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

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

data_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1552733'
_audit_update_record             
;
2017-05-28 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT094_a_sq                
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.43 Report
RESPONSE: Not all electron density related to disordered guests has been removed by SQUEEZE routine
;
_vrf_PLAT420_a_sq                
;
PROBLEM: D-H Without Acceptor       O1W    --  H1WA   ...     Please Check
RESPONSE: The data crystal contained a very large region of highly disordered solvent comprising approximately 41% of the unit cell.  The program SQUEEZE in PLATON was used to remove the contribution to the scattering due to the disordered solvent.
;
_vrf_PLAT420_a_sq_2              
;
PROBLEM: D-H Without Acceptor       O1W    -- *H1WB   ...     Please Check
RESPONSE: The data crystal contained a very large region of highly disordered solvent comprising approximately 41% of the unit cell.  The program SQUEEZE in PLATON was used to remove the contribution to the scattering due to the disordered solvent.
;
# Added during the CSD deposition process: Sunday 28 May 2017 12:50 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C108 H64 Ca4 O21'
_chemical_formula_sum            'C108 H64 Ca4 O21'
_chemical_formula_weight         1857.91

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2490 0.3510 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   13.5460(19)
_cell_length_b                   13.5460(19)
_cell_length_c                   34.908(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6405(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    46635
_cell_measurement_theta_min      0.90
_cell_measurement_theta_max      30.91

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    0.963
_exptl_crystal_F_000             1920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.255
_shelx_estimated_absorpt_T_min   0.975
_shelx_estimated_absorpt_T_max   0.987
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995, 1997)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.750
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  
;
Beijing Synchrotron Radiation Facility, beam line station 
1W2B equipped with a MarCCD-165 detector (the monochrome 
X-ray source is produced by accelerator and selected by 
a double crystal monochromator)
;
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            11487
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.435
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_full        26.744
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3190
_reflns_number_gt                2448
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
marccd, control software for MarCCD-165 detector
;
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger., SQUEEZE, SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0752P)²+5.9324P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3190
_refine_ls_number_parameters     160
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1447
_refine_ls_wR_factor_gt          0.1367
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.39203(4) 0.35193(4) 0.0000 0.02386(18) Uani 1 2 d S T P . .
O1 O 0.5000 0.5000 0.0000 0.0329(10) Uani 1 8 d S T P . .
O2 O 0.53845(13) 0.32408(16) 0.04412(6) 0.0594(6) Uani 1 1 d . . . . .
O3 O 0.40968(13) 0.22858(12) 0.05069(4) 0.0372(4) Uani 1 1 d . . . . .
O1W O 0.2311(2) 0.2818(3) 0.0000 0.0978(14) Uani 1 2 d DS T P . .
H1WA H 0.1547(18) 0.301(4) 0.0000 0.098 Uiso 1 2 d DS U P . .
H1WB H 0.208(4) 0.226(3) -0.0139(17) 0.098 Uiso 0.5 1 d D U P . .
C1 C 0.49426(17) 0.25451(15) 0.06093(6) 0.0289(5) Uani 1 1 d . . . . .
C2 C 0.54348(16) 0.20500(16) 0.09412(6) 0.0291(5) Uani 1 1 d . . . . .
C3 C 0.64096(18) 0.22839(18) 0.10385(7) 0.0399(6) Uani 1 1 d . . . . .
H3 H 0.6748 0.2788 0.0902 0.048 Uiso 1 1 calc R U . . .
C4 C 0.68863(18) 0.17848(19) 0.13328(8) 0.0412(6) Uani 1 1 d . . . . .
H4 H 0.7548 0.1943 0.1398 0.049 Uiso 1 1 calc R U . . .
C5 C 0.63801(16) 0.10488(16) 0.15306(6) 0.0300(5) Uani 1 1 d . . . . .
C6 C 0.53950(16) 0.08441(14) 0.14398(6) 0.0249(5) Uani 1 1 d . . . . .
C7 C 0.49202(16) 0.13337(14) 0.11476(6) 0.0256(5) Uani 1 1 d . . . . .
H7 H 0.4252 0.1186 0.1087 0.031 Uiso 1 1 calc R U . . .
C8 C 0.5000 0.0000 0.16870(8) 0.0247(6) Uani 1 2 d S T P . .
C9 C 0.59181(16) -0.02709(15) 0.19167(6) 0.0260(5) Uani 1 1 d . . . . .
C10 C 0.67045(17) 0.03517(16) 0.18264(6) 0.0302(5) Uani 1 1 d . . . . .
C11 C 0.76235(18) 0.02310(19) 0.19981(7) 0.0382(6) Uani 1 1 d . . . . .
H11 H 0.8156 0.0659 0.1936 0.046 Uiso 1 1 calc R U . . .
C12 C 0.77478(19) -0.0528(2) 0.22622(7) 0.0417(6) Uani 1 1 d . . . . .
H12 H 0.8369 -0.0619 0.2384 0.050 Uiso 1 1 calc R U . . .
C13 C 0.69657(19) -0.11557(18) 0.23491(7) 0.0388(6) Uani 1 1 d . . . . .
H13 H 0.7060 -0.1674 0.2529 0.047 Uiso 1 1 calc R U . . .
C14 C 0.60446(18) -0.10363(17) 0.21764(6) 0.0322(5) Uani 1 1 d . . . . .
H14 H 0.5515 -0.1470 0.2235 0.039 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
Ca1 O2 2.3292(17) 4_565 ?
Ca1 O2 2.3292(17) 11_565 ?
Ca1 O1W 2.378(3) . ?
Ca1 O3 2.4452(16) 10 ?
Ca1 O3 2.4453(16) . ?
Ca1 O1 2.4824(7) . ?
Ca1 O2 2.5394(19) . ?
Ca1 O2 2.5395(19) 10 ?
Ca1 C1 2.861(2) 10 ?
Ca1 Ca1 3.5106(9) 11_565 ?
Ca1 Ca1 3.5107(9) 3_655 ?
Ca1 H1WB 3.06(4) . ?
O1 Ca1 2.4824(7) 9_665 ?
O1 Ca1 2.4824(7) 11_565 ?
O1 Ca1 2.4824(7) 3_655 ?
O2 C1 1.261(3) . ?
O2 Ca1 2.3291(17) 3_655 ?
O3 C1 1.251(3) . ?
O1W H1WA 1.067(19) . ?
O1W H1WB 0.95(2) . ?
C1 C2 1.495(3) . ?
C2 C7 1.395(3) . ?
C2 C3 1.400(3) . ?
C3 C4 1.389(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.399(3) . ?
C5 C10 1.467(3) . ?
C6 C7 1.376(3) . ?
C6 C8 1.529(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.525(3) . ?
C8 C9 1.525(3) 2_655 ?
C8 C6 1.529(2) 2_655 ?
C9 C14 1.388(3) . ?
C9 C10 1.395(3) . ?
C10 C11 1.391(3) . ?
C11 C12 1.392(3) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(3) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ca1 O2 82.80(11) 4_565 11_565 ?
O2 Ca1 O1W 83.81(9) 4_565 . ?
O2 Ca1 O1W 83.81(9) 11_565 . ?
O2 Ca1 O3 162.32(8) 4_565 10 ?
O2 Ca1 O3 89.76(7) 11_565 10 ?
O1W Ca1 O3 79.45(8) . 10 ?
O2 Ca1 O3 89.75(6) 4_565 . ?
O2 Ca1 O3 162.32(8) 11_565 . ?
O1W Ca1 O3 79.45(8) . . ?
O3 Ca1 O3 92.70(8) 10 . ?
O2 Ca1 O1 73.60(5) 4_565 . ?
O2 Ca1 O1 73.60(5) 11_565 . ?
O1W Ca1 O1 149.63(10) . . ?
O3 Ca1 O1 119.64(4) 10 . ?
O3 Ca1 O1 119.64(4) . . ?
O2 Ca1 O2 90.13(12) 4_565 . ?
O2 Ca1 O2 143.56(8) 11_565 . ?
O1W Ca1 O2 131.06(7) . . ?
O3 Ca1 O2 105.13(7) 10 . ?
O3 Ca1 O2 51.92(6) . . ?
O1 Ca1 O2 70.11(4) . . ?
O2 Ca1 O2 143.56(8) 4_565 10 ?
O2 Ca1 O2 90.13(12) 11_565 10 ?
O1W Ca1 O2 131.06(7) . 10 ?
O3 Ca1 O2 51.92(6) 10 10 ?
O3 Ca1 O2 105.13(7) . 10 ?
O1 Ca1 O2 70.11(4) . 10 ?
O2 Ca1 O2 74.68(10) . 10 ?
O2 Ca1 C1 167.72(7) 4_565 10 ?
O2 Ca1 C1 89.64(7) 11_565 10 ?
O1W Ca1 C1 105.05(8) . 10 ?
O3 Ca1 C1 25.77(6) 10 10 ?
O3 Ca1 C1 100.11(6) . 10 ?
O1 Ca1 C1 95.02(5) . 10 ?
O2 Ca1 C1 90.25(7) . 10 ?
O2 Ca1 C1 26.15(6) 10 10 ?
O2 Ca1 Ca1 46.29(5) 4_565 11_565 ?
O2 Ca1 Ca1 46.29(5) 11_565 11_565 ?
O1W Ca1 Ca1 104.63(10) . 11_565 ?
O3 Ca1 Ca1 133.65(4) 10 11_565 ?
O3 Ca1 Ca1 133.64(4) . 11_565 ?
O1 Ca1 Ca1 45.0 . 11_565 ?
O2 Ca1 Ca1 105.52(5) . 11_565 ?
O2 Ca1 Ca1 105.52(5) 10 11_565 ?
C1 Ca1 Ca1 122.05(4) 10 11_565 ?
O2 Ca1 Ca1 106.96(6) 4_565 3_655 ?
O2 Ca1 Ca1 106.96(6) 11_565 3_655 ?
O1W Ca1 Ca1 165.37(10) . 3_655 ?
O3 Ca1 Ca1 90.52(5) 10 3_655 ?
O3 Ca1 Ca1 90.52(5) . 3_655 ?
O1 Ca1 Ca1 45.0 . 3_655 ?
O2 Ca1 Ca1 41.53(4) . 3_655 ?
O2 Ca1 Ca1 41.53(4) 10 3_655 ?
C1 Ca1 Ca1 65.99(5) 10 3_655 ?
Ca1 Ca1 Ca1 90.0 11_565 3_655 ?
O2 Ca1 H1WB 97.9(8) 4_565 . ?
O2 Ca1 H1WB 85.8(11) 11_565 . ?
O1W Ca1 H1WB 14.0(8) . . ?
O3 Ca1 H1WB 65.5(8) 10 . ?
O3 Ca1 H1WB 79.4(12) . . ?
O1 Ca1 H1WB 158.4(10) . . ?
O2 Ca1 H1WB 130.7(11) . . ?
O2 Ca1 H1WB 117.3(9) 10 . ?
C1 Ca1 H1WB 91.2(8) 10 . ?
Ca1 Ca1 H1WB 115.0(9) 11_565 . ?
Ca1 Ca1 H1WB 153.2(7) 3_655 . ?
Ca1 O1 Ca1 180.0 . 9_665 ?
Ca1 O1 Ca1 90.0 . 11_565 ?
Ca1 O1 Ca1 90.0 9_665 11_565 ?
Ca1 O1 Ca1 90.0 . 3_655 ?
Ca1 O1 Ca1 90.0 9_665 3_655 ?
Ca1 O1 Ca1 180.0 11_565 3_655 ?
C1 O2 Ca1 154.9(2) . 3_655 ?
C1 O2 Ca1 91.28(14) . . ?
Ca1 O2 Ca1 92.19(6) 3_655 . ?
C1 O3 Ca1 96.00(13) . . ?
Ca1 O1W H1WA 142(3) . . ?
Ca1 O1W H1WB 128(3) . . ?
H1WA O1W H1WB 82.6(19) . . ?
O3 C1 O2 120.8(2) . . ?
O3 C1 C2 120.27(19) . . ?
O2 C1 C2 118.9(2) . . ?
C7 C2 C3 120.2(2) . . ?
C7 C2 C1 119.3(2) . . ?
C3 C2 C1 120.48(19) . . ?
C2 C3 C4 120.5(2) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 119.1(2) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C4 C5 C6 119.9(2) . . ?
C4 C5 C10 131.5(2) . . ?
C6 C5 C10 108.52(19) . . ?
C7 C6 C5 121.21(19) . . ?
C7 C6 C8 127.96(18) . . ?
C5 C6 C8 110.73(17) . . ?
C6 C7 C2 119.0(2) . . ?
C6 C7 H7 120.5 . . ?
C2 C7 H7 120.5 . . ?
C9 C8 C9 116.5(2) . 2_655 ?
C9 C8 C6 113.72(11) . 2_655 ?
C9 C8 C6 101.03(11) 2_655 2_655 ?
C9 C8 C6 101.03(11) . . ?
C9 C8 C6 113.72(11) 2_655 . ?
C6 C8 C6 111.3(2) 2_655 . ?
C14 C9 C10 120.3(2) . . ?
C14 C9 C8 128.61(19) . . ?
C10 C9 C8 111.02(17) . . ?
C11 C10 C9 121.0(2) . . ?
C11 C10 C5 130.3(2) . . ?
C9 C10 C5 108.64(19) . . ?
C10 C11 C12 118.7(2) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 120.2(2) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 121.1(2) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C9 C14 C13 118.6(2) . . ?
C9 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?

_refine_diff_density_max         1.324
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.055



_exptl_crystal_recrystallization_method 'Solvothermal method'
####################################################################### 
# 
# 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_a_sq
_database_code_depnum_ccdc_archive 'CCDC 1470061'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_RINTA01_a_sq                
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: The crystal was minute in one direction, and Rint value is biased by the large number of weak reflections measured. Enough data was measured to solve the structure to meet the reqiurement of Chemistry study.
;
_vrf_THETM01_a_sq                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
RESPONSE: The data was collected at BRSF (synchrotron) with a wavelength of 0.7200 angstroms. 
;
# Added during the CSD deposition process: Tuesday 23 May 2017 09:41 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H26 Ca O7'
_chemical_formula_weight         538.59

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.263(2)
_cell_length_b                   15.960(3)
_cell_length_c                   33.531(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5492.3(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    105(2)
_cell_measurement_reflns_used    2728
_cell_measurement_theta_min      0.90
_cell_measurement_theta_max      25.00

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.274
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.997
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9865
_exptl_absorpt_correction_T_max  0.9973
_exptl_absorpt_process_details   
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995, 1997)
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      105(2)
_diffrn_radiation_wavelength     0.720
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  
;
Beijing Synchrotron Radiation Facility, beam line station 
1W2B equipped with a MarCCD-165 detector (the monochrome 
X-ray source is produced by accelerator and selected by 
a double crystal monochromator)
;
_diffrn_measurement_method       'phi scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14681
_diffrn_reflns_av_unetI/netI     0.1191
_diffrn_reflns_av_R_equivalents  0.1724
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.357
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4651
_reflns_number_gt                2910
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
marccd, control software for MarCCD-165 detector
;
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger., SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1164P)²+8.8053P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0033(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4651
_refine_ls_number_parameters     359
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1371
_refine_ls_R_factor_gt           0.0858
_refine_ls_wR_factor_ref         0.2403
_refine_ls_wR_factor_gt          0.2028
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.30797(10) 0.93713(6) 0.74236(3) 0.0212(3) Uani 1 1 d . . . . .
O1 O 0.4872(4) 0.9111(2) 0.79806(11) 0.0253(9) Uani 1 1 d . . . . .
O2 O 0.3650(4) 0.8091(2) 0.77447(12) 0.0277(9) Uani 1 1 d . . . . .
O3 O 0.1323(4) 0.9807(2) 0.78199(11) 0.0259(9) Uani 1 1 d . . . . .
O4 O -0.0138(4) 1.0770(2) 0.80065(11) 0.0246(9) Uani 1 1 d . . . . .
O5 O 0.1489(4) 0.8293(3) 0.72639(13) 0.0329(10) Uani 1 1 d . . . . .
H5A H 0.147(7) 0.786(5) 0.747(2) 0.05(2) Uiso 1 1 d . . . . .
O6 O 0.1987(4) 0.9932(3) 0.68547(11) 0.0292(9) Uani 1 1 d . . . . .
H6A H 0.123(8) 1.035(5) 0.690(2) 0.06(2) Uiso 1 1 d . . . . .
O7 O 0.3912(4) 1.0748(2) 0.74991(12) 0.0290(9) Uani 1 1 d D . . . .
H7A H 0.483(2) 1.073(3) 0.7415(16) 0.035 Uiso 1 1 d D U . . .
C1 C 0.4460(5) 0.8368(3) 0.79978(16) 0.0225(12) Uani 1 1 d . . . . .
C2 C 0.4863(5) 0.7807(3) 0.83296(16) 0.0228(12) Uani 1 1 d . . . . .
C3 C 0.4173(6) 0.7061(3) 0.83953(18) 0.0276(13) Uani 1 1 d . . . . .
H3 H 0.3457 0.6923 0.8228 0.033 Uiso 1 1 calc R U . . .
C4 C 0.4524(6) 0.6520(4) 0.87030(18) 0.0303(13) Uani 1 1 d . . . . .
H4 H 0.4051 0.6018 0.8749 0.036 Uiso 1 1 calc R U . . .
C5 C 0.5578(6) 0.6730(3) 0.89406(17) 0.0258(12) Uani 1 1 d . . . . .
C6 C 0.6296(5) 0.7463(3) 0.88703(16) 0.0218(11) Uani 1 1 d . . . . .
C7 C 0.5928(5) 0.8006(3) 0.85667(15) 0.0190(11) Uani 1 1 d . . . . .
H7 H 0.6401 0.8508 0.8522 0.023 Uiso 1 1 calc R U . . .
C8 C 0.7500 0.7500 0.9134(2) 0.0227(16) Uani 1 2 d S T P . .
C9 C 0.7352(6) 0.6691(3) 0.93767(16) 0.0224(12) Uani 1 1 d . . . . .
C10 C 0.6225(5) 0.6256(3) 0.92600(16) 0.0233(12) Uani 1 1 d . . . . .
C11 C 0.5910(6) 0.5501(3) 0.94385(17) 0.0283(13) Uani 1 1 d . . . . .
H11 H 0.5131 0.5214 0.9368 0.034 Uiso 1 1 calc R U . . .
C12 C 0.6761(6) 0.5166(4) 0.97251(18) 0.0303(13) Uani 1 1 d . . . . .
H12 H 0.6570 0.4640 0.9844 0.036 Uiso 1 1 calc R U . . .
C13 C 0.7868(6) 0.5591(4) 0.98349(16) 0.0273(13) Uani 1 1 d . . . . .
H13 H 0.8426 0.5359 1.0032 0.033 Uiso 1 1 calc R U . . .
C14 C 0.8188(6) 0.6363(3) 0.96601(16) 0.0256(12) Uani 1 1 d . . . . .
H14 H 0.8959 0.6652 0.9734 0.031 Uiso 1 1 calc R U . . .
C15 C 0.0946(5) 1.0403(3) 0.80415(16) 0.0221(12) Uani 1 1 d . . . . .
C16 C 0.1825(5) 1.0674(3) 0.83753(15) 0.0219(11) Uani 1 1 d . . . . .
C17 C 0.2864(5) 1.0165(3) 0.84901(16) 0.0241(12) Uani 1 1 d . . . . .
H17 H 0.2989 0.9641 0.8361 0.029 Uiso 1 1 calc R U . . .
C18 C 0.3707(5) 1.0405(3) 0.87846(18) 0.0281(13) Uani 1 1 d . . . . .
H18 H 0.4396 1.0044 0.8864 0.034 Uiso 1 1 calc R U . . .
C19 C 0.3546(5) 1.1184(3) 0.89680(17) 0.0231(12) Uani 1 1 d . . . . .
C20 C 0.2499(5) 1.1687(3) 0.88560(16) 0.0199(11) Uani 1 1 d . . . . .
C21 C 0.1629(5) 1.1441(3) 0.85668(16) 0.0225(12) Uani 1 1 d . . . . .
H21 H 0.0909 1.1787 0.8498 0.027 Uiso 1 1 calc R U . . .
C22 C 0.2500 1.2500 0.9101(2) 0.0206(16) Uani 1 2 d S T P . .
C23 C 0.3728(5) 1.2396(3) 0.93481(16) 0.0210(11) Uani 1 1 d . . . . .
C24 C 0.4323(5) 1.1616(3) 0.92691(16) 0.0216(11) Uani 1 1 d . . . . .
C25 C 0.5451(5) 1.1396(4) 0.94662(17) 0.0289(13) Uani 1 1 d . . . . .
H25 H 0.5849 1.0869 0.9416 0.035 Uiso 1 1 calc R U . . .
C26 C 0.6005(6) 1.1948(4) 0.97403(19) 0.0323(14) Uani 1 1 d . . . . .
H26 H 0.6782 1.1798 0.9877 0.039 Uiso 1 1 calc R U . . .
C27 C 0.5423(6) 1.2714(4) 0.98132(18) 0.0312(14) Uani 1 1 d . . . . .
H27 H 0.5815 1.3090 0.9997 0.037 Uiso 1 1 calc R U . . .
C28 C 0.4273(5) 1.2947(3) 0.96224(16) 0.0245(12) Uani 1 1 d . . . . .
H28 H 0.3870 1.3470 0.9678 0.029 Uiso 1 1 calc R U . . .
C29 C 0.0801(7) 0.8038(4) 0.6918(2) 0.0392(16) Uani 1 1 d . . . . .
H29A H 0.0085 0.8430 0.6867 0.059 Uiso 1 1 calc R U . . .
H29B H 0.0448 0.7474 0.6959 0.059 Uiso 1 1 calc R U . . .
H29C H 0.1395 0.8034 0.6689 0.059 Uiso 1 1 calc R U . . .
C30 C 0.2335(8) 0.9793(5) 0.64505(19) 0.0510(19) Uani 1 1 d . . . . .
H30A H 0.3043 0.9382 0.6438 0.076 Uiso 1 1 calc R U . . .
H30B H 0.2624 1.0321 0.6330 0.076 Uiso 1 1 calc R U . . .
H30C H 0.1578 0.9579 0.6304 0.076 Uiso 1 1 calc R U . . .
C31 C 0.3310(6) 1.1505(4) 0.7375(2) 0.0420(17) Uani 1 1 d D . . . .
H31A H 0.3398 1.1565 0.7086 0.063 Uiso 1 1 calc R U . . .
H31B H 0.3732 1.1980 0.7508 0.063 Uiso 1 1 calc R U . . .
H31C H 0.2384 1.1492 0.7447 0.063 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
Ca1 O4 2.340(4) 3_576 ?
Ca1 O3 2.346(4) . ?
Ca1 O7 2.371(4) . ?
Ca1 O2 2.383(4) . ?
Ca1 O6 2.387(4) . ?
Ca1 O5 2.432(4) . ?
Ca1 O1 2.654(4) . ?
Ca1 C1 2.877(5) . ?
O1 C1 1.260(6) . ?
O2 C1 1.268(7) . ?
O3 C15 1.266(6) . ?
O4 C15 1.263(7) . ?
O4 Ca1 2.340(4) 3_476 ?
O5 C29 1.417(7) . ?
O5 H5A 0.98(7) . ?
O6 C30 1.419(7) . ?
O6 H6A 1.03(8) . ?
O7 C31 1.419(7) . ?
O7 H7A 0.986(19) . ?
C1 C2 1.486(8) . ?
C2 C7 1.388(8) . ?
C2 C3 1.403(8) . ?
C3 C4 1.393(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.385(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.402(8) . ?
C5 C10 1.469(8) . ?
C6 C7 1.389(7) . ?
C6 C8 1.521(7) . ?
C7 H7 0.9500 . ?
C8 C6 1.521(7) 2_665 ?
C8 C9 1.534(7) 2_665 ?
C8 C9 1.534(7) . ?
C9 C14 1.383(8) . ?
C9 C10 1.404(8) . ?
C10 C11 1.385(8) . ?
C11 C12 1.405(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.373(8) . ?
C12 H12 0.9500 . ?
C13 C14 1.403(8) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C16 1.501(8) . ?
C16 C17 1.394(7) . ?
C16 C21 1.398(8) . ?
C17 C18 1.368(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.397(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.393(7) . ?
C19 C24 1.460(8) . ?
C20 C21 1.375(8) . ?
C20 C22 1.536(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.518(7) . ?
C22 C23 1.518(7) 2_575 ?
C22 C20 1.535(6) 2_575 ?
C23 C28 1.390(8) . ?
C23 C24 1.411(8) . ?
C24 C25 1.378(8) . ?
C25 C26 1.395(9) . ?
C25 H25 0.9500 . ?
C26 C27 1.383(9) . ?
C26 H26 0.9500 . ?
C27 C28 1.393(8) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 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
O4 Ca1 O3 168.12(14) 3_576 . ?
O4 Ca1 O7 82.71(14) 3_576 . ?
O3 Ca1 O7 86.66(14) . . ?
O4 Ca1 O2 90.23(14) 3_576 . ?
O3 Ca1 O2 100.79(15) . . ?
O7 Ca1 O2 131.14(14) . . ?
O4 Ca1 O6 84.89(14) 3_576 . ?
O3 Ca1 O6 88.87(14) . . ?
O7 Ca1 O6 84.68(14) . . ?
O2 Ca1 O6 142.95(14) . . ?
O4 Ca1 O5 108.73(15) 3_576 . ?
O3 Ca1 O5 79.55(14) . . ?
O7 Ca1 O5 157.12(14) . . ?
O2 Ca1 O5 69.97(14) . . ?
O6 Ca1 O5 76.94(14) . . ?
O4 Ca1 O1 82.94(13) 3_576 . ?
O3 Ca1 O1 100.40(13) . . ?
O7 Ca1 O1 79.65(13) . . ?
O2 Ca1 O1 51.49(12) . . ?
O6 Ca1 O1 161.22(13) . . ?
O5 Ca1 O1 120.61(13) . . ?
O4 Ca1 C1 88.52(14) 3_576 . ?
O3 Ca1 C1 99.46(14) . . ?
O7 Ca1 C1 105.47(15) . . ?
O2 Ca1 C1 25.76(14) . . ?
O6 Ca1 C1 167.12(15) . . ?
O5 Ca1 C1 94.81(15) . . ?
O1 Ca1 C1 25.93(13) . . ?
C1 O1 Ca1 87.0(3) . . ?
C1 O2 Ca1 99.4(3) . . ?
C15 O3 Ca1 142.1(3) . . ?
C15 O4 Ca1 134.5(3) . 3_476 ?
C29 O5 Ca1 135.9(4) . . ?
C29 O5 H5A 111(4) . . ?
Ca1 O5 H5A 111(4) . . ?
C30 O6 Ca1 125.8(4) . . ?
C30 O6 H6A 116(4) . . ?
Ca1 O6 H6A 118(4) . . ?
C31 O7 Ca1 126.9(4) . . ?
C31 O7 H7A 111(2) . . ?
Ca1 O7 H7A 107(3) . . ?
O1 C1 O2 121.2(5) . . ?
O1 C1 C2 120.5(5) . . ?
O2 C1 C2 118.2(5) . . ?
O1 C1 Ca1 67.1(3) . . ?
O2 C1 Ca1 54.8(3) . . ?
C2 C1 Ca1 166.6(4) . . ?
C7 C2 C3 120.1(5) . . ?
C7 C2 C1 120.7(5) . . ?
C3 C2 C1 119.2(5) . . ?
C4 C3 C2 120.8(5) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 118.6(5) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 H4 120.7 . . ?
C4 C5 C6 121.0(5) . . ?
C4 C5 C10 130.4(5) . . ?
C6 C5 C10 108.3(5) . . ?
C7 C6 C5 120.1(5) . . ?
C7 C6 C8 128.5(5) . . ?
C5 C6 C8 111.2(4) . . ?
C2 C7 C6 119.4(5) . . ?
C2 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C6 C8 C6 108.9(6) . 2_665 ?
C6 C8 C9 114.9(3) . 2_665 ?
C6 C8 C9 101.3(3) 2_665 2_665 ?
C6 C8 C9 101.3(3) . . ?
C6 C8 C9 114.9(3) 2_665 . ?
C9 C8 C9 115.9(6) 2_665 . ?
C14 C9 C10 121.0(5) . . ?
C14 C9 C8 128.5(5) . . ?
C10 C9 C8 110.4(4) . . ?
C11 C10 C9 120.2(5) . . ?
C11 C10 C5 131.1(5) . . ?
C9 C10 C5 108.7(5) . . ?
C10 C11 C12 118.8(5) . . ?
C10 C11 H11 120.6 . . ?
C12 C11 H11 120.6 . . ?
C13 C12 C11 120.7(5) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C12 C13 C14 121.0(5) . . ?
C12 C13 H13 119.5 . . ?
C14 C13 H13 119.5 . . ?
C9 C14 C13 118.3(5) . . ?
C9 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
O4 C15 O3 124.2(5) . . ?
O4 C15 C16 117.7(5) . . ?
O3 C15 C16 118.1(5) . . ?
C17 C16 C21 119.6(5) . . ?
C17 C16 C15 119.8(5) . . ?
C21 C16 C15 120.6(5) . . ?
C18 C17 C16 121.3(5) . . ?
C18 C17 H17 119.3 . . ?
C16 C17 H17 119.3 . . ?
C17 C18 C19 119.5(5) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C18 C19 C20 119.0(5) . . ?
C18 C19 C24 131.3(5) . . ?
C20 C19 C24 109.6(5) . . ?
C21 C20 C19 121.8(5) . . ?
C21 C20 C22 128.2(5) . . ?
C19 C20 C22 110.0(4) . . ?
C20 C21 C16 118.7(5) . . ?
C20 C21 H21 120.6 . . ?
C16 C21 H21 120.6 . . ?
C23 C22 C23 113.8(6) . 2_575 ?
C23 C22 C20 112.6(3) . 2_575 ?
C23 C22 C20 101.6(3) 2_575 2_575 ?
C23 C22 C20 101.5(3) . . ?
C23 C22 C20 112.6(3) 2_575 . ?
C20 C22 C20 115.3(6) 2_575 . ?
C28 C23 C24 120.6(5) . . ?
C28 C23 C22 128.7(4) . . ?
C24 C23 C22 110.7(4) . . ?
C25 C24 C23 119.9(5) . . ?
C25 C24 C19 132.1(5) . . ?
C23 C24 C19 108.1(5) . . ?
C24 C25 C26 119.8(5) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 H25 120.1 . . ?
C27 C26 C25 119.9(5) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C28 121.4(6) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C23 C28 C27 118.4(5) . . ?
C23 C28 H28 120.8 . . ?
C27 C28 H28 120.8 . . ?
O5 C29 H29A 109.5 . . ?
O5 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
O5 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O6 C30 H30A 109.5 . . ?
O6 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
O6 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O7 C31 H31A 109.5 . . ?
O7 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
O7 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 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 C1 O2 9.2(5) . . . . ?
Ca1 O1 C1 C2 -167.7(5) . . . . ?
Ca1 O2 C1 O1 -10.3(6) . . . . ?
Ca1 O2 C1 C2 166.5(4) . . . . ?
O1 C1 C2 C7 -16.2(8) . . . . ?
O2 C1 C2 C7 166.9(5) . . . . ?
Ca1 C1 C2 C7 -137.9(14) . . . . ?
O1 C1 C2 C3 165.3(5) . . . . ?
O2 C1 C2 C3 -11.6(8) . . . . ?
Ca1 C1 C2 C3 43.7(18) . . . . ?
C7 C2 C3 C4 1.5(9) . . . . ?
C1 C2 C3 C4 179.9(5) . . . . ?
C2 C3 C4 C5 -0.6(9) . . . . ?
C3 C4 C5 C6 -1.1(9) . . . . ?
C3 C4 C5 C10 -174.5(6) . . . . ?
C4 C5 C6 C7 2.1(8) . . . . ?
C10 C5 C6 C7 176.8(5) . . . . ?
C4 C5 C6 C8 -172.7(5) . . . . ?
C10 C5 C6 C8 1.9(6) . . . . ?
C3 C2 C7 C6 -0.5(8) . . . . ?
C1 C2 C7 C6 -178.9(5) . . . . ?
C5 C6 C7 C2 -1.3(8) . . . . ?
C8 C6 C7 C2 172.6(5) . . . . ?
C7 C6 C8 C6 -54.4(5) . . . 2_665 ?
C5 C6 C8 C6 119.9(5) . . . 2_665 ?
C7 C6 C8 C9 58.4(8) . . . 2_665 ?
C5 C6 C8 C9 -127.3(5) . . . 2_665 ?
C7 C6 C8 C9 -175.9(5) . . . . ?
C5 C6 C8 C9 -1.6(6) . . . . ?
C6 C8 C9 C14 177.5(5) . . . . ?
C6 C8 C9 C14 60.3(8) 2_665 . . . ?
C9 C8 C9 C14 -57.5(5) 2_665 . . . ?
C6 C8 C9 C10 0.7(6) . . . . ?
C6 C8 C9 C10 -116.5(5) 2_665 . . . ?
C9 C8 C9 C10 125.8(5) 2_665 . . . ?
C14 C9 C10 C11 2.3(8) . . . . ?
C8 C9 C10 C11 179.3(5) . . . . ?
C14 C9 C10 C5 -176.7(5) . . . . ?
C8 C9 C10 C5 0.4(6) . . . . ?
C4 C5 C10 C11 -6.2(11) . . . . ?
C6 C5 C10 C11 179.8(6) . . . . ?
C4 C5 C10 C9 172.6(6) . . . . ?
C6 C5 C10 C9 -1.4(6) . . . . ?
C9 C10 C11 C12 -2.5(8) . . . . ?
C5 C10 C11 C12 176.2(6) . . . . ?
C10 C11 C12 C13 1.8(9) . . . . ?
C11 C12 C13 C14 -1.0(9) . . . . ?
C10 C9 C14 C13 -1.3(8) . . . . ?
C8 C9 C14 C13 -177.8(5) . . . . ?
C12 C13 C14 C9 0.7(8) . . . . ?
Ca1 O4 C15 O3 0.0(8) 3_476 . . . ?
Ca1 O4 C15 C16 -178.1(3) 3_476 . . . ?
Ca1 O3 C15 O4 128.9(5) . . . . ?
Ca1 O3 C15 C16 -53.1(8) . . . . ?
O4 C15 C16 C17 164.0(5) . . . . ?
O3 C15 C16 C17 -14.2(7) . . . . ?
O4 C15 C16 C21 -17.4(7) . . . . ?
O3 C15 C16 C21 164.4(5) . . . . ?
C21 C16 C17 C18 -0.6(8) . . . . ?
C15 C16 C17 C18 178.0(5) . . . . ?
C16 C17 C18 C19 -1.6(8) . . . . ?
C17 C18 C19 C20 2.3(8) . . . . ?
C17 C18 C19 C24 -176.2(6) . . . . ?
C18 C19 C20 C21 -0.8(8) . . . . ?
C24 C19 C20 C21 178.1(5) . . . . ?
C18 C19 C20 C22 178.8(5) . . . . ?
C24 C19 C20 C22 -2.4(6) . . . . ?
C19 C20 C21 C16 -1.5(8) . . . . ?
C22 C20 C21 C16 179.0(5) . . . . ?
C17 C16 C21 C20 2.2(8) . . . . ?
C15 C16 C21 C20 -176.4(5) . . . . ?
C21 C20 C22 C23 -177.7(5) . . . . ?
C19 C20 C22 C23 2.7(6) . . . . ?
C21 C20 C22 C23 60.2(8) . . . 2_575 ?
C19 C20 C22 C23 -119.4(5) . . . 2_575 ?
C21 C20 C22 C20 -55.7(5) . . . 2_575 ?
C19 C20 C22 C20 124.7(5) . . . 2_575 ?
C23 C22 C23 C28 -60.7(5) 2_575 . . . ?
C20 C22 C23 C28 54.2(8) 2_575 . . . ?
C20 C22 C23 C28 178.1(5) . . . . ?
C23 C22 C23 C24 119.1(4) 2_575 . . . ?
C20 C22 C23 C24 -126.1(5) 2_575 . . . ?
C20 C22 C23 C24 -2.2(6) . . . . ?
C28 C23 C24 C25 0.3(8) . . . . ?
C22 C23 C24 C25 -179.5(5) . . . . ?
C28 C23 C24 C19 -179.3(5) . . . . ?
C22 C23 C24 C19 0.9(6) . . . . ?
C18 C19 C24 C25 0.1(10) . . . . ?
C20 C19 C24 C25 -178.6(6) . . . . ?
C18 C19 C24 C23 179.6(6) . . . . ?
C20 C19 C24 C23 0.9(6) . . . . ?
C23 C24 C25 C26 -0.6(8) . . . . ?
C19 C24 C25 C26 178.9(6) . . . . ?
C24 C25 C26 C27 0.0(9) . . . . ?
C25 C26 C27 C28 1.0(10) . . . . ?
C24 C23 C28 C27 0.6(8) . . . . ?
C22 C23 C28 C27 -179.6(5) . . . . ?
C26 C27 C28 C23 -1.3(9) . . . . ?

_refine_diff_density_max         0.603
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.113



_exptl_crystal_recrystallization_method 'single crystal to single crystal'
####################################################################### 
# 
# 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_130621b_0m_sq
_database_code_depnum_ccdc_archive 'CCDC 1424463'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-06-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT026_130621b_0m_sq       
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         39 %
RESPONSE: The crystal was minute in one direction, and there were a large number of weak reflections due to the presence of disordered solvents, but enough data was measured to solve the structure.
;
_vrf_PLAT245_130621b_0m_sq       
;
PROBLEM: U(iso) H1W     Smaller than U(eq) O1W     by ...      0.085 AngSq
RESPONSE: The data crystal contained a very large region of highly disordered solvent comprising approximately 41% of the unit cell.  The program SQUEEZE in PLATON was used to remove the contribution to the scattering due to the disordered solvent.
;
_vrf_PLAT420_130621b_0m_sq       
;
PROBLEM: D-H Without Acceptor       O1W    --  H1W    ...     Please Check
RESPONSE: The data crystal contained a very large region of highly disordered solvent comprising approximately 41% of the unit cell.  The program SQUEEZE in PLATON was used to remove the contribution to the scattering due to the disordered solvent.
;
_vrf_RINTA01_130621b_0m_sq       
;
PROBLEM: The value of Rint is greater than 0.12
RESPONSE: Rint value is (correctly) biased by the large number of weak data measured. See PLAT026
;
_vrf_PLAT020_130621b_0m_sq       
;
PROBLEM: The value of Rint is greater than 0.12 .........      0.150 Report
RESPONSE: Rint value is (correctly) biased by the large number of weak data measured. See PLAT026
;
# Added during the CSD deposition process: Tuesday 23 May 2017 04:06 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C108 H64 Ca4 O21'
_chemical_formula_weight         1857.91

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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           87
_space_group_name_H-M_alt        'I 4/m'
_space_group_name_Hall           '-I 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   13.3902(12)
_cell_length_b                   13.3902(12)
_cell_length_c                   35.510(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6366.8(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    625
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      16.82

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    0.969
_exptl_crystal_F_000             1920
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.224
_shelx_estimated_absorpt_T_min   0.985
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9845
_exptl_absorpt_correction_T_max  0.9933
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16181
_diffrn_reflns_av_unetI/netI     0.1180
_diffrn_reflns_av_R_equivalents  0.1505
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         1.625
_diffrn_reflns_theta_max         25.003
_diffrn_reflns_theta_full        25.003
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2864
_reflns_number_gt                1104
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger., SQUEEZE
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1000P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0036(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2864
_refine_ls_number_parameters     159
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1896
_refine_ls_R_factor_gt           0.0852
_refine_ls_wR_factor_ref         0.2407
_refine_ls_wR_factor_gt          0.2069
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.15766(14) 1.12615(15) 0.5000 0.0869(8) Uani 1 2 d S T P . .
O1 O 0.0000 1.0000 0.5000 0.054(2) Uani 1 8 d S T P . .
O2 O 0.2717(3) 1.0963(3) 0.54990(10) 0.0752(12) Uani 1 1 d . . . . .
O3 O 0.1738(3) 0.9646(3) 0.54217(10) 0.0774(12) Uani 1 1 d . . . . .
O1W O 0.2073(7) 1.2935(10) 0.5000 0.182(4) Uani 1 2 d DS T P . .
C1 C 0.2423(4) 1.0112(5) 0.55965(15) 0.0646(15) Uani 1 1 d . . . . .
C2 C 0.2902(4) 0.9621(4) 0.59314(13) 0.0544(13) Uani 1 1 d . . . . .
C3 C 0.2622(4) 0.8667(4) 0.60411(16) 0.0739(17) Uani 1 1 d . . . . .
H3 H 0.2105 0.8348 0.5914 0.089 Uiso 1 1 calc R U . . .
C4 C 0.3093(4) 0.8183(4) 0.63336(16) 0.0784(18) Uani 1 1 d . . . . .
H4 H 0.2893 0.7544 0.6404 0.094 Uiso 1 1 calc R U . . .
C5 C 0.3861(4) 0.8653(4) 0.65200(14) 0.0579(14) Uani 1 1 d . . . . .
C6 C 0.4124(3) 0.9624(4) 0.64182(12) 0.0508(13) Uani 1 1 d . . . . .
C7 C 0.3650(4) 1.0104(4) 0.61271(13) 0.0540(13) Uani 1 1 d . . . . .
H7 H 0.3832 1.0751 0.6062 0.065 Uiso 1 1 calc R U . . .
C8 C 0.5000 1.0000 0.66529(17) 0.0467(17) Uani 1 2 d S T P . .
C9 C 0.5225(3) 0.9071(4) 0.68863(12) 0.0474(12) Uani 1 1 d . . . . .
C10 C 0.4556(4) 0.8308(4) 0.68143(13) 0.0543(13) Uani 1 1 d . . . . .
C11 C 0.4626(4) 0.7401(4) 0.69942(16) 0.0741(17) Uani 1 1 d . . . . .
H11 H 0.4169 0.6895 0.6944 0.089 Uiso 1 1 calc R U . . .
C12 C 0.5385(5) 0.7257(5) 0.72489(16) 0.0756(17) Uani 1 1 d . . . . .
H12 H 0.5440 0.6648 0.7373 0.091 Uiso 1 1 calc R U . . .
C13 C 0.6072(5) 0.8010(5) 0.73243(15) 0.0752(17) Uani 1 1 d . . . . .
H13 H 0.6585 0.7900 0.7496 0.090 Uiso 1 1 calc R U . . .
C14 C 0.5995(4) 0.8923(4) 0.71438(14) 0.0645(15) Uani 1 1 d . . . . .
H14 H 0.6450 0.9431 0.7194 0.077 Uiso 1 1 calc R U . . .
H1W H 0.228(4) 1.348(3) 0.5184(14) 0.097 Uiso 1 1 d D 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
Ca1 O1W 2.337(14) . ?
Ca1 O3 2.309(4) 12_666 ?
Ca1 O3 2.309(4) 3_665 ?
Ca1 O2 2.373(4) 10_556 ?
Ca1 O2 2.373(4) . ?
Ca1 O3 2.640(4) . ?
Ca1 O3 2.640(4) 10_556 ?
Ca1 O1 2.704(2) . ?
Ca1 C1 2.853(6) 10_556 ?
Ca1 C1 2.853(6) . ?
Ca1 Ca1 3.824(3) 11_466 ?
Ca1 Ca1 3.824(3) 3_665 ?
O1 Ca1 2.704(2) 9_576 ?
O1 Ca1 2.704(2) 11_466 ?
O1 Ca1 2.704(2) 3_665 ?
O2 C1 1.255(6) . ?
O3 C1 1.271(6) . ?
O3 Ca1 2.309(4) 11_466 ?
O1W H1W 1.017(19) . ?
C1 C2 1.502(7) . ?
C2 C7 1.380(6) . ?
C2 C3 1.387(7) . ?
C3 C4 1.377(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.376(7) . ?
C4 H4 0.9300 . ?
C5 C6 1.395(6) . ?
C5 C10 1.473(7) . ?
C6 C7 1.373(6) . ?
C6 C8 1.524(5) . ?
C7 H7 0.9300 . ?
C8 C6 1.524(5) 2_675 ?
C8 C9 1.525(5) 2_675 ?
C8 C9 1.525(5) . ?
C9 C10 1.382(6) . ?
C9 C14 1.392(6) . ?
C10 C11 1.376(7) . ?
C11 C12 1.373(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.391(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.384(7) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?

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
O1W Ca1 O3 86.4(2) . 12_666 ?
O1W Ca1 O3 86.4(2) . 3_665 ?
O3 Ca1 O3 80.9(2) 12_666 3_665 ?
O1W Ca1 O2 88.8(2) . 10_556 ?
O3 Ca1 O2 91.06(13) 12_666 10_556 ?
O3 Ca1 O2 170.81(15) 3_665 10_556 ?
O1W Ca1 O2 88.8(2) . . ?
O3 Ca1 O2 170.81(15) 12_666 . ?
O3 Ca1 O2 91.06(13) 3_665 . ?
O2 Ca1 O2 96.61(19) 10_556 . ?
O1W Ca1 O3 139.67(15) . . ?
O3 Ca1 O3 130.75(18) 12_666 . ?
O3 Ca1 O3 85.23(18) 3_665 . ?
O2 Ca1 O3 103.47(14) 10_556 . ?
O2 Ca1 O3 52.11(13) . . ?
O1W Ca1 O3 139.66(15) . 10_556 ?
O3 Ca1 O3 85.23(18) 12_666 10_556 ?
O3 Ca1 O3 130.75(18) 3_665 10_556 ?
O2 Ca1 O3 52.11(13) 10_556 10_556 ?
O2 Ca1 O3 103.47(14) . 10_556 ?
O3 Ca1 O3 69.12(16) . 10_556 ?
O1W Ca1 O1 145.2(3) . . ?
O3 Ca1 O1 67.61(10) 12_666 . ?
O3 Ca1 O1 67.61(10) 3_665 . ?
O2 Ca1 O1 113.42(12) 10_556 . ?
O2 Ca1 O1 113.42(12) . . ?
O3 Ca1 O1 63.39(10) . . ?
O3 Ca1 O1 63.39(10) 10_556 . ?
O1W Ca1 C1 113.8(2) . 10_556 ?
O3 Ca1 C1 87.11(15) 12_666 10_556 ?
O3 Ca1 C1 155.85(19) 3_665 10_556 ?
O2 Ca1 C1 25.75(13) 10_556 10_556 ?
O2 Ca1 C1 101.99(14) . 10_556 ?
O3 Ca1 C1 86.93(15) . 10_556 ?
O3 Ca1 C1 26.39(13) 10_556 10_556 ?
O1 Ca1 C1 88.47(14) . 10_556 ?
O1W Ca1 C1 113.8(2) . . ?
O3 Ca1 C1 155.85(19) 12_666 . ?
O3 Ca1 C1 87.11(15) 3_665 . ?
O2 Ca1 C1 101.99(14) 10_556 . ?
O2 Ca1 C1 25.74(13) . . ?
O3 Ca1 C1 26.39(13) . . ?
O3 Ca1 C1 86.93(15) 10_556 . ?
O1 Ca1 C1 88.47(14) . . ?
C1 Ca1 C1 95.9(2) 10_556 . ?
O1W Ca1 Ca1 169.8(3) . 11_466 ?
O3 Ca1 Ca1 101.34(10) 12_666 11_466 ?
O3 Ca1 Ca1 101.34(10) 3_665 11_466 ?
O2 Ca1 Ca1 84.48(12) 10_556 11_466 ?
O2 Ca1 Ca1 84.48(12) . 11_466 ?
O3 Ca1 Ca1 36.35(9) . 11_466 ?
O3 Ca1 Ca1 36.35(9) 10_556 11_466 ?
O1 Ca1 Ca1 45.0 . 11_466 ?
C1 Ca1 Ca1 60.50(14) 10_556 11_466 ?
C1 Ca1 Ca1 60.50(14) . 11_466 ?
O1W Ca1 Ca1 100.2(3) . 3_665 ?
O3 Ca1 Ca1 42.67(10) 12_666 3_665 ?
O3 Ca1 Ca1 42.67(10) 3_665 3_665 ?
O2 Ca1 Ca1 131.16(10) 10_556 3_665 ?
O2 Ca1 Ca1 131.16(10) . 3_665 ?
O3 Ca1 Ca1 99.90(9) . 3_665 ?
O3 Ca1 Ca1 99.90(9) 10_556 3_665 ?
O1 Ca1 Ca1 45.0 . 3_665 ?
C1 Ca1 Ca1 117.03(12) 10_556 3_665 ?
C1 Ca1 Ca1 117.03(12) . 3_665 ?
Ca1 Ca1 Ca1 90.001(1) 11_466 3_665 ?
Ca1 O1 Ca1 180.0 . 9_576 ?
Ca1 O1 Ca1 90.0 . 11_466 ?
Ca1 O1 Ca1 90.0 9_576 11_466 ?
Ca1 O1 Ca1 90.0 . 3_665 ?
Ca1 O1 Ca1 90.000(1) 9_576 3_665 ?
Ca1 O1 Ca1 180.0 11_466 3_665 ?
C1 O2 Ca1 99.0(3) . . ?
C1 O3 Ca1 149.8(4) . 11_466 ?
C1 O3 Ca1 86.2(4) . . ?
Ca1 O3 Ca1 100.98(14) 11_466 . ?
Ca1 O1W H1W 140(4) . . ?
O3 C1 O2 122.5(5) . . ?
O3 C1 C2 118.7(6) . . ?
O2 C1 C2 118.8(5) . . ?
O3 C1 Ca1 67.4(3) . . ?
O2 C1 Ca1 55.2(3) . . ?
C2 C1 Ca1 173.3(4) . . ?
C7 C2 C3 119.1(5) . . ?
C7 C2 C1 120.2(5) . . ?
C3 C2 C1 120.7(5) . . ?
C4 C3 C2 121.5(5) . . ?
C4 C3 H3 119.3 . . ?
C2 C3 H3 119.3 . . ?
C5 C4 C3 119.3(5) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 119.4(5) . . ?
C4 C5 C10 132.1(5) . . ?
C6 C5 C10 108.5(4) . . ?
C7 C6 C5 121.0(5) . . ?
C7 C6 C8 127.9(4) . . ?
C5 C6 C8 111.1(4) . . ?
C2 C7 C6 119.8(5) . . ?
C2 C7 H7 120.1 . . ?
C6 C7 H7 120.1 . . ?
C6 C8 C6 113.7(5) . 2_675 ?
C6 C8 C9 114.5(2) . 2_675 ?
C6 C8 C9 100.4(3) 2_675 2_675 ?
C6 C8 C9 100.4(3) . . ?
C6 C8 C9 114.5(2) 2_675 . ?
C9 C8 C9 114.2(5) 2_675 . ?
C10 C9 C14 119.8(5) . . ?
C10 C9 C8 112.0(4) . . ?
C14 C9 C8 128.3(4) . . ?
C9 C10 C11 121.5(5) . . ?
C9 C10 C5 108.0(4) . . ?
C11 C10 C5 130.5(5) . . ?
C10 C11 C12 118.7(6) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C13 C12 C11 120.9(5) . . ?
C13 C12 H12 119.5 . . ?
C11 C12 H12 119.5 . . ?
C12 C13 C14 120.1(5) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C9 C14 C13 119.0(5) . . ?
C9 C14 H14 120.5 . . ?
C13 C14 H14 120.5 . . ?

_refine_diff_density_max         0.799
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.071



_exptl_crystal_recrystallization_method 'Solvothermal method'
