#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/06/7110617.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7110617
loop_
_publ_author_name
'Fromm, Katharina M.'
_publ_section_title
;
 Synthesis and crystal structure of
 Li[{Ca7(μ3-OH)8I6(thf)12}2(μ-I)]·3THF, a unique H-bound dimer of
 a Ca7-cluster on the way to sol--gels
;
_journal_issue                   17
_journal_name_full               'Chemical Communications'
_journal_page_first              1659
_journal_paper_doi               10.1039/a904560k
_journal_year                    1999
_chemical_formula_moiety         'C108 H232 Ca14 I13 O43'
_chemical_formula_sum            'C54 H116 Ca7 I6.5 O21.5'
_chemical_formula_weight         2214.88
_chemical_name_common            Ca7-Cluster-Dimer
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   21.592(3)
_cell_length_b                   21.592(3)
_cell_length_c                   36.839(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_volume                     14874(4)
_computing_molecular_graphics    'SCHAKAL (E.Keller, Uni Freiburg) '
_computing_publication_material  'WORD 97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  Enraf-Nonius
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0651
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            7165
_diffrn_reflns_theta_full        26.93
_diffrn_reflns_theta_max         26.93
_diffrn_reflns_theta_min         2.25
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.447
_exptl_absorpt_correction_type   'face indexation '
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             6579
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .3
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         7165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1208
_refine_ls_R_factor_gt           0.0668
_refine_ls_shift/su_max          0.063
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1090P)²+72.2258P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.2057
_reflns_number_gt                4307
_reflns_number_total             7165
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904560ksup1.cif
_cod_data_source_block           Ca7-Dimer
_cod_original_sg_symbol_H-M      R(-3)
_cod_original_formula_sum        'C54 H116 Ca7 I6.50 O21.50'
_cod_database_code               7110617
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
I1 I 0.0000 0.0000 0.0000 0.0545(4) Uani 1 6 d S
I2 I -0.19580(3) -0.22237(3) 0.183355(16) 0.0568(2) Uani 1 1 d .
I3 I 0.21555(5) 0.15575(5) 0.34061(3) 0.0989(4) Uani 1 1 d .
Ca1 Ca -0.08790(8) -0.10252(8) 0.13011(4) 0.0362(4) Uani 1 1 d .
Ca2 Ca 0.08563(8) 0.10397(8) 0.28686(4) 0.0376(4) Uani 1 1 d .
Ca3 Ca 0.0000 0.0000 0.20857(6) 0.0344(6) Uani 1 3 d S
O1 O 0.0000 0.0000 0.0999(2) 0.0294(18) Uani 1 3 d S
H1 H 0.0000 0.0000 0.0727 0.035 Uiso 1 3 calc SR
O2 O -0.0865(2) -0.0123(3) 0.16447(13) 0.0318(11) Uani 1 1 d .
H2 H -0.1332 -0.0189 0.1733 0.038 Uiso 1 1 calc R
O3 O -0.0154(3) 0.0720(3) 0.25189(13) 0.0337(11) Uani 1 1 d .
H3 H -0.0237 0.1110 0.2429 0.040 Uiso 1 1 calc R
O4 O 0.0000 0.0000 0.3166(2) 0.039(2) Uani 1 3 d S
H4 H 0.0000 0.0000 0.3437 0.046 Uiso 1 3 calc SR
O5 O -0.0797(4) -0.1902(3) 0.09294(17) 0.0601(17) Uani 1 1 d .
O6 O -0.1898(3) -0.1254(4) 0.09351(18) 0.0660(19) Uani 1 1 d .
O7 O 0.0655(4) 0.1959(4) 0.31334(18) 0.0630(18) Uani 1 1 d .
O8 O 0.1660(4) 0.1890(4) 0.2424(2) 0.072(2) Uani 1 1 d .
C13 C 0.1672(6) 0.2533(5) 0.2315(3) 0.063(3) Uani 1 1 d .
H13A H 0.1671 0.2808 0.2530 0.075 Uiso 1 1 calc R
H13B H 0.1254 0.2422 0.2161 0.075 Uiso 1 1 calc R
C14 C 0.2341(10) 0.2935(9) 0.2109(5) 0.134(7) Uani 1 1 d .
H14A H 0.2251 0.2853 0.1845 0.160 Uiso 1 1 calc R
H14B H 0.2565 0.3454 0.2158 0.160 Uiso 1 1 calc R
C15 C 0.2793(9) 0.2667(9) 0.2233(7) 0.159(9) Uani 1 1 d .
H15A H 0.3112 0.2690 0.2034 0.191 Uiso 1 1 calc R
H15B H 0.3093 0.2961 0.2437 0.191 Uiso 1 1 calc R
C16 C 0.2354(6) 0.1948(8) 0.2347(5) 0.105(5) Uani 1 1 d .
H16A H 0.2552 0.1847 0.2566 0.126 Uiso 1 1 calc R
H16B H 0.2308 0.1611 0.2152 0.126 Uiso 1 1 calc R
C9 C 0.0256(7) 0.2253(6) 0.2970(3) 0.071(3) Uani 1 1 d .
H9A H -0.0244 0.1871 0.2929 0.086 Uiso 1 1 calc R
H9B H 0.0469 0.2472 0.2733 0.086 Uiso 1 1 calc R
C10 C 0.0273(9) 0.2788(9) 0.3213(4) 0.122(6) Uani 1 1 d .
H10A H -0.0213 0.2717 0.3247 0.147 Uiso 1 1 calc R
H10B H 0.0587 0.3274 0.3114 0.147 Uiso 1 1 calc R
C11 C 0.0561(10) 0.2693(11) 0.3563(5) 0.146(8) Uani 1 1 d .
H11A H 0.1004 0.3139 0.3628 0.175 Uiso 1 1 calc R
H11B H 0.0206 0.2578 0.3759 0.175 Uiso 1 1 calc R
C12 C 0.0714(9) 0.2104(9) 0.3518(3) 0.110(6) Uani 1 1 d .
H12A H 0.1201 0.2248 0.3606 0.132 Uiso 1 1 calc R
H12B H 0.0364 0.1675 0.3654 0.132 Uiso 1 1 calc R
C1 C -0.0943(10) -0.2589(7) 0.1044(4) 0.122(7) Uani 1 1 d .
H1A H -0.1435 -0.2863 0.1142 0.146 Uiso 1 1 calc R
H1B H -0.0604 -0.2545 0.1237 0.146 Uiso 1 1 calc R
C2 C -0.0866(10) -0.2958(7) 0.0729(4) 0.113(6) Uani 1 1 d .
H2A H -0.0527 -0.3128 0.0783 0.136 Uiso 1 1 calc R
H2B H -0.1334 -0.3375 0.0663 0.136 Uiso 1 1 calc R
C3 C -0.0626(19) -0.2499(11) 0.0464(5) 0.255(18) Uani 1 1 d .
H3A H -0.0979 -0.2677 0.0264 0.306 Uiso 1 1 calc R
H3B H -0.0178 -0.2459 0.0371 0.306 Uiso 1 1 calc R
C4 C -0.0484(12) -0.1771(8) 0.0575(4) 0.138(8) Uani 1 1 d .
H4A H 0.0035 -0.1424 0.0584 0.166 Uiso 1 1 calc R
H4B H -0.0717 -0.1591 0.0408 0.166 Uiso 1 1 calc R
C5 C -0.2561(8) -0.1417(11) 0.1067(4) 0.127(7) Uani 1 1 d .
H5A H -0.2609 -0.0985 0.1063 0.152 Uiso 1 1 calc R
H5B H -0.2611 -0.1584 0.1322 0.152 Uiso 1 1 calc R
C6 C -0.3102(10) -0.1959(13) 0.0851(8) 0.187(11) Uani 1 1 d .
H6A H -0.3225 -0.2440 0.0939 0.224 Uiso 1 1 calc R
H6B H -0.3539 -0.1918 0.0850 0.224 Uiso 1 1 calc R
C7 C -0.2801(11) -0.1835(19) 0.0507(6) 0.238(19) Uani 1 1 d .
H7A H -0.2884 -0.1485 0.0373 0.285 Uiso 1 1 calc R
H7B H -0.3006 -0.2284 0.0365 0.285 Uiso 1 1 calc R
C8 C -0.2021(12) -0.1543(18) 0.0573(5) 0.225(15) Uani 1 1 d .
H8A H -0.1897 -0.1926 0.0556 0.269 Uiso 1 1 calc R
H8B H -0.1730 -0.1164 0.0395 0.269 Uiso 1 1 calc R
O10 O 0.0653(13) 0.6149(17) 0.1031(6) 0.133(9) Uani 0.50 1 d P
C17 C 0.0830(17) 0.6789(16) 0.1176(11) 0.120(13) Uani 0.50 1 d P
H17A H 0.0410 0.6762 0.1300 0.144 Uiso 0.50 1 calc PR
H17B H 0.0983 0.7154 0.0982 0.144 Uiso 0.50 1 calc PR
C18 C 0.1397(16) 0.6986(18) 0.1429(13) 0.19(3) Uani 0.50 1 d P
H18A H 0.1872 0.7211 0.1311 0.226 Uiso 0.50 1 calc PR
H18B H 0.1394 0.7297 0.1626 0.226 Uiso 0.50 1 calc PR
C19 C 0.119(3) 0.635(3) 0.1538(11) 0.21(3) Uani 0.50 1 d P
H19A H 0.0826 0.6207 0.1732 0.248 Uiso 0.50 1 calc PR
H19B H 0.1598 0.6310 0.1634 0.248 Uiso 0.50 1 calc PR
C20 C 0.091(3) 0.5933(19) 0.126(2) 0.22(3) Uani 0.50 1 d P
H20A H 0.1293 0.5875 0.1137 0.268 Uiso 0.50 1 calc PR
H20B H 0.0540 0.5455 0.1340 0.268 Uiso 0.50 1 calc PR
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Ca1 O2 82.0(2) 2 .
O2 Ca1 O1 78.60(18) 2 .
O2 Ca1 O1 78.56(18) . .
O2 Ca1 O6 177.0(2) 2 .
O2 Ca1 O6 96.0(2) . .
O1 Ca1 O6 98.8(2) . .
O2 Ca1 O5 95.3(2) 2 .
O2 Ca1 O5 175.5(2) . .
O1 Ca1 O5 97.4(2) . .
O6 Ca1 O5 86.5(3) . .
O2 Ca1 I2 94.93(13) 2 .
O2 Ca1 I2 92.53(13) . .
O1 Ca1 I2 169.57(17) . .
O6 Ca1 I2 87.45(18) . .
O5 Ca1 I2 91.33(15) . .
O2 Ca1 Ca3 41.61(12) 2 .
O2 Ca1 Ca3 41.62(12) . .
O1 Ca1 Ca3 82.57(17) . .
O6 Ca1 Ca3 136.90(19) . .
O5 Ca1 Ca3 136.35(18) . .
I2 Ca1 Ca3 87.17(5) . .
O2 Ca1 Ca1 83.05(12) 2 3
O2 Ca1 Ca1 38.95(13) . 3
O1 Ca1 Ca1 40.27(11) . 3
O6 Ca1 Ca1 94.0(2) . 3
O5 Ca1 Ca1 137.27(15) . 3
I2 Ca1 Ca1 131.40(5) . 3
Ca3 Ca1 Ca1 59.68(3) . 3
O2 Ca1 Ca1 39.00(12) 2 2
O2 Ca1 Ca1 83.02(12) . 2
O1 Ca1 Ca1 40.27(11) . 2
O6 Ca1 Ca1 138.60(18) . 2
O5 Ca1 Ca1 92.59(18) . 2
I2 Ca1 Ca1 133.93(5) . 2
Ca3 Ca1 Ca1 59.68(3) . 2
Ca1 Ca1 Ca1 60.0 3 2
O3 Ca2 O3 81.2(2) . 3
O3 Ca2 O4 78.50(19) . .
O3 Ca2 O4 78.49(19) 3 .
O3 Ca2 O8 93.5(2) . .
O3 Ca2 O8 87.1(2) 3 .
O4 Ca2 O8 164.3(3) . .
O3 Ca2 O7 86.6(2) . .
O3 Ca2 O7 167.4(2) 3 .
O4 Ca2 O7 102.5(2) . .
O8 Ca2 O7 90.3(3) . .
O3 Ca2 I3 173.20(14) . .
O3 Ca2 I3 105.22(13) 3 .
O4 Ca2 I3 100.52(16) . .
O8 Ca2 I3 89.0(2) . .
O7 Ca2 I3 87.07(16) . .
O3 Ca2 Ca3 41.16(12) . .
O3 Ca2 Ca3 41.16(12) 3 .
O4 Ca2 Ca3 82.05(19) . .
O8 Ca2 Ca3 83.1(2) . .
O7 Ca2 Ca3 126.23(16) . .
I3 Ca2 Ca3 145.59(6) . .
O3 Ca2 Ca2 39.29(13) . 2
O3 Ca2 Ca2 82.94(13) 3 2
O4 Ca2 Ca2 39.99(12) . 2
O8 Ca2 Ca2 132.63(19) . 2
O7 Ca2 Ca2 89.84(18) . 2
I3 Ca2 Ca2 138.28(4) . 2
Ca3 Ca2 Ca2 59.61(3) . 2
O3 Ca2 Ca2 82.94(12) . 3
O3 Ca2 Ca2 39.28(13) 3 3
O4 Ca2 Ca2 39.99(12) . 3
O8 Ca2 Ca2 126.25(19) . 3
O7 Ca2 Ca2 142.40(18) . 3
I3 Ca2 Ca2 100.69(6) . 3
Ca3 Ca2 Ca2 59.61(3) . 3
Ca2 Ca2 Ca2 60.0 2 3
O3 Ca3 O3 79.47(19) . 3
O3 Ca3 O3 79.47(19) . 2
O3 Ca3 O3 79.47(19) 3 2
O3 Ca3 O2 99.93(16) . .
O3 Ca3 O2 178.48(18) 3 .
O3 Ca3 O2 101.81(16) 2 .
O3 Ca3 O2 101.81(16) . 3
O3 Ca3 O2 99.93(16) 3 3
O3 Ca3 O2 178.48(17) 2 3
O2 Ca3 O2 78.81(18) . 3
O3 Ca3 O2 178.48(17) . 2
O3 Ca3 O2 101.81(16) 3 2
O3 Ca3 O2 99.93(16) 2 2
O2 Ca3 O2 78.81(18) . 2
O2 Ca3 O2 78.81(18) 3 2
O3 Ca3 Ca2 40.25(13) . .
O3 Ca3 Ca2 40.26(12) 3 .
O3 Ca3 Ca2 83.31(14) 2 .
O2 Ca3 Ca2 138.87(12) . .
O2 Ca3 Ca2 97.14(12) 3 .
O2 Ca3 Ca2 141.16(12) 2 .
O3 Ca3 Ca2 40.26(13) . 2
O3 Ca3 Ca2 83.31(14) 3 2
O3 Ca3 Ca2 40.25(13) 2 2
O2 Ca3 Ca2 97.14(12) . 2
O2 Ca3 Ca2 141.16(12) 3 2
O2 Ca3 Ca2 138.87(12) 2 2
Ca2 Ca3 Ca2 60.77(6) . 2
O3 Ca3 Ca2 83.31(14) . 3
O3 Ca3 Ca2 40.25(13) 3 3
O3 Ca3 Ca2 40.26(12) 2 3
O2 Ca3 Ca2 141.16(12) . 3
O2 Ca3 Ca2 138.87(12) 3 3
O2 Ca3 Ca2 97.14(12) 2 3
Ca2 Ca3 Ca2 60.77(6) . 3
Ca2 Ca3 Ca2 60.77(6) 2 3
O3 Ca3 Ca1 138.65(13) . .
O3 Ca3 Ca1 140.87(12) 3 .
O3 Ca3 Ca1 96.78(12) 2 .
O2 Ca3 Ca1 40.00(12) . .
O2 Ca3 Ca1 82.80(13) 3 .
O2 Ca3 Ca1 39.94(12) 2 .
Ca2 Ca3 Ca1 178.87(4) . .
Ca2 Ca3 Ca1 118.64(4) 2 .
Ca2 Ca3 Ca1 119.95(4) 3 .
O3 Ca3 Ca1 96.78(12) . 3
O3 Ca3 Ca1 138.65(13) 3 3
O3 Ca3 Ca1 140.87(12) 2 3
O2 Ca3 Ca1 39.94(12) . 3
O2 Ca3 Ca1 40.00(12) 3 3
O2 Ca3 Ca1 82.80(13) 2 3
Ca2 Ca3 Ca1 118.64(4) . 3
Ca2 Ca3 Ca1 119.95(4) 2 3
Ca2 Ca3 Ca1 178.87(4) 3 3
Ca1 Ca3 Ca1 60.65(5) . 3
O3 Ca3 Ca1 140.87(12) . 2
O3 Ca3 Ca1 96.78(12) 3 2
O3 Ca3 Ca1 138.65(12) 2 2
O2 Ca3 Ca1 82.80(13) . 2
O2 Ca3 Ca1 39.94(12) 3 2
O2 Ca3 Ca1 40.00(12) 2 2
Ca2 Ca3 Ca1 119.95(4) . 2
Ca2 Ca3 Ca1 178.87(4) 2 2
Ca2 Ca3 Ca1 118.64(4) 3 2
Ca1 Ca3 Ca1 60.65(5) . 2
Ca1 Ca3 Ca1 60.65(5) 3 2
Ca1 O1 Ca1 99.5(2) 3 .
Ca1 O1 Ca1 99.5(2) 3 2
Ca1 O1 Ca1 99.5(2) . 2
Ca1 O1 H1 118.2 3 .
Ca1 O1 H1 118.2 . .
Ca1 O1 H1 118.2 2 .
Ca1 O2 Ca1 102.05(19) 3 .
Ca1 O2 Ca3 98.45(18) 3 .
Ca1 O2 Ca3 98.38(18) . .
Ca1 O2 H2 118.1 3 .
Ca1 O2 H2 118.1 . .
Ca3 O2 H2 118.1 . .
Ca2 O3 Ca2 101.4(2) . 2
Ca2 O3 Ca3 98.59(19) . .
Ca2 O3 Ca3 98.58(19) 2 .
Ca2 O3 H3 118.2 . .
Ca2 O3 H3 118.2 2 .
Ca3 O3 H3 118.2 . .
Ca2 O4 Ca2 100.0(2) 2 .
Ca2 O4 Ca2 100.0(2) 2 3
Ca2 O4 Ca2 100.0(2) . 3
Ca2 O4 H4 117.8 2 .
Ca2 O4 H4 117.8 . .
Ca2 O4 H4 117.8 3 .
C1 O5 C4 108.2(9) . .
C1 O5 Ca1 125.9(6) . .
C4 O5 Ca1 125.1(7) . .
C5 O6 C8 105.9(12) . .
C5 O6 Ca1 125.3(8) . .
C8 O6 Ca1 123.9(9) . .
C9 O7 C12 108.8(8) . .
C9 O7 Ca2 125.8(6) . .
C12 O7 Ca2 122.5(7) . .
C13 O8 C16 109.8(8) . .
C13 O8 Ca2 125.7(6) . .
C16 O8 Ca2 120.6(7) . .
O8 C13 C14 104.7(9) . .
O8 C13 H13A 110.8 . .
C14 C13 H13A 110.8 . .
O8 C13 H13B 110.8 . .
C14 C13 H13B 110.8 . .
H13A C13 H13B 108.9 . .
C15 C14 C13 105.1(11) . .
C15 C14 H14A 110.7 . .
C13 C14 H14A 110.7 . .
C15 C14 H14B 110.7 . .
C13 C14 H14B 110.7 . .
H14A C14 H14B 108.8 . .
C16 C15 C14 108.6(14) . .
C16 C15 H15A 110.0 . .
C14 C15 H15A 110.0 . .
C16 C15 H15B 110.0 . .
C14 C15 H15B 110.0 . .
H15A C15 H15B 108.4 . .
C15 C16 O8 104.2(11) . .
C15 C16 H16A 110.9 . .
O8 C16 H16A 110.9 . .
C15 C16 H16B 110.9 . .
O8 C16 H16B 110.9 . .
H16A C16 H16B 108.9 . .
O7 C9 C10 108.3(10) . .
O7 C9 H9A 110.0 . .
C10 C9 H9A 110.0 . .
O7 C9 H9B 110.0 . .
C10 C9 H9B 110.0 . .
H9A C9 H9B 108.4 . .
C9 C10 C11 105.6(11) . .
C9 C10 H10A 110.6 . .
C11 C10 H10A 110.6 . .
C9 C10 H10B 110.6 . .
C11 C10 H10B 110.6 . .
H10A C10 H10B 108.7 . .
C12 C11 C10 108.1(10) . .
C12 C11 H11A 110.1 . .
C10 C11 H11A 110.1 . .
C12 C11 H11B 110.1 . .
C10 C11 H11B 110.1 . .
H11A C11 H11B 108.4 . .
O7 C12 C11 105.2(11) . .
O7 C12 H12A 110.7 . .
C11 C12 H12A 110.7 . .
O7 C12 H12B 110.7 . .
C11 C12 H12B 110.7 . .
H12A C12 H12B 108.8 . .
O5 C1 C2 107.9(10) . .
O5 C1 H1A 110.1 . .
C2 C1 H1A 110.1 . .
O5 C1 H1B 110.1 . .
C2 C1 H1B 110.1 . .
H1A C1 H1B 108.4 . .
C3 C2 C1 106.9(11) . .
C3 C2 H2A 110.3 . .
C1 C2 H2A 110.3 . .
C3 C2 H2B 110.4 . .
C1 C2 H2B 110.3 . .
H2A C2 H2B 108.6 . .
C2 C3 C4 112.9(13) . .
C2 C3 H3A 109.0 . .
C4 C3 H3A 109.0 . .
C2 C3 H3B 109.0 . .
C4 C3 H3B 109.0 . .
H3A C3 H3B 107.8 . .
O5 C4 C3 102.4(13) . .
O5 C4 H4A 111.3 . .
C3 C4 H4A 111.3 . .
O5 C4 H4B 111.3 . .
C3 C4 H4B 111.3 . .
H4A C4 H4B 109.2 . .
O6 C5 C6 109.5(17) . .
O6 C5 H5A 109.8 . .
C6 C5 H5A 109.8 . .
O6 C5 H5B 109.8 . .
C6 C5 H5B 109.8 . .
H5A C5 H5B 108.2 . .
C7 C6 C5 104.0(19) . .
C7 C6 H6A 111.0 . .
C5 C6 H6A 110.9 . .
C7 C6 H6B 110.9 . .
C5 C6 H6B 110.9 . .
H6A C6 H6B 109.0 . .
C6 C7 C8 104.6(18) . .
C6 C7 H7A 110.9 . .
C8 C7 H7A 110.9 . .
C6 C7 H7B 110.7 . .
C8 C7 H7B 110.8 . .
H7A C7 H7B 108.9 . .
O6 C8 C7 105.0(16) . .
O6 C8 H8A 110.7 . .
C7 C8 H8A 110.8 . .
O6 C8 H8B 110.8 . .
C7 C8 H8B 110.7 . .
H8A C8 H8B 108.8 . .
C20 O10 C17 100(3) . .
O10 C17 C18 109(3) . .
O10 C17 C20 37(2) . .
C18 C17 C20 73(3) . .
O10 C17 C19 76(2) . .
C18 C17 C19 40(2) . .
C20 C17 C19 38(2) . .
O10 C17 H17A 109.9 . .
C18 C17 H17A 109.9 . .
C20 C17 H17A 112.8 . .
C19 C17 H17A 103.0 . .
O10 C17 H17B 109.9 . .
C18 C17 H17B 109.9 . .
C20 C17 H17B 134.6 . .
C19 C17 H17B 143.4 . .
H17A C17 H17B 108.3 . .
C19 C18 C17 96(3) . .
C19 C18 H18A 112.6 . .
C17 C18 H18A 112.6 . .
C19 C18 H18B 112.6 . .
C17 C18 H18B 112.6 . .
H18A C18 H18B 110.1 . .
C18 C19 C20 106(4) . .
C18 C19 C17 45(2) . .
C20 C19 C17 69(3) . .
C18 C19 H19A 110.5 . .
C20 C19 H19A 110.5 . .
C17 C19 H19A 100.9 . .
C18 C19 H19B 110.5 . .
C20 C19 H19B 110.5 . .
C17 C19 H19B 147.8 . .
H19A C19 H19B 108.7 . .
O10 C20 C19 115(4) . .
O10 C20 C17 42(2) . .
C19 C20 C17 73(3) . .
O10 C20 H20A 108.6 . .
C19 C20 H20A 108.6 . .
C17 C20 H20A 121.6 . .
O10 C20 H20B 108.6 . .
C19 C20 H20B 108.5 . .
C17 C20 H20B 128.0 . .
H20A C20 H20B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I2 Ca1 3.1531(17) .
I3 Ca2 3.1470(17) .
Ca1 O2 2.309(5) 2
Ca1 O2 2.312(5) .
Ca1 O1 2.354(4) .
Ca1 O6 2.411(6) .
Ca1 O5 2.413(6) .
Ca1 Ca3 3.557(2) .
Ca1 Ca1 3.592(3) 3
Ca1 Ca1 3.592(3) 2
Ca2 O3 2.322(5) .
Ca2 O3 2.322(5) 3
Ca2 O4 2.346(4) .
Ca2 O8 2.425(7) .
Ca2 O7 2.438(7) .
Ca2 Ca3 3.553(2) .
Ca2 Ca2 3.595(3) 2
Ca2 Ca2 3.595(3) 3
Ca3 O3 2.365(5) .
Ca3 O3 2.365(5) 3
Ca3 O3 2.365(5) 2
Ca3 O2 2.388(5) .
Ca3 O2 2.388(5) 3
Ca3 O2 2.388(5) 2
Ca3 Ca2 3.553(2) 2
Ca3 Ca2 3.553(2) 3
Ca3 Ca1 3.557(2) 3
Ca3 Ca1 3.557(2) 2
O1 Ca1 2.354(4) 3
O1 Ca1 2.354(4) 2
O1 H1 1.0000 .
O2 Ca1 2.309(5) 3
O2 H2 1.0000 .
O3 Ca2 2.322(5) 2
O3 H3 1.0000 .
O4 Ca2 2.346(4) 2
O4 Ca2 2.346(4) 3
O4 H4 1.0000 .
O5 C1 1.419(13) .
O5 C4 1.431(15) .
O6 C5 1.381(15) .
O6 C8 1.438(18) .
O7 C9 1.432(12) .
O7 C12 1.442(12) .
O8 C13 1.431(12) .
O8 C16 1.468(13) .
C13 C14 1.472(16) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 C15 1.44(2) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C16 1.418(19) .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C9 C10 1.446(16) .
C9 H9A 0.9900 .
C9 H9B 0.9900 .
C10 C11 1.49(2) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.48(2) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C1 C2 1.463(16) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C3 1.30(2) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.50(2) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 C6 1.42(2) .
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C7 1.39(3) .
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.50(3) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 H8A 0.9900 .
C8 H8B 0.9900 .
O10 C20 1.22(6) .
O10 C17 1.35(4) .
C17 C18 1.42(6) .
C17 C20 1.97(5) .
C17 C19 2.01(5) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C18 C19 1.29(5) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.30(6) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
