# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2016

####################################################################### 
# 
# 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. 
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#######################################################################

data_03115
_database_code_depnum_ccdc_archive 'CCDC 1482630'
_audit_update_record             
;
2016-05-30 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;


_vrf_PLAT242_                    
; 
PROBLEM: _C Note: Check Low Ueq as Compared to Neighbors for C10. 
RESPONSE: IThis alert arises from the thermal motion of an atom
 in one of the ethyl groups. In the explanation offered by IUCR,
 "False alarms may occur for terminal groups such as the t-butyl moiety." 
;

_vrf_PLAT301_                    
; 
PROBLEM: _G Note: Main Residue Disorder ................... 8 Perc. 
RESPONSE: Yes, there is main residue disorder; it was modeled. 
;

_vrf_PLAT860_                    
; 
PROBLEM: _G Note: Number of Least-Squares Restraints ....... 3 
RESPONSE: These restraints arose from the modeling of disorder 
in the ethyl groups. 
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            03115
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H80 Ca I2 N8 O4'
_chemical_formula_sum            'C36 H80 Ca I2 N8 O4'
_chemical_formula_weight         982.96

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   16.066(2)
_cell_length_b                   19.561(2)
_cell_length_c                   15.994(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.274(2)
_cell_angle_gamma                90.00
_cell_volume                     4961(1)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2017
_cell_measurement_theta_min      1.97
_cell_measurement_theta_max      27.53

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2040
_exptl_absorpt_coefficient_mu    1.411
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.883840
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26985
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.97
_diffrn_reflns_theta_max         27.53
_reflns_number_total             5667
_reflns_number_gt                4824
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, Bruker'
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_solution    SIR97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  ?

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0338P)²+4.7446P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5667
_refine_ls_number_parameters     249
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0254
_refine_ls_wR_factor_ref         0.0681
_refine_ls_wR_factor_gt          0.0629
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_refine_ls_shift/su_max          0.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.5000 0.69574(3) 0.7500 0.02746(11) Uani 1 2 d S . .
I1 I 0.466873(9) 0.716955(7) 0.547860(8) 0.04052(6) Uani 1 1 d . . .
O1 O 0.35797(8) 0.68783(8) 0.75389(9) 0.0402(3) Uani 1 1 d . . .
O2 O 0.5000 0.57937(10) 0.7500 0.0370(4) Uani 1 2 d S . .
O3 O 0.5000 0.81234(11) 0.7500 0.0470(5) Uani 1 2 d S . .
N1 N 0.25444(11) 0.66522(9) 0.83224(10) 0.0377(4) Uani 1 1 d D . .
N2 N 0.22670(11) 0.72799(11) 0.70593(13) 0.0470(5) Uani 1 1 d . . .
N3 N 0.47293(11) 0.48080(9) 0.67658(11) 0.0368(4) Uani 1 1 d . . .
N4 N 0.45843(17) 0.91194(10) 0.80376(13) 0.0593(6) Uani 1 1 d . . .
C1 C 0.28339(12) 0.69384(10) 0.76333(13) 0.0338(4) Uani 1 1 d . A .
C2 C 0.5000 0.51555(14) 0.7500 0.0319(5) Uani 1 2 d S . .
C3 C 0.5000 0.87530(16) 0.7500 0.0435(7) Uani 1 2 d S . .
C4 C 0.31052(15) 0.61487(13) 0.88195(15) 0.0503(6) Uani 1 1 d . A .
H4A H 0.2967 0.6125 0.9400 0.060 Uiso 1 1 calc R . .
H4B H 0.3696 0.6306 0.8864 0.060 Uiso 1 1 calc R . .
C5 C 0.3032(2) 0.54517(15) 0.8439(2) 0.0710(8) Uani 1 1 d . . .
H5A H 0.3400 0.5136 0.8803 0.107 Uiso 1 1 calc R A .
H5B H 0.3201 0.5466 0.7877 0.107 Uiso 1 1 calc R . .
H5C H 0.2446 0.5295 0.8385 0.107 Uiso 1 1 calc R . .
C6 C 0.1974(4) 0.7038(3) 0.8784(4) 0.0534(13) Uani 0.739(13) 1 d PD A 1
H6A H 0.1753 0.7439 0.8441 0.064 Uiso 0.739(13) 1 calc PR A 1
H6B H 0.2300 0.7209 0.9322 0.064 Uiso 0.739(13) 1 calc PR A 1
C7 C 0.1237(4) 0.6613(4) 0.8981(5) 0.0768(19) Uani 0.739(13) 1 d PD A 1
H7A H 0.0888 0.6891 0.9299 0.115 Uiso 0.739(13) 1 calc PR A 1
H7B H 0.1451 0.6214 0.9320 0.115 Uiso 0.739(13) 1 calc PR A 1
H7C H 0.0895 0.6460 0.8450 0.115 Uiso 0.739(13) 1 calc PR A 1
C6' C 0.2248(12) 0.7142(7) 0.8903(11) 0.0534(13) Uani 0.261(13) 1 d PD A 5
H6C H 0.2034 0.7557 0.8586 0.064 Uiso 0.261(13) 1 calc PR A 5
H6D H 0.2725 0.7278 0.9343 0.064 Uiso 0.261(13) 1 calc PR A 5
C7' C 0.1553(12) 0.6836(10) 0.9324(12) 0.0768(19) Uani 0.261(13) 1 d PD A 5
H7D H 0.1374 0.7170 0.9716 0.115 Uiso 0.261(13) 1 calc PR A 5
H7E H 0.1764 0.6424 0.9637 0.115 Uiso 0.261(13) 1 calc PR A 5
H7F H 0.1072 0.6716 0.8890 0.115 Uiso 0.261(13) 1 calc PR A 5
C8 C 0.25728(19) 0.76417(19) 0.6358(2) 0.0740(10) Uani 1 1 d . A .
H8A H 0.2324 0.7426 0.5815 0.089 Uiso 1 1 calc R . .
H8B H 0.3193 0.7591 0.6423 0.089 Uiso 1 1 calc R . .
C9 C 0.2356(2) 0.83855(17) 0.6326(2) 0.0817(10) Uani 1 1 d . . .
H9A H 0.2567 0.8599 0.5847 0.123 Uiso 1 1 calc R A .
H9B H 0.2618 0.8606 0.6854 0.123 Uiso 1 1 calc R . .
H9C H 0.1742 0.8440 0.6257 0.123 Uiso 1 1 calc R . .
C10 C 0.13828(15) 0.70818(14) 0.68762(19) 0.0556(6) Uani 1 1 d . A .
H10A H 0.1061 0.7433 0.6513 0.067 Uiso 1 1 calc R . .
H10B H 0.1150 0.7055 0.7412 0.067 Uiso 1 1 calc R . .
C11 C 0.1283(3) 0.64038(18) 0.6435(3) 0.1024(14) Uani 1 1 d . . .
H11A H 0.0683 0.6287 0.6305 0.154 Uiso 1 1 calc R A .
H11B H 0.1581 0.6052 0.6805 0.154 Uiso 1 1 calc R . .
H11C H 0.1520 0.6429 0.5909 0.154 Uiso 1 1 calc R . .
C12 C 0.43783(15) 0.52184(12) 0.60148(14) 0.0441(5) Uani 1 1 d . . .
H12A H 0.4402 0.4944 0.5499 0.053 Uiso 1 1 calc R . .
H12B H 0.4738 0.5626 0.5990 0.053 Uiso 1 1 calc R . .
C13 C 0.34808(16) 0.54498(14) 0.60086(17) 0.0577(6) Uani 1 1 d . . .
H13A H 0.3283 0.5701 0.5484 0.087 Uiso 1 1 calc R . .
H13B H 0.3457 0.5748 0.6496 0.087 Uiso 1 1 calc R . .
H13C H 0.3120 0.5050 0.6041 0.087 Uiso 1 1 calc R . .
C14 C 0.50254(15) 0.41263(11) 0.65664(14) 0.0441(5) Uani 1 1 d . . .
H14A H 0.5424 0.3955 0.7059 0.053 Uiso 1 1 calc R . .
H14B H 0.5335 0.4164 0.6081 0.053 Uiso 1 1 calc R . .
C15 C 0.43149(19) 0.36129(13) 0.63500(17) 0.0589(7) Uani 1 1 d . . .
H15A H 0.4549 0.3170 0.6219 0.088 Uiso 1 1 calc R . .
H15B H 0.3922 0.3775 0.5857 0.088 Uiso 1 1 calc R . .
H15C H 0.4016 0.3562 0.6834 0.088 Uiso 1 1 calc R . .
C16 C 0.5016(3) 0.97046(15) 0.84899(19) 0.0795(10) Uani 1 1 d . . .
H16A H 0.4590 1.0019 0.8659 0.095 Uiso 1 1 calc R . .
H16B H 0.5329 0.9956 0.8102 0.095 Uiso 1 1 calc R . .
C17 C 0.5617(3) 0.9498(2) 0.9260(3) 0.1180(16) Uani 1 1 d . . .
H17A H 0.5904 0.9904 0.9524 0.177 Uiso 1 1 calc R . .
H17B H 0.6034 0.9180 0.9098 0.177 Uiso 1 1 calc R . .
H17C H 0.5306 0.9275 0.9663 0.177 Uiso 1 1 calc R . .
C18 C 0.40059(19) 0.87395(14) 0.84820(18) 0.0615(7) Uani 1 1 d . . .
H18A H 0.4311 0.8584 0.9037 0.074 Uiso 1 1 calc R . .
H18B H 0.3802 0.8329 0.8148 0.074 Uiso 1 1 calc R . .
C19 C 0.3259(2) 0.9170(2) 0.8621(2) 0.0850(11) Uani 1 1 d . . .
H19A H 0.2856 0.8885 0.8864 0.127 Uiso 1 1 calc R . .
H19B H 0.2984 0.9358 0.8078 0.127 Uiso 1 1 calc R . .
H19C H 0.3452 0.9545 0.9011 0.127 Uiso 1 1 calc R . .


_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 2.276(2) . ?
Ca1 O3 2.281(2) . ?
Ca1 O1 2.2978(14) 2_656 ?
Ca1 O1 2.2978(14) . ?
Ca1 I1 3.2177(4) 2_656 ?
Ca1 I1 3.2177(4) . ?
O1 C1 1.237(2) . ?
O2 C2 1.248(3) . ?
O3 C3 1.232(4) . ?
N1 C1 1.382(3) . ?
N1 C6' 1.466(8) . ?
N1 C6 1.473(4) . ?
N1 C4 1.478(3) . ?
N2 C1 1.360(3) . ?
N2 C10 1.456(3) . ?
N2 C8 1.475(3) . ?
N3 C2 1.366(2) . ?
N3 C14 1.468(3) . ?
N3 C12 1.479(3) . ?
N4 C3 1.373(3) . ?
N4 C18 1.461(4) . ?
N4 C16 1.467(4) . ?
C2 N3 1.366(2) 2_656 ?
C3 N4 1.373(3) 2_656 ?
C4 C5 1.490(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.521(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C6' C7' 1.516(10) . ?
C6' H6C 0.9900 . ?
C6' H6D 0.9900 . ?
C7' H7D 0.9800 . ?
C7' H7E 0.9800 . ?
C7' H7F 0.9800 . ?
C8 C9 1.495(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.498(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.510(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.518(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.492(5) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.511(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 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
O2 Ca1 O3 180.000(1) . . ?
O2 Ca1 O1 86.14(4) . 2_656 ?
O3 Ca1 O1 93.86(4) . 2_656 ?
O2 Ca1 O1 86.14(4) . . ?
O3 Ca1 O1 93.86(4) . . ?
O1 Ca1 O1 172.28(8) 2_656 . ?
O2 Ca1 I1 97.411(10) . 2_656 ?
O3 Ca1 I1 82.589(10) . 2_656 ?
O1 Ca1 I1 91.82(4) 2_656 2_656 ?
O1 Ca1 I1 89.18(4) . 2_656 ?
O2 Ca1 I1 97.411(10) . . ?
O3 Ca1 I1 82.589(10) . . ?
O1 Ca1 I1 89.18(4) 2_656 . ?
O1 Ca1 I1 91.82(4) . . ?
I1 Ca1 I1 165.178(19) 2_656 . ?
C1 O1 Ca1 169.22(15) . . ?
C2 O2 Ca1 180.000(1) . . ?
C3 O3 Ca1 180.000(1) . . ?
C1 N1 C6' 115.2(7) . . ?
C1 N1 C6 120.6(3) . . ?
C1 N1 C4 116.41(17) . . ?
C6' N1 C4 109.1(9) . . ?
C6 N1 C4 116.5(3) . . ?
C1 N2 C10 122.05(19) . . ?
C1 N2 C8 118.68(19) . . ?
C10 N2 C8 114.1(2) . . ?
C2 N3 C14 124.70(18) . . ?
C2 N3 C12 117.07(18) . . ?
C14 N3 C12 114.28(17) . . ?
C3 N4 C18 116.8(2) . . ?
C3 N4 C16 118.5(2) . . ?
C18 N4 C16 116.4(2) . . ?
O1 C1 N2 121.38(19) . . ?
O1 C1 N1 121.05(18) . . ?
N2 C1 N1 117.56(17) . . ?
O2 C2 N3 119.84(12) . . ?
O2 C2 N3 119.84(12) . 2_656 ?
N3 C2 N3 120.3(2) . 2_656 ?
O3 C3 N4 121.48(14) . 2_656 ?
O3 C3 N4 121.48(14) . . ?
N4 C3 N4 117.0(3) 2_656 . ?
N1 C4 C5 112.9(2) . . ?
N1 C4 H4A 109.0 . . ?
C5 C4 H4A 109.0 . . ?
N1 C4 H4B 109.0 . . ?
C5 C4 H4B 109.0 . . ?
H4A C4 H4B 107.8 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C7 113.1(4) . . ?
N1 C6 H6A 109.0 . . ?
C7 C6 H6A 109.0 . . ?
N1 C6 H6B 109.0 . . ?
C7 C6 H6B 109.0 . . ?
H6A C6 H6B 107.8 . . ?
N1 C6' C7' 111.1(10) . . ?
N1 C6' H6C 109.4 . . ?
C7' C6' H6C 109.4 . . ?
N1 C6' H6D 109.4 . . ?
C7' C6' H6D 109.4 . . ?
H6C C6' H6D 108.0 . . ?
N2 C8 C9 112.9(3) . . ?
N2 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
N2 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 110.9(3) . . ?
N2 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
N2 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.0 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N3 C12 C13 114.01(19) . . ?
N3 C12 H12A 108.8 . . ?
C13 C12 H12A 108.7 . . ?
N3 C12 H12B 108.7 . . ?
C13 C12 H12B 108.8 . . ?
H12A C12 H12B 107.6 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 C15 113.1(2) . . ?
N3 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
N3 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N4 C16 C17 112.8(3) . . ?
N4 C16 H16A 109.0 . . ?
C17 C16 H16A 109.0 . . ?
N4 C16 H16B 109.0 . . ?
C17 C16 H16B 109.0 . . ?
H16A C16 H16B 107.8 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N4 C18 C19 111.8(3) . . ?
N4 C18 H18A 109.3 . . ?
C19 C18 H18A 109.3 . . ?
N4 C18 H18B 109.3 . . ?
C19 C18 H18B 109.3 . . ?
H18A C18 H18B 107.9 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 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
O3 Ca1 O1 C1 -30.2(8) . . . . ?
I1 Ca1 O1 C1 52.3(8) 2_656 . . . ?
I1 Ca1 O1 C1 -112.9(8) . . . . ?
Ca1 O1 C1 N2 88.9(8) . . . . ?
Ca1 O1 C1 N1 -91.9(8) . . . . ?
C10 N2 C1 O1 147.0(2) . . . . ?
C8 N2 C1 O1 -6.1(4) . . . . ?
C10 N2 C1 N1 -32.2(3) . . . . ?
C8 N2 C1 N1 174.7(2) . . . . ?
C6' N1 C1 O1 116.0(9) . . . . ?
C6 N1 C1 O1 137.1(4) . . . . ?
C4 N1 C1 O1 -13.6(3) . . . . ?
C6' N1 C1 N2 -64.9(9) . . . . ?
C6 N1 C1 N2 -43.8(4) . . . . ?
C4 N1 C1 N2 165.6(2) . . . . ?
C14 N3 C2 O2 151.23(15) . . . . ?
C12 N3 C2 O2 -5.07(19) . . . . ?
C14 N3 C2 N3 -28.77(15) . . . 2_656 ?
C12 N3 C2 N3 174.93(19) . . . 2_656 ?
C18 N4 C3 O3 -12.1(3) . . . . ?
C16 N4 C3 O3 135.10(19) . . . . ?
C18 N4 C3 N4 167.9(3) . . . 2_656 ?
C16 N4 C3 N4 -44.90(19) . . . 2_656 ?
C1 N1 C4 C5 -82.1(3) . . . . ?
C6' N1 C4 C5 145.5(7) . . . . ?
C6 N1 C4 C5 126.0(4) . . . . ?
C1 N1 C6 C7 135.0(4) . . . . ?
C6' N1 C6 C7 -146(3) . . . . ?
C4 N1 C6 C7 -74.3(4) . . . . ?
C1 N1 C6' C7' 149.4(12) . . . . ?
C6 N1 C6' C7' 39(2) . . . . ?
C4 N1 C6' C7' -77.5(14) . . . . ?
C1 N2 C8 C9 -123.1(3) . . . . ?
C10 N2 C8 C9 81.7(3) . . . . ?
C1 N2 C10 C11 -67.9(3) . . . . ?
C8 N2 C10 C11 86.3(3) . . . . ?
C2 N3 C12 C13 -78.9(2) . . . . ?
C14 N3 C12 C13 122.4(2) . . . . ?
C2 N3 C14 C15 124.2(2) . . . . ?
C12 N3 C14 C15 -78.9(2) . . . . ?
C3 N4 C16 C17 -81.2(4) . . . . ?
C18 N4 C16 C17 66.2(4) . . . . ?
C3 N4 C18 C19 -146.8(2) . . . . ?
C16 N4 C18 C19 65.3(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.064



_exptl_crystal_recrystallization_method 'From the Melt'
####################################################################### 
# 
# 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_02250a
_database_code_depnum_ccdc_archive 'CCDC 1482631'
_audit_update_record             
;
2016-05-30 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            02250a
_chemical_melting_point          376-379
_chemical_formula_moiety         'C24 H38 Ca N2 O7, 2(I)'
_chemical_formula_sum            'C24 H38 Ca I2 N2 O7'
_chemical_formula_weight         760.44

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   14.340(2)
_cell_length_b                   15.857(2)
_cell_length_c                   14.444(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.616(3)
_cell_angle_gamma                90.00
_cell_volume                     3163.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3039
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      25.054

_exptl_crystal_description       Needle
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512
_exptl_absorpt_coefficient_mu    2.190
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4390
_exptl_absorpt_correction_T_max  0.9175
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'

_exptl_special_details           'L. Fitts / T. Hanusa - Vanderbilt University'

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker CCD platform'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12297
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0383
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.96
_diffrn_reflns_theta_max         25.06
_reflns_number_total             2811
_reflns_number_gt                2229
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SIR-97
_computing_structure_refinement  'Bruker SHELXTL'
_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0473P)²+6.7699P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2811
_refine_ls_number_parameters     170
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0936
_refine_ls_wR_factor_gt          0.0861
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.100
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.28962(2) 0.11046(2) 0.90295(2) 0.03648(14) Uani 1 1 d . . .
Ca1 Ca 0.0000 0.28569(7) 0.7500 0.0226(3) Uani 1 2 d S . .
O1 O 0.0436(2) 0.15480(18) 0.6861(2) 0.0295(7) Uani 1 1 d . . .
N1 N 0.0215(3) 0.0840(2) 0.7157(3) 0.0248(8) Uani 1 1 d . . .
C1 C 0.0386(3) 0.0080(3) 0.6674(3) 0.0237(9) Uani 1 1 d . . .
C2 C 0.1326(3) -0.0127(3) 0.6714(3) 0.0339(11) Uani 1 1 d . . .
H2A H 0.1851 0.0199 0.7083 0.041 Uiso 1 1 calc R . .
C3 C 0.1485(4) -0.0822(3) 0.6203(4) 0.0440(13) Uani 1 1 d . . .
H3A H 0.2128 -0.0988 0.6229 0.053 Uiso 1 1 calc R . .
C4 C 0.0711(4) -0.1279(3) 0.5653(4) 0.0421(13) Uani 1 1 d . . .
H4A H 0.0824 -0.1758 0.5302 0.050 Uiso 1 1 calc R . .
C5 C -0.0221(4) -0.1042(3) 0.5611(4) 0.0411(13) Uani 1 1 d . . .
H5A H -0.0749 -0.1353 0.5222 0.049 Uiso 1 1 calc R . .
C6 C -0.0397(3) -0.0359(3) 0.6129(3) 0.0320(11) Uani 1 1 d . . .
H6A H -0.1040 -0.0196 0.6109 0.038 Uiso 1 1 calc R . .
O2 O 0.1096(2) 0.3169(2) 0.6561(2) 0.0373(8) Uani 1 1 d . . .
C7 C 0.2012(4) 0.2760(4) 0.6685(4) 0.0440(13) Uani 1 1 d . . .
H7A H 0.1928 0.2194 0.6383 0.053 Uiso 1 1 calc R . .
H7B H 0.2352 0.2699 0.7376 0.053 Uiso 1 1 calc R . .
C8 C 0.2559(5) 0.3330(4) 0.6196(4) 0.0522(15) Uani 1 1 d . . .
H8A H 0.2849 0.3808 0.6616 0.063 Uiso 1 1 calc R . .
H8B H 0.3077 0.3021 0.6004 0.063 Uiso 1 1 calc R . .
C9 C 0.1800(5) 0.3625(4) 0.5341(4) 0.0529(15) Uani 1 1 d . . .
H9A H 0.1704 0.3217 0.4805 0.063 Uiso 1 1 calc R . .
H9B H 0.1967 0.4182 0.5121 0.063 Uiso 1 1 calc R . .
C10 C 0.0911(5) 0.3681(4) 0.5706(4) 0.0516(15) Uani 1 1 d . . .
H10A H 0.0790 0.4273 0.5857 0.062 Uiso 1 1 calc R . .
H10B H 0.0337 0.3469 0.5215 0.062 Uiso 1 1 calc R . .
O3 O 0.0000 0.4361(3) 0.7500 0.0340(11) Uani 1 2 d S . .
C11 C 0.0806(4) 0.4897(3) 0.7971(4) 0.0414(13) Uani 1 1 d . . .
H11A H 0.1314 0.4878 0.7623 0.050 Uiso 1 1 calc R . .
H11B H 0.1091 0.4707 0.8640 0.050 Uiso 1 1 calc R . .
C12 C 0.0419(4) 0.5768(3) 0.7961(4) 0.0477(14) Uani 1 1 d . . .
H12A H 0.0914 0.6194 0.7929 0.057 Uiso 1 1 calc R . .
H12B H 0.0185 0.5876 0.8535 0.057 Uiso 1 1 calc R . .
O4 O 0.1350(2) 0.2830(2) 0.8829(2) 0.0370(8) Uani 1 1 d D . .
H4B H 0.155(4) 0.306(3) 0.9372(19) 0.055 Uiso 1 1 d D . .
H4C H 0.168(4) 0.238(2) 0.888(4) 0.055 Uiso 1 1 d 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 O4 2.330(3) 2_556 ?
Ca1 O4 2.330(3) . ?
Ca1 O3 2.385(4) . ?
Ca1 O2 2.388(3) 2_556 ?
Ca1 O2 2.388(3) . ?
Ca1 O1 2.421(3) . ?
Ca1 O1 2.421(3) 2_556 ?
Ca1 H4C 2.78(5) . ?
O1 N1 1.271(5) . ?
N1 N1 1.301(7) 2_556 ?
N1 C1 1.446(5) . ?
C1 C2 1.372(6) . ?
C1 C6 1.375(6) . ?
C2 C3 1.380(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.383(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.373(8) . ?
C4 H4A 0.9500 . ?
C5 C6 1.378(7) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
O2 C7 1.432(6) . ?
O2 C10 1.443(6) . ?
C7 C8 1.494(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.485(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.507(8) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
O3 C11 1.448(5) . ?
O3 C11 1.448(5) 2_556 ?
C11 C12 1.487(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C12 1.535(11) 2_556 ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O4 H4B 0.840(5) . ?
O4 H4C 0.840(5) . ?

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 O4 177.91(18) 2_556 . ?
O4 Ca1 O3 91.04(9) 2_556 . ?
O4 Ca1 O3 91.04(9) . . ?
O4 Ca1 O2 86.77(12) 2_556 2_556 ?
O4 Ca1 O2 93.67(12) . 2_556 ?
O3 Ca1 O2 78.05(9) . 2_556 ?
O4 Ca1 O2 93.67(12) 2_556 . ?
O4 Ca1 O2 86.77(12) . . ?
O3 Ca1 O2 78.05(9) . . ?
O2 Ca1 O2 156.11(17) 2_556 . ?
O4 Ca1 O1 85.00(12) 2_556 . ?
O4 Ca1 O1 93.20(11) . . ?
O3 Ca1 O1 149.01(7) . . ?
O2 Ca1 O1 132.15(11) 2_556 . ?
O2 Ca1 O1 71.57(11) . . ?
O4 Ca1 O1 93.20(11) 2_556 2_556 ?
O4 Ca1 O1 85.00(12) . 2_556 ?
O3 Ca1 O1 149.01(7) . 2_556 ?
O2 Ca1 O1 71.57(11) 2_556 2_556 ?
O2 Ca1 O1 132.15(11) . 2_556 ?
O1 Ca1 O1 61.97(14) . 2_556 ?
O4 Ca1 H4C 162.0(8) 2_556 . ?
O4 Ca1 H4C 16.1(8) . . ?
O3 Ca1 H4C 105.6(9) . . ?
O2 Ca1 H4C 103.0(11) 2_556 . ?
O2 Ca1 H4C 83.5(12) . . ?
O1 Ca1 H4C 77.2(8) . . ?
O1 Ca1 H4C 76.0(11) 2_556 . ?
N1 O1 Ca1 121.0(2) . . ?
O1 N1 N1 117.9(2) . 2_556 ?
O1 N1 C1 118.9(3) . . ?
N1 N1 C1 123.0(2) 2_556 . ?
C2 C1 C6 123.0(4) . . ?
C2 C1 N1 118.1(4) . . ?
C6 C1 N1 118.6(4) . . ?
C1 C2 C3 118.1(5) . . ?
C1 C2 H2A 121.0 . . ?
C3 C2 H2A 121.0 . . ?
C2 C3 C4 120.2(5) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 120.2(5) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
C4 C5 C6 120.6(5) . . ?
C4 C5 H5A 119.7 . . ?
C6 C5 H5A 119.7 . . ?
C1 C6 C5 117.9(4) . . ?
C1 C6 H6A 121.0 . . ?
C5 C6 H6A 121.0 . . ?
C7 O2 C10 108.3(4) . . ?
C7 O2 Ca1 123.9(3) . . ?
C10 O2 Ca1 127.3(3) . . ?
O2 C7 C8 104.3(4) . . ?
O2 C7 H7A 110.9 . . ?
C8 C7 H7A 110.9 . . ?
O2 C7 H7B 110.9 . . ?
C8 C7 H7B 110.9 . . ?
H7A C7 H7B 108.9 . . ?
C9 C8 C7 102.9(5) . . ?
C9 C8 H8A 111.2 . . ?
C7 C8 H8A 111.2 . . ?
C9 C8 H8B 111.2 . . ?
C7 C8 H8B 111.2 . . ?
H8A C8 H8B 109.1 . . ?
C8 C9 C10 103.1(5) . . ?
C8 C9 H9A 111.1 . . ?
C10 C9 H9A 111.1 . . ?
C8 C9 H9B 111.1 . . ?
C10 C9 H9B 111.1 . . ?
H9A C9 H9B 109.1 . . ?
O2 C10 C9 106.8(5) . . ?
O2 C10 H10A 110.4 . . ?
C9 C10 H10A 110.4 . . ?
O2 C10 H10B 110.4 . . ?
C9 C10 H10B 110.4 . . ?
H10A C10 H10B 108.6 . . ?
C11 O3 C11 108.1(5) . 2_556 ?
C11 O3 Ca1 125.9(2) . . ?
C11 O3 Ca1 125.9(2) 2_556 . ?
O3 C11 C12 107.0(4) . . ?
O3 C11 H11A 110.3 . . ?
C12 C11 H11A 110.3 . . ?
O3 C11 H11B 110.3 . . ?
C12 C11 H11B 110.3 . . ?
H11A C11 H11B 108.6 . . ?
C11 C12 C12 102.2(3) . 2_556 ?
C11 C12 H12A 111.3 . . ?
C12 C12 H12A 111.3 2_556 . ?
C11 C12 H12B 111.3 . . ?
C12 C12 H12B 111.3 2_556 . ?
H12A C12 H12B 109.2 . . ?
Ca1 O4 H4B 139(4) . . ?
Ca1 O4 H4C 114(4) . . ?
H4B O4 H4C 104(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
O4 Ca1 O1 N1 -95.2(3) 2_556 . . . ?
O4 Ca1 O1 N1 83.7(3) . . . . ?
O3 Ca1 O1 N1 -178.9(2) . . . . ?
O2 Ca1 O1 N1 -14.2(3) 2_556 . . . ?
O2 Ca1 O1 N1 169.2(3) . . . . ?
O1 Ca1 O1 N1 1.1(2) 2_556 . . . ?
Ca1 O1 N1 N1 -3.1(6) . . . 2_556 ?
Ca1 O1 N1 C1 172.7(3) . . . . ?
O1 N1 C1 C2 64.3(5) . . . . ?
N1 N1 C1 C2 -120.2(6) 2_556 . . . ?
O1 N1 C1 C6 -110.0(5) . . . . ?
N1 N1 C1 C6 65.5(7) 2_556 . . . ?
C6 C1 C2 C3 -1.9(7) . . . . ?
N1 C1 C2 C3 -175.9(4) . . . . ?
C1 C2 C3 C4 1.4(8) . . . . ?
C2 C3 C4 C5 0.1(9) . . . . ?
C3 C4 C5 C6 -1.2(8) . . . . ?
C2 C1 C6 C5 0.8(7) . . . . ?
N1 C1 C6 C5 174.8(4) . . . . ?
C4 C5 C6 C1 0.8(8) . . . . ?
O4 Ca1 O2 C7 -135.3(4) 2_556 . . . ?
O4 Ca1 O2 C7 42.6(4) . . . . ?
O3 Ca1 O2 C7 134.4(4) . . . . ?
O2 Ca1 O2 C7 134.4(4) 2_556 . . . ?
O1 Ca1 O2 C7 -51.8(4) . . . . ?
O1 Ca1 O2 C7 -37.6(4) 2_556 . . . ?
O4 Ca1 O2 C10 34.5(4) 2_556 . . . ?
O4 Ca1 O2 C10 -147.5(4) . . . . ?
O3 Ca1 O2 C10 -55.8(4) . . . . ?
O2 Ca1 O2 C10 -55.8(4) 2_556 . . . ?
O1 Ca1 O2 C10 118.0(4) . . . . ?
O1 Ca1 O2 C10 132.2(4) 2_556 . . . ?
C10 O2 C7 C8 26.3(6) . . . . ?
Ca1 O2 C7 C8 -162.2(3) . . . . ?
O2 C7 C8 C9 -38.0(6) . . . . ?
C7 C8 C9 C10 34.6(6) . . . . ?
C7 O2 C10 C9 -4.4(6) . . . . ?
Ca1 O2 C10 C9 -175.5(3) . . . . ?
C8 C9 C10 O2 -19.3(6) . . . . ?
O4 Ca1 O3 C11 -161.4(3) 2_556 . . . ?
O4 Ca1 O3 C11 18.6(3) . . . . ?
O2 Ca1 O3 C11 112.1(3) 2_556 . . . ?
O2 Ca1 O3 C11 -67.9(3) . . . . ?
O1 Ca1 O3 C11 -79.4(3) . . . . ?
O1 Ca1 O3 C11 100.6(3) 2_556 . . . ?
O4 Ca1 O3 C11 18.6(3) 2_556 . . 2_556 ?
O4 Ca1 O3 C11 -161.4(3) . . . 2_556 ?
O2 Ca1 O3 C11 -67.9(3) 2_556 . . 2_556 ?
O2 Ca1 O3 C11 112.1(3) . . . 2_556 ?
O1 Ca1 O3 C11 100.6(3) . . . 2_556 ?
O1 Ca1 O3 C11 -79.4(3) 2_556 . . 2_556 ?
C11 O3 C11 C12 12.0(3) 2_556 . . . ?
Ca1 O3 C11 C12 -168.0(3) . . . . ?
O3 C11 C12 C12 -30.1(7) . . . 2_556 ?

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
O4 H4C I1 0.840(5) 2.650(10) 3.485(3) 173(5) .
O4 H4B I1 0.840(5) 2.597(8) 3.434(3) 174(5) 7_557

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.06
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.003
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.120


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method THF/toluene
####################################################################### 
# 
# 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_99290
_database_code_depnum_ccdc_archive 'CCDC 1482632'
_audit_update_record             
;
2016-05-30 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;

_vrf_PLAT601_vand90              
; 
PROBLEM: _C Structure Contains Solvent Accessible VOIDS of .         42 Ang3 
RESPONSE: This may be a result of slight ligand disorder; there is no evidence
for included solvent. Other PLATON alerts re Hirshfeld tests, short bond lengths
are also likely consequences of disorder.

;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            99290
_chemical_melting_point          436-440
_chemical_formula_moiety         'I, C45 H105 Ca I O5 P5'
_chemical_formula_sum            'C45 H105 Ca I2 O5 P5'
_chemical_formula_weight         1175.02

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'
P P 0.1023 0.0942 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   13.0031(8)
_cell_length_b                   17.628(1)
_cell_length_c                   28.160(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6454.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8192
_cell_measurement_theta_min      1.45
_cell_measurement_theta_max      27.53

_exptl_crystal_description       'irregular block'
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.152
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.884602
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART Platform CCD'
_diffrn_measurement_method       'area detector, omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44664
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.45
_diffrn_reflns_theta_max         27.53
_reflns_number_total             14683
_reflns_number_gt                9472
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART, Bruker'
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  ?

_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0582P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_number_reflns         14683
_refine_ls_number_parameters     538
_refine_ls_number_restraints     399
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1148
_refine_ls_wR_factor_gt          0.1010
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.002
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.89309(3) 1.13756(2) 0.045646(16) 0.05851(13) Uani 1 1 d . . .
I2 I 0.23034(3) 0.75189(2) 0.148374(13) 0.05200(11) Uani 1 1 d . . .
Ca1 Ca 0.71618(9) 1.03082(7) 0.09383(4) 0.0396(3) Uani 1 1 d . . .
O1 O 0.5871(4) 0.9650(3) 0.13271(18) 0.0725(14) Uani 1 1 d D . .
P1 P 0.49217(16) 0.91813(13) 0.13025(9) 0.0803(7) Uani 1 1 d D . .
C1 C 0.5138(7) 0.8216(5) 0.1145(5) 0.150(6) Uani 1 1 d D . .
H1A H 0.4554 0.7920 0.1273 0.180 Uiso 1 1 calc R . .
H1B H 0.5090 0.8186 0.0794 0.180 Uiso 1 1 calc R . .
C2 C 0.6009(9) 0.7846(5) 0.1272(6) 0.155(6) Uani 1 1 d D . .
H2A H 0.6087 0.7899 0.1620 0.186 Uiso 1 1 calc R . .
H2B H 0.6596 0.8114 0.1124 0.186 Uiso 1 1 calc R . .
C3 C 0.6115(11) 0.7011(5) 0.1153(4) 0.142(5) Uani 1 1 d D . .
H3A H 0.5529 0.6731 0.1285 0.212 Uiso 1 1 calc R . .
H3B H 0.6755 0.6814 0.1290 0.212 Uiso 1 1 calc R . .
H3C H 0.6131 0.6946 0.0807 0.212 Uiso 1 1 calc R . .
C4 C 0.4182(6) 0.9219(4) 0.1842(2) 0.074(2) Uani 1 1 d D . .
H4A H 0.4004 0.9756 0.1906 0.089 Uiso 1 1 calc R . .
H4B H 0.3530 0.8942 0.1791 0.089 Uiso 1 1 calc R . .
C5 C 0.4686(8) 0.8905(6) 0.2270(3) 0.122(4) Uani 1 1 d D . .
H5A H 0.5370 0.9144 0.2311 0.146 Uiso 1 1 calc R . .
H5B H 0.4789 0.8352 0.2229 0.146 Uiso 1 1 calc R . .
C6 C 0.4009(10) 0.9056(6) 0.2721(3) 0.144(5) Uani 1 1 d D . .
H6A H 0.3961 0.9603 0.2777 0.215 Uiso 1 1 calc R . .
H6B H 0.4325 0.8810 0.2997 0.215 Uiso 1 1 calc R . .
H6C H 0.3319 0.8848 0.2670 0.215 Uiso 1 1 calc R . .
C7 C 0.4051(8) 0.9510(6) 0.0836(3) 0.119(4) Uani 1 1 d D . .
H7A H 0.4401 0.9455 0.0526 0.143 Uiso 1 1 calc R . .
H7B H 0.3438 0.9177 0.0832 0.143 Uiso 1 1 calc R . .
C8 C 0.3717(8) 1.0278(7) 0.0886(4) 0.133(5) Uani 1 1 d D . .
H8A H 0.4324 1.0611 0.0927 0.159 Uiso 1 1 calc R . .
H8B H 0.3285 1.0324 0.1174 0.159 Uiso 1 1 calc R . .
C9 C 0.3092(8) 1.0544(8) 0.0448(4) 0.184(7) Uani 1 1 d D . .
H9A H 0.3516 1.0884 0.0254 0.276 Uiso 1 1 calc R . .
H9B H 0.2474 1.0814 0.0554 0.276 Uiso 1 1 calc R . .
H9C H 0.2891 1.0102 0.0258 0.276 Uiso 1 1 calc R . .
O2 O 0.8385(3) 0.9371(3) 0.10587(18) 0.0639(13) Uani 1 1 d D . .
P2 P 0.94190(14) 0.91819(12) 0.12544(7) 0.0625(5) Uani 1 1 d D . .
C10 C 0.9994(5) 0.9975(5) 0.1550(3) 0.083(3) Uani 1 1 d D . .
H10A H 1.0023 1.0403 0.1322 0.099 Uiso 1 1 calc R . .
H10B H 0.9533 1.0131 0.1812 0.099 Uiso 1 1 calc R . .
C11 C 1.1062(6) 0.9864(6) 0.1753(3) 0.107(3) Uani 1 1 d D . .
H11A H 1.1042 0.9457 0.1995 0.129 Uiso 1 1 calc R . .
H11B H 1.1533 0.9701 0.1496 0.129 Uiso 1 1 calc R . .
C12 C 1.1469(8) 1.0583(7) 0.1976(5) 0.178(7) Uani 1 1 d D . .
H12A H 1.1370 1.1009 0.1757 0.267 Uiso 1 1 calc R . .
H12B H 1.2204 1.0523 0.2044 0.267 Uiso 1 1 calc R . .
H12C H 1.1099 1.0683 0.2273 0.267 Uiso 1 1 calc R . .
C13 C 1.0299(5) 0.8871(4) 0.0804(3) 0.073(2) Uani 1 1 d D . .
H13A H 1.0972 0.8764 0.0953 0.088 Uiso 1 1 calc R . .
H13B H 1.0040 0.8392 0.0666 0.088 Uiso 1 1 calc R . .
C14 C 1.0450(6) 0.9429(4) 0.0417(3) 0.074(2) Uani 1 1 d D . .
H14A H 1.0821 0.9875 0.0545 0.088 Uiso 1 1 calc R . .
H14B H 0.9769 0.9604 0.0304 0.088 Uiso 1 1 calc R . .
C15 C 1.1059(8) 0.9105(6) -0.0008(3) 0.124(4) Uani 1 1 d D . .
H15A H 1.1796 0.9116 0.0065 0.186 Uiso 1 1 calc R . .
H15B H 1.0924 0.9414 -0.0290 0.186 Uiso 1 1 calc R . .
H15C H 1.0842 0.8581 -0.0067 0.186 Uiso 1 1 calc R . .
C16 C 0.9373(7) 0.8473(6) 0.1710(4) 0.118(4) Uani 1 1 d D . .
H16A H 1.0084 0.8285 0.1754 0.141 Uiso 1 1 calc R . .
H16B H 0.9178 0.8734 0.2008 0.141 Uiso 1 1 calc R . .
C17 C 0.8780(11) 0.7876(8) 0.1673(6) 0.245(11) Uani 1 1 d D . .
H17A H 0.9033 0.7579 0.1398 0.294 Uiso 1 1 calc R . .
H17B H 0.8085 0.8061 0.1588 0.294 Uiso 1 1 calc R . .
C18 C 0.8654(9) 0.7330(6) 0.2082(4) 0.146(5) Uani 1 1 d D . .
H18A H 0.9298 0.7301 0.2261 0.219 Uiso 1 1 calc R . .
H18B H 0.8479 0.6826 0.1959 0.219 Uiso 1 1 calc R . .
H18C H 0.8102 0.7509 0.2291 0.219 Uiso 1 1 calc R . .
O3 O 0.7640(3) 1.0766(2) 0.16656(12) 0.0614(12) Uani 1 1 d D . .
P3 P 0.73691(14) 1.11536(10) 0.21188(6) 0.0606(5) Uani 1 1 d D . .
C19 C 0.7786(5) 1.2116(2) 0.2124(2) 0.083(2) Uani 1 1 d D . .
H19A H 0.7341 1.2409 0.1906 0.100 Uiso 1 1 calc R . .
H19B H 0.7681 1.2322 0.2448 0.100 Uiso 1 1 calc R . .
C20 C 0.8842(5) 1.2243(4) 0.1991(3) 0.103(3) Uani 1 1 d D . .
H20A H 0.8950 1.2034 0.1669 0.124 Uiso 1 1 calc R . .
H20B H 0.9288 1.1954 0.2211 0.124 Uiso 1 1 calc R . .
C21 C 0.9186(8) 1.3064(4) 0.1993(3) 0.127(4) Uani 1 1 d D . .
H21A H 0.8991 1.3304 0.1692 0.190 Uiso 1 1 calc R . .
H21B H 0.9935 1.3088 0.2030 0.190 Uiso 1 1 calc R . .
H21C H 0.8855 1.3332 0.2257 0.190 Uiso 1 1 calc R . .
C22 C 0.7915(6) 1.0673(3) 0.26205(17) 0.080(2) Uani 1 1 d D . .
H22A H 0.8673 1.0722 0.2603 0.096 Uiso 1 1 calc R . .
H22B H 0.7687 1.0937 0.2912 0.096 Uiso 1 1 calc R . .
C23 C 0.7667(6) 0.9880(3) 0.2667(2) 0.086(3) Uani 1 1 d D . .
H23A H 0.7723 0.9639 0.2351 0.103 Uiso 1 1 calc R . .
H23B H 0.6942 0.9835 0.2771 0.103 Uiso 1 1 calc R . .
C24 C 0.8342(8) 0.9446(5) 0.3014(3) 0.121(4) Uani 1 1 d D . .
H24A H 0.9067 0.9535 0.2937 0.182 Uiso 1 1 calc R . .
H24B H 0.8192 0.8902 0.2989 0.182 Uiso 1 1 calc R . .
H24C H 0.8201 0.9619 0.3338 0.182 Uiso 1 1 calc R . .
C25 C 0.5992(3) 1.1119(4) 0.2177(3) 0.118(4) Uani 1 1 d D . .
H25A H 0.5702 1.1273 0.1866 0.141 Uiso 1 1 calc R . .
H25B H 0.5804 1.0580 0.2224 0.141 Uiso 1 1 calc R . .
C26 C 0.5466(5) 1.1541(7) 0.2529(4) 0.154(5) Uani 1 1 d D . .
H26A H 0.5655 1.2082 0.2495 0.185 Uiso 1 1 calc R . .
H26B H 0.5704 1.1370 0.2845 0.185 Uiso 1 1 calc R . .
C27 C 0.4300(5) 1.1474(6) 0.2511(3) 0.103(3) Uani 1 1 d D . .
H27A H 0.4037 1.1758 0.2237 0.155 Uiso 1 1 calc R . .
H27B H 0.4005 1.1683 0.2803 0.155 Uiso 1 1 calc R . .
H27C H 0.4105 1.0940 0.2480 0.155 Uiso 1 1 calc R . .
O4 O 0.6063(3) 1.1341(2) 0.08295(13) 0.0566(10) Uani 1 1 d D . .
P4 P 0.58816(13) 1.21013(10) 0.06135(5) 0.0525(4) Uani 1 1 d D . .
C28 C 0.6042(4) 1.2094(3) -0.00204(13) 0.0518(15) Uani 1 1 d D . .
H28A H 0.5906 1.2612 -0.0140 0.062 Uiso 1 1 calc R . .
H28B H 0.6770 1.1975 -0.0091 0.062 Uiso 1 1 calc R . .
C29 C 0.5403(5) 1.1570(4) -0.02837(17) 0.0634(19) Uani 1 1 d D . .
H29A H 0.4673 1.1685 -0.0214 0.076 Uiso 1 1 calc R . .
H29B H 0.5543 1.1049 -0.0169 0.076 Uiso 1 1 calc R . .
C30 C 0.5559(6) 1.1589(5) -0.08185(18) 0.082(2) Uani 1 1 d D . .
H30A H 0.5441 1.2105 -0.0936 0.123 Uiso 1 1 calc R . .
H30B H 0.5072 1.1240 -0.0970 0.123 Uiso 1 1 calc R . .
H30C H 0.6264 1.1433 -0.0894 0.123 Uiso 1 1 calc R . .
C31 C 0.6718(4) 1.2818(3) 0.0849(2) 0.0644(19) Uani 1 1 d D . .
H31A H 0.6564 1.2870 0.1192 0.077 Uiso 1 1 calc R . .
H31B H 0.7432 1.2629 0.0823 0.077 Uiso 1 1 calc R . .
C32 C 0.6685(6) 1.3565(3) 0.0642(3) 0.089(3) Uani 1 1 d D . .
H32A H 0.5965 1.3747 0.0648 0.106 Uiso 1 1 calc R . .
H32B H 0.6898 1.3527 0.0305 0.106 Uiso 1 1 calc R . .
C33 C 0.7361(7) 1.4155(4) 0.0886(3) 0.098(3) Uani 1 1 d D . .
H33A H 0.7014 1.4341 0.1172 0.147 Uiso 1 1 calc R . .
H33B H 0.7484 1.4580 0.0669 0.147 Uiso 1 1 calc R . .
H33C H 0.8019 1.3924 0.0974 0.147 Uiso 1 1 calc R . .
C34 C 0.4586(3) 1.2415(4) 0.07318(17) 0.0673(19) Uani 1 1 d D . .
H34A H 0.4504 1.2932 0.0599 0.081 Uiso 1 1 calc R . .
H34B H 0.4106 1.2078 0.0558 0.081 Uiso 1 1 calc R . .
C35 C 0.4281(5) 1.2432(6) 0.1224(2) 0.110(4) Uani 1 1 d D . .
H35A H 0.4714 1.2808 0.1392 0.132 Uiso 1 1 calc R . .
H35B H 0.4423 1.1929 0.1366 0.132 Uiso 1 1 calc R . .
C36 C 0.3157(6) 1.2628(7) 0.1313(3) 0.147(5) Uani 1 1 d D . .
H36A H 0.2993 1.3111 0.1159 0.220 Uiso 1 1 calc R . .
H36B H 0.3036 1.2671 0.1655 0.220 Uiso 1 1 calc R . .
H36C H 0.2718 1.2227 0.1182 0.220 Uiso 1 1 calc R . .
O5 O 0.6698(3) 0.9729(3) 0.02179(14) 0.0731(14) Uani 1 1 d D . .
P5 P 0.7005(2) 0.93671(13) -0.02350(7) 0.0873(8) Uani 1 1 d D . .
C37 C 0.8021(6) 0.9889(4) -0.0527(2) 0.135(4) Uani 1 1 d D . .
H37A H 0.7754 1.0403 -0.0598 0.162 Uiso 1 1 calc R . .
H37B H 0.8588 0.9952 -0.0296 0.162 Uiso 1 1 calc R . .
C38 C 0.8452(8) 0.9589(6) -0.0955(3) 0.151(5) Uani 1 1 d D . .
H38A H 0.7890 0.9503 -0.1186 0.181 Uiso 1 1 calc R . .
H38B H 0.8769 0.9091 -0.0884 0.181 Uiso 1 1 calc R . .
C39 C 0.9258(10) 1.0098(8) -0.1183(4) 0.206(8) Uani 1 1 d D . .
H39A H 0.8921 1.0542 -0.1324 0.308 Uiso 1 1 calc R . .
H39B H 0.9621 0.9815 -0.1432 0.308 Uiso 1 1 calc R . .
H39C H 0.9751 1.0265 -0.0942 0.308 Uiso 1 1 calc R . .
C40 C 0.6018(6) 0.9400(6) -0.0682(3) 0.192(7) Uani 1 1 d D . .
H40A H 0.5873 0.9943 -0.0738 0.231 Uiso 1 1 calc R . .
H40B H 0.6335 0.9204 -0.0977 0.231 Uiso 1 1 calc R . .
C41 C 0.5061(7) 0.9041(10) -0.0643(4) 0.251(11) Uani 1 1 d D . .
H41A H 0.4712 0.9225 -0.0352 0.301 Uiso 1 1 calc R . .
H41B H 0.5170 0.8488 -0.0607 0.301 Uiso 1 1 calc R . .
C42 C 0.4360(7) 0.9182(7) -0.1070(4) 0.156(6) Uani 1 1 d D . .
H42A H 0.4232 0.9727 -0.1102 0.235 Uiso 1 1 calc R . .
H42B H 0.3706 0.8916 -0.1022 0.235 Uiso 1 1 calc R . .
H42C H 0.4693 0.8992 -0.1358 0.235 Uiso 1 1 calc R . .
C43 C 0.7382(8) 0.8405(3) -0.0186(3) 0.200(7) Uani 1 1 d DU . .
H43A H 0.6741 0.8103 -0.0180 0.240 Uiso 1 1 calc R . .
H43B H 0.7737 0.8276 -0.0487 0.240 Uiso 1 1 calc R . .
C44 C 0.8005(14) 0.8126(6) 0.0183(4) 0.236(8) Uani 1 1 d DU . .
H44A H 0.7622 0.8169 0.0486 0.283 Uiso 1 1 calc R . .
H44B H 0.8624 0.8450 0.0209 0.283 Uiso 1 1 calc R . .
C45 C 0.8343(8) 0.7309(4) 0.0120(4) 0.131(4) Uani 1 1 d D . .
H45A H 0.7842 0.6972 0.0272 0.197 Uiso 1 1 calc R . .
H45B H 0.9019 0.7237 0.0267 0.197 Uiso 1 1 calc R . .
H45C H 0.8385 0.7191 -0.0219 0.197 Uiso 1 1 calc R . .


_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
I1 Ca1 3.2670(12) . ?
Ca1 O3 2.287(3) . ?
Ca1 O1 2.316(4) . ?
Ca1 O2 2.319(4) . ?
Ca1 O4 2.335(4) . ?
Ca1 O5 2.349(4) . ?
O1 P1 1.487(5) . ?
P1 C1 1.781(9) . ?
P1 C4 1.800(7) . ?
P1 C7 1.828(9) . ?
C1 C2 1.355(12) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.516(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.478(10) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.569(11) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.430(12) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.550(11) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
O2 P2 1.491(4) . ?
P2 C10 1.791(7) . ?
P2 C16 1.793(8) . ?
P2 C13 1.793(7) . ?
C10 C11 1.514(9) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.511(11) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.481(9) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 C15 1.544(9) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.308(12) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C18 1.511(12) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O3 P3 1.490(3) . ?
P3 C19 1.781(4) . ?
P3 C22 1.794(4) . ?
P3 C25 1.798(4) . ?
C19 C20 1.440(5) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 C21 1.516(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.441(5) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.520(5) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C26 1.415(5) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.522(5) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
O4 P4 1.490(3) . ?
P4 C31 1.794(4) . ?
P4 C28 1.797(4) . ?
P4 C34 1.804(4) . ?
C28 C29 1.447(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.520(5) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.442(5) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.525(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.442(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.522(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
O5 P5 1.481(4) . ?
P5 C43 1.771(4) . ?
P5 C40 1.798(4) . ?
P5 C37 1.807(4) . ?
C37 C38 1.432(5) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C38 C39 1.522(6) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 C41 1.401(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 C42 1.528(6) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 C44 1.407(5) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 C45 1.516(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 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
O3 Ca1 O1 87.16(16) . . ?
O3 Ca1 O2 86.20(16) . . ?
O1 Ca1 O2 94.07(17) . . ?
O3 Ca1 O4 90.52(15) . . ?
O1 Ca1 O4 90.53(16) . . ?
O2 Ca1 O4 174.21(16) . . ?
O3 Ca1 O5 174.90(17) . . ?
O1 Ca1 O5 90.26(18) . . ?
O2 Ca1 O5 89.59(17) . . ?
O4 Ca1 O5 93.91(15) . . ?
O3 Ca1 I1 88.69(11) . . ?
O1 Ca1 I1 174.46(14) . . ?
O2 Ca1 I1 89.32(12) . . ?
O4 Ca1 I1 85.83(10) . . ?
O5 Ca1 I1 94.14(13) . . ?
P1 O1 Ca1 149.1(3) . . ?
O1 P1 C1 114.3(4) . . ?
O1 P1 C4 112.5(3) . . ?
C1 P1 C4 109.3(5) . . ?
O1 P1 C7 111.8(4) . . ?
C1 P1 C7 102.8(6) . . ?
C4 P1 C7 105.3(4) . . ?
C2 C1 P1 121.8(8) . . ?
C2 C1 H1A 106.9 . . ?
P1 C1 H1A 106.9 . . ?
C2 C1 H1B 106.9 . . ?
P1 C1 H1B 106.9 . . ?
H1A C1 H1B 106.7 . . ?
C1 C2 C3 119.0(11) . . ?
C1 C2 H2A 107.6 . . ?
C3 C2 H2A 107.6 . . ?
C1 C2 H2B 107.6 . . ?
C3 C2 H2B 107.6 . . ?
H2A C2 H2B 107.0 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C4 P1 115.9(6) . . ?
C5 C4 H4A 108.3 . . ?
P1 C4 H4A 108.3 . . ?
C5 C4 H4B 108.3 . . ?
P1 C4 H4B 108.3 . . ?
H4A C4 H4B 107.4 . . ?
C4 C5 C6 110.3(8) . . ?
C4 C5 H5A 109.6 . . ?
C6 C5 H5A 109.6 . . ?
C4 C5 H5B 109.6 . . ?
C6 C5 H5B 109.6 . . ?
H5A C5 H5B 108.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 P1 114.6(7) . . ?
C8 C7 H7A 108.6 . . ?
P1 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
P1 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C7 C8 C9 111.5(11) . . ?
C7 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
C7 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P2 O2 Ca1 146.3(3) . . ?
O2 P2 C10 111.9(3) . . ?
O2 P2 C16 113.0(4) . . ?
C10 P2 C16 103.1(5) . . ?
O2 P2 C13 112.5(3) . . ?
C10 P2 C13 107.5(4) . . ?
C16 P2 C13 108.4(4) . . ?
C11 C10 P2 117.2(6) . . ?
C11 C10 H10A 108.0 . . ?
P2 C10 H10A 108.0 . . ?
C11 C10 H10B 108.0 . . ?
P2 C10 H10B 108.0 . . ?
H10A C10 H10B 107.2 . . ?
C12 C11 C10 111.7(8) . . ?
C12 C11 H11A 109.3 . . ?
C10 C11 H11A 109.3 . . ?
C12 C11 H11B 109.3 . . ?
C10 C11 H11B 109.3 . . ?
H11A C11 H11B 107.9 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 P2 113.7(5) . . ?
C14 C13 H13A 108.8 . . ?
P2 C13 H13A 108.8 . . ?
C14 C13 H13B 108.8 . . ?
P2 C13 H13B 108.8 . . ?
H13A C13 H13B 107.7 . . ?
C13 C14 C15 113.1(7) . . ?
C13 C14 H14A 109.0 . . ?
C15 C14 H14A 109.0 . . ?
C13 C14 H14B 109.0 . . ?
C15 C14 H14B 109.0 . . ?
H14A C14 H14B 107.8 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 P2 121.5(9) . . ?
C17 C16 H16A 107.0 . . ?
P2 C16 H16A 107.0 . . ?
C17 C16 H16B 107.0 . . ?
P2 C16 H16B 107.0 . . ?
H16A C16 H16B 106.7 . . ?
C16 C17 C18 121.0(12) . . ?
C16 C17 H17A 107.1 . . ?
C18 C17 H17A 107.1 . . ?
C16 C17 H17B 107.1 . . ?
C18 C17 H17B 107.1 . . ?
H17A C17 H17B 106.8 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P3 O3 Ca1 149.8(3) . . ?
O3 P3 C19 111.8(3) . . ?
O3 P3 C22 111.4(3) . . ?
C19 P3 C22 108.8(3) . . ?
O3 P3 C25 107.3(3) . . ?
C19 P3 C25 109.5(3) . . ?
C22 P3 C25 107.9(3) . . ?
C20 C19 P3 115.8(4) . . ?
C20 C19 H19A 108.3 . . ?
P3 C19 H19A 108.3 . . ?
C20 C19 H19B 108.3 . . ?
P3 C19 H19B 108.3 . . ?
H19A C19 H19B 107.4 . . ?
C19 C20 C21 115.4(6) . . ?
C19 C20 H20A 108.4 . . ?
C21 C20 H20A 108.4 . . ?
C19 C20 H20B 108.4 . . ?
C21 C20 H20B 108.4 . . ?
H20A C20 H20B 107.5 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 P3 116.2(4) . . ?
C23 C22 H22A 108.2 . . ?
P3 C22 H22A 108.2 . . ?
C23 C22 H22B 108.2 . . ?
P3 C22 H22B 108.2 . . ?
H22A C22 H22B 107.4 . . ?
C22 C23 C24 114.7(5) . . ?
C22 C23 H23A 108.6 . . ?
C24 C23 H23A 108.6 . . ?
C22 C23 H23B 108.6 . . ?
C24 C23 H23B 108.6 . . ?
H23A C23 H23B 107.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 P3 121.8(5) . . ?
C26 C25 H25A 106.9 . . ?
P3 C25 H25A 106.9 . . ?
C26 C25 H25B 106.9 . . ?
P3 C25 H25B 106.9 . . ?
H25A C25 H25B 106.7 . . ?
C25 C26 C27 114.8(6) . . ?
C25 C26 H26A 108.6 . . ?
C27 C26 H26A 108.6 . . ?
C25 C26 H26B 108.6 . . ?
C27 C26 H26B 108.6 . . ?
H26A C26 H26B 107.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
P4 O4 Ca1 148.4(2) . . ?
O4 P4 C31 112.7(2) . . ?
O4 P4 C28 112.4(2) . . ?
C31 P4 C28 107.6(2) . . ?
O4 P4 C34 110.4(3) . . ?
C31 P4 C34 106.4(3) . . ?
C28 P4 C34 107.1(2) . . ?
C29 C28 P4 116.5(3) . . ?
C29 C28 H28A 108.2 . . ?
P4 C28 H28A 108.2 . . ?
C29 C28 H28B 108.2 . . ?
P4 C28 H28B 108.2 . . ?
H28A C28 H28B 107.3 . . ?
C28 C29 C30 114.7(5) . . ?
C28 C29 H29A 108.6 . . ?
C30 C29 H29A 108.6 . . ?
C28 C29 H29B 108.6 . . ?
C30 C29 H29B 108.6 . . ?
H29A C29 H29B 107.6 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 P4 118.4(4) . . ?
C32 C31 H31A 107.7 . . ?
P4 C31 H31A 107.7 . . ?
C32 C31 H31B 107.7 . . ?
P4 C31 H31B 107.7 . . ?
H31A C31 H31B 107.1 . . ?
C31 C32 C33 115.1(5) . . ?
C31 C32 H32A 108.5 . . ?
C33 C32 H32A 108.5 . . ?
C31 C32 H32B 108.5 . . ?
C33 C32 H32B 108.5 . . ?
H32A C32 H32B 107.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 P4 116.1(4) . . ?
C35 C34 H34A 108.2 . . ?
P4 C34 H34A 108.2 . . ?
C35 C34 H34B 108.2 . . ?
P4 C34 H34B 108.2 . . ?
H34A C34 H34B 107.4 . . ?
C34 C35 C36 115.3(5) . . ?
C34 C35 H35A 108.5 . . ?
C36 C35 H35A 108.5 . . ?
C34 C35 H35B 108.5 . . ?
C36 C35 H35B 108.5 . . ?
H35A C35 H35B 107.5 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
P5 O5 Ca1 149.5(3) . . ?
O5 P5 C43 114.9(3) . . ?
O5 P5 C40 113.4(3) . . ?
C43 P5 C40 106.4(4) . . ?
O5 P5 C37 111.6(3) . . ?
C43 P5 C37 108.7(4) . . ?
C40 P5 C37 100.8(3) . . ?
C38 C37 P5 118.7(5) . . ?
C38 C37 H37A 107.6 . . ?
P5 C37 H37A 107.6 . . ?
C38 C37 H37B 107.6 . . ?
P5 C37 H37B 107.6 . . ?
H37A C37 H37B 107.1 . . ?
C37 C38 C39 114.1(6) . . ?
C37 C38 H38A 108.7 . . ?
C39 C38 H38A 108.7 . . ?
C37 C38 H38B 108.7 . . ?
C39 C38 H38B 108.7 . . ?
H38A C38 H38B 107.6 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C41 C40 P5 124.4(6) . . ?
C41 C40 H40A 106.2 . . ?
P5 C40 H40A 106.2 . . ?
C41 C40 H40B 106.2 . . ?
P5 C40 H40B 106.2 . . ?
H40A C40 H40B 106.4 . . ?
C40 C41 C42 113.3(6) . . ?
C40 C41 H41A 108.9 . . ?
C42 C41 H41A 108.9 . . ?
C40 C41 H41B 108.9 . . ?
C42 C41 H41B 108.9 . . ?
H41A C41 H41B 107.7 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C44 C43 P5 123.5(6) . . ?
C44 C43 H43A 106.5 . . ?
P5 C43 H43A 106.5 . . ?
C44 C43 H43B 106.5 . . ?
P5 C43 H43B 106.5 . . ?
H43A C43 H43B 106.5 . . ?
C43 C44 C45 114.3(6) . . ?
C43 C44 H44A 108.7 . . ?
C45 C44 H44A 108.7 . . ?
C43 C44 H44B 108.7 . . ?
C45 C44 H44B 108.7 . . ?
H44A C44 H44B 107.6 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 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
O3 Ca1 O1 P1 170.5(6) . . . . ?
O2 Ca1 O1 P1 -103.5(6) . . . . ?
O4 Ca1 O1 P1 80.0(6) . . . . ?
O5 Ca1 O1 P1 -13.9(6) . . . . ?
Ca1 O1 P1 C1 76.8(8) . . . . ?
Ca1 O1 P1 C4 -157.7(6) . . . . ?
Ca1 O1 P1 C7 -39.4(8) . . . . ?
O1 P1 C1 C2 32.4(15) . . . . ?
C4 P1 C1 C2 -94.7(12) . . . . ?
C7 P1 C1 C2 153.7(12) . . . . ?
P1 C1 C2 C3 176.2(10) . . . . ?
O1 P1 C4 C5 -63.9(7) . . . . ?
C1 P1 C4 C5 64.2(8) . . . . ?
C7 P1 C4 C5 174.0(7) . . . . ?
P1 C4 C5 C6 173.8(7) . . . . ?
O1 P1 C7 C8 -59.0(10) . . . . ?
C1 P1 C7 C8 177.9(9) . . . . ?
C4 P1 C7 C8 63.5(9) . . . . ?
P1 C7 C8 C9 173.1(7) . . . . ?
O3 Ca1 O2 P2 -36.9(5) . . . . ?
O1 Ca1 O2 P2 -123.8(5) . . . . ?
O5 Ca1 O2 P2 146.0(6) . . . . ?
I1 Ca1 O2 P2 51.8(5) . . . . ?
Ca1 O2 P2 C10 4.0(7) . . . . ?
Ca1 O2 P2 C16 119.8(6) . . . . ?
Ca1 O2 P2 C13 -117.1(6) . . . . ?
O2 P2 C10 C11 -178.3(6) . . . . ?
C16 P2 C10 C11 60.0(8) . . . . ?
C13 P2 C10 C11 -54.4(8) . . . . ?
P2 C10 C11 C12 178.0(9) . . . . ?
O2 P2 C13 C14 57.5(7) . . . . ?
C10 P2 C13 C14 -66.1(7) . . . . ?
C16 P2 C13 C14 -176.9(6) . . . . ?
P2 C13 C14 C15 -170.3(6) . . . . ?
O2 P2 C16 C17 41.8(15) . . . . ?
C10 P2 C16 C17 162.8(13) . . . . ?
C13 P2 C16 C17 -83.5(13) . . . . ?
P2 C16 C17 C18 -172.8(11) . . . . ?
O1 Ca1 O3 P3 -52.8(5) . . . . ?
O2 Ca1 O3 P3 -147.1(5) . . . . ?
O4 Ca1 O3 P3 37.7(5) . . . . ?
I1 Ca1 O3 P3 123.5(5) . . . . ?
Ca1 O3 P3 C19 -103.0(5) . . . . ?
Ca1 O3 P3 C22 135.0(5) . . . . ?
Ca1 O3 P3 C25 17.2(6) . . . . ?
O3 P3 C19 C20 -49.8(7) . . . . ?
C22 P3 C19 C20 73.6(7) . . . . ?
C25 P3 C19 C20 -168.6(6) . . . . ?
P3 C19 C20 C21 179.5(6) . . . . ?
O3 P3 C22 C23 -55.4(7) . . . . ?
C19 P3 C22 C23 -179.1(6) . . . . ?
C25 P3 C22 C23 62.1(7) . . . . ?
P3 C22 C23 C24 165.2(6) . . . . ?
O3 P3 C25 C26 -169.7(9) . . . . ?
C19 P3 C25 C26 -48.1(10) . . . . ?
C22 P3 C25 C26 70.2(9) . . . . ?
P3 C25 C26 C27 177.1(8) . . . . ?
O3 Ca1 O4 P4 99.2(5) . . . . ?
O1 Ca1 O4 P4 -173.7(5) . . . . ?
O5 Ca1 O4 P4 -83.4(5) . . . . ?
I1 Ca1 O4 P4 10.5(5) . . . . ?
Ca1 O4 P4 C31 -65.7(5) . . . . ?
Ca1 O4 P4 C28 56.1(5) . . . . ?
Ca1 O4 P4 C34 175.6(4) . . . . ?
O4 P4 C28 C29 57.5(5) . . . . ?
C31 P4 C28 C29 -177.8(5) . . . . ?
C34 P4 C28 C29 -63.8(6) . . . . ?
P4 C28 C29 C30 179.5(5) . . . . ?
O4 P4 C31 C32 174.7(6) . . . . ?
C28 P4 C31 C32 50.3(7) . . . . ?
C34 P4 C31 C32 -64.2(7) . . . . ?
P4 C31 C32 C33 175.7(6) . . . . ?
O4 P4 C34 C35 54.9(8) . . . . ?
C31 P4 C34 C35 -67.6(8) . . . . ?
C28 P4 C34 C35 177.5(7) . . . . ?
P4 C34 C35 C36 -174.6(9) . . . . ?
O1 Ca1 O5 P5 -138.9(6) . . . . ?
O2 Ca1 O5 P5 -44.8(6) . . . . ?
O4 Ca1 O5 P5 130.6(6) . . . . ?
I1 Ca1 O5 P5 44.5(6) . . . . ?
Ca1 O5 P5 C43 79.4(7) . . . . ?
Ca1 O5 P5 C40 -158.0(6) . . . . ?
Ca1 O5 P5 C37 -45.0(7) . . . . ?
O5 P5 C37 C38 176.2(8) . . . . ?
C43 P5 C37 C38 48.4(9) . . . . ?
C40 P5 C37 C38 -63.2(9) . . . . ?
P5 C37 C38 C39 176.8(10) . . . . ?
O5 P5 C40 C41 -63.6(14) . . . . ?
C43 P5 C40 C41 63.6(15) . . . . ?
C37 P5 C40 C41 177.0(13) . . . . ?
P5 C40 C41 C42 178.4(9) . . . . ?
O5 P5 C43 C44 -41.9(15) . . . . ?
C40 P5 C43 C44 -168.2(13) . . . . ?
C37 P5 C43 C44 84.0(14) . . . . ?
P5 C43 C44 C45 -172.5(10) . . . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.53
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.079


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method THF/toluene
####################################################################### 
# 
# 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_vand79
_database_code_depnum_ccdc_archive 'CCDC 1482633'
_audit_update_record             
;
2016-05-30 deposited with the CCDC.
2016-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          458-464
_chemical_formula_moiety         ?
_chemical_formula_sum            'C90 H75 Ba I2 O5 P5'
_chemical_formula_weight         1782.49

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'
P P 0.1023 0.0942 '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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)

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

_cell_length_a                   12.1294(3)
_cell_length_b                   14.6056(3)
_cell_length_c                   22.7585(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.5360(10)
_cell_angle_gamma                90.00
_cell_volume                     3935.71(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9900
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      26.38

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1784
_exptl_absorpt_coefficient_mu    1.443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.222
_exptl_absorpt_correction_T_max  0.322
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_reflns_number            29775
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.54
_diffrn_reflns_theta_max         26.41
_reflns_number_total             15029
_reflns_number_gt                14357
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0074P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.021(5)
_refine_ls_number_reflns         15029
_refine_ls_number_parameters     928
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0248
_refine_ls_R_factor_gt           0.0229
_refine_ls_wR_factor_ref         0.0451
_refine_ls_wR_factor_gt          0.0444
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_restrained_S_all      0.991
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.419676(12) 0.771439(10) 0.726924(6) 0.01282(4) Uani 1 1 d . . .
I1 I 0.618065(15) 0.791112(13) 0.634565(8) 0.02341(5) Uani 1 1 d . . .
I3 I 0.950662(17) 0.231532(14) 0.881289(9) 0.02859(5) Uani 1 1 d . . .
P1 P 0.19507(6) 0.73580(6) 0.83432(3) 0.01712(15) Uani 1 1 d . . .
P2 P 0.26365(6) 0.57983(5) 0.60459(3) 0.01501(15) Uani 1 1 d . . .
P3 P 0.55038(6) 0.96431(5) 0.84668(3) 0.01793(16) Uani 1 1 d . . .
P4 P 0.20721(6) 0.96363(5) 0.62608(3) 0.01795(16) Uani 1 1 d . . .
P5 P 0.58431(6) 0.55043(5) 0.81454(3) 0.01789(16) Uani 1 1 d . . .
O1 O 0.26700(14) 0.75584(13) 0.79031(7) 0.0200(4) Uani 1 1 d . . .
O2 O 0.33946(15) 0.63797(13) 0.64993(8) 0.0189(4) Uani 1 1 d . . .
O3 O 0.51438(16) 0.87464(14) 0.81750(8) 0.0226(5) Uani 1 1 d . . .
O4 O 0.28042(16) 0.90084(14) 0.66957(8) 0.0240(5) Uani 1 1 d . . .
O5 O 0.53453(16) 0.64140(14) 0.79457(9) 0.0250(5) Uani 1 1 d . . .
C1 C 0.1376(2) 0.62202(19) 0.82306(12) 0.0171(6) Uani 1 1 d . . .
C2 C 0.1754(2) 0.5643(2) 0.78320(12) 0.0197(6) Uani 1 1 d . . .
H2A H 0.2304 0.5852 0.7623 0.024 Uiso 1 1 calc R . .
C3 C 0.1328(2) 0.4761(2) 0.77395(12) 0.0235(7) Uani 1 1 d . . .
H3A H 0.1582 0.4368 0.7464 0.028 Uiso 1 1 calc R . .
C4 C 0.0539(2) 0.4455(2) 0.80459(12) 0.0252(7) Uani 1 1 d . . .
H4A H 0.0257 0.3848 0.7985 0.030 Uiso 1 1 calc R . .
C5 C 0.0156(2) 0.5026(2) 0.84412(13) 0.0280(8) Uani 1 1 d . . .
H5A H -0.0391 0.4812 0.8651 0.034 Uiso 1 1 calc R . .
C6 C 0.0566(2) 0.5905(2) 0.85322(13) 0.0243(7) Uani 1 1 d . . .
H6A H 0.0295 0.6299 0.8802 0.029 Uiso 1 1 calc R . .
C7 C 0.0781(2) 0.8134(2) 0.82981(12) 0.0192(6) Uani 1 1 d . . .
C8 C 0.0952(3) 0.8972(2) 0.85980(13) 0.0248(7) Uani 1 1 d . . .
H8A H 0.1675 0.9115 0.8837 0.030 Uiso 1 1 calc R . .
C9 C 0.0083(3) 0.9594(2) 0.85516(13) 0.0275(7) Uani 1 1 d . . .
H9A H 0.0210 1.0163 0.8758 0.033 Uiso 1 1 calc R . .
C10 C -0.0977(3) 0.9392(2) 0.82032(14) 0.0320(8) Uani 1 1 d . . .
H10A H -0.1578 0.9818 0.8174 0.038 Uiso 1 1 calc R . .
C11 C -0.1155(3) 0.8565(2) 0.78975(15) 0.0361(8) Uani 1 1 d . . .
H11A H -0.1876 0.8429 0.7654 0.043 Uiso 1 1 calc R . .
C12 C -0.0287(2) 0.7939(2) 0.79461(12) 0.0286(7) Uani 1 1 d . . .
H12A H -0.0418 0.7371 0.7739 0.034 Uiso 1 1 calc R . .
C13 C 0.2742(2) 0.74644(19) 0.91115(11) 0.0184(6) Uani 1 1 d . . .
C14 C 0.3906(2) 0.7594(2) 0.92234(12) 0.0233(7) Uani 1 1 d . . .
H14A H 0.4281 0.7611 0.8898 0.028 Uiso 1 1 calc R . .
C15 C 0.4516(2) 0.7697(3) 0.98063(12) 0.0310(7) Uani 1 1 d . . .
H15A H 0.5310 0.7789 0.9880 0.037 Uiso 1 1 calc R . .
C16 C 0.3983(2) 0.7667(2) 1.02813(12) 0.0298(7) Uani 1 1 d . . .
H16A H 0.4410 0.7729 1.0682 0.036 Uiso 1 1 calc R . .
C17 C 0.2822(2) 0.7546(2) 1.01764(12) 0.0269(7) Uani 1 1 d . . .
H17A H 0.2453 0.7532 1.0504 0.032 Uiso 1 1 calc R . .
C18 C 0.2209(2) 0.7448(2) 0.95987(12) 0.0228(7) Uani 1 1 d . . .
H18A H 0.1414 0.7367 0.9528 0.027 Uiso 1 1 calc R . .
C19 C 0.2462(2) 0.62454(19) 0.52958(12) 0.0163(6) Uani 1 1 d . . .
C20 C 0.1615(2) 0.5903(2) 0.48301(12) 0.0213(6) Uani 1 1 d . . .
H20A H 0.1124 0.5435 0.4911 0.026 Uiso 1 1 calc R . .
C21 C 0.1490(2) 0.6239(2) 0.42579(13) 0.0237(7) Uani 1 1 d . . .
H21A H 0.0918 0.5999 0.3942 0.028 Uiso 1 1 calc R . .
C22 C 0.2198(2) 0.6929(2) 0.41391(13) 0.0262(7) Uani 1 1 d . . .
H22A H 0.2102 0.7169 0.3743 0.031 Uiso 1 1 calc R . .
C23 C 0.3046(2) 0.7268(2) 0.45962(12) 0.0252(7) Uani 1 1 d . . .
H23A H 0.3535 0.7735 0.4512 0.030 Uiso 1 1 calc R . .
C24 C 0.3182(2) 0.6932(2) 0.51734(13) 0.0202(6) Uani 1 1 d . . .
H24A H 0.3762 0.7166 0.5486 0.024 Uiso 1 1 calc R . .
C25 C 0.3146(2) 0.46415(19) 0.60171(12) 0.0154(6) Uani 1 1 d . . .
C26 C 0.3442(2) 0.4280(2) 0.55069(13) 0.0202(6) Uani 1 1 d . . .
H26A H 0.3357 0.4642 0.5153 0.024 Uiso 1 1 calc R . .
C27 C 0.3864(2) 0.3389(2) 0.55115(13) 0.0238(7) Uani 1 1 d . . .
H27A H 0.4062 0.3146 0.5161 0.029 Uiso 1 1 calc R . .
C28 C 0.3992(2) 0.2863(2) 0.60286(12) 0.0241(6) Uani 1 1 d . . .
H28A H 0.4278 0.2257 0.6033 0.029 Uiso 1 1 calc R . .
C29 C 0.3704(2) 0.3221(2) 0.65423(13) 0.0220(7) Uani 1 1 d . . .
H29A H 0.3788 0.2857 0.6895 0.026 Uiso 1 1 calc R . .
C30 C 0.3295(2) 0.41058(19) 0.65402(12) 0.0185(6) Uani 1 1 d . . .
H30A H 0.3114 0.4351 0.6894 0.022 Uiso 1 1 calc R . .
C31 C 0.1247(2) 0.5726(2) 0.61980(12) 0.0172(6) Uani 1 1 d . . .
C32 C 0.0797(2) 0.6527(2) 0.63947(12) 0.0212(6) Uani 1 1 d . . .
H32A H 0.1218 0.7081 0.6437 0.025 Uiso 1 1 calc R . .
C33 C -0.0268(2) 0.6505(2) 0.65267(12) 0.0240(7) Uani 1 1 d . . .
H33A H -0.0578 0.7044 0.6659 0.029 Uiso 1 1 calc R . .
C34 C -0.0874(2) 0.5705(2) 0.64667(13) 0.0299(8) Uani 1 1 d . . .
H34A H -0.1594 0.5692 0.6567 0.036 Uiso 1 1 calc R . .
C35 C -0.0449(3) 0.4920(2) 0.62614(13) 0.0298(8) Uani 1 1 d . . .
H35A H -0.0882 0.4372 0.6214 0.036 Uiso 1 1 calc R . .
C36 C 0.0612(2) 0.4929(2) 0.61249(12) 0.0225(7) Uani 1 1 d . . .
H36A H 0.0903 0.4390 0.5981 0.027 Uiso 1 1 calc R . .
C37 C 0.4432(2) 1.0218(2) 0.87681(13) 0.0191(6) Uani 1 1 d . . .
C38 C 0.4522(2) 1.0351(2) 0.93777(13) 0.0276(7) Uani 1 1 d . . .
H38A H 0.5162 1.0122 0.9656 0.033 Uiso 1 1 calc R . .
C39 C 0.3691(3) 1.0813(2) 0.95857(14) 0.0318(8) Uani 1 1 d . . .
H39A H 0.3759 1.0893 1.0006 0.038 Uiso 1 1 calc R . .
C40 C 0.2765(3) 1.1158(2) 0.91876(14) 0.0272(7) Uani 1 1 d . . .
H40A H 0.2203 1.1488 0.9332 0.033 Uiso 1 1 calc R . .
C41 C 0.2656(3) 1.1025(2) 0.85825(14) 0.0274(7) Uani 1 1 d . . .
H41A H 0.2013 1.1259 0.8309 0.033 Uiso 1 1 calc R . .
C42 C 0.3471(2) 1.0552(2) 0.83640(13) 0.0263(7) Uani 1 1 d . . .
H42A H 0.3382 1.0453 0.7944 0.032 Uiso 1 1 calc R . .
C43 C 0.5865(2) 1.0432(2) 0.79304(13) 0.0193(6) Uani 1 1 d . . .
C44 C 0.6191(2) 1.0085(2) 0.74325(12) 0.0231(7) Uani 1 1 d . . .
H44A H 0.6232 0.9441 0.7383 0.028 Uiso 1 1 calc R . .
C45 C 0.6462(3) 1.0664(2) 0.70024(15) 0.0331(8) Uani 1 1 d . . .
H45A H 0.6690 1.0419 0.6661 0.040 Uiso 1 1 calc R . .
C46 C 0.6397(3) 1.1597(3) 0.70741(16) 0.0396(9) Uani 1 1 d . . .
H46A H 0.6559 1.1998 0.6775 0.048 Uiso 1 1 calc R . .
C47 C 0.6096(3) 1.1953(3) 0.75820(17) 0.0451(10) Uani 1 1 d . . .
H47A H 0.6080 1.2597 0.7637 0.054 Uiso 1 1 calc R . .
C48 C 0.5821(3) 1.1373(2) 0.80076(14) 0.0289(7) Uani 1 1 d . . .
H48A H 0.5602 1.1617 0.8352 0.035 Uiso 1 1 calc R . .
C49 C 0.7389(2) 1.0265(2) 0.93009(14) 0.0267(7) Uani 1 1 d . . .
H49A H 0.7231 1.0852 0.9123 0.032 Uiso 1 1 calc R . .
C50 C 0.8289(3) 1.0148(3) 0.97848(15) 0.0332(8) Uani 1 1 d . . .
H50A H 0.8745 1.0658 0.9943 0.040 Uiso 1 1 calc R . .
C51 C 0.8528(3) 0.9296(3) 1.00372(14) 0.0329(8) Uani 1 1 d . . .
H51A H 0.9154 0.9219 1.0366 0.040 Uiso 1 1 calc R . .
C52 C 0.7869(3) 0.8553(2) 0.98183(13) 0.0287(7) Uani 1 1 d . . .
H52A H 0.8036 0.7968 0.9999 0.034 Uiso 1 1 calc R . .
C53 C 0.6962(2) 0.8658(2) 0.93339(12) 0.0218(7) Uani 1 1 d . . .
H53A H 0.6511 0.8144 0.9179 0.026 Uiso 1 1 calc R . .
C54 C 0.6712(2) 0.9517(2) 0.90750(12) 0.0184(6) Uani 1 1 d . . .
C55 C 0.0882(2) 0.90452(19) 0.57963(12) 0.0194(6) Uani 1 1 d . . .
C56 C -0.0168(2) 0.8961(2) 0.59543(13) 0.0217(7) Uani 1 1 d . . .
H56A H -0.0290 0.9257 0.6306 0.026 Uiso 1 1 calc R . .
C57 C -0.1022(2) 0.8457(2) 0.56068(13) 0.0241(7) Uani 1 1 d . . .
H57A H -0.1732 0.8410 0.5717 0.029 Uiso 1 1 calc R . .
C58 C -0.0845(2) 0.8017(2) 0.50946(13) 0.0249(7) Uani 1 1 d . . .
H58A H -0.1437 0.7670 0.4853 0.030 Uiso 1 1 calc R . .
C59 C 0.0188(2) 0.8080(2) 0.49357(13) 0.0265(7) Uani 1 1 d . . .
H59A H 0.0310 0.7773 0.4588 0.032 Uiso 1 1 calc R . .
C60 C 0.1041(2) 0.8591(2) 0.52826(13) 0.0226(7) Uani 1 1 d . . .
H60A H 0.1749 0.8634 0.5170 0.027 Uiso 1 1 calc R . .
C61 C 0.1492(2) 1.0560(2) 0.66251(12) 0.0203(6) Uani 1 1 d . . .
C62 C 0.0916(2) 1.0360(2) 0.70849(12) 0.0246(7) Uani 1 1 d . . .
H62A H 0.0886 0.9747 0.7221 0.030 Uiso 1 1 calc R . .
C63 C 0.0394(3) 1.1054(2) 0.73389(13) 0.0284(7) Uani 1 1 d . . .
H63A H -0.0025 1.0908 0.7634 0.034 Uiso 1 1 calc R . .
C64 C 0.0476(2) 1.1953(2) 0.71689(13) 0.0281(7) Uani 1 1 d . . .
H64A H 0.0122 1.2425 0.7348 0.034 Uiso 1 1 calc R . .
C65 C 0.1080(2) 1.2161(2) 0.67348(13) 0.0293(7) Uani 1 1 d . . .
H65A H 0.1159 1.2780 0.6624 0.035 Uiso 1 1 calc R . .
C66 C 0.1570(2) 1.1472(2) 0.64624(13) 0.0228(7) Uani 1 1 d . . .
H66A H 0.1966 1.1624 0.6159 0.027 Uiso 1 1 calc R . .
C67 C 0.2288(2) 1.0642(2) 0.52379(12) 0.0204(6) Uani 1 1 d . . .
H67A H 0.1489 1.0706 0.5150 0.024 Uiso 1 1 calc R . .
C68 C 0.2915(2) 1.1041(2) 0.48655(12) 0.0219(7) Uani 1 1 d . . .
H68A H 0.2545 1.1386 0.4526 0.026 Uiso 1 1 calc R . .
C69 C 0.4076(2) 1.0939(2) 0.49852(13) 0.0231(7) Uani 1 1 d . . .
H69A H 0.4504 1.1217 0.4730 0.028 Uiso 1 1 calc R . .
C70 C 0.4614(2) 1.0431(2) 0.54790(14) 0.0264(7) Uani 1 1 d . . .
H70A H 0.5410 1.0354 0.5558 0.032 Uiso 1 1 calc R . .
C71 C 0.3993(2) 1.0036(2) 0.58577(13) 0.0220(7) Uani 1 1 d . . .
H71A H 0.4365 0.9688 0.6196 0.026 Uiso 1 1 calc R . .
C72 C 0.2828(2) 1.0147(2) 0.57424(12) 0.0186(6) Uani 1 1 d . . .
C73 C 0.7017(2) 0.5587(2) 0.87789(13) 0.0235(7) Uani 1 1 d . . .
C74 C 0.7332(3) 0.4847(3) 0.91675(13) 0.0349(8) Uani 1 1 d . . .
H74A H 0.6920 0.4290 0.9102 0.042 Uiso 1 1 calc R . .
C75 C 0.8245(3) 0.4928(3) 0.96475(15) 0.0484(11) Uani 1 1 d . . .
H75A H 0.8463 0.4422 0.9909 0.058 Uiso 1 1 calc R . .
C76 C 0.8823(3) 0.5712(4) 0.97463(17) 0.0571(14) Uani 1 1 d . . .
H76A H 0.9432 0.5760 1.0087 0.068 Uiso 1 1 calc R . .
C77 C 0.8556(3) 0.6460(3) 0.9363(2) 0.0546(13) Uani 1 1 d . . .
H77A H 0.8989 0.7006 0.9433 0.066 Uiso 1 1 calc R . .
C78 C 0.7630(3) 0.6389(2) 0.88702(15) 0.0359(9) Uani 1 1 d . . .
H78A H 0.7429 0.6890 0.8603 0.043 Uiso 1 1 calc R . .
C79 C 0.6361(2) 0.4926(2) 0.75615(12) 0.0183(6) Uani 1 1 d . . .
C80 C 0.5873(2) 0.5143(2) 0.69638(12) 0.0205(6) Uani 1 1 d . . .
H80A H 0.5294 0.5592 0.6877 0.025 Uiso 1 1 calc R . .
C81 C 0.6230(2) 0.4709(2) 0.64997(13) 0.0251(7) Uani 1 1 d . . .
H81A H 0.5898 0.4862 0.6094 0.030 Uiso 1 1 calc R . .
C82 C 0.7071(2) 0.4052(2) 0.66234(14) 0.0278(7) Uani 1 1 d . . .
H82A H 0.7307 0.3747 0.6303 0.033 Uiso 1 1 calc R . .
C83 C 0.7570(2) 0.3840(2) 0.72179(14) 0.0271(7) Uani 1 1 d . . .
H83A H 0.8156 0.3397 0.7303 0.033 Uiso 1 1 calc R . .
C84 C 0.7217(2) 0.4269(2) 0.76832(13) 0.0237(7) Uani 1 1 d . . .
H84A H 0.7557 0.4119 0.8088 0.028 Uiso 1 1 calc R . .
C85 C 0.4844(2) 0.4758(2) 0.83883(12) 0.0183(6) Uani 1 1 d . . .
C86 C 0.4346(3) 0.5063(2) 0.88540(13) 0.0254(7) Uani 1 1 d . . .
H86A H 0.4543 0.5645 0.9032 0.030 Uiso 1 1 calc R . .
C87 C 0.3571(3) 0.4522(2) 0.90543(13) 0.0300(8) Uani 1 1 d . . .
H87A H 0.3240 0.4732 0.9372 0.036 Uiso 1 1 calc R . .
C88 C 0.3274(2) 0.3678(2) 0.87958(13) 0.0284(8) Uani 1 1 d . . .
H88A H 0.2738 0.3309 0.8935 0.034 Uiso 1 1 calc R . .
C89 C 0.3758(2) 0.3367(2) 0.83328(13) 0.0282(7) Uani 1 1 d . . .
H89A H 0.3557 0.2785 0.8156 0.034 Uiso 1 1 calc R . .
C90 C 0.4536(2) 0.3912(2) 0.81308(13) 0.0234(7) Uani 1 1 d . . .
H90A H 0.4862 0.3702 0.7812 0.028 Uiso 1 1 calc R . .


_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
Ba1 O1 2.5927(16) . ?
Ba1 O3 2.6102(18) . ?
Ba1 O5 2.6433(19) . ?
Ba1 O2 2.6603(19) . ?
Ba1 O4 2.6780(19) . ?
Ba1 I1 3.5337(2) . ?
P1 O1 1.4932(17) . ?
P1 C1 1.799(3) . ?
P1 C7 1.801(3) . ?
P1 C13 1.809(3) . ?
P2 O2 1.4898(19) . ?
P2 C31 1.795(3) . ?
P2 C19 1.797(3) . ?
P2 C25 1.805(3) . ?
P3 O3 1.490(2) . ?
P3 C54 1.794(3) . ?
P3 C43 1.800(3) . ?
P3 C37 1.803(3) . ?
P4 O4 1.492(2) . ?
P4 C72 1.805(3) . ?
P4 C61 1.805(3) . ?
P4 C55 1.812(3) . ?
P5 O5 1.489(2) . ?
P5 C73 1.797(3) . ?
P5 C79 1.799(3) . ?
P5 C85 1.803(3) . ?
C1 C2 1.387(4) . ?
C1 C6 1.393(4) . ?
C2 C3 1.387(4) . ?
C3 C4 1.376(4) . ?
C4 C5 1.379(4) . ?
C5 C6 1.376(4) . ?
C7 C8 1.395(4) . ?
C7 C12 1.397(4) . ?
C8 C9 1.378(4) . ?
C9 C10 1.388(4) . ?
C10 C11 1.387(5) . ?
C11 C12 1.380(4) . ?
C13 C14 1.393(4) . ?
C13 C18 1.399(3) . ?
C14 C15 1.380(4) . ?
C15 C16 1.376(4) . ?
C16 C17 1.387(4) . ?
C17 C18 1.370(4) . ?
C19 C24 1.396(4) . ?
C19 C20 1.399(4) . ?
C20 C21 1.369(4) . ?
C21 C22 1.389(4) . ?
C22 C23 1.386(4) . ?
C23 C24 1.379(4) . ?
C25 C26 1.391(4) . ?
C25 C30 1.403(4) . ?
C26 C27 1.397(4) . ?
C27 C28 1.386(4) . ?
C28 C29 1.393(4) . ?
C29 C30 1.384(4) . ?
C31 C36 1.386(4) . ?
C31 C32 1.405(4) . ?
C32 C33 1.389(4) . ?
C33 C34 1.370(4) . ?
C34 C35 1.381(5) . ?
C35 C36 1.388(4) . ?
C37 C38 1.381(4) . ?
C37 C42 1.406(4) . ?
C38 C39 1.380(4) . ?
C39 C40 1.377(4) . ?
C40 C41 1.369(4) . ?
C41 C42 1.384(4) . ?
C43 C44 1.376(4) . ?
C43 C48 1.388(4) . ?
C44 C45 1.386(4) . ?
C45 C46 1.378(5) . ?
C46 C47 1.387(5) . ?
C47 C48 1.381(4) . ?
C49 C50 1.383(4) . ?
C49 C54 1.394(4) . ?
C50 C51 1.375(5) . ?
C51 C52 1.375(5) . ?
C52 C53 1.387(4) . ?
C53 C54 1.392(4) . ?
C55 C60 1.394(4) . ?
C55 C56 1.401(4) . ?
C56 C57 1.373(4) . ?
C57 C58 1.388(4) . ?
C58 C59 1.381(4) . ?
C59 C60 1.377(4) . ?
C61 C66 1.391(4) . ?
C61 C62 1.409(4) . ?
C62 C63 1.387(4) . ?
C63 C64 1.378(4) . ?
C64 C65 1.386(4) . ?
C65 C66 1.381(4) . ?
C67 C68 1.384(4) . ?
C67 C72 1.394(4) . ?
C68 C69 1.383(4) . ?
C69 C70 1.386(4) . ?
C70 C71 1.388(4) . ?
C71 C72 1.390(4) . ?
C73 C78 1.378(4) . ?
C73 C74 1.396(4) . ?
C74 C75 1.381(4) . ?
C75 C76 1.336(6) . ?
C76 C77 1.391(6) . ?
C77 C78 1.409(5) . ?
C79 C80 1.397(4) . ?
C79 C84 1.397(4) . ?
C80 C81 1.379(4) . ?
C81 C82 1.384(4) . ?
C82 C83 1.392(4) . ?
C83 C84 1.376(4) . ?
C85 C90 1.384(4) . ?
C85 C86 1.402(4) . ?
C86 C87 1.380(4) . ?
C87 C88 1.380(5) . ?
C88 C89 1.389(4) . ?
C89 C90 1.388(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ba1 O3 81.74(6) . . ?
O1 Ba1 O5 87.86(6) . . ?
O3 Ba1 O5 82.47(6) . . ?
O1 Ba1 O2 95.67(6) . . ?
O3 Ba1 O2 168.16(6) . . ?
O5 Ba1 O2 85.89(6) . . ?
O1 Ba1 O4 83.23(6) . . ?
O3 Ba1 O4 95.76(6) . . ?
O5 Ba1 O4 171.08(6) . . ?
O2 Ba1 O4 95.41(6) . . ?
O1 Ba1 I1 177.39(4) . . ?
O3 Ba1 I1 100.55(4) . . ?
O5 Ba1 I1 93.67(4) . . ?
O2 Ba1 I1 82.34(4) . . ?
O4 Ba1 I1 95.25(4) . . ?
O1 P1 C1 110.51(12) . . ?
O1 P1 C7 113.96(12) . . ?
C1 P1 C7 107.26(13) . . ?
O1 P1 C13 111.53(11) . . ?
C1 P1 C13 108.96(13) . . ?
C7 P1 C13 104.30(13) . . ?
O2 P2 C31 111.33(12) . . ?
O2 P2 C19 112.24(12) . . ?
C31 P2 C19 106.43(12) . . ?
O2 P2 C25 113.19(12) . . ?
C31 P2 C25 107.19(13) . . ?
C19 P2 C25 106.04(13) . . ?
O3 P3 C54 111.42(13) . . ?
O3 P3 C43 110.55(12) . . ?
C54 P3 C43 108.07(13) . . ?
O3 P3 C37 114.40(13) . . ?
C54 P3 C37 106.86(13) . . ?
C43 P3 C37 105.15(14) . . ?
O4 P4 C72 111.96(12) . . ?
O4 P4 C61 112.96(12) . . ?
C72 P4 C61 107.16(14) . . ?
O4 P4 C55 112.22(12) . . ?
C72 P4 C55 105.60(13) . . ?
C61 P4 C55 106.46(13) . . ?
O5 P5 C73 112.51(14) . . ?
O5 P5 C79 112.15(13) . . ?
C73 P5 C79 106.34(13) . . ?
O5 P5 C85 112.19(12) . . ?
C73 P5 C85 105.25(13) . . ?
C79 P5 C85 107.95(14) . . ?
P1 O1 Ba1 169.22(11) . . ?
P2 O2 Ba1 163.02(11) . . ?
P3 O3 Ba1 153.58(12) . . ?
P4 O4 Ba1 168.07(12) . . ?
P5 O5 Ba1 161.16(13) . . ?
C2 C1 C6 119.4(3) . . ?
C2 C1 P1 118.8(2) . . ?
C6 C1 P1 121.9(2) . . ?
C1 C2 C3 119.9(3) . . ?
C4 C3 C2 120.1(3) . . ?
C3 C4 C5 120.3(3) . . ?
C6 C5 C4 120.0(3) . . ?
C5 C6 C1 120.3(3) . . ?
C8 C7 C12 118.7(3) . . ?
C8 C7 P1 119.5(2) . . ?
C12 C7 P1 121.7(2) . . ?
C9 C8 C7 120.8(3) . . ?
C8 C9 C10 120.0(3) . . ?
C11 C10 C9 119.8(3) . . ?
C12 C11 C10 120.2(3) . . ?
C11 C12 C7 120.5(3) . . ?
C14 C13 C18 118.8(2) . . ?
C14 C13 P1 119.49(19) . . ?
C18 C13 P1 121.7(2) . . ?
C15 C14 C13 120.1(2) . . ?
C16 C15 C14 120.4(3) . . ?
C15 C16 C17 120.1(3) . . ?
C18 C17 C16 119.8(3) . . ?
C17 C18 C13 120.7(3) . . ?
C24 C19 C20 119.6(3) . . ?
C24 C19 P2 120.1(2) . . ?
C20 C19 P2 120.3(2) . . ?
C21 C20 C19 120.3(3) . . ?
C20 C21 C22 120.0(3) . . ?
C23 C22 C21 120.2(3) . . ?
C24 C23 C22 120.2(3) . . ?
C23 C24 C19 119.7(3) . . ?
C26 C25 C30 119.2(3) . . ?
C26 C25 P2 122.5(2) . . ?
C30 C25 P2 118.2(2) . . ?
C25 C26 C27 120.5(3) . . ?
C28 C27 C26 119.8(3) . . ?
C27 C28 C29 120.1(3) . . ?
C30 C29 C28 120.2(3) . . ?
C29 C30 C25 120.2(3) . . ?
C36 C31 C32 119.5(3) . . ?
C36 C31 P2 123.1(2) . . ?
C32 C31 P2 117.3(2) . . ?
C33 C32 C31 119.6(3) . . ?
C34 C33 C32 120.2(3) . . ?
C33 C34 C35 120.7(3) . . ?
C34 C35 C36 120.0(3) . . ?
C31 C36 C35 120.0(3) . . ?
C38 C37 C42 118.8(3) . . ?
C38 C37 P3 122.7(2) . . ?
C42 C37 P3 118.5(2) . . ?
C39 C38 C37 120.6(3) . . ?
C40 C39 C38 120.4(3) . . ?
C41 C40 C39 119.7(3) . . ?
C40 C41 C42 120.8(3) . . ?
C41 C42 C37 119.6(3) . . ?
C44 C43 C48 119.7(3) . . ?
C44 C43 P3 118.6(2) . . ?
C48 C43 P3 121.7(2) . . ?
C43 C44 C45 120.8(3) . . ?
C46 C45 C44 119.5(3) . . ?
C45 C46 C47 120.1(3) . . ?
C48 C47 C46 120.2(3) . . ?
C47 C48 C43 119.8(3) . . ?
C50 C49 C54 119.8(3) . . ?
C51 C50 C49 120.2(3) . . ?
C52 C51 C50 120.7(3) . . ?
C51 C52 C53 119.9(3) . . ?
C52 C53 C54 119.9(3) . . ?
C53 C54 C49 119.6(3) . . ?
C53 C54 P3 119.0(2) . . ?
C49 C54 P3 121.4(2) . . ?
C60 C55 C56 118.2(3) . . ?
C60 C55 P4 118.5(2) . . ?
C56 C55 P4 123.0(2) . . ?
C57 C56 C55 120.9(3) . . ?
C56 C57 C58 119.8(3) . . ?
C59 C58 C57 120.2(3) . . ?
C60 C59 C58 119.9(3) . . ?
C59 C60 C55 121.0(3) . . ?
C66 C61 C62 118.0(3) . . ?
C66 C61 P4 122.5(2) . . ?
C62 C61 P4 119.4(2) . . ?
C63 C62 C61 120.1(3) . . ?
C64 C63 C62 120.8(3) . . ?
C63 C64 C65 119.4(3) . . ?
C66 C65 C64 120.4(3) . . ?
C65 C66 C61 121.1(3) . . ?
C68 C67 C72 120.0(3) . . ?
C67 C68 C69 120.4(3) . . ?
C68 C69 C70 119.8(3) . . ?
C69 C70 C71 120.2(3) . . ?
C70 C71 C72 120.0(3) . . ?
C71 C72 C67 119.5(3) . . ?
C71 C72 P4 117.9(2) . . ?
C67 C72 P4 122.6(2) . . ?
C78 C73 C74 119.8(3) . . ?
C78 C73 P5 119.1(3) . . ?
C74 C73 P5 121.1(2) . . ?
C75 C74 C73 119.8(4) . . ?
C76 C75 C74 120.5(4) . . ?
C75 C76 C77 121.7(4) . . ?
C76 C77 C78 118.6(4) . . ?
C73 C78 C77 119.5(4) . . ?
C80 C79 C84 119.2(3) . . ?
C80 C79 P5 118.1(2) . . ?
C84 C79 P5 122.7(2) . . ?
C81 C80 C79 120.3(3) . . ?
C80 C81 C82 120.2(3) . . ?
C81 C82 C83 119.9(3) . . ?
C84 C83 C82 120.3(3) . . ?
C83 C84 C79 120.1(3) . . ?
C90 C85 C86 118.9(3) . . ?
C90 C85 P5 123.2(2) . . ?
C86 C85 P5 117.9(2) . . ?
C87 C86 C85 120.3(3) . . ?
C88 C87 C86 120.3(3) . . ?
C87 C88 C89 120.1(3) . . ?
C90 C89 C88 119.6(3) . . ?
C85 C90 C89 120.8(3) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.058
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method THF/toluene
