20                                                                
 1.3 with sigma of 0.01                                                         
 O7-C7 = O8-C7 = O126-C125 = C20-O20 = C20-O21                                  
 1.25 with sigma of 0.008                                                       
 Ca3-H3BA \\sim Ca3-H3BB                                                        
 with sigma of 0.02                                                             
3. Uiso/Uaniso restraints and constraints                                       
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim O7 \\sim O8:     
within 2A with sigma of 0.008 and sigma for terminal atoms of 0.016 within 2A   
C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim O20 \\sim 
O21: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within 
2A                                                                              
C314 \\sim C315 \\sim C316 \\sim C317 \\sim C318 \\sim C319 \\sim O320 \\sim    
C320 \\sim O321 \\sim O5: within 2A with sigma of 0.004 and sigma for terminal  
atoms of 0.008 within 2A                                                        
4. Others                                                                       
 Sof(C1)=Sof(C3)=Sof(H3)=Sof(C2)=Sof(H2)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=       
 Sof(H6)=Sof(C7)=Sof(O7)=Sof(O8)=1-FVAR(1)                                      
 Sof(C119)=Sof(C120)=Sof(H120)=Sof(C121)=Sof(H121)=Sof(C122)=Sof(C123)=         
 Sof(H123)=Sof(C124)=Sof(H124)=Sof(C125)=Sof(O125)=Sof(O126)=FVAR(1)            
 Fixed Sof: C14(0.5) C15(0.5) H15(0.5) C16(0.5) H16(0.5) C17(0.5) C18(0.5)      
 H18(0.5) C19(0.5) H19(0.5) C20(0.5) O20(0.5) O21(0.5) C314(0.5) C319(0.5)      
 H319(0.5) C318(0.5) H318(0.5) C317(0.5) C316(0.5) H316(0.5) C315(0.5)          
 H315(0.5) C320(0.5) O320(0.5) O321(0.5)                                        
5.a Free rotating group:                                                        
 O3B(H3BA,H3BB)                                                                 
5.b Aromatic/amide H refined with riding coordinates:                           
 C3(H3), C2(H2), C5(H5), C6(H6), C15(H15), C16(H16), C18(H18), C19(H19),        
 C104(H104), C105(H105), C107(H107), C108(H108), C110(H110), C112(H112),        
 C115(H115), C117(H117), C130(H130), C131(H131), C133(H133), C134(H134),        
 C138(H138), C139(H139), C141(H141), C142(H142), C204(H204), C205(H205),        
 C207(H207), C208(H208), C210(H210), C212(H212), C215(H215), C217(H217),        
 C220(H220), C221(H221), C223(H223), C224(H224), C230(H230), C231(H231),        
 C233(H233), C234(H234), C238(H238), C239(H239), C241(H241), C242(H242),        
 C304(H304), C305(H305), C307(H307), C308(H308), C310(H310), C312(H312),        
 C404(H404), C405(H405), C407(H407), C408(H408), C410(H410), C412(H412),        
 C415(H415), C416(H416), C418(H418), C419(H419), C120(H120), C121(H121),        
 C123(H123), C124(H124), C319(H319), C318(H318), C316(H316), C315(H315)         
5.c Fitted hexagon refined as free rotating group:                              
 C1(C3,C2,C4,C5,C6), C14(C15,C16,C17,C18,C19), C314(C319,C318,C317,C316,C315)   
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0462(11) 1.0025(7) 0.3011(11) 0.069(4) Uani 0.380(11) 1 d DG U P A 2
C3 C 0.0076(10) 0.9545(10) 0.2875(11) 0.063(4) Uani 0.380(11) 1 d G U P A 2
H3 H -0.038426 0.968947 0.277666 0.076 Uiso 0.380(11) 1 calc R U P A 2
C2 C 0.0363(13) 0.8853(9) 0.2882(13) 0.055(4) Uani 0.380(11) 1 d G U P A 2
H2 H 0.009989 0.852434 0.278844 0.066 Uiso 0.380(11) 1 calc R U P A 2
C4 C 0.1037(15) 0.8641(10) 0.3025(17) 0.053(5) Uani 0.380(11) 1 d G U P A 2
C5 C 0.1422(13) 0.9121(13) 0.3162(18) 0.054(5) Uani 0.380(11) 1 d G U P A 2
H5 H 0.188253 0.897670 0.325996 0.064 Uiso 0.380(11) 1 calc R U P A 2
C6 C 0.1135(12) 0.9813(11) 0.3155(14) 0.061(5) Uani 0.380(11) 1 d G U P A 2
H6 H 0.139840 1.014184 0.324819 0.073 Uiso 0.380(11) 1 calc R U P A 2
Ca1 Ca 0.41538(6) 0.68206(8) 0.66288(8) 0.0666(4) Uani 1 1 d . . . . .
O1 O 0.4461(4) 0.5542(3) 0.7213(3) 0.0983(16) Uani 1 1 d . . . . .
Ca2 Ca 0.20530(7) 0.67363(11) 0.75260(8) 0.0845(5) Uani 1 1 d . . . . .
O2 O 0.1471(5) 0.5444(6) 0.8312(4) 0.158(4) Uani 1 1 d . . . . .
Ca3 Ca -0.07458(7) 0.74013(7) 0.76920(7) 0.0655(3) Uani 1 1 d D . . . .
O3A O -0.1952(3) 0.7309(3) 0.8707(3) 0.0775(12) Uani 1 1 d . . . . .
O3B O -0.1508(2) 0.7555(3) 0.6991(3) 0.0682(10) Uani 1 1 d G . . . .
H3BA H -0.159187 0.722250 0.683783 0.102 Uiso 1 1 d DG U . . .
H3BB H -0.188454 0.785249 0.697087 0.102 Uiso 1 1 d DG U . . .
Ca4 Ca 0.49592(5) 0.22783(7) 0.26394(6) 0.0523(3) Uani 1 1 d . . . . .
Ca5 Ca 1.39106(6) 0.15435(7) 0.19210(6) 0.0571(3) Uani 1 1 d . . . . .
C7 C 0.0277(7) 1.0742(8) 0.2914(15) 0.067(4) Uani 0.380(11) 1 d D U P A 2
O7 O 0.0725(14) 1.1281(13) 0.2782(17) 0.066(5) Uani 0.380(11) 1 d D U P A 2
O8 O -0.0421(6) 1.0916(7) 0.3024(9) 0.092(5) Uani 0.380(11) 1 d D U P A 2
C14 C 1.1821(10) 0.0094(11) 0.0558(10) 0.080(4) Uani 0.5 1 d G U P B 2
C15 C 1.2240(12) -0.0504(9) 0.0839(11) 0.080(4) Uani 0.5 1 d G U P B 2
H15 H 1.221730 -0.096525 0.077973 0.096 Uiso 0.5 1 calc R U P B 2
C16 C 1.2691(11) -0.0428(9) 0.1207(10) 0.085(4) Uani 0.5 1 d G U P B 2
H16 H 1.297723 -0.083708 0.139885 0.102 Uiso 0.5 1 calc R U P B 2
C17 C 1.2724(10) 0.0246(10) 0.1294(9) 0.092(3) Uani 0.5 1 d DG U P B 2
C18 C 1.2306(10) 0.0844(8) 0.1013(9) 0.088(4) Uani 0.5 1 d G U P B 2
H18 H 1.232808 0.130472 0.107231 0.105 Uiso 0.5 1 calc R U P B 2
C19 C 1.1854(10) 0.0768(9) 0.0645(9) 0.086(4) Uani 0.5 1 d G U P B 2
H19 H 1.156814 0.117657 0.045318 0.104 Uiso 0.5 1 calc R U P B 2
C20 C 1.3186(10) 0.0201(11) 0.1665(11) 0.103(4) Uani 0.5 1 d D U P B 2
O20 O 1.3672(8) -0.0277(9) 0.1813(8) 0.105(4) Uani 0.5 1 d D U P B 2
O21 O 1.3140(10) 0.0744(10) 0.1860(9) 0.109(4) Uani 0.5 1 d D U P B 2
O101 O 0.0383(2) 0.7580(4) 0.6711(3) 0.0890(16) Uani 1 1 d . . . . .
C102 C 0.1036(3) 0.7398(5) 0.6368(4) 0.0761(19) Uani 1 1 d . . . . .
O102 O 0.1580(3) 0.7273(5) 0.6606(3) 0.122(3) Uani 1 1 d . . . . .
C103 C 0.1173(3) 0.7372(4) 0.5631(3) 0.0599(13) Uani 1 1 d . . . . .
C104 C 0.1916(4) 0.7281(4) 0.5181(3) 0.0658(15) Uani 1 1 d . . . . .
H104 H 0.233401 0.723475 0.534637 0.079 Uiso 1 1 calc R U . . .
C105 C 0.2053(3) 0.7256(3) 0.4502(3) 0.0607(14) Uani 1 1 d . . . . .
H105 H 0.256556 0.719527 0.419989 0.073 Uiso 1 1 calc R U . . .
C106 C 0.1448(3) 0.7319(3) 0.4247(3) 0.0581(13) Uani 1 1 d . . . . .
C107 C 0.0695(3) 0.7403(3) 0.4710(3) 0.0574(13) Uani 1 1 d . . . . .
H107 H 0.027308 0.743774 0.455334 0.069 Uiso 1 1 calc R U . . .
C108 C 0.0567(3) 0.7433(3) 0.5381(3) 0.0591(13) Uani 1 1 d . . . . .
H108 H 0.005639 0.749668 0.568442 0.071 Uiso 1 1 calc R U . . .
C109 C 0.1605(3) 0.7283(3) 0.3516(3) 0.0567(13) Uani 1 1 d . . . . .
C110 C 0.1994(4) 0.6688(3) 0.3368(3) 0.0600(13) Uani 1 1 d . . . . .
H110 H 0.214002 0.630976 0.374900 0.072 Uiso 1 1 calc R U . . .
C111 C 0.2186(4) 0.6612(3) 0.2679(3) 0.0556(13) Uani 1 1 d . . . . .
C112 C 0.2586(3) 0.6007(3) 0.2522(3) 0.0557(12) Uani 1 1 d . . . . .
H112 H 0.274602 0.562987 0.289188 0.067 Uiso 1 1 calc R U . . .
C113 C 0.2748(3) 0.5949(3) 0.1856(3) 0.0529(12) Uani 1 1 d . . . . .
C114 C 0.2535(3) 0.6528(3) 0.1280(3) 0.0524(12) Uani 1 1 d . . . . .
C115 C 0.2131(3) 0.7109(3) 0.1421(3) 0.0525(12) Uani 1 1 d . . . . .
H115 H 0.197840 0.748291 0.104339 0.063 Uiso 1 1 calc R U . . .
C116 C 0.1934(3) 0.7167(3) 0.2120(3) 0.0541(12) Uani 1 1 d . . . . .
C117 C 0.1524(3) 0.7762(3) 0.2284(3) 0.0526(12) Uani 1 1 d . . . . .
H117 H 0.134803 0.812478 0.191902 0.063 Uiso 1 1 calc R U . . .
C118 C 0.1367(3) 0.7847(3) 0.2940(3) 0.0545(12) Uani 1 1 d . . . . .
O127 O 0.2909(3) 0.6328(3) -0.1844(3) 0.0826(14) Uani 1 1 d . . . . .
C128 C 0.3422(3) 0.6491(3) -0.1668(3) 0.0580(13) Uani 1 1 d . . . . .
O128 O 0.4119(2) 0.6704(2) -0.2126(2) 0.0659(10) Uani 1 1 d . . . . .
C129 C 0.3204(3) 0.6486(3) -0.0898(3) 0.0519(12) Uani 1 1 d . . . . .
C130 C 0.2415(3) 0.6432(3) -0.0434(3) 0.0559(12) Uani 1 1 d . . . . .
H130 H 0.202508 0.637864 -0.060325 0.067 Uiso 1 1 calc R U . . .
C131 C 0.2196(3) 0.6455(3) 0.0255(3) 0.0560(12) Uani 1 1 d . . . . .
H131 H 0.165697 0.643001 0.055683 0.067 Uiso 1 1 calc R U . . .
C132 C 0.2771(3) 0.6517(3) 0.0520(3) 0.0531(12) Uani 1 1 d . . . . .
C133 C 0.3550(3) 0.6554(3) 0.0065(3) 0.0538(12) Uani 1 1 d . . . . .
H133 H 0.394197 0.658372 0.024153 0.065 Uiso 1 1 calc R U . . .
C134 C 0.3766(3) 0.6548(3) -0.0635(3) 0.0548(12) Uani 1 1 d . . . . .
H134 H 0.430415 0.658751 -0.094352 0.066 Uiso 1 1 calc R U . . .
O135 O 0.3375(3) 0.2774(3) 0.1436(3) 0.0759(12) Uani 1 1 d . . . . .
C136 C 0.3751(3) 0.3106(3) 0.1645(3) 0.0579(13) Uani 1 1 d . . . . .
O136 O 0.4286(2) 0.2798(2) 0.1867(2) 0.0608(9) Uani 1 1 d . . . . .
C137 C 0.3541(3) 0.3870(3) 0.1652(3) 0.0534(12) Uani 1 1 d . . . . .
C138 C 0.2899(3) 0.4173(3) 0.1492(3) 0.0534(12) Uani 1 1 d . . . . .
H138 H 0.262092 0.391032 0.134765 0.064 Uiso 1 1 calc R U . . .
C139 C 0.2661(3) 0.4858(3) 0.1542(3) 0.0545(12) Uani 1 1 d . . . . .
H139 H 0.221946 0.506299 0.143148 0.065 Uiso 1 1 calc R U . . .
C140 C 0.3063(3) 0.5247(3) 0.1753(3) 0.0509(11) Uani 1 1 d . . . . .
C141 C 0.3715(3) 0.4955(3) 0.1900(3) 0.0560(12) Uani 1 1 d . . . . .
H141 H 0.399925 0.522012 0.203731 0.067 Uiso 1 1 calc R U . . .
C142 C 0.3953(3) 0.4264(3) 0.1845(3) 0.0560(12) Uani 1 1 d . . . . .
H142 H 0.440335 0.406416 0.194029 0.067 Uiso 1 1 calc R U . . .
O201 O -0.1149(3) 0.2944(5) 1.1555(3) 0.119(2) Uani 1 1 d . . . . .
C202 C -0.0481(3) 0.2702(4) 1.1346(4) 0.0670(16) Uani 1 1 d . . . . .
O202 O -0.0068(3) 0.2518(3) 1.1735(3) 0.0768(12) Uani 1 1 d . . . . .
C203 C -0.0183(3) 0.2609(4) 1.0622(3) 0.0611(14) Uani 1 1 d . . . . .
C204 C 0.0604(4) 0.2564(4) 1.0255(4) 0.0728(17) Uani 1 1 d . . . . .
H204 H 0.095723 0.257058 1.048070 0.087 Uiso 1 1 calc R U . . .
C205 C 0.0883(4) 0.2511(4) 0.9569(4) 0.0729(17) Uani 1 1 d . . . . .
H205 H 0.142556 0.247567 0.933033 0.087 Uiso 1 1 calc R U . . .
C206 C 0.0382(3) 0.2507(3) 0.9217(3) 0.0591(13) Uani 1 1 d . . . . .
C207 C -0.0417(3) 0.2534(4) 0.9595(3) 0.0606(14) Uani 1 1 d . . . . .
H207 H -0.077193 0.251515 0.937524 0.073 Uiso 1 1 calc R U . . .
C208 C -0.0695(3) 0.2588(4) 1.0286(3) 0.0644(15) Uani 1 1 d . . . . .
H208 H -0.123927 0.261022 1.053400 0.077 Uiso 1 1 calc R U . . .
C209 C 0.0680(3) 0.2432(4) 0.8482(3) 0.0591(13) Uani 1 1 d . . . . .
C210 C 0.1098(3) 0.1822(4) 0.8425(3) 0.0610(14) Uani 1 1 d . . . . .
H210 H 0.120570 0.147771 0.884754 0.073 Uiso 1 1 calc R U . . .
C211 C 0.1375(3) 0.1689(3) 0.7758(3) 0.0591(13) Uani 1 1 d . . . . .
C212 C 0.1789(4) 0.1042(3) 0.7711(3) 0.0648(15) Uani 1 1 d . . . . .
H212 H 0.190785 0.070030 0.812813 0.078 Uiso 1 1 calc R U . . .
C213 C 0.2020(4) 0.0906(3) 0.7062(3) 0.0613(14) Uani 1 1 d . . . . .
C214 C 0.1880(3) 0.1448(3) 0.6424(3) 0.0563(13) Uani 1 1 d . . . . .
C215 C 0.1475(3) 0.2062(3) 0.6473(3) 0.0546(12) Uani 1 1 d . . . . .
H215 H 0.136808 0.240626 0.605008 0.066 Uiso 1 1 calc R U . . .
C216 C 0.1210(3) 0.2201(3) 0.7135(3) 0.0520(12) Uani 1 1 d . . . . .
C217 C 0.0801(3) 0.2829(3) 0.7192(3) 0.0528(12) Uani 1 1 d . . . . .
H217 H 0.070198 0.317789 0.676592 0.063 Uiso 1 1 calc R U . . .
C218 C 0.0531(3) 0.2971(3) 0.7839(3) 0.0529(12) Uani 1 1 d . . . . .
C219 C 0.0142(3) 0.3685(3) 0.7821(3) 0.0539(12) Uani 1 1 d . . . . .
C220 C -0.0350(3) 0.3941(3) 0.7423(3) 0.0558(13) Uani 1 1 d . . . . .
H220 H -0.046822 0.363561 0.720985 0.067 Uiso 1 1 calc R U . . .
C221 C -0.0670(3) 0.4640(3) 0.7334(3) 0.0627(14) Uani 1 1 d . . . . .
H221 H -0.100006 0.479615 0.705886 0.075 Uiso 1 1 calc R U . . .
C222 C -0.0529(3) 0.5115(3) 0.7627(3) 0.0634(14) Uani 1 1 d D . . . .
C223 C -0.0051(3) 0.4843(3) 0.8039(3) 0.0613(14) Uani 1 1 d . . . . .
H223 H 0.004808 0.514284 0.826615 0.074 Uiso 1 1 calc R U . . .
C224 C 0.0292(3) 0.4140(3) 0.8133(3) 0.0574(13) Uani 1 1 d . . . . .
H224 H 0.062258 0.398318 0.840832 0.069 Uiso 1 1 calc R U . . .
C225 C -0.0842(3) 0.5830(3) 0.7518(4) 0.0666(15) Uani 1 1 d D . . . .
O225 O -0.0868(3) 0.6139(3) 0.7952(3) 0.0756(12) Uani 1 1 d . . . . .
O226 O -0.1089(3) 0.6158(3) 0.6983(3) 0.0763(12) Uani 1 1 d . . . . .
O227 O 0.2784(2) 0.1551(3) 0.3054(2) 0.0718(12) Uani 1 1 d . . . . .
C228 C 0.3186(3) 0.1418(4) 0.3452(3) 0.0579(13) Uani 1 1 d . . . . .
O228 O 0.39201(19) 0.1330(2) 0.3188(2) 0.0554(9) Uani 1 1 d . . . . .
C229 C 0.2827(3) 0.1379(4) 0.4239(3) 0.0580(13) Uani 1 1 d . . . . .
C230 C 0.2047(3) 0.1505(4) 0.4543(3) 0.0667(15) Uani 1 1 d . . . . .
H230 H 0.172831 0.160434 0.425946 0.080 Uiso 1 1 calc R U . . .
C231 C 0.1733(3) 0.1484(4) 0.5282(3) 0.0673(16) Uani 1 1 d . . . . .
H231 H 0.119374 0.154468 0.550188 0.081 Uiso 1 1 calc R U . . .
C232 C 0.2185(3) 0.1379(3) 0.5684(3) 0.0550(12) Uani 1 1 d . . . . .
C233 C 0.2984(3) 0.1263(3) 0.5364(3) 0.0590(13) Uani 1 1 d . . . . .
H233 H 0.330647 0.119085 0.564002 0.071 Uiso 1 1 calc R U . . .
C234 C 0.3292(3) 0.1255(3) 0.4664(3) 0.0570(13) Uani 1 1 d . . . . .
H234 H 0.382525 0.116540 0.446034 0.068 Uiso 1 1 calc R U . . .
O235 O 0.3118(3) -0.2298(3) 0.6842(3) 0.0836(14) Uani 1 1 d . . . . .
C236 C 0.3506(3) -0.1780(4) 0.6820(3) 0.0616(14) Uani 1 1 d . . . . .
O236 O 0.4220(2) -0.1822(3) 0.6704(2) 0.0681(11) Uani 1 1 d . . . . .
C237 C 0.3116(3) -0.1102(4) 0.6917(3) 0.0618(14) Uani 1 1 d . . . . .
C238 C 0.2384(4) -0.0985(5) 0.6910(6) 0.097(3) Uani 1 1 d . . . . .
H238 H 0.211896 -0.134947 0.685965 0.117 Uiso 1 1 calc R U . . .
C239 C 0.2019(4) -0.0340(5) 0.6974(5) 0.091(2) Uani 1 1 d . . . . .
H239 H 0.151012 -0.026771 0.696738 0.109 Uiso 1 1 calc R U . . .
C240 C 0.2399(4) 0.0194(4) 0.7049(3) 0.0641(15) Uani 1 1 d . . . . .
C241 C 0.3132(4) 0.0070(4) 0.7079(3) 0.0663(15) Uani 1 1 d . . . . .
H241 H 0.338700 0.042111 0.715373 0.080 Uiso 1 1 calc R U . . .
C242 C 0.3493(4) -0.0569(3) 0.7001(3) 0.0640(15) Uani 1 1 d . . . . .
H242 H 0.400288 -0.064167 0.700542 0.077 Uiso 1 1 calc R U . . .
O301 O 0.5403(2) 0.1651(2) 0.1857(2) 0.0638(10) Uani 1 1 d . . . . .
C302 C 0.5468(3) 0.1057(4) 0.1733(3) 0.0612(14) Uani 1 1 d . . . . .
O302 O 0.4893(2) 0.0619(3) 0.1909(3) 0.0803(13) Uani 1 1 d . . . . .
C303 C 0.6278(3) 0.0869(3) 0.1355(3) 0.0524(12) Uani 1 1 d . . . . .
C304 C 0.6398(3) 0.0163(3) 0.1300(3) 0.0580(13) Uani 1 1 d . . . . .
H304 H 0.596230 -0.019392 0.149804 0.070 Uiso 1 1 calc R U . . .
C305 C 0.7138(3) -0.0020(3) 0.0964(3) 0.0562(13) Uani 1 1 d . . . . .
H305 H 0.720901 -0.050760 0.094707 0.067 Uiso 1 1 calc R U . . .
C306 C 0.7776(3) 0.0495(3) 0.0652(3) 0.0502(12) Uani 1 1 d . . . . .
C307 C 0.7658(3) 0.1204(3) 0.0705(3) 0.0531(12) Uani 1 1 d . . . . .
H307 H 0.809221 0.156684 0.049491 0.064 Uiso 1 1 calc R U . . .
C308 C 0.6920(3) 0.1379(3) 0.1057(3) 0.0525(12) Uani 1 1 d . . . . .
H308 H 0.685189 0.185724 0.109507 0.063 Uiso 1 1 calc R U . . .
C309 C 0.8586(3) 0.0310(3) 0.0285(3) 0.0526(12) Uani 1 1 d . . . . .
C310 C 0.9145(3) 0.0420(3) 0.0506(3) 0.0559(13) Uani 1 1 d . . . . .
H310 H 0.902169 0.066262 0.084472 0.067 Uiso 1 1 calc R U . . .
C311 C 0.9916(3) 0.0184(3) 0.0250(3) 0.0567(13) Uani 1 1 d . . . . .
C312 C 1.0493(3) 0.0281(3) 0.0492(3) 0.0587(14) Uani 1 1 d . . . . .
H312 H 1.037040 0.051417 0.083850 0.070 Uiso 1 1 calc R U . . .
C313 C 1.1235(3) 0.0047(3) 0.0241(3) 0.0549(12) Uani 1 1 d . . . . .
O401 O 0.2979(2) 0.6174(3) 0.6785(2) 0.0728(12) Uani 1 1 d . . . . .
C402 C 0.3298(3) 0.6058(4) 0.6191(3) 0.0608(14) Uani 1 1 d . . . . .
O402 O 0.4006(2) 0.6263(3) 0.5784(3) 0.0832(14) Uani 1 1 d . . . . .
C403 C 0.2814(3) 0.5696(3) 0.5968(3) 0.0516(12) Uani 1 1 d . . . . .
C404 C 0.2040(3) 0.5425(3) 0.6442(3) 0.0520(12) Uani 1 1 d . . . . .
H404 H 0.183912 0.542330 0.693274 0.062 Uiso 1 1 calc R U . . .
C405 C 0.1563(3) 0.5161(3) 0.6215(3) 0.0487(11) Uani 1 1 d . . . . .
H405 H 0.103820 0.497431 0.655212 0.058 Uiso 1 1 calc R U . . .
C406 C 0.1836(3) 0.5161(3) 0.5494(3) 0.0416(10) Uani 1 1 d . . . . .
C407 C 0.2618(3) 0.5400(3) 0.5027(3) 0.0430(10) Uani 1 1 d . . . . .
H407 H 0.282026 0.538119 0.454384 0.052 Uiso 1 1 calc R U . . .
C408 C 0.3104(3) 0.5663(3) 0.5256(3) 0.0494(11) Uani 1 1 d . . . . .
H408 H 0.363742 0.582282 0.493032 0.059 Uiso 1 1 calc R U . . .
C409 C 0.1243(3) 0.4980(3) 0.5253(2) 0.0414(10) Uani 1 1 d . . . . .
C410 C 0.0563(3) 0.5350(3) 0.5385(3) 0.0439(10) Uani 1 1 d . . . . .
H410 H 0.050651 0.568864 0.562506 0.053 Uiso 1 1 calc R U . . .
C411 C -0.0041(3) 0.5250(3) 0.5182(3) 0.0408(10) Uani 1 1 d . . . . .
C412 C -0.0741(3) 0.5627(3) 0.5326(3) 0.0432(10) Uani 1 1 d . . . . .
H412 H -0.079909 0.596291 0.556932 0.052 Uiso 1 1 calc R U . . .
C413 C -0.1334(2) 0.5525(3) 0.5127(2) 0.0398(9) Uani 1 1 d . . . . .
C414 C -0.2043(3) 0.5952(3) 0.5308(3) 0.0425(10) Uani 1 1 d . . . . .
C415 C -0.2312(3) 0.6060(3) 0.5982(3) 0.0482(11) Uani 1 1 d . . . . .
H415 H -0.204100 0.586805 0.631271 0.058 Uiso 1 1 calc R U . . .
C416 C -0.2971(3) 0.6446(3) 0.6169(3) 0.0478(11) Uani 1 1 d . . . . .
H416 H -0.313842 0.653098 0.661769 0.057 Uiso 1 1 calc R U . . .
C417 C -0.3387(3) 0.6708(3) 0.5705(3) 0.0491(11) Uani 1 1 d . . . . .
C418 C -0.3103(3) 0.6631(3) 0.5019(3) 0.0497(11) Uani 1 1 d . . . . .
H418 H -0.337042 0.683434 0.468547 0.060 Uiso 1 1 calc R U . . .
C419 C -0.2432(3) 0.6258(3) 0.4819(3) 0.0456(11) Uani 1 1 d . . . . .
H419 H -0.224050 0.621317 0.434807 0.055 Uiso 1 1 calc R U . . .
C420 C -0.4150(3) 0.7038(3) 0.5955(3) 0.0597(14) Uani 1 1 d . . . . .
O420 O -0.4580(2) 0.7149(3) 0.5601(3) 0.0730(11) Uani 1 1 d . . . . .
O421 O -0.4384(2) 0.7127(2) 0.6566(2) 0.0645(10) Uani 1 1 d . . . . .
C119 C 0.1038(9) 0.8513(7) 0.2977(9) 0.044(3) Uani 0.620(11) 1 d . . P A 1
C120 C 0.0447(8) 0.8789(8) 0.2698(8) 0.055(3) Uani 0.620(11) 1 d . . P A 1
H120 H 0.019292 0.846741 0.258899 0.066 Uiso 0.620(11) 1 calc R U P A 1
C121 C 0.0231(7) 0.9523(7) 0.2580(7) 0.060(3) Uani 0.620(11) 1 d . . P A 1
H121 H -0.016978 0.969573 0.239076 0.072 Uiso 0.620(11) 1 calc R U P A 1
C122 C 0.0597(6) 1.0031(5) 0.2736(6) 0.055(3) Uani 0.620(11) 1 d D . P A 1
C123 C 0.1174(9) 0.9722(9) 0.3034(8) 0.055(3) Uani 0.620(11) 1 d . . P A 1
H123 H 0.143398 1.003237 0.314874 0.066 Uiso 0.620(11) 1 calc R U P A 1
C124 C 0.1375(9) 0.8961(8) 0.3167(11) 0.051(3) Uani 0.620(11) 1 d . . P A 1
H124 H 0.174645 0.876282 0.339067 0.061 Uiso 0.620(11) 1 calc R U P A 1
C125 C 0.0434(6) 1.0773(5) 0.2513(7) 0.067(3) Uani 0.620(11) 1 d D . P A 1
O125 O 0.0728(12) 1.1232(10) 0.2652(11) 0.087(5) Uani 0.620(11) 1 d . . P A 1
O126 O 0.0008(5) 1.1039(4) 0.2126(5) 0.084(3) Uani 0.620(11) 1 d D . P A 1
C314 C 1.1798(8) 0.0126(7) 0.0592(7) 0.049(3) Uani 0.5 1 d G U P B 1
C319 C 1.2214(9) -0.0507(6) 0.0786(8) 0.048(3) Uani 0.5 1 d G U P B 1
H319 H 1.218105 -0.091290 0.064703 0.057 Uiso 0.5 1 calc R U P B 1
C318 C 1.2678(8) -0.0547(6) 0.1182(8) 0.051(3) Uani 0.5 1 d G U P B 1
H318 H 1.296187 -0.097967 0.131460 0.062 Uiso 0.5 1 calc R U P B 1
C317 C 1.2726(7) 0.0046(6) 0.1385(7) 0.057(2) Uani 0.5 1 d G U P B 1
C316 C 1.2310(8) 0.0680(5) 0.1191(7) 0.054(2) Uani 0.5 1 d G U P B 1
H316 H 1.234244 0.108515 0.132982 0.065 Uiso 0.5 1 calc R U P B 1
C315 C 1.1846(7) 0.0719(6) 0.0795(7) 0.056(3) Uani 0.5 1 d G U P B 1
H315 H 1.156161 0.115194 0.066225 0.067 Uiso 0.5 1 calc R U P B 1
C320 C 1.3160(9) 0.0019(8) 0.1913(8) 0.062(2) Uani 0.5 1 d . U P B 1
O320 O 1.3458(7) -0.0632(7) 0.2149(7) 0.083(3) Uani 0.5 1 d . U P B 1
O321 O 1.3143(7) 0.0516(6) 0.2128(5) 0.060(2) Uani 0.5 1 d . U P B 1
O5 O 1.4555(4) 0.1927(4) 0.0609(3) 0.124(2) 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 C3 1.3900 . ?
C1 C6 1.3900 . ?
C1 C7 1.345(9) . ?
C3 H3 0.9500 . ?
C3 C2 1.3900 . ?
C2 H2 0.9500 . ?
C2 C4 1.3900 . ?
C4 C5 1.3900 . ?
C4 C118 1.651(13) . ?
C5 H5 0.9500 . ?
C5 C6 1.3900 . ?
C6 H6 0.9500 . ?
Ca1 O1 2.395(6) . ?
Ca1 O127 2.952(5) 1_556 ?
Ca1 O128 2.505(4) 1_556 ?
Ca1 O235 2.491(4) 1_565 ?
Ca1 C236 2.972(6) 1_565 ?
Ca1 O236 2.694(4) 1_565 ?
Ca1 O401 2.447(4) . ?
Ca1 C402 2.851(5) . ?
Ca1 O402 2.517(4) . ?
Ca1 C420 2.904(5) 1_655 ?
Ca1 O420 2.414(4) 1_655 ?
Ca1 O421 2.774(4) 1_655 ?
Ca2 O2 2.410(9) . ?
Ca2 O102 2.260(6) . ?
Ca2 O127 2.339(5) 1_556 ?
Ca2 O201 2.286(4) 2_567 ?
Ca2 O235 2.385(5) 1_565 ?
Ca2 O401 2.358(4) . ?
Ca3 O3A 2.384(4) . ?
Ca3 O3B 2.334(4) . ?
Ca3 O7 2.31(2) 2_576 ?
Ca3 O101 2.232(4) . ?
Ca3 O202 2.313(5) 2_567 ?
Ca3 C225 3.213(6) . ?
Ca3 O225 2.273(5) . ?
Ca3 O125 2.427(17) 2_576 ?
O3B H3BA 0.8699 . ?
O3B H3BB 0.8700 . ?
Ca4 Ca5 3.5378(14) 1_455 ?
Ca4 O128 2.313(4) 2_665 ?
Ca4 O136 2.287(4) . ?
Ca4 O228 2.356(4) . ?
Ca4 O236 2.327(4) 2_656 ?
Ca4 O301 2.288(3) . ?
Ca4 O421 2.282(3) 2_566 ?
Ca5 O21 2.257(17) . ?
Ca5 O135 2.463(5) 1_655 ?
Ca5 C136 2.833(6) 1_655 ?
Ca5 O136 2.513(4) 1_655 ?
Ca5 O227 2.497(4) 1_655 ?
Ca5 C228 2.878(5) 1_655 ?
Ca5 O228 2.526(4) 1_655 ?
Ca5 O301 2.748(4) 1_655 ?
Ca5 C302 2.899(5) 1_655 ?
Ca5 O302 2.443(4) 1_655 ?
Ca5 O321 2.329(11) . ?
Ca5 O5 2.348(5) . ?
C7 O7 1.256(8) . ?
C7 O8 1.269(8) . ?
C14 C15 1.3900 . ?
C14 C19 1.3900 . ?
C14 C313 1.505(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.3900 . ?
C16 H16 0.9500 . ?
C16 C17 1.3900 . ?
C17 C18 1.3900 . ?
C17 C20 1.341(9) . ?
C18 H18 0.9500 . ?
C18 C19 1.3900 . ?
C19 H19 0.9500 . ?
C20 O20 1.267(8) . ?
C20 O21 1.255(8) . ?
O101 C102 1.258(7) . ?
C102 O102 1.256(8) . ?
C102 C103 1.489(8) . ?
C103 C104 1.388(7) . ?
C103 C108 1.393(8) . ?
C104 H104 0.9500 . ?
C104 C105 1.368(8) . ?
C105 H105 0.9500 . ?
C105 C106 1.398(8) . ?
C106 C107 1.405(8) . ?
C106 C109 1.479(7) . ?
C107 H107 0.9500 . ?
C107 C108 1.359(8) . ?
C108 H108 0.9500 . ?
C109 C110 1.382(8) . ?
C109 C118 1.449(8) . ?
C110 H110 0.9500 . ?
C110 C111 1.415(7) . ?
C111 C112 1.413(7) . ?
C111 C116 1.434(8) . ?
C112 H112 0.9500 . ?
C112 C113 1.361(7) . ?
C113 C114 1.434(8) . ?
C113 C140 1.491(7) . ?
C114 C115 1.365(7) . ?
C114 C132 1.491(7) . ?
C115 H115 0.9500 . ?
C115 C116 1.417(7) . ?
C116 C117 1.410(7) . ?
C117 H117 0.9500 . ?
C117 C118 1.367(7) . ?
C118 C119 1.393(14) . ?
O127 C128 1.248(7) . ?
C128 O128 1.257(7) . ?
C128 C129 1.502(7) . ?
C129 C130 1.399(7) . ?
C129 C134 1.389(8) . ?
C130 H130 0.9500 . ?
C130 C131 1.362(7) . ?
C131 H131 0.9500 . ?
C131 C132 1.414(8) . ?
C132 C133 1.384(8) . ?
C133 H133 0.9500 . ?
C133 C134 1.371(7) . ?
C134 H134 0.9500 . ?
O135 C136 1.274(7) . ?
C136 O136 1.263(7) . ?
C136 C137 1.494(8) . ?
C137 C138 1.384(8) . ?
C137 C142 1.379(8) . ?
C138 H138 0.9500 . ?
C138 C139 1.389(7) . ?
C139 H139 0.9500 . ?
C139 C140 1.389(8) . ?
C140 C141 1.385(8) . ?
C141 H141 0.9500 . ?
C141 C142 1.402(8) . ?
C142 H142 0.9500 . ?
O201 C202 1.266(7) . ?
C202 O202 1.260(7) . ?
C202 C203 1.485(7) . ?
C203 C204 1.382(8) . ?
C203 C208 1.396(8) . ?
C204 H204 0.9500 . ?
C204 C205 1.374(8) . ?
C205 H205 0.9500 . ?
C205 C206 1.396(9) . ?
C206 C207 1.397(8) . ?
C206 C209 1.488(7) . ?
C207 H207 0.9500 . ?
C207 C208 1.385(7) . ?
C208 H208 0.9500 . ?
C209 C210 1.374(8) . ?
C209 C218 1.442(8) . ?
C210 H210 0.9500 . ?
C210 C211 1.414(7) . ?
C211 C212 1.428(7) . ?
C211 C216 1.410(8) . ?
C212 H212 0.9500 . ?
C212 C213 1.388(8) . ?
C213 C214 1.427(8) . ?
C213 C240 1.494(7) . ?
C214 C215 1.367(7) . ?
C214 C232 1.492(7) . ?
C215 H215 0.9500 . ?
C215 C216 1.411(7) . ?
C216 C217 1.398(7) . ?
C217 H217 0.9500 . ?
C217 C218 1.386(7) . ?
C218 C219 1.492(7) . ?
C219 C220 1.400(8) . ?
C219 C224 1.387(8) . ?
C220 H220 0.9500 . ?
C220 C221 1.395(8) . ?
C221 H221 0.9500 . ?
C221 C222 1.379(9) . ?
C222 C223 1.399(9) . ?
C222 C225 1.413(6) . ?
C223 H223 0.9500 . ?
C223 C224 1.418(8) . ?
C224 H224 0.9500 . ?
C225 O225 1.257(7) . ?
C225 O226 1.282(8) . ?
O227 C228 1.263(7) . ?
C228 O228 1.287(6) . ?
C228 C229 1.497(7) . ?
C229 C230 1.390(7) . ?
C229 C234 1.409(8) . ?
C230 H230 0.9500 . ?
C230 C231 1.415(8) . ?
C231 H231 0.9500 . ?
C231 C232 1.355(8) . ?
C232 C233 1.417(7) . ?
C233 H233 0.9500 . ?
C233 C234 1.363(7) . ?
C234 H234 0.9500 . ?
O235 C236 1.253(8) . ?
C236 O236 1.257(7) . ?
C236 C237 1.489(7) . ?
C237 C238 1.366(9) . ?
C237 C242 1.392(9) . ?
C238 H238 0.9500 . ?
C238 C239 1.395(9) . ?
C239 H239 0.9500 . ?
C239 C240 1.384(10) . ?
C240 C241 1.385(9) . ?
C241 H241 0.9500 . ?
C241 C242 1.389(8) . ?
C242 H242 0.9500 . ?
O301 C302 1.258(7) . ?
C302 O302 1.258(8) . ?
C302 C303 1.501(6) . ?
C303 C304 1.401(7) . ?
C303 C308 1.378(8) . ?
C304 H304 0.9500 . ?
C304 C305 1.376(7) . ?
C305 H305 0.9500 . ?
C305 C306 1.373(8) . ?
C306 C307 1.405(7) . ?
C306 C309 1.494(6) . ?
C307 H307 0.9500 . ?
C307 C308 1.374(7) . ?
C308 H308 0.9500 . ?
C309 C310 1.353(8) . ?
C309 C313 1.447(7) 2_755 ?
C310 H310 0.9500 . ?
C310 C311 1.432(7) . ?
C311 C311 1.421(10) 2_755 ?
C311 C312 1.404(8) . ?
C312 H312 0.9500 . ?
C312 C313 1.384(7) . ?
C313 C314 1.540(11) . ?
O401 C402 1.261(6) . ?
C402 O402 1.251(7) . ?
C402 C403 1.484(7) . ?
C403 C404 1.391(7) . ?
C403 C408 1.408(7) . ?
C404 H404 0.9500 . ?
C404 C405 1.367(7) . ?
C405 H405 0.9500 . ?
C405 C406 1.398(6) . ?
C406 C407 1.391(6) . ?
C406 C409 1.493(7) . ?
C407 H407 0.9500 . ?
C407 C408 1.384(7) . ?
C408 H408 0.9500 . ?
C409 C410 1.388(6) . ?
C409 C413 1.450(6) 2_566 ?
C410 H410 0.9500 . ?
C410 C411 1.397(7) . ?
C411 C411 1.421(8) 2_566 ?
C411 C412 1.426(6) . ?
C412 H412 0.9500 . ?
C412 C413 1.375(7) . ?
C413 C414 1.500(6) . ?
C414 C415 1.404(6) . ?
C414 C419 1.391(7) . ?
C415 H415 0.9500 . ?
C415 C416 1.388(6) . ?
C416 H416 0.9500 . ?
C416 C417 1.383(7) . ?
C417 C418 1.397(7) . ?
C417 C420 1.498(6) . ?
C418 H418 0.9500 . ?
C418 C419 1.395(6) . ?
C419 H419 0.9500 . ?
C420 O420 1.239(7) . ?
C420 O421 1.264(7) . ?
C119 C120 1.407(15) . ?
C119 C124 1.362(15) . ?
C120 H120 0.9500 . ?
C120 C121 1.385(15) . ?
C121 H121 0.9500 . ?
C121 C122 1.437(15) . ?
C122 C123 1.417(14) . ?
C122 C125 1.358(7) . ?
C123 H123 0.9500 . ?
C123 C124 1.421(15) . ?
C124 H124 0.9500 . ?
C125 O125 1.254(16) . ?
C125 O126 1.281(7) . ?
C314 C319 1.3900 . ?
C314 C315 1.3900 . ?
C319 H319 0.9500 . ?
C319 C318 1.3900 . ?
C318 H318 0.9500 . ?
C318 C317 1.3900 . ?
C317 C316 1.3900 . ?
C317 C320 1.586(16) . ?
C316 H316 0.9500 . ?
C316 C315 1.3900 . ?
C315 H315 0.9500 . ?
C320 O320 1.310(18) . ?
C320 O321 1.205(15) . ?

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
C3 C1 C6 120.0 . . ?
C7 C1 C3 122.8(14) . . ?
C7 C1 C6 116.6(14) . . ?
C1 C3 H3 120.0 . . ?
C1 C3 C2 120.0 . . ?
C2 C3 H3 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C2 C3 120.0 . . ?
C4 C2 H2 120.0 . . ?
C2 C4 C5 120.0 . . ?
C2 C4 C118 115.5(14) . . ?
C5 C4 C118 124.3(14) . . ?
C4 C5 H5 120.0 . . ?
C4 C5 C6 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 H6 120.0 . . ?
C5 C6 C1 120.0 . . ?
C5 C6 H6 120.0 . . ?
O1 Ca1 O127 79.45(18) . 1_556 ?
O1 Ca1 O128 75.14(16) . 1_556 ?
O1 Ca1 O235 141.5(2) . 1_565 ?
O1 Ca1 C236 147.29(18) . 1_565 ?
O1 Ca1 O236 138.40(17) . 1_565 ?
O1 Ca1 O401 83.2(2) . . ?
O1 Ca1 C402 81.08(19) . . ?
O1 Ca1 O402 80.13(19) . . ?
O1 Ca1 C420 79.9(2) . 1_655 ?
O1 Ca1 O420 91.86(18) . 1_655 ?
O1 Ca1 O421 80.47(18) . 1_655 ?
O127 Ca1 C236 72.66(17) 1_556 1_565 ?
O128 Ca1 O127 46.62(12) 1_556 1_556 ?
O128 Ca1 C236 73.37(15) 1_556 1_565 ?
O128 Ca1 O236 66.62(14) 1_556 1_565 ?
O128 Ca1 C402 134.18(17) 1_556 . ?
O128 Ca1 O402 152.04(18) 1_556 . ?
O128 Ca1 C420 92.18(15) 1_556 1_655 ?
O128 Ca1 O421 67.44(12) 1_556 1_655 ?
O235 Ca1 O127 62.65(18) 1_565 1_556 ?
O235 Ca1 O128 83.07(16) 1_565 1_556 ?
O235 Ca1 C236 24.56(16) 1_565 1_565 ?
O235 Ca1 O236 49.58(14) 1_565 1_565 ?
O235 Ca1 C402 92.51(16) 1_565 . ?
O235 Ca1 O402 109.57(17) 1_565 . ?
O235 Ca1 C420 133.05(17) 1_565 1_655 ?
O235 Ca1 O421 119.80(14) 1_565 1_655 ?
O236 Ca1 O127 85.76(14) 1_565 1_556 ?
O236 Ca1 C236 25.03(14) 1_565 1_565 ?
O236 Ca1 C402 138.27(16) 1_565 . ?
O236 Ca1 C420 85.68(14) 1_565 1_655 ?
O236 Ca1 O421 70.45(11) 1_565 1_655 ?
O401 Ca1 O127 65.76(13) . 1_556 ?
O401 Ca1 O128 111.29(14) . 1_556 ?
O401 Ca1 O235 75.55(16) . 1_565 ?
O401 Ca1 C236 100.10(16) . 1_565 ?
O401 Ca1 O236 125.13(14) . 1_565 ?
O401 Ca1 C402 26.14(14) . . ?
O401 Ca1 O402 52.14(13) . . ?
O401 Ca1 C420 146.36(14) . 1_655 ?
O401 Ca1 O421 163.40(15) . 1_655 ?
C402 Ca1 O127 91.11(14) . 1_556 ?
C402 Ca1 C236 115.64(16) . 1_565 ?
C402 Ca1 C420 121.56(15) . 1_655 ?
O402 Ca1 O127 116.15(14) . 1_556 ?
O402 Ca1 C236 127.53(18) . 1_565 ?
O402 Ca1 O236 140.51(17) . 1_565 ?
O402 Ca1 C402 26.01(14) . . ?
O402 Ca1 C420 96.15(15) . 1_655 ?
O402 Ca1 O421 121.11(12) . 1_655 ?
C420 Ca1 O127 137.52(16) 1_655 1_556 ?
C420 Ca1 C236 109.82(17) 1_655 1_565 ?
O420 Ca1 O127 162.34(15) 1_655 1_556 ?
O420 Ca1 O128 116.40(14) 1_655 1_556 ?
O420 Ca1 O235 126.45(18) 1_655 1_565 ?
O420 Ca1 C236 109.88(18) 1_655 1_565 ?
O420 Ca1 O236 90.85(15) 1_655 1_565 ?
O420 Ca1 O401 128.89(14) 1_655 . ?
O420 Ca1 C402 102.78(15) 1_655 . ?
O420 Ca1 O402 76.84(14) 1_655 . ?
O420 Ca1 C420 24.83(16) 1_655 1_655 ?
O420 Ca1 O421 48.97(13) 1_655 1_655 ?
O421 Ca1 O127 113.91(12) 1_655 1_556 ?
O421 Ca1 C236 95.35(14) 1_655 1_565 ?
O421 Ca1 C402 145.29(13) 1_655 . ?
O421 Ca1 C420 25.61(13) 1_655 1_655 ?
O2 Ca2 Ca1 112.1(2) . . ?
O102 Ca2 Ca1 107.84(15) . . ?
O102 Ca2 O2 109.5(3) . . ?
O102 Ca2 O127 162.2(2) . 1_556 ?
O102 Ca2 O201 99.7(2) . 2_567 ?
O102 Ca2 O235 90.7(2) . 1_565 ?
O102 Ca2 O401 89.63(17) . . ?
O127 Ca2 Ca1 54.54(11) 1_556 . ?
O127 Ca2 O2 82.3(2) 1_556 . ?
O127 Ca2 O235 74.43(18) 1_556 1_565 ?
O127 Ca2 O401 78.19(15) 1_556 . ?
O201 Ca2 Ca1 138.24(14) 2_567 . ?
O201 Ca2 O2 86.3(3) 2_567 . ?
O201 Ca2 O127 94.13(17) 2_567 1_556 ?
O201 Ca2 O235 107.3(2) 2_567 1_565 ?
O201 Ca2 O401 168.4(3) 2_567 . ?
O235 Ca2 Ca1 43.36(10) 1_565 . ?
O235 Ca2 O2 153.7(3) 1_565 . ?
O401 Ca2 Ca1 42.22(10) . . ?
O401 Ca2 O2 84.0(3) . . ?
O401 Ca2 O235 79.28(16) . 1_565 ?
O3A Ca3 C225 102.85(16) . . ?
O3A Ca3 O125 85.9(5) . 2_576 ?
O3B Ca3 O3A 85.55(16) . . ?
O3B Ca3 C225 72.09(16) . . ?
O3B Ca3 O125 87.9(5) . 2_576 ?
O7 Ca3 O3A 89.6(7) 2_576 . ?
O7 Ca3 O3B 82.0(7) 2_576 . ?
O7 Ca3 C225 150.0(8) 2_576 . ?
O7 Ca3 O125 7.3(11) 2_576 2_576 ?
O101 Ca3 O3A 175.8(2) . . ?
O101 Ca3 O3B 93.93(17) . . ?
O101 Ca3 O7 86.2(7) . 2_576 ?
O101 Ca3 O202 82.87(17) . 2_567 ?
O101 Ca3 C225 80.91(18) . . ?
O101 Ca3 O225 91.5(2) . . ?
O101 Ca3 O125 90.0(5) . 2_576 ?
O202 Ca3 O3A 96.92(17) 2_567 . ?
O202 Ca3 O3B 169.76(18) 2_567 . ?
O202 Ca3 O7 88.0(7) 2_567 2_576 ?
O202 Ca3 C225 116.73(17) 2_567 . ?
O202 Ca3 O125 82.4(5) 2_567 2_576 ?
O225 Ca3 O3A 92.59(17) . . ?
O225 Ca3 O3B 85.35(17) . . ?
O225 Ca3 O7 167.0(8) . 2_576 ?
O225 Ca3 O202 104.41(18) . 2_567 ?
O225 Ca3 C225 17.75(17) . . ?
O225 Ca3 O125 173.2(5) . 2_576 ?
O125 Ca3 C225 157.2(4) 2_576 . ?
Ca3 O3B H3BA 125.6 . . ?
Ca3 O3B H3BB 126.6 . . ?
H3BA O3B H3BB 104.5 . . ?
Ca5 Ca4 Ca1 173.18(4) 1_455 2_666 ?
O128 Ca4 Ca1 44.52(10) 2_665 2_666 ?
O128 Ca4 Ca5 134.80(11) 2_665 1_455 ?
O128 Ca4 O228 174.01(13) 2_665 . ?
O128 Ca4 O236 76.09(17) 2_665 2_656 ?
O136 Ca4 Ca1 129.23(11) . 2_666 ?
O136 Ca4 Ca5 45.07(10) . 1_455 ?
O136 Ca4 O128 98.50(16) . 2_665 ?
O136 Ca4 O228 78.45(14) . . ?
O136 Ca4 O236 173.09(16) . 2_656 ?
O136 Ca4 O301 78.83(14) . . ?
O228 Ca4 Ca1 134.19(10) . 2_666 ?
O228 Ca4 Ca5 45.50(9) . 1_455 ?
O236 Ca4 Ca1 49.21(11) 2_656 2_666 ?
O236 Ca4 Ca5 137.02(12) 2_656 1_455 ?
O236 Ca4 O228 107.33(16) 2_656 . ?
O301 Ca4 Ca1 135.01(11) . 2_666 ?
O301 Ca4 Ca5 50.94(10) . 1_455 ?
O301 Ca4 O128 105.52(14) . 2_665 ?
O301 Ca4 O228 79.07(14) . . ?
O301 Ca4 O236 98.32(14) . 2_656 ?
O421 Ca4 Ca1 51.20(11) 2_566 2_666 ?
O421 Ca4 Ca5 122.90(11) 2_566 1_455 ?
O421 Ca4 O128 79.50(14) 2_566 2_665 ?
O421 Ca4 O136 96.96(14) 2_566 . ?
O421 Ca4 O228 95.67(14) 2_566 . ?
O421 Ca4 O236 86.37(14) 2_566 2_656 ?
O421 Ca4 O301 173.79(15) 2_566 . ?
O21 Ca5 O5 85.7(4) . . ?
O135 Ca5 C136 26.67(14) 1_655 1_655 ?
O135 Ca5 O136 52.90(13) 1_655 1_655 ?
O135 Ca5 O227 76.04(16) 1_655 1_655 ?
O135 Ca5 C228 92.05(16) 1_655 1_655 ?
O135 Ca5 O228 108.34(13) 1_655 1_655 ?
O135 Ca5 O301 115.06(15) 1_655 1_655 ?
O135 Ca5 C302 134.87(19) 1_655 1_655 ?
C136 Ca5 C228 80.12(17) 1_655 1_655 ?
C136 Ca5 C302 115.79(18) 1_655 1_655 ?
O136 Ca5 C136 26.47(14) 1_655 1_655 ?
O136 Ca5 C228 74.66(15) 1_655 1_655 ?
O136 Ca5 O228 71.27(13) 1_655 1_655 ?
O136 Ca5 O301 66.86(12) 1_655 1_655 ?
O136 Ca5 C302 91.95(15) 1_655 1_655 ?
O227 Ca5 C136 74.70(16) 1_655 1_655 ?
O227 Ca5 O136 81.30(14) 1_655 1_655 ?
O227 Ca5 C228 25.95(14) 1_655 1_655 ?
O227 Ca5 O228 52.50(12) 1_655 1_655 ?
O227 Ca5 O301 118.95(12) 1_655 1_655 ?
O227 Ca5 C302 131.51(15) 1_655 1_655 ?
C228 Ca5 C302 105.99(16) 1_655 1_655 ?
O228 Ca5 C136 87.86(14) 1_655 1_655 ?
O228 Ca5 C228 26.55(13) 1_655 1_655 ?
O228 Ca5 O301 68.05(11) 1_655 1_655 ?
O228 Ca5 C302 79.74(13) 1_655 1_655 ?
O301 Ca5 C136 91.95(14) 1_655 1_655 ?
O301 Ca5 C228 93.78(13) 1_655 1_655 ?
O301 Ca5 C302 25.56(14) 1_655 1_655 ?
O302 Ca5 O135 156.00(18) 1_655 1_655 ?
O302 Ca5 C136 141.23(17) 1_655 1_655 ?
O302 Ca5 O136 116.96(14) 1_655 1_655 ?
O302 Ca5 O227 126.57(17) 1_655 1_655 ?
O302 Ca5 C228 106.57(17) 1_655 1_655 ?
O302 Ca5 O228 84.60(14) 1_655 1_655 ?
O302 Ca5 O301 50.10(14) 1_655 1_655 ?
O302 Ca5 C302 25.45(17) 1_655 1_655 ?
O321 Ca5 O135 112.4(3) . 1_655 ?
O321 Ca5 C136 136.7(3) . 1_655 ?
O321 Ca5 O136 160.4(3) . 1_655 ?
O321 Ca5 O227 82.4(3) . 1_655 ?
O321 Ca5 C228 94.9(3) . 1_655 ?
O321 Ca5 O228 106.6(2) . 1_655 ?
O321 Ca5 O301 131.3(3) . 1_655 ?
O321 Ca5 C302 107.0(3) . 1_655 ?
O321 Ca5 O302 81.6(3) . 1_655 ?
O321 Ca5 O5 96.2(3) . . ?
O5 Ca5 O135 78.5(2) . 1_655 ?
O5 Ca5 C136 87.9(2) . 1_655 ?
O5 Ca5 O136 93.1(2) . 1_655 ?
O5 Ca5 O227 151.7(2) . 1_655 ?
O5 Ca5 C228 167.6(2) . 1_655 ?
O5 Ca5 O228 150.7(2) . 1_655 ?
O5 Ca5 O301 83.2(2) . 1_655 ?
O5 Ca5 C302 76.1(2) . 1_655 ?
O5 Ca5 O302 80.7(2) . 1_655 ?
O7 C7 C1 126.0(18) . . ?
O7 C7 O8 112.7(17) . . ?
O8 C7 C1 120.9(14) . . ?
C15 C14 C19 120.0 . . ?
C15 C14 C313 125.0(12) . . ?
C19 C14 C313 114.6(12) . . ?
C14 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C16 C15 H15 120.0 . . ?
C15 C16 H16 120.0 . . ?
C15 C16 C17 120.0 . . ?
C17 C16 H16 120.0 . . ?
C16 C17 C18 120.0 . . ?
C20 C17 C16 110.6(13) . . ?
C20 C17 C18 129.4(13) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0 . . ?
C19 C18 H18 120.0 . . ?
C14 C19 H19 120.0 . . ?
C18 C19 C14 120.0 . . ?
C18 C19 H19 120.0 . . ?
O20 C20 C17 130.3(16) . . ?
O21 C20 C17 112.9(14) . . ?
O21 C20 O20 116.7(14) . . ?
C20 O21 Ca5 140.3(13) . . ?
C102 O101 Ca3 154.6(6) . . ?
O101 C102 C103 117.6(6) . . ?
O102 C102 O101 122.7(6) . . ?
O102 C102 C103 119.6(5) . . ?
C102 O102 Ca2 152.5(6) . . ?
C104 C103 C102 119.7(5) . . ?
C104 C103 C108 118.8(5) . . ?
C108 C103 C102 121.4(5) . . ?
C103 C104 H104 119.7 . . ?
C105 C104 C103 120.6(6) . . ?
C105 C104 H104 119.7 . . ?
C104 C105 H105 119.6 . . ?
C104 C105 C106 120.9(5) . . ?
C106 C105 H105 119.6 . . ?
C105 C106 C107 118.2(5) . . ?
C105 C106 C109 120.2(5) . . ?
C107 C106 C109 121.6(5) . . ?
C106 C107 H107 119.8 . . ?
C108 C107 C106 120.5(5) . . ?
C108 C107 H107 119.8 . . ?
C103 C108 H108 119.5 . . ?
C107 C108 C103 121.1(5) . . ?
C107 C108 H108 119.5 . . ?
C110 C109 C106 119.1(5) . . ?
C110 C109 C118 118.0(5) . . ?
C118 C109 C106 122.8(5) . . ?
C109 C110 H110 118.3 . . ?
C109 C110 C111 123.3(5) . . ?
C111 C110 H110 118.3 . . ?
C110 C111 C116 118.0(5) . . ?
C112 C111 C110 123.8(5) . . ?
C112 C111 C116 118.2(5) . . ?
C111 C112 H112 119.0 . . ?
C113 C112 C111 121.9(5) . . ?
C113 C112 H112 119.0 . . ?
C112 C113 C114 119.8(5) . . ?
C112 C113 C140 120.4(5) . . ?
C114 C113 C140 119.5(4) . . ?
C113 C114 C132 120.9(5) . . ?
C115 C114 C113 119.7(5) . . ?
C115 C114 C132 119.4(5) . . ?
C114 C115 H115 119.3 . . ?
C114 C115 C116 121.3(5) . . ?
C116 C115 H115 119.3 . . ?
C115 C116 C111 118.9(5) . . ?
C117 C116 C111 118.0(5) . . ?
C117 C116 C115 123.0(5) . . ?
C116 C117 H117 118.2 . . ?
C118 C117 C116 123.6(5) . . ?
C118 C117 H117 118.2 . . ?
C109 C118 C4 119.7(11) . . ?
C117 C118 C4 120.7(11) . . ?
C117 C118 C109 119.0(5) . . ?
C117 C118 C119 116.3(8) . . ?
C119 C118 C109 124.5(8) . . ?
Ca2 O127 Ca1 85.27(14) 1_554 1_554 ?
C128 O127 Ca1 84.6(3) . 1_554 ?
C128 O127 Ca2 148.9(5) . 1_554 ?
O127 C128 Ca1 71.7(3) . 1_554 ?
O127 C128 O128 122.6(5) . . ?
O127 C128 C129 119.9(5) . . ?
O128 C128 Ca1 51.1(3) . 1_554 ?
O128 C128 C129 117.4(5) . . ?
C129 C128 Ca1 166.3(4) . 1_554 ?
Ca4 O128 Ca1 95.12(15) 2_665 1_554 ?
C128 O128 Ca1 105.9(3) . 1_554 ?
C128 O128 Ca4 139.5(4) . 2_665 ?
C130 C129 C128 119.6(5) . . ?
C134 C129 C128 121.9(5) . . ?
C134 C129 C130 118.5(5) . . ?
C129 C130 H130 119.4 . . ?
C131 C130 C129 121.3(5) . . ?
C131 C130 H130 119.4 . . ?
C130 C131 H131 120.1 . . ?
C130 C131 C132 119.9(5) . . ?
C132 C131 H131 120.1 . . ?
C131 C132 C114 120.2(5) . . ?
C133 C132 C114 121.2(5) . . ?
C133 C132 C131 118.6(5) . . ?
C132 C133 H133 119.5 . . ?
C134 C133 C132 121.1(5) . . ?
C134 C133 H133 119.5 . . ?
C129 C134 H134 119.7 . . ?
C133 C134 C129 120.6(5) . . ?
C133 C134 H134 119.7 . . ?
C136 O135 Ca5 93.1(3) . 1_455 ?
O135 C136 Ca5 60.3(3) . 1_455 ?
O135 C136 C137 119.6(5) . . ?
O136 C136 Ca5 62.5(3) . 1_455 ?
O136 C136 O135 121.9(5) . . ?
O136 C136 C137 118.5(5) . . ?
C137 C136 Ca5 168.7(4) . 1_455 ?
Ca4 O136 Ca5 94.82(15) . 1_455 ?
C136 O136 Ca4 160.2(4) . . ?
C136 O136 Ca5 91.0(3) . 1_455 ?
C138 C137 C136 118.9(5) . . ?
C142 C137 C136 121.6(5) . . ?
C142 C137 C138 119.5(5) . . ?
C137 C138 H138 119.9 . . ?
C137 C138 C139 120.2(5) . . ?
C139 C138 H138 119.9 . . ?
C138 C139 H139 119.8 . . ?
C138 C139 C140 120.5(5) . . ?
C140 C139 H139 119.8 . . ?
C139 C140 C113 118.3(5) . . ?
C141 C140 C113 121.9(5) . . ?
C141 C140 C139 119.6(5) . . ?
C140 C141 H141 120.3 . . ?
C140 C141 C142 119.4(5) . . ?
C142 C141 H141 120.3 . . ?
C137 C142 C141 120.8(5) . . ?
C137 C142 H142 119.6 . . ?
C141 C142 H142 119.6 . . ?
C202 O201 Ca2 144.7(4) . 2_567 ?
O201 C202 C203 118.6(5) . . ?
O202 C202 O201 122.8(5) . . ?
O202 C202 C203 118.6(5) . . ?
C202 O202 Ca3 161.8(5) . 2_567 ?
C204 C203 C202 121.1(5) . . ?
C204 C203 C208 118.7(5) . . ?
C208 C203 C202 120.2(5) . . ?
C203 C204 H204 119.5 . . ?
C205 C204 C203 121.0(6) . . ?
C205 C204 H204 119.5 . . ?
C204 C205 H205 119.5 . . ?
C204 C205 C206 121.1(5) . . ?
C206 C205 H205 119.5 . . ?
C205 C206 C207 118.0(5) . . ?
C205 C206 C209 121.2(5) . . ?
C207 C206 C209 120.8(5) . . ?
C206 C207 H207 119.6 . . ?
C208 C207 C206 120.7(5) . . ?
C208 C207 H207 119.6 . . ?
C203 C208 H208 119.7 . . ?
C207 C208 C203 120.5(5) . . ?
C207 C208 H208 119.7 . . ?
C210 C209 C206 118.7(5) . . ?
C210 C209 C218 119.5(5) . . ?
C218 C209 C206 121.9(5) . . ?
C209 C210 H210 118.8 . . ?
C209 C210 C211 122.3(5) . . ?
C211 C210 H210 118.8 . . ?
C210 C211 C212 121.9(5) . . ?
C216 C211 C210 118.5(5) . . ?
C216 C211 C212 119.5(5) . . ?
C211 C212 H212 119.7 . . ?
C213 C212 C211 120.6(5) . . ?
C213 C212 H212 119.7 . . ?
C212 C213 C214 119.1(5) . . ?
C212 C213 C240 119.5(5) . . ?
C214 C213 C240 121.4(5) . . ?
C213 C214 C232 121.8(5) . . ?
C215 C214 C213 120.1(5) . . ?
C215 C214 C232 118.1(5) . . ?
C214 C215 H215 119.0 . . ?
C214 C215 C216 121.9(5) . . ?
C216 C215 H215 119.0 . . ?
C211 C216 C215 118.6(5) . . ?
C217 C216 C211 118.7(5) . . ?
C217 C216 C215 122.7(5) . . ?
C216 C217 H217 118.3 . . ?
C218 C217 C216 123.5(5) . . ?
C218 C217 H217 118.3 . . ?
C209 C218 C219 123.7(4) . . ?
C217 C218 C209 117.5(5) . . ?
C217 C218 C219 118.7(5) . . ?
C220 C219 C218 119.0(5) . . ?
C224 C219 C218 122.8(5) . . ?
C224 C219 C220 118.0(5) . . ?
C219 C220 H220 119.6 . . ?
C221 C220 C219 120.8(5) . . ?
C221 C220 H220 119.6 . . ?
C220 C221 H221 118.4 . . ?
C222 C221 C220 123.1(6) . . ?
C222 C221 H221 118.4 . . ?
C221 C222 C223 115.4(5) . . ?
C221 C222 C225 122.5(6) . . ?
C223 C222 C225 122.1(6) . . ?
C222 C223 H223 118.4 . . ?
C222 C223 C224 123.1(5) . . ?
C224 C223 H223 118.4 . . ?
C219 C224 C223 119.5(6) . . ?
C219 C224 H224 120.3 . . ?
C223 C224 H224 120.3 . . ?
C222 C225 Ca3 143.9(5) . . ?
O225 C225 Ca3 33.4(3) . . ?
O225 C225 C222 118.8(6) . . ?
O225 C225 O226 120.9(5) . . ?
O226 C225 Ca3 91.6(4) . . ?
O226 C225 C222 120.3(6) . . ?
C225 O225 Ca3 128.8(4) . . ?
C228 O227 Ca5 94.1(3) . 1_455 ?
O227 C228 Ca5 60.0(3) . 1_455 ?
O227 C228 O228 121.3(5) . . ?
O227 C228 C229 120.9(5) . . ?
O228 C228 Ca5 61.3(3) . 1_455 ?
O228 C228 C229 117.8(5) . . ?
C229 C228 Ca5 177.9(4) . 1_455 ?
Ca4 O228 Ca5 92.81(13) . 1_455 ?
C228 O228 Ca4 126.4(4) . . ?
C228 O228 Ca5 92.1(3) . 1_455 ?
C230 C229 C228 120.6(5) . . ?
C230 C229 C234 119.3(5) . . ?
C234 C229 C228 120.0(4) . . ?
C229 C230 H230 120.5 . . ?
C229 C230 C231 119.0(5) . . ?
C231 C230 H230 120.5 . . ?
C230 C231 H231 119.2 . . ?
C232 C231 C230 121.5(5) . . ?
C232 C231 H231 119.2 . . ?
C231 C232 C214 121.6(5) . . ?
C231 C232 C233 119.0(5) . . ?
C233 C232 C214 119.2(5) . . ?
C232 C233 H233 119.8 . . ?
C234 C233 C232 120.5(5) . . ?
C234 C233 H233 119.8 . . ?
C229 C234 H234 119.7 . . ?
C233 C234 C229 120.6(5) . . ?
C233 C234 H234 119.7 . . ?
Ca2 O235 Ca1 95.55(17) 1_545 1_545 ?
C236 O235 Ca1 99.7(3) . 1_545 ?
C236 O235 Ca2 149.3(5) . 1_545 ?
O235 C236 Ca1 55.7(3) . 1_545 ?
O235 C236 O236 120.7(5) . . ?
O235 C236 C237 119.2(5) . . ?
O236 C236 Ca1 65.0(3) . 1_545 ?
O236 C236 C237 120.1(6) . . ?
C237 C236 Ca1 174.9(4) . 1_545 ?
Ca4 O236 Ca1 89.96(14) 2_656 1_545 ?
C236 O236 Ca1 90.0(4) . 1_545 ?
C236 O236 Ca4 140.6(4) . 2_656 ?
C238 C237 C236 120.4(6) . . ?
C238 C237 C242 118.8(5) . . ?
C242 C237 C236 120.8(5) . . ?
C237 C238 H238 119.4 . . ?
C237 C238 C239 121.3(7) . . ?
C239 C238 H238 119.4 . . ?
C238 C239 H239 120.1 . . ?
C240 C239 C238 119.8(6) . . ?
C240 C239 H239 120.1 . . ?
C239 C240 C213 118.8(6) . . ?
C239 C240 C241 119.4(5) . . ?
C241 C240 C213 121.8(6) . . ?
C240 C241 H241 120.0 . . ?
C240 C241 C242 120.1(6) . . ?
C242 C241 H241 120.0 . . ?
C237 C242 H242 119.7 . . ?
C241 C242 C237 120.6(6) . . ?
C241 C242 H242 119.7 . . ?
Ca4 O301 Ca5 88.77(11) . 1_455 ?
C302 O301 Ca4 152.2(4) . . ?
C302 O301 Ca5 84.0(3) . 1_455 ?
O301 C302 Ca5 70.5(3) . 1_455 ?
O301 C302 O302 123.3(5) . . ?
O301 C302 C303 117.7(5) . . ?
O302 C302 Ca5 56.5(3) . 1_455 ?
O302 C302 C303 119.0(5) . . ?
C303 C302 Ca5 158.9(4) . 1_455 ?
C302 O302 Ca5 98.0(4) . 1_455 ?
C304 C303 C302 120.4(5) . . ?
C308 C303 C302 121.4(5) . . ?
C308 C303 C304 118.2(4) . . ?
C303 C304 H304 119.5 . . ?
C305 C304 C303 121.0(5) . . ?
C305 C304 H304 119.5 . . ?
C304 C305 H305 119.6 . . ?
C306 C305 C304 120.7(5) . . ?
C306 C305 H305 119.6 . . ?
C305 C306 C307 118.4(4) . . ?
C305 C306 C309 121.7(5) . . ?
C307 C306 C309 119.8(5) . . ?
C306 C307 H307 119.6 . . ?
C308 C307 C306 120.7(5) . . ?
C308 C307 H307 119.6 . . ?
C303 C308 H308 119.6 . . ?
C307 C308 C303 120.9(5) . . ?
C307 C308 H308 119.6 . . ?
C310 C309 C306 118.2(4) . . ?
C310 C309 C313 119.6(4) . 2_755 ?
C313 C309 C306 121.9(5) 2_755 . ?
C309 C310 H310 118.7 . . ?
C309 C310 C311 122.6(4) . . ?
C311 C310 H310 118.7 . . ?
C311 C311 C310 117.6(6) 2_755 . ?
C312 C311 C310 122.8(4) . . ?
C312 C311 C311 119.6(6) . 2_755 ?
C311 C312 H312 119.0 . . ?
C313 C312 C311 122.0(5) . . ?
C313 C312 H312 119.0 . . ?
C309 C313 C14 120.1(8) 2_755 . ?
C309 C313 C314 123.9(6) 2_755 . ?
C312 C313 C14 121.1(8) . . ?
C312 C313 C309 118.5(5) . 2_755 ?
C312 C313 C314 117.4(6) . . ?
Ca2 O401 Ca1 97.44(14) . . ?
C402 O401 Ca1 95.1(3) . . ?
C402 O401 Ca2 152.0(4) . . ?
O401 C402 Ca1 58.8(3) . . ?
O401 C402 C403 118.9(5) . . ?
O402 C402 Ca1 61.9(3) . . ?
O402 C402 O401 120.6(5) . . ?
O402 C402 C403 120.4(5) . . ?
C403 C402 Ca1 176.4(4) . . ?
C402 O402 Ca1 92.1(3) . . ?
C404 C403 C402 120.6(4) . . ?
C404 C403 C408 118.0(4) . . ?
C408 C403 C402 121.3(5) . . ?
C403 C404 H404 119.3 . . ?
C405 C404 C403 121.4(4) . . ?
C405 C404 H404 119.3 . . ?
C404 C405 H405 119.5 . . ?
C404 C405 C406 121.0(5) . . ?
C406 C405 H405 119.5 . . ?
C405 C406 C409 117.0(4) . . ?
C407 C406 C405 118.3(4) . . ?
C407 C406 C409 124.4(4) . . ?
C406 C407 H407 119.6 . . ?
C408 C407 C406 120.8(4) . . ?
C408 C407 H407 119.6 . . ?
C403 C408 H408 119.8 . . ?
C407 C408 C403 120.4(4) . . ?
C407 C408 H408 119.8 . . ?
C410 C409 C406 116.3(4) . . ?
C410 C409 C413 118.2(4) . 2_566 ?
C413 C409 C406 125.4(4) 2_566 . ?
C409 C410 H410 118.4 . . ?
C409 C410 C411 123.2(4) . . ?
C411 C410 H410 118.4 . . ?
C410 C411 C411 118.8(5) . 2_566 ?
C410 C411 C412 122.9(4) . . ?
C411 C411 C412 118.3(5) 2_566 . ?
C411 C412 H412 118.7 . . ?
C413 C412 C411 122.7(4) . . ?
C413 C412 H412 118.7 . . ?
C409 C413 C414 123.3(4) 2_566 . ?
C412 C413 C409 118.8(4) . 2_566 ?
C412 C413 C414 117.9(4) . . ?
C415 C414 C413 119.2(4) . . ?
C419 C414 C413 121.8(4) . . ?
C419 C414 C415 119.1(4) . . ?
C414 C415 H415 119.8 . . ?
C416 C415 C414 120.4(5) . . ?
C416 C415 H415 119.8 . . ?
C415 C416 H416 119.8 . . ?
C417 C416 C415 120.5(4) . . ?
C417 C416 H416 119.8 . . ?
C416 C417 C418 119.2(4) . . ?
C416 C417 C420 120.2(4) . . ?
C418 C417 C420 120.5(5) . . ?
C417 C418 H418 119.7 . . ?
C419 C418 C417 120.6(5) . . ?
C419 C418 H418 119.7 . . ?
C414 C419 C418 119.9(4) . . ?
C414 C419 H419 120.0 . . ?
C418 C419 H419 120.0 . . ?
C417 C420 Ca1 148.5(4) . 1_455 ?
O420 C420 Ca1 54.9(3) . 1_455 ?
O420 C420 C417 119.5(5) . . ?
O420 C420 O421 120.6(5) . . ?
O421 C420 Ca1 71.4(3) . 1_455 ?
O421 C420 C417 119.5(5) . . ?
C420 O420 Ca1 100.3(4) . 1_455 ?
Ca4 O421 Ca1 88.92(11) 2_566 1_455 ?
C420 O421 Ca1 83.0(3) . 1_455 ?
C420 O421 Ca4 156.6(4) . 2_566 ?
C118 C119 C120 120.1(12) . . ?
C124 C119 C118 119.4(12) . . ?
C124 C119 C120 119.6(9) . . ?
C119 C120 H120 119.6 . . ?
C121 C120 C119 120.8(10) . . ?
C121 C120 H120 119.6 . . ?
C120 C121 H121 119.1 . . ?
C120 C121 C122 121.7(9) . . ?
C122 C121 H121 119.1 . . ?
C123 C122 C121 115.5(8) . . ?
C125 C122 C121 118.6(10) . . ?
C125 C122 C123 125.5(10) . . ?
C122 C123 H123 119.0 . . ?
C122 C123 C124 122.0(11) . . ?
C124 C123 H123 119.0 . . ?
C119 C124 C123 120.3(10) . . ?
C119 C124 H124 119.8 . . ?
C123 C124 H124 119.8 . . ?
O125 C125 C122 120.7(13) . . ?
O125 C125 O126 117.6(12) . . ?
O126 C125 C122 121.7(10) . . ?
C125 O125 Ca3 134.9(14) . 2_576 ?
C319 C314 C313 114.1(7) . . ?
C319 C314 C315 120.0 . . ?
C315 C314 C313 125.5(7) . . ?
C314 C319 H319 120.0 . . ?
C318 C319 C314 120.0 . . ?
C318 C319 H319 120.0 . . ?
C319 C318 H318 120.0 . . ?
C317 C318 C319 120.0 . . ?
C317 C318 H318 120.0 . . ?
C318 C317 C316 120.0 . . ?
C318 C317 C320 124.0(8) . . ?
C316 C317 C320 115.7(8) . . ?
C317 C316 H316 120.0 . . ?
C315 C316 C317 120.0 . . ?
C315 C316 H316 120.0 . . ?
C314 C315 H315 120.0 . . ?
C316 C315 C314 120.0 . . ?
C316 C315 H315 120.0 . . ?
O320 C320 C317 112.5(11) . . ?
O321 C320 C317 122.7(11) . . ?
O321 C320 O320 124.4(13) . . ?
C320 O321 Ca5 141.7(10) . . ?

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
_geom_hbond_publ_flag
O3B H3BA O226 0.87 2.13 2.740(6) 126.2 . yes
O3B H3BB O227 0.87 1.96 2.824(6) 175.3 2_566 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C3 C2 C4 0.0 . . . . ?
C1 C7 O7 Ca3 162(2) . . . 2_576 ?
C3 C1 C6 C5 0.0 . . . . ?
C3 C1 C7 O7 -155(2) . . . . ?
C3 C1 C7 O8 32(3) . . . . ?
C3 C2 C4 C5 0.0 . . . . ?
C3 C2 C4 C118 -174(2) . . . . ?
C2 C4 C5 C6 0.0 . . . . ?
C2 C4 C118 C109 -134.4(11) . . . . ?
C2 C4 C118 C117 55.0(18) . . . . ?
C4 C5 C6 C1 0.0 . . . . ?
C5 C4 C118 C109 51.4(16) . . . . ?
C5 C4 C118 C117 -119.2(13) . . . . ?
C6 C1 C3 C2 0.0 . . . . ?
C6 C1 C7 O7 16(3) . . . . ?
C6 C1 C7 O8 -157(2) . . . . ?
Ca1 O127 C128 O128 -4.1(6) 1_554 . . . ?
Ca1 O127 C128 C129 172.0(5) 1_554 . . . ?
Ca1 C128 O128 Ca4 118.5(6) 1_554 . . 2_665 ?
Ca1 C128 C129 C130 134.7(15) 1_554 . . . ?
Ca1 C128 C129 C134 -43.9(19) 1_554 . . . ?
Ca1 O235 C236 O236 0.8(7) 1_545 . . . ?
Ca1 O235 C236 C237 179.4(5) 1_545 . . . ?
Ca1 C236 O236 Ca4 -89.9(5) 1_545 . . 2_656 ?
Ca1 O401 C402 O402 1.4(7) . . . . ?
Ca1 O401 C402 C403 -176.7(5) . . . . ?
Ca1 C420 O421 Ca4 -70.5(9) 1_455 . . 2_566 ?
Ca2 O127 C128 Ca1 -71.6(6) 1_554 . . 1_554 ?
Ca2 O127 C128 O128 -75.7(9) 1_554 . . . ?
Ca2 O127 C128 C129 100.5(8) 1_554 . . . ?
Ca2 O201 C202 O202 2.3(16) 2_567 . . . ?
Ca2 O201 C202 C203 -179.5(7) 2_567 . . . ?
Ca2 O235 C236 Ca1 118.8(8) 1_545 . . 1_545 ?
Ca2 O235 C236 O236 119.5(7) 1_545 . . . ?
Ca2 O235 C236 C237 -61.8(11) 1_545 . . . ?
Ca2 O401 C402 Ca1 116.4(9) . . . . ?
Ca2 O401 C402 O402 117.8(8) . . . . ?
Ca2 O401 C402 C403 -60.4(12) . . . . ?
Ca3 O101 C102 O102 -60.7(15) . . . . ?
Ca3 O101 C102 C103 122.6(9) . . . . ?
Ca4 O301 C302 Ca5 75.7(7) . . . 1_455 ?
Ca4 O301 C302 O302 54.7(11) . . . . ?
Ca4 O301 C302 C303 -125.5(7) . . . . ?
Ca5 O135 C136 O136 11.2(6) 1_455 . . . ?
Ca5 O135 C136 C137 -166.9(5) 1_455 . . . ?
Ca5 C136 O136 Ca4 -107.3(12) 1_455 . . . ?
Ca5 C136 C137 C138 -81(2) 1_455 . . . ?
Ca5 C136 C137 C142 96.6(19) 1_455 . . . ?
Ca5 O227 C228 O228 -0.6(6) 1_455 . . . ?
Ca5 O227 C228 C229 177.7(5) 1_455 . . . ?
Ca5 C228 O228 Ca4 95.1(3) 1_455 . . . ?
Ca5 O301 C302 O302 -21.0(6) 1_455 . . . ?
Ca5 O301 C302 C303 158.7(5) 1_455 . . . ?
Ca5 C302 C303 C304 -81.2(13) 1_455 . . . ?
Ca5 C302 C303 C308 99.1(12) 1_455 . . . ?
C7 C1 C3 C2 171(2) . . . . ?
C7 C1 C6 C5 -171.4(19) . . . . ?
O8 C7 O7 Ca3 -25(4) . . . 2_576 ?
C14 C15 C16 C17 0.0 . . . . ?
C15 C14 C19 C18 0.0 . . . . ?
C15 C14 C313 C309 -45.5(14) . . . 2_755 ?
C15 C14 C313 C312 128.9(10) . . . . ?
C15 C16 C17 C18 0.0 . . . . ?
C15 C16 C17 C20 179.7(16) . . . . ?
C16 C17 C18 C19 0.0 . . . . ?
C16 C17 C20 O20 14(3) . . . . ?
C16 C17 C20 O21 -169.6(15) . . . . ?
C17 C18 C19 C14 0.0 . . . . ?
C17 C20 O21 Ca5 -138.9(16) . . . . ?
C18 C17 C20 O20 -166.6(18) . . . . ?
C18 C17 C20 O21 10(3) . . . . ?
C19 C14 C15 C16 0.0 . . . . ?
C19 C14 C313 C309 142.4(8) . . . 2_755 ?
C19 C14 C313 C312 -43.2(13) . . . . ?
C20 C17 C18 C19 -179.6(19) . . . . ?
O20 C20 O21 Ca5 38(3) . . . . ?
O101 C102 O102 Ca2 46.3(18) . . . . ?
O101 C102 C103 C104 170.9(7) . . . . ?
O101 C102 C103 C108 -9.5(11) . . . . ?
C102 C103 C104 C105 -180.0(6) . . . . ?
C102 C103 C108 C107 -179.5(6) . . . . ?
O102 C102 C103 C104 -5.9(11) . . . . ?
O102 C102 C103 C108 173.7(7) . . . . ?
C103 C102 O102 Ca2 -137.1(9) . . . . ?
C103 C104 C105 C106 -0.2(10) . . . . ?
C104 C103 C108 C107 0.2(9) . . . . ?
C104 C105 C106 C107 -0.5(9) . . . . ?
C104 C105 C106 C109 -179.3(6) . . . . ?
C105 C106 C107 C108 1.1(9) . . . . ?
C105 C106 C109 C110 50.4(8) . . . . ?
C105 C106 C109 C118 -129.6(6) . . . . ?
C106 C107 C108 C103 -0.9(9) . . . . ?
C106 C109 C110 C111 -178.5(6) . . . . ?
C106 C109 C118 C4 10.3(13) . . . . ?
C106 C109 C118 C117 -179.0(5) . . . . ?
C106 C109 C118 C119 6.3(12) . . . . ?
C107 C106 C109 C110 -128.3(6) . . . . ?
C107 C106 C109 C118 51.7(8) . . . . ?
C108 C103 C104 C105 0.4(10) . . . . ?
C109 C106 C107 C108 179.8(5) . . . . ?
C109 C110 C111 C112 179.9(6) . . . . ?
C109 C110 C111 C116 -2.7(9) . . . . ?
C109 C118 C119 C120 -143.2(9) . . . . ?
C109 C118 C119 C124 47.5(13) . . . . ?
C110 C109 C118 C4 -169.7(12) . . . . ?
C110 C109 C118 C117 1.1(8) . . . . ?
C110 C109 C118 C119 -173.7(9) . . . . ?
C110 C111 C112 C113 178.9(6) . . . . ?
C110 C111 C116 C115 179.0(5) . . . . ?
C110 C111 C116 C117 1.3(8) . . . . ?
C111 C112 C113 C114 2.1(9) . . . . ?
C111 C112 C113 C140 -170.9(5) . . . . ?
C111 C116 C117 C118 1.2(9) . . . . ?
C112 C111 C116 C115 -3.3(8) . . . . ?
C112 C111 C116 C117 179.0(5) . . . . ?
C112 C113 C114 C115 -3.7(8) . . . . ?
C112 C113 C114 C132 174.3(5) . . . . ?
C112 C113 C140 C139 124.1(6) . . . . ?
C112 C113 C140 C141 -52.4(8) . . . . ?
C113 C114 C115 C116 1.7(8) . . . . ?
C113 C114 C132 C131 119.2(6) . . . . ?
C113 C114 C132 C133 -59.7(7) . . . . ?
C113 C140 C141 C142 175.6(5) . . . . ?
C114 C113 C140 C139 -49.0(7) . . . . ?
C114 C113 C140 C141 134.5(6) . . . . ?
C114 C115 C116 C111 1.8(8) . . . . ?
C114 C115 C116 C117 179.4(5) . . . . ?
C114 C132 C133 C134 -179.6(5) . . . . ?
C115 C114 C132 C131 -62.7(7) . . . . ?
C115 C114 C132 C133 118.3(6) . . . . ?
C115 C116 C117 C118 -176.4(5) . . . . ?
C116 C111 C112 C113 1.4(9) . . . . ?
C116 C117 C118 C4 168.3(12) . . . . ?
C116 C117 C118 C109 -2.4(9) . . . . ?
C116 C117 C118 C119 172.8(9) . . . . ?
C117 C118 C119 C120 41.9(14) . . . . ?
C117 C118 C119 C124 -127.4(10) . . . . ?
C118 C4 C5 C6 174(2) . . . . ?
C118 C109 C110 C111 1.5(9) . . . . ?
C118 C119 C120 C121 -166.1(12) . . . . ?
C118 C119 C124 C123 164.7(14) . . . . ?
O127 C128 O128 Ca1 5.0(7) . . . 1_554 ?
O127 C128 O128 Ca4 123.5(6) . . . 2_665 ?
O127 C128 C129 C130 -11.4(9) . . . . ?
O127 C128 C129 C134 170.0(6) . . . . ?
C128 C129 C130 C131 -177.4(5) . . . . ?
C128 C129 C134 C133 178.9(5) . . . . ?
O128 C128 C129 C130 165.0(5) . . . . ?
O128 C128 C129 C134 -13.7(8) . . . . ?
C129 C128 O128 Ca1 -171.2(4) . . . 1_554 ?
C129 C128 O128 Ca4 -52.7(8) . . . 2_665 ?
C129 C130 C131 C132 -1.5(9) . . . . ?
C130 C129 C134 C133 0.3(8) . . . . ?
C130 C131 C132 C114 -178.8(5) . . . . ?
C130 C131 C132 C133 0.1(8) . . . . ?
C131 C132 C133 C134 1.4(8) . . . . ?
C132 C114 C115 C116 -176.3(5) . . . . ?
C132 C133 C134 C129 -1.6(9) . . . . ?
C134 C129 C130 C131 1.3(9) . . . . ?
O135 C136 O136 Ca4 -118.3(10) . . . . ?
O135 C136 O136 Ca5 -10.9(6) . . . 1_455 ?
O135 C136 C137 C138 5.4(8) . . . . ?
O135 C136 C137 C142 -177.3(5) . . . . ?
C136 C137 C138 C139 175.9(5) . . . . ?
C136 C137 C142 C141 -175.5(5) . . . . ?
O136 C136 C137 C138 -172.8(5) . . . . ?
O136 C136 C137 C142 4.6(8) . . . . ?
C137 C136 O136 Ca4 59.9(14) . . . . ?
C137 C136 O136 Ca5 167.2(5) . . . 1_455 ?
C137 C138 C139 C140 0.0(8) . . . . ?
C138 C137 C142 C141 1.8(8) . . . . ?
C138 C139 C140 C113 -175.4(5) . . . . ?
C138 C139 C140 C141 1.3(8) . . . . ?
C139 C140 C141 C142 -1.0(8) . . . . ?
C140 C113 C114 C115 169.4(5) . . . . ?
C140 C113 C114 C132 -12.6(8) . . . . ?
C140 C141 C142 C137 -0.6(8) . . . . ?
C142 C137 C138 C139 -1.5(8) . . . . ?
O201 C202 O202 Ca3 -74.7(16) . . . 2_567 ?
O201 C202 C203 C204 161.1(7) . . . . ?
O201 C202 C203 C208 -17.0(11) . . . . ?
C202 C203 C204 C205 -177.2(7) . . . . ?
C202 C203 C208 C207 177.2(6) . . . . ?
O202 C202 C203 C204 -20.6(10) . . . . ?
O202 C202 C203 C208 161.3(6) . . . . ?
C203 C202 O202 Ca3 107.1(12) . . . 2_567 ?
C203 C204 C205 C206 0.6(12) . . . . ?
C204 C203 C208 C207 -0.9(10) . . . . ?
C204 C205 C206 C207 -2.1(10) . . . . ?
C204 C205 C206 C209 -178.6(7) . . . . ?
C205 C206 C207 C208 2.1(10) . . . . ?
C205 C206 C209 C210 54.3(9) . . . . ?
C205 C206 C209 C218 -126.7(7) . . . . ?
C206 C207 C208 C203 -0.6(10) . . . . ?
C206 C209 C210 C211 177.3(6) . . . . ?
C206 C209 C218 C217 -176.9(5) . . . . ?
C206 C209 C218 C219 6.3(9) . . . . ?
C207 C206 C209 C210 -122.1(7) . . . . ?
C207 C206 C209 C218 56.9(9) . . . . ?
C208 C203 C204 C205 0.9(11) . . . . ?
C209 C206 C207 C208 178.6(6) . . . . ?
C209 C210 C211 C212 -178.1(6) . . . . ?
C209 C210 C211 C216 -0.3(10) . . . . ?
C209 C218 C219 C220 -145.0(6) . . . . ?
C209 C218 C219 C224 40.0(8) . . . . ?
C210 C209 C218 C217 2.1(8) . . . . ?
C210 C209 C218 C219 -174.7(5) . . . . ?
C210 C211 C212 C213 176.8(6) . . . . ?
C210 C211 C216 C215 -179.0(6) . . . . ?
C210 C211 C216 C217 1.8(9) . . . . ?
C211 C212 C213 C214 3.8(10) . . . . ?
C211 C212 C213 C240 -175.4(6) . . . . ?
C211 C216 C217 C218 -1.4(9) . . . . ?
C212 C211 C216 C215 -1.1(9) . . . . ?
C212 C211 C216 C217 179.7(6) . . . . ?
C212 C213 C214 C215 -4.6(10) . . . . ?
C212 C213 C214 C232 173.6(6) . . . . ?
C212 C213 C240 C239 115.4(8) . . . . ?
C212 C213 C240 C241 -67.1(8) . . . . ?
C213 C214 C215 C216 2.5(9) . . . . ?
C213 C214 C232 C231 135.5(7) . . . . ?
C213 C214 C232 C233 -49.7(8) . . . . ?
C213 C240 C241 C242 -174.5(5) . . . . ?
C214 C213 C240 C239 -63.7(9) . . . . ?
C214 C213 C240 C241 113.7(7) . . . . ?
C214 C215 C216 C211 0.3(9) . . . . ?
C214 C215 C216 C217 179.5(6) . . . . ?
C214 C232 C233 C234 -175.1(5) . . . . ?
C215 C214 C232 C231 -46.3(9) . . . . ?
C215 C214 C232 C233 128.5(6) . . . . ?
C215 C216 C217 C218 179.5(5) . . . . ?
C216 C211 C212 C213 -0.9(10) . . . . ?
C216 C217 C218 C209 -0.6(8) . . . . ?
C216 C217 C218 C219 176.4(5) . . . . ?
C217 C218 C219 C220 38.1(7) . . . . ?
C217 C218 C219 C224 -136.8(6) . . . . ?
C218 C209 C210 C211 -1.7(9) . . . . ?
C218 C219 C220 C221 -174.2(5) . . . . ?
C218 C219 C224 C223 174.8(5) . . . . ?
C219 C220 C221 C222 -0.2(8) . . . . ?
C220 C219 C224 C223 -0.2(8) . . . . ?
C220 C221 C222 C223 -1.3(8) . . . . ?
C220 C221 C222 C225 178.5(5) . . . . ?
C221 C222 C223 C224 2.1(8) . . . . ?
C221 C222 C225 Ca3 -168.1(5) . . . . ?
C221 C222 C225 O225 161.4(6) . . . . ?
C221 C222 C225 O226 -19.0(9) . . . . ?
C222 C223 C224 C219 -1.4(8) . . . . ?
C222 C225 O225 Ca3 147.2(4) . . . . ?
C223 C222 C225 Ca3 11.6(10) . . . . ?
C223 C222 C225 O225 -18.9(9) . . . . ?
C223 C222 C225 O226 160.7(5) . . . . ?
C224 C219 C220 C221 0.9(8) . . . . ?
C225 C222 C223 C224 -177.6(5) . . . . ?
O226 C225 O225 Ca3 -32.5(8) . . . . ?
O227 C228 O228 Ca4 95.6(6) . . . . ?
O227 C228 O228 Ca5 0.6(6) . . . 1_455 ?
O227 C228 C229 C230 -1.4(10) . . . . ?
O227 C228 C229 C234 -177.9(6) . . . . ?
C228 C229 C230 C231 -178.3(6) . . . . ?
C228 C229 C234 C233 176.1(6) . . . . ?
O228 C228 C229 C230 176.9(6) . . . . ?
O228 C228 C229 C234 0.5(9) . . . . ?
C229 C228 O228 Ca4 -82.7(6) . . . . ?
C229 C228 O228 Ca5 -177.8(5) . . . 1_455 ?
C229 C230 C231 C232 3.1(10) . . . . ?
C230 C229 C234 C233 -0.4(9) . . . . ?
C230 C231 C232 C214 172.7(6) . . . . ?
C230 C231 C232 C233 -2.1(10) . . . . ?
C231 C232 C233 C234 -0.2(9) . . . . ?
C232 C214 C215 C216 -175.7(5) . . . . ?
C232 C233 C234 C229 1.4(9) . . . . ?
C234 C229 C230 C231 -1.8(10) . . . . ?
O235 C236 O236 Ca1 -0.7(6) . . . 1_545 ?
O235 C236 O236 Ca4 -90.6(7) . . . 2_656 ?
O235 C236 C237 C238 -10.2(10) . . . . ?
O235 C236 C237 C242 171.0(6) . . . . ?
C236 C237 C238 C239 -177.9(8) . . . . ?
C236 C237 C242 C241 179.0(6) . . . . ?
O236 C236 C237 C238 168.4(7) . . . . ?
O236 C236 C237 C242 -10.4(9) . . . . ?
C237 C236 O236 Ca1 -179.3(5) . . . 1_545 ?
C237 C236 O236 Ca4 90.8(8) . . . 2_656 ?
C237 C238 C239 C240 -0.1(14) . . . . ?
C238 C237 C242 C241 0.2(10) . . . . ?
C238 C239 C240 C213 175.7(7) . . . . ?
C238 C239 C240 C241 -1.8(12) . . . . ?
C239 C240 C241 C242 2.9(10) . . . . ?
C240 C213 C214 C215 174.6(6) . . . . ?
C240 C213 C214 C232 -7.2(9) . . . . ?
C240 C241 C242 C237 -2.1(9) . . . . ?
C242 C237 C238 C239 0.9(13) . . . . ?
O301 C302 O302 Ca5 23.9(7) . . . 1_455 ?
O301 C302 C303 C304 170.7(5) . . . . ?
O301 C302 C303 C308 -9.0(8) . . . . ?
C302 C303 C304 C305 -179.1(5) . . . . ?
C302 C303 C308 C307 -179.3(5) . . . . ?
O302 C302 C303 C304 -9.5(8) . . . . ?
O302 C302 C303 C308 170.8(6) . . . . ?
C303 C302 O302 Ca5 -155.9(5) . . . 1_455 ?
C303 C304 C305 C306 -2.0(9) . . . . ?
C304 C303 C308 C307 0.9(8) . . . . ?
C304 C305 C306 C307 1.8(8) . . . . ?
C304 C305 C306 C309 179.9(5) . . . . ?
C305 C306 C307 C308 -0.3(8) . . . . ?
C305 C306 C309 C310 -128.4(6) . . . . ?
C305 C306 C309 C313 45.7(8) . . . 2_755 ?
C306 C307 C308 C303 -1.1(8) . . . . ?
C306 C309 C310 C311 173.1(5) . . . . ?
C307 C306 C309 C310 49.7(7) . . . . ?
C307 C306 C309 C313 -136.2(6) . . . 2_755 ?
C308 C303 C304 C305 0.6(8) . . . . ?
C309 C306 C307 C308 -178.4(5) . . . . ?
C309 C310 C311 C311 -0.6(11) . . . 2_755 ?
C309 C310 C311 C312 -178.5(6) . . . . ?
C309 C313 C314 C319 -39.1(10) 2_755 . . . ?
C309 C313 C314 C315 148.4(8) 2_755 . . . ?
C310 C311 C312 C313 179.7(6) . . . . ?
C311 C311 C312 C313 1.9(11) 2_755 . . . ?
C311 C312 C313 C14 -174.7(10) . . . . ?
C311 C312 C313 C309 -0.2(9) . . . 2_755 ?
C311 C312 C313 C314 -175.4(7) . . . . ?
C312 C313 C314 C319 135.9(7) . . . . ?
C312 C313 C314 C315 -36.6(12) . . . . ?
C313 C14 C15 C16 -171.7(15) . . . . ?
C313 C14 C19 C18 172.5(14) . . . . ?
C313 C309 C310 C311 -1.1(9) 2_755 . . . ?
C313 C314 C319 C318 -172.9(11) . . . . ?
C313 C314 C315 C316 172.1(12) . . . . ?
O401 C402 O402 Ca1 -1.4(7) . . . . ?
O401 C402 C403 C404 -5.9(9) . . . . ?
O401 C402 C403 C408 169.8(6) . . . . ?
C402 C403 C404 C405 173.3(5) . . . . ?
C402 C403 C408 C407 -172.9(5) . . . . ?
O402 C402 C403 C404 176.0(6) . . . . ?
O402 C402 C403 C408 -8.4(9) . . . . ?
C403 C402 O402 Ca1 176.7(5) . . . . ?
C403 C404 C405 C406 -0.6(8) . . . . ?
C404 C403 C408 C407 2.9(8) . . . . ?
C404 C405 C406 C407 3.4(7) . . . . ?
C404 C405 C406 C409 -170.6(5) . . . . ?
C405 C406 C407 C408 -3.0(7) . . . . ?
C405 C406 C409 C410 46.3(6) . . . . ?
C405 C406 C409 C413 -136.0(5) . . . 2_566 ?
C406 C407 C408 C403 -0.1(8) . . . . ?
C406 C409 C410 C411 179.0(4) . . . . ?
C407 C406 C409 C410 -127.2(5) . . . . ?
C407 C406 C409 C413 50.5(7) . . . 2_566 ?
C408 C403 C404 C405 -2.5(8) . . . . ?
C409 C406 C407 C408 170.5(5) . . . . ?
C409 C410 C411 C411 -0.4(9) . . . 2_566 ?
C409 C410 C411 C412 179.4(5) . . . . ?
C409 C413 C414 C415 144.2(5) 2_566 . . . ?
C409 C413 C414 C419 -37.1(7) 2_566 . . . ?
C410 C411 C412 C413 -179.8(5) . . . . ?
C411 C411 C412 C413 0.0(8) 2_566 . . . ?
C411 C412 C413 C409 -0.8(7) . . . 2_566 ?
C411 C412 C413 C414 180.0(4) . . . . ?
C412 C413 C414 C415 -36.5(7) . . . . ?
C412 C413 C414 C419 142.1(5) . . . . ?
C413 C409 C410 C411 1.2(7) 2_566 . . . ?
C413 C414 C415 C416 -179.3(4) . . . . ?
C413 C414 C419 C418 178.0(5) . . . . ?
C414 C415 C416 C417 2.1(8) . . . . ?
C415 C414 C419 C418 -3.4(7) . . . . ?
C415 C416 C417 C418 -4.7(8) . . . . ?
C415 C416 C417 C420 172.5(5) . . . . ?
C416 C417 C418 C419 3.4(8) . . . . ?
C416 C417 C420 Ca1 -97.7(8) . . . 1_455 ?
C416 C417 C420 O420 -167.7(6) . . . . ?
C416 C417 C420 O421 5.3(8) . . . . ?
C417 C418 C419 C414 0.7(8) . . . . ?
C417 C420 O420 Ca1 143.1(5) . . . 1_455 ?
C417 C420 O421 Ca1 -147.5(5) . . . 1_455 ?
C417 C420 O421 Ca4 141.9(7) . . . 2_566 ?
C418 C417 C420 Ca1 79.4(9) . . . 1_455 ?
C418 C417 C420 O420 9.5(9) . . . . ?
C418 C417 C420 O421 -177.6(5) . . . . ?
C419 C414 C415 C416 2.0(8) . . . . ?
C420 C417 C418 C419 -173.8(5) . . . . ?
O420 C420 O421 Ca1 25.3(6) . . . 1_455 ?
O420 C420 O421 Ca4 -45.2(14) . . . 2_566 ?
O421 C420 O420 Ca1 -29.8(7) . . . 1_455 ?
C119 C120 C121 C122 0.0(16) . . . . ?
C120 C119 C124 C123 -4.6(15) . . . . ?
C120 C121 C122 C123 -1.6(15) . . . . ?
C120 C121 C122 C125 171.3(10) . . . . ?
C121 C122 C123 C124 0.1(15) . . . . ?
C121 C122 C125 O125 178.5(14) . . . . ?
C121 C122 C125 O126 -4.9(16) . . . . ?
C122 C123 C124 C119 3.0(16) . . . . ?
C122 C125 O125 Ca3 173.4(11) . . . 2_576 ?
C123 C122 C125 O125 -9(2) . . . . ?
C123 C122 C125 O126 167.2(12) . . . . ?
C124 C119 C120 C121 3.2(14) . . . . ?
C125 C122 C123 C124 -172.2(12) . . . . ?
O126 C125 O125 Ca3 -3(3) . . . 2_576 ?
C314 C319 C318 C317 0.0 . . . . ?
C319 C314 C315 C316 0.0 . . . . ?
C319 C318 C317 C316 0.0 . . . . ?
C319 C318 C317 C320 173.0(12) . . . . ?
C318 C317 C316 C315 0.0 . . . . ?
C318 C317 C320 O320 -1.2(16) . . . . ?
C318 C317 C320 O321 -174.2(11) . . . . ?
C317 C316 C315 C314 0.0 . . . . ?
C317 C320 O321 Ca5 -105.1(16) . . . . ?
C316 C317 C320 O320 172.1(10) . . . . ?
C316 C317 C320 O321 -0.9(17) . . . . ?
C315 C314 C319 C318 0.0 . . . . ?
C320 C317 C316 C315 -173.5(11) . . . . ?
O320 C320 O321 Ca5 82.8(19) . . . . ?

_platon_squeeze_details          
;
Electron density in the voids were initially modelled as up to 15 partially
occupied water molecules with no major improvement in the refinement R values 
so the refinement was eventually completed using the Squeeze algorithm in
Platon giving the details in the table below.

Taking the volume of H20 to be about 40 and the number of electrons as 18 

31 waters would be 31 x 18 = 558 electrons
31 waters have a volume of 31 x 40 = 1240

The unit cell contains 31 water molecules which have been treated as a diffuse 
contribution to the overall scattering without specific atom positions as 
calculated by SQUEEZE routine in PLATON then the structure refined with Olex2. 
;
# SQUEEZE RESULTS (Version = 250724)                                            
# Note: Data are Listed for all Voids in the P1 Unit Cell                       
# i.e. Centre of Gravity, Solvent Accessible Volume,                            
# Recovered number of Electrons in the Void and                                 
# Details about the Squeezed Material                                         
_platon_squeeze_special_details  ?
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 -0.013 0.006 0.503 1976 551 ' '

_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'
