# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5b

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         "'C19 H14 Cl N O3"
_chemical_formula_sum            'C19 H14 Cl N O3'
_chemical_formula_weight         339.76
_chemical_absolute_configuration ad

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   P212121
_symmetry_space_group_name_Hall  'P 2ac 2ab'

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

_cell_length_a                   5.70670(10)
_cell_length_b                   13.4355(2)
_cell_length_c                   20.8250(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1596.70(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    228(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             704
_exptl_absorpt_coefficient_mu    2.265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4644
_exptl_absorpt_correction_T_max  0.8396
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      228(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'BRUKER SMART APEXII CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19107
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.92
_diffrn_reflns_theta_max         68.38
_reflns_number_total             2884
_reflns_number_gt                2787
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_cell_refinement       'APEX2 (Bruker, 2010); SAINT (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009);XPREP(Sheldrick,2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008), OLEX2 (2009)'
_computing_molecular_graphics    ?
_computing_publication_material  'OLEX2 (Dolomanov,2009)'
_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)+(0.0400P)²+0.2759P] 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     SHELXL
_refine_ls_extinction_coef       0.0020(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(13)
_refine_ls_number_reflns         2884
_refine_ls_number_parameters     218
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0281
_refine_ls_wR_factor_ref         0.0736
_refine_ls_wR_factor_gt          0.0726
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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
Cl1 Cl -0.20611(9) 0.60229(4) 0.24232(2) 0.05101(15) Uani 1 1 d . . .
O1 O 0.3717(3) 0.81651(9) 0.40282(7) 0.0489(3) Uani 1 1 d . . .
O2 O -0.0366(2) 0.56643(9) 0.39466(5) 0.0360(3) Uani 1 1 d . . .
C1 C 0.3687(3) 0.51168(12) 0.39685(8) 0.0346(4) Uani 1 1 d . . .
O3 O 0.4362(2) 0.53246(10) 0.45035(6) 0.0454(3) Uani 1 1 d . . .
C2 C 0.0516(4) 0.72461(13) 0.44156(9) 0.0402(4) Uani 1 1 d . . .
H2 H 0.0128 0.7714 0.4734 0.048 Uiso 1 1 calc R . .
C3 C 0.2436(3) 0.74471(11) 0.39863(8) 0.0335(4) Uani 1 1 d . . .
C4 C 0.2633(3) 0.67336(11) 0.34267(8) 0.0335(4) Uani 1 1 d . . .
H4A H 0.4274 0.6701 0.3290 0.040 Uiso 1 1 calc R . .
H4B H 0.1714 0.6995 0.3067 0.040 Uiso 1 1 calc R . .
C5 C 0.1783(3) 0.56787(11) 0.35817(7) 0.0304(3) Uani 1 1 d . . .
N5 N 0.4473(3) 0.43521(10) 0.35936(7) 0.0378(3) Uani 1 1 d . . .
C6 C 0.6273(3) 0.36433(13) 0.37868(10) 0.0431(4) Uani 1 1 d . . .
H6A H 0.7124 0.3914 0.4156 0.052 Uiso 1 1 calc R . .
H6B H 0.7394 0.3565 0.3434 0.052 Uiso 1 1 calc R . .
C7 C 0.5313(3) 0.26316(12) 0.39633(8) 0.0357(4) Uani 1 1 d . . .
C8 C 0.6627(4) 0.17903(14) 0.38435(10) 0.0502(5) Uani 1 1 d . . .
H8 H 0.8058 0.1846 0.3623 0.060 Uiso 1 1 calc R . .
C9 C 0.5860(5) 0.08652(15) 0.40450(12) 0.0639(6) Uani 1 1 d . . .
H9 H 0.6789 0.0300 0.3968 0.077 Uiso 1 1 calc R . .
C10 C 0.3759(5) 0.07663(14) 0.43552(10) 0.0564(6) Uani 1 1 d . . .
H10 H 0.3238 0.0136 0.4489 0.068 Uiso 1 1 calc R . .
C11 C -0.0721(3) 0.64084(13) 0.43689(8) 0.0387(4) Uani 1 1 d . . .
H11 H -0.1966 0.6329 0.4660 0.046 Uiso 1 1 calc R . .
C12 C 0.2423(4) 0.15932(14) 0.44689(9) 0.0488(5) Uani 1 1 d . . .
H12 H 0.0973 0.1529 0.4679 0.059 Uiso 1 1 calc R . .
C13 C 0.3193(4) 0.25238(13) 0.42769(9) 0.0421(4) Uani 1 1 d . . .
H13 H 0.2266 0.3087 0.4360 0.051 Uiso 1 1 calc R . .
C14 C 0.3193(3) 0.42851(11) 0.30209(8) 0.0340(3) Uani 1 1 d . . .
C15 C 0.1505(3) 0.50364(11) 0.29974(7) 0.0310(3) Uani 1 1 d . . .
C16 C 0.0037(3) 0.50866(12) 0.24777(8) 0.0353(4) Uani 1 1 d . . .
C17 C 0.0213(4) 0.44021(14) 0.19810(8) 0.0431(4) Uani 1 1 d . . .
H17 H -0.0823 0.4428 0.1630 0.052 Uiso 1 1 calc R . .
C18 C 0.1943(4) 0.36795(13) 0.20110(9) 0.0461(4) Uani 1 1 d . . .
H18 H 0.2095 0.3226 0.1670 0.055 Uiso 1 1 calc R . .
C19 C 0.3452(3) 0.36064(12) 0.25288(9) 0.0426(4) Uani 1 1 d . . .
H19 H 0.4615 0.3111 0.2545 0.051 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
Cl1 C16 1.7402(17) . ?
O1 C3 1.213(2) . ?
O2 C11 1.347(2) . ?
O2 C5 1.4424(19) . ?
C1 O3 1.212(2) . ?
C1 N5 1.366(2) . ?
C1 C5 1.549(2) . ?
C2 C11 1.332(3) . ?
C2 C3 1.440(3) . ?
C2 H2 0.9400 . ?
C3 C4 1.513(2) . ?
C4 C5 1.532(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C5 C15 1.500(2) . ?
N5 C14 1.402(2) . ?
N5 C6 1.457(2) . ?
C6 C7 1.511(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C7 C8 1.379(3) . ?
C7 C13 1.382(3) . ?
C8 C9 1.383(3) . ?
C8 H8 0.9400 . ?
C9 C10 1.368(4) . ?
C9 H9 0.9400 . ?
C10 C12 1.368(3) . ?
C10 H10 0.9400 . ?
C11 H11 0.9400 . ?
C12 C13 1.384(3) . ?
C12 H12 0.9400 . ?
C13 H13 0.9400 . ?
C14 C19 1.380(2) . ?
C14 C15 1.396(2) . ?
C15 C16 1.371(2) . ?
C16 C17 1.388(2) . ?
C17 C18 1.386(3) . ?
C17 H17 0.9400 . ?
C18 C19 1.384(3) . ?
C18 H18 0.9400 . ?
C19 H19 0.9400 . ?

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
C11 O2 C5 117.51(12) . . ?
O3 C1 N5 126.46(17) . . ?
O3 C1 C5 126.09(16) . . ?
N5 C1 C5 107.45(14) . . ?
C11 C2 C3 121.09(15) . . ?
C11 C2 H2 119.5 . . ?
C3 C2 H2 119.5 . . ?
O1 C3 C2 124.25(16) . . ?
O1 C3 C4 120.97(15) . . ?
C2 C3 C4 114.56(14) . . ?
C3 C4 C5 113.59(12) . . ?
C3 C4 H4A 108.8 . . ?
C5 C4 H4A 108.8 . . ?
C3 C4 H4B 108.8 . . ?
C5 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
O2 C5 C15 109.27(13) . . ?
O2 C5 C4 113.10(13) . . ?
C15 C5 C4 113.24(12) . . ?
O2 C5 C1 108.40(12) . . ?
C15 C5 C1 102.44(13) . . ?
C4 C5 C1 109.77(13) . . ?
C1 N5 C14 111.30(15) . . ?
C1 N5 C6 124.42(15) . . ?
C14 N5 C6 124.08(15) . . ?
N5 C6 C7 113.56(15) . . ?
N5 C6 H6A 108.9 . . ?
C7 C6 H6A 108.9 . . ?
N5 C6 H6B 108.9 . . ?
C7 C6 H6B 108.9 . . ?
H6A C6 H6B 107.7 . . ?
C8 C7 C13 118.38(17) . . ?
C8 C7 C6 119.75(17) . . ?
C13 C7 C6 121.77(16) . . ?
C7 C8 C9 120.6(2) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 H8 119.7 . . ?
C10 C9 C8 120.5(2) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C12 C10 C9 119.42(19) . . ?
C12 C10 H10 120.3 . . ?
C9 C10 H10 120.3 . . ?
C2 C11 O2 126.52(16) . . ?
C2 C11 H11 116.7 . . ?
O2 C11 H11 116.7 . . ?
C10 C12 C13 120.4(2) . . ?
C10 C12 H12 119.8 . . ?
C13 C12 H12 119.8 . . ?
C7 C13 C12 120.60(18) . . ?
C7 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C19 C14 C15 121.74(16) . . ?
C19 C14 N5 128.20(16) . . ?
C15 C14 N5 110.06(14) . . ?
C16 C15 C14 119.02(14) . . ?
C16 C15 C5 132.59(15) . . ?
C14 C15 C5 108.35(14) . . ?
C15 C16 C17 120.78(16) . . ?
C15 C16 Cl1 120.51(13) . . ?
C17 C16 Cl1 118.71(14) . . ?
C18 C17 C16 118.83(17) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C19 C18 C17 121.88(16) . . ?
C19 C18 H18 119.1 . . ?
C17 C18 H18 119.1 . . ?
C14 C19 C18 117.71(17) . . ?
C14 C19 H19 121.1 . . ?
C18 C19 H19 121.1 . . ?

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
C11 C2 C3 O1 -175.33(19) . . . . ?
C11 C2 C3 C4 10.0(3) . . . . ?
O1 C3 C4 C5 153.77(17) . . . . ?
C2 C3 C4 C5 -31.4(2) . . . . ?
C11 O2 C5 C15 -160.33(14) . . . . ?
C11 O2 C5 C4 -33.20(19) . . . . ?
C11 O2 C5 C1 88.77(17) . . . . ?
C3 C4 C5 O2 42.9(2) . . . . ?
C3 C4 C5 C15 167.93(14) . . . . ?
C3 C4 C5 C1 -78.28(17) . . . . ?
O3 C1 C5 O2 -58.8(2) . . . . ?
N5 C1 C5 O2 121.69(13) . . . . ?
O3 C1 C5 C15 -174.26(16) . . . . ?
N5 C1 C5 C15 6.26(16) . . . . ?
O3 C1 C5 C4 65.2(2) . . . . ?
N5 C1 C5 C4 -114.32(14) . . . . ?
O3 C1 N5 C14 175.79(16) . . . . ?
C5 C1 N5 C14 -4.73(17) . . . . ?
O3 C1 N5 C6 0.8(3) . . . . ?
C5 C1 N5 C6 -179.76(14) . . . . ?
C1 N5 C6 C7 104.74(19) . . . . ?
C14 N5 C6 C7 -69.7(2) . . . . ?
N5 C6 C7 C8 147.41(18) . . . . ?
N5 C6 C7 C13 -36.3(2) . . . . ?
C13 C7 C8 C9 -1.3(3) . . . . ?
C6 C7 C8 C9 175.1(2) . . . . ?
C7 C8 C9 C10 1.4(4) . . . . ?
C8 C9 C10 C12 -0.4(3) . . . . ?
C3 C2 C11 O2 0.9(3) . . . . ?
C5 O2 C11 C2 11.7(3) . . . . ?
C9 C10 C12 C13 -0.5(3) . . . . ?
C8 C7 C13 C12 0.4(3) . . . . ?
C6 C7 C13 C12 -175.93(18) . . . . ?
C10 C12 C13 C7 0.5(3) . . . . ?
C1 N5 C14 C19 -179.22(16) . . . . ?
C6 N5 C14 C19 -4.2(3) . . . . ?
C1 N5 C14 C15 1.05(19) . . . . ?
C6 N5 C14 C15 176.10(14) . . . . ?
C19 C14 C15 C16 1.4(2) . . . . ?
N5 C14 C15 C16 -178.82(14) . . . . ?
C19 C14 C15 C5 -176.51(15) . . . . ?
N5 C14 C15 C5 3.25(18) . . . . ?
O2 C5 C15 C16 62.0(2) . . . . ?
C4 C5 C15 C16 -65.1(2) . . . . ?
C1 C5 C15 C16 176.80(17) . . . . ?
O2 C5 C15 C14 -120.46(14) . . . . ?
C4 C5 C15 C14 112.49(16) . . . . ?
C1 C5 C15 C14 -5.65(16) . . . . ?
C14 C15 C16 C17 0.1(2) . . . . ?
C5 C15 C16 C17 177.44(17) . . . . ?
C14 C15 C16 Cl1 -179.00(12) . . . . ?
C5 C15 C16 Cl1 -1.7(2) . . . . ?
C15 C16 C17 C18 -1.6(3) . . . . ?
Cl1 C16 C17 C18 177.47(14) . . . . ?
C16 C17 C18 C19 1.8(3) . . . . ?
C15 C14 C19 C18 -1.3(3) . . . . ?
N5 C14 C19 C18 178.97(17) . . . . ?
C17 C18 C19 C14 -0.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        68.38
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.159
_refine_diff_density_rms         0.032
_database_code_depnum_ccdc_archive 'CCDC 1009077'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ca[P4]2

_audit_creation_method           SHELXL-2012
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H64 Ca O12 P2, C H4 O, C H4 O, H2 O'
_chemical_formula_sum            'C86 H74 Ca O15 P2'
_chemical_formula_weight         1449.47

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.3641 1.2855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

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

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

_cell_length_a                   8.2594(3)
_cell_length_b                   13.6877(5)
_cell_length_c                   32.5308(11)
_cell_angle_alpha                90
_cell_angle_beta                 90.290(2)
_cell_angle_gamma                90
_cell_volume                     3677.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             1520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    1.708
_shelx_estimated_absorpt_T_min   0.848
_shelx_estimated_absorpt_T_max   0.967
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6376
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2003)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'INCOATEC Imus micro-focus source'
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_reflns_number            52231
_diffrn_reflns_av_unetI/netI     0.0981
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         3.503
_diffrn_reflns_theta_max         66.500
_diffrn_reflns_theta_full        66.650
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measured_fraction_theta_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_point_group_measured_fraction_full 0.965
_reflns_number_total             52231
_reflns_number_gt                45390
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.885
_reflns_Friedel_fraction_max     0.952
_reflns_Friedel_fraction_full    0.949

_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. These statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'APEX2(Bruker, 2012'
_computing_cell_refinement       'APEX2(Bruker,2012);SAINT 8.18C(Bruker,2012)'
_computing_data_reduction        'SAINT (Bruker,2012);XPREP(Sheldrick,2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  SHELXL-2012Beta(Sheldrick,2012),OLEX2(2009)
_computing_molecular_graphics    ?
_computing_publication_material  'OLEX2 (Dolomanov,2009)'

_refine_special_details          
;
Refined as a 2-component pseudo-merohedral twin. Basf = 0.153(2)
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0167P)²+13.8003P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 4726 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.036(6)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         52231
_refine_ls_number_parameters     962
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0756
_refine_ls_wR_factor_ref         0.1736
_refine_ls_wR_factor_gt          0.1641
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.058
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.5996(2) 0.65921(17) 0.24942(6) 0.0233(5) Uani 1 1 d . . . . .
P2 P 0.8579(3) 0.6610(2) 0.33962(7) 0.0165(5) Uani 1 1 d . . . . .
P1 P 0.3451(3) 0.60040(19) 0.16485(8) 0.0177(6) Uani 1 1 d . . . . .
O1 O 0.4117(8) 0.5114(5) 0.1372(2) 0.0164(15) Uani 1 1 d . . . . .
O6 O 0.7661(8) 0.5934(5) 0.37253(19) 0.0169(15) Uani 1 1 d . . . . .
O2 O 0.2638(7) 0.6711(5) 0.13051(18) 0.0148(15) Uani 1 1 d . . . . .
O7 O 0.9136(8) 0.7522(5) 0.3675(2) 0.0150(15) Uani 1 1 d . . . . .
O4 O 0.4892(9) 0.6456(5) 0.1843(2) 0.0255(17) Uani 1 1 d . . . . .
O5 O 0.7353(9) 0.6903(5) 0.3091(2) 0.0223(17) Uani 1 1 d . . . . .
O8 O 1.0100(8) 0.6147(5) 0.3261(2) 0.0240(17) Uani 1 1 d D . . . .
O3 O 0.2089(9) 0.5686(5) 0.1908(2) 0.0262(18) Uani 1 1 d . . . . .
O15 O 1.1040(8) 0.6869(6) 0.2531(2) 0.038(2) Uani 1 1 d D . . . .
O10 O 0.7399(9) 0.5143(6) 0.2373(2) 0.0334(19) Uani 1 1 d D . . . .
O9 O 0.4369(10) 0.5559(6) 0.2894(2) 0.033(2) Uani 1 1 d D . . . .
O13 O 0.9099(10) 0.4985(7) 0.1685(3) 0.047(2) Uani 1 1 d . . . . .
H13 H 1.0113 0.5024 0.1678 0.071 Uiso 1 1 calc R U . . .
O12 O 0.8174(10) 0.7441(6) 0.2196(2) 0.036(2) Uani 1 1 d D . . . .
C9 C 0.1326(13) 0.4765(8) 0.0506(3) 0.020(2) Uani 1 1 d . . . . .
C49 C 0.9168(13) 0.6402(8) 0.4779(3) 0.023(3) Uani 1 1 d . . . . .
C41 C 0.8394(11) 0.5794(7) 0.4108(3) 0.012(2) Uani 1 1 d . . . . .
C40 C 0.4397(13) 0.2946(8) 0.1712(4) 0.024(3) Uani 1 1 d . . . . .
O11 O 0.3895(11) 0.7764(7) 0.2607(3) 0.051(3) Uani 1 1 d D . . . .
C45 C 1.0858(15) 0.5351(8) 0.5225(3) 0.026(3) Uani 1 1 d . . . . .
H45 H 1.1445 0.4763 0.5268 0.031 Uiso 1 1 calc R U . . .
C42 C 0.9214(13) 0.4888(7) 0.4173(3) 0.017(2) Uani 1 1 d . . . . .
C46 C 1.0845(15) 0.6049(9) 0.5525(4) 0.031(3) Uani 1 1 d . . . . .
H46 H 1.1377 0.5935 0.5780 0.037 Uiso 1 1 calc R U . . .
C15 C 0.4995(13) 0.7184(8) 0.0186(3) 0.021(2) Uani 1 1 d . . . . .
C12 C 0.3405(12) 0.6856(7) 0.0934(3) 0.015(2) Uani 1 1 d . . . . .
C52 C 0.7967(12) 0.7950(8) 0.3929(3) 0.017(2) Uani 1 1 d . . . . .
C53 C 0.7325(13) 0.8844(8) 0.3800(3) 0.021(2) Uani 1 1 d . . . . .
C2 C 0.2399(13) 0.3750(8) 0.1224(3) 0.019(2) Uani 1 1 d . . . . .
C35 C 0.4776(14) 0.2507(9) 0.2099(3) 0.025(3) Uani 1 1 d . . . . .
C11 C 0.3402(12) 0.6092(8) 0.0649(3) 0.019(2) Uani 1 1 d . . . . .
C38 C 0.7188(14) 0.2675(8) 0.1522(3) 0.024(3) Uani 1 1 d . . . . .
H38 H 0.8036 0.2725 0.1326 0.029 Uiso 1 1 calc R U . . .
C48 C 0.9238(14) 0.7113(8) 0.5089(3) 0.028(3) Uani 1 1 d . . . . .
H48 H 0.8723 0.7726 0.5046 0.033 Uiso 1 1 calc R U . . .
C55 C 0.5565(14) 0.8779(9) 0.4399(3) 0.026(3) Uani 1 1 d . . . . .
C51 C 0.7531(12) 0.7479(8) 0.4280(3) 0.018(2) Uani 1 1 d . . . . .
C50 C 0.8335(11) 0.6530(8) 0.4391(3) 0.018(2) Uani 1 1 d . . . . .
C4 C 0.0680(14) 0.3818(9) 0.0618(3) 0.024(3) Uani 1 1 d . . . . .
C17 C 0.5857(15) 0.6632(10) -0.0477(3) 0.035(3) Uani 1 1 d . . . . .
H17 H 0.6369 0.6764 -0.0732 0.042 Uiso 1 1 calc R U . . .
C5 C -0.0690(16) 0.3478(11) 0.0385(4) 0.043(4) Uani 1 1 d . . . . .
H5 H -0.1147 0.2862 0.0453 0.051 Uiso 1 1 calc R U . . .
C65 C 0.9715(14) 0.9974(8) 0.2910(3) 0.026(3) Uani 1 1 d . . . . .
C14 C 0.4867(12) 0.7917(7) 0.0486(3) 0.017(2) Uani 1 1 d . . . . .
H14 H 0.5357 0.8533 0.0436 0.020 Uiso 1 1 calc R U . . .
C43 C 1.0017(13) 0.4774(8) 0.4540(3) 0.022(3) Uani 1 1 d . . . . .
H43 H 1.0603 0.4187 0.4586 0.026 Uiso 1 1 calc R U . . .
C71 C 0.9214(14) 0.4097(7) 0.3864(3) 0.022(3) Uani 1 1 d . . . . .
C61 C 0.7772(13) 0.9277(8) 0.3393(3) 0.021(2) Uani 1 1 d . . . . .
C60 C 0.6192(13) 0.7863(8) 0.4513(3) 0.020(2) Uani 1 1 d . . . . .
C13 C 0.4051(13) 0.7771(8) 0.0851(3) 0.019(2) Uani 1 1 d . . . . .
C33 C 0.1947(14) 0.2715(9) 0.2287(4) 0.029(3) Uani 1 1 d . . . . .
H33 H 0.1090 0.2637 0.2478 0.035 Uiso 1 1 calc R U . . .
C70 C 0.9360(13) 0.9599(8) 0.3306(3) 0.020(2) Uani 1 1 d . . . . .
C80 C 0.7806(14) 0.3518(8) 0.3788(3) 0.023(3) Uani 1 1 d . . . . .
C20 C 0.4258(14) 0.6241(7) 0.0268(3) 0.020(3) Uani 1 1 d . . . . .
C19 C 0.4384(15) 0.5503(9) -0.0037(4) 0.033(3) Uani 1 1 d . . . . .
H19 H 0.3913 0.4879 0.0008 0.040 Uiso 1 1 calc R U . . .
C44 C 1.0015(12) 0.5488(8) 0.4851(3) 0.018(2) Uani 1 1 d . . . . .
C76 C 0.6542(16) 0.2084(8) 0.3479(4) 0.032(3) Uani 1 1 d . . . . .
H76 H 0.6597 0.1520 0.3309 0.038 Uiso 1 1 calc R U . . .
C62 C 0.6592(15) 0.9333(8) 0.3090(4) 0.028(3) Uani 1 1 d . . . . .
H62 H 0.5525 0.9113 0.3146 0.034 Uiso 1 1 calc R U . . .
C1 C 0.3050(13) 0.4668(7) 0.1107(3) 0.016(2) Uani 1 1 d . . . . .
C79 C 0.6283(15) 0.3740(9) 0.3966(4) 0.029(3) Uani 1 1 d . . . . .
H79 H 0.6165 0.4307 0.4132 0.035 Uiso 1 1 calc R U . . .
C18 C 0.5189(18) 0.5691(9) -0.0397(4) 0.045(4) Uani 1 1 d . . . . .
H18 H 0.5301 0.5187 -0.0596 0.053 Uiso 1 1 calc R U . . .
C10 C 0.2599(12) 0.5171(8) 0.0748(3) 0.020(2) Uani 1 1 d . . . . .
C68 C 1.2134(15) 0.9925(9) 0.3511(4) 0.036(3) Uani 1 1 d . . . . .
H68 H 1.2966 0.9916 0.3714 0.043 Uiso 1 1 calc R U . . .
C54 C 0.6144(14) 0.9256(8) 0.4045(4) 0.025(3) Uani 1 1 d . . . . .
H54 H 0.5713 0.9877 0.3973 0.030 Uiso 1 1 calc R U . . .
C34 C 0.3466(14) 0.2401(9) 0.2389(4) 0.033(3) Uani 1 1 d . . . . .
H34 H 0.3663 0.2114 0.2650 0.040 Uiso 1 1 calc R U . . .
C59 C 0.5456(14) 0.7346(10) 0.4847(3) 0.032(3) Uani 1 1 d . . . . .
H59 H 0.5869 0.6727 0.4928 0.038 Uiso 1 1 calc R U . . .
C3 C 0.1248(14) 0.3346(8) 0.0961(3) 0.024(3) Uani 1 1 d . . . . .
H3 H 0.0838 0.2714 0.1022 0.029 Uiso 1 1 calc R U . . .
C32 C 0.1632(15) 0.3148(8) 0.1907(4) 0.030(3) Uani 1 1 d . . . . .
H32 H 0.0561 0.3361 0.1848 0.036 Uiso 1 1 calc R U . . .
C47 C 1.0032(15) 0.6944(8) 0.5453(3) 0.028(3) Uani 1 1 d . . . . .
H47 H 1.0037 0.7434 0.5660 0.034 Uiso 1 1 calc R U . . .
C75 C 0.7966(15) 0.2664(8) 0.3529(3) 0.026(3) Uani 1 1 d . . . . .
C72 C 1.0652(14) 0.3838(8) 0.3675(4) 0.025(3) Uani 1 1 d . . . . .
H72 H 1.1591 0.4220 0.3726 0.030 Uiso 1 1 calc R U . . .
C66 C 1.1326(16) 1.0298(9) 0.2828(4) 0.038(3) Uani 1 1 d . . . . .
H66 H 1.1583 1.0542 0.2563 0.046 Uiso 1 1 calc R U . . .
C7 C -0.0734(17) 0.4924(11) -0.0019(4) 0.044(4) Uani 1 1 d . . . . .
H7 H -0.1253 0.5310 -0.0223 0.053 Uiso 1 1 calc R U . . .
C37 C 0.7504(16) 0.2241(9) 0.1912(4) 0.033(3) Uani 1 1 d . . . . .
H37 H 0.8554 0.2001 0.1978 0.040 Uiso 1 1 calc R U . . .
C39 C 0.5727(14) 0.3009(8) 0.1427(4) 0.024(3) Uani 1 1 d . . . . .
H39 H 0.5550 0.3297 0.1165 0.029 Uiso 1 1 calc R U . . .
C73 C 1.0766(16) 0.3028(8) 0.3410(3) 0.031(3) Uani 1 1 d . . . . .
H73 H 1.1756 0.2885 0.3275 0.037 Uiso 1 1 calc R U . . .
C63 C 0.6949(17) 0.9708(9) 0.2702(4) 0.039(3) Uani 1 1 d . . . . .
H63 H 0.6123 0.9753 0.2499 0.047 Uiso 1 1 calc R U . . .
C69 C 1.0612(14) 0.9597(9) 0.3617(4) 0.030(3) Uani 1 1 d . . . . .
H69 H 1.0393 0.9376 0.3887 0.036 Uiso 1 1 calc R U . . .
C22 C 0.2194(17) 0.9071(9) 0.1144(4) 0.035(3) Uani 1 1 d . U . . .
C36 C 0.6307(13) 0.2175(8) 0.2185(4) 0.027(3) Uani 1 1 d . . . . .
H36 H 0.6522 0.1891 0.2446 0.032 Uiso 1 1 calc R U . . .
C77 C 0.5169(18) 0.2290(9) 0.3654(4) 0.041(3) Uani 1 1 d . . . . .
H77 H 0.4276 0.1861 0.3618 0.049 Uiso 1 1 calc R U . . .
C31 C 0.2805(13) 0.3278(8) 0.1615(3) 0.019(2) Uani 1 1 d . . . . .
C21 C 0.3772(15) 0.8638(8) 0.1130(3) 0.026(3) Uani 1 1 d . . . . .
C57 C 0.3550(18) 0.8641(12) 0.4936(4) 0.051(4) Uani 1 1 d . . . . .
H57 H 0.2654 0.8901 0.5081 0.061 Uiso 1 1 calc R U . . .
C8 C 0.0584(14) 0.5274(10) 0.0176(3) 0.032(3) Uani 1 1 d . . . . .
H8 H 0.1029 0.5880 0.0090 0.038 Uiso 1 1 calc R U . . .
C81 C 0.3686(16) 0.4638(10) 0.2786(4) 0.041(3) Uani 1 1 d D . . . .
H81A H 0.4152 0.4128 0.2962 0.062 Uiso 1 1 calc R U . . .
H81B H 0.3925 0.4494 0.2498 0.062 Uiso 1 1 calc R U . . .
H81C H 0.2511 0.4659 0.2825 0.062 Uiso 1 1 calc R U . . .
C64 C 0.8469(17) 1.0010(9) 0.2615(3) 0.036(3) Uani 1 1 d . . . . .
H64 H 0.8698 1.0252 0.2348 0.043 Uiso 1 1 calc R U . . .
C82 C 0.805(2) 0.4456(10) 0.2666(4) 0.057(4) Uani 1 1 d D . . . .
H82A H 0.7617 0.4601 0.2939 0.085 Uiso 1 1 calc R U . . .
H82B H 0.9231 0.4509 0.2672 0.085 Uiso 1 1 calc R U . . .
H82C H 0.7737 0.3792 0.2586 0.085 Uiso 1 1 calc R U . . .
C74 C 0.9426(16) 0.2445(9) 0.3349(4) 0.037(3) Uani 1 1 d . . . . .
H74 H 0.9512 0.1882 0.3179 0.044 Uiso 1 1 calc R U . . .
C087 C 0.8420(16) 0.5388(11) 0.1305(5) 0.051(4) Uani 1 1 d . . . . .
H08A H 0.7653 0.5910 0.1371 0.077 Uiso 1 1 calc DR U . . .
H08B H 0.7856 0.4870 0.1153 0.077 Uiso 1 1 calc R U . . .
H08C H 0.9295 0.5652 0.1136 0.077 Uiso 1 1 calc R U . . .
C56 C 0.4198(16) 0.9159(10) 0.4622(4) 0.039(3) Uani 1 1 d . . . . .
H56 H 0.3750 0.9774 0.4549 0.046 Uiso 1 1 calc R U . . .
C58 C 0.4175(17) 0.7734(11) 0.5048(4) 0.047(4) Uani 1 1 d . . . . .
H58 H 0.3698 0.7383 0.5268 0.056 Uiso 1 1 calc R U . . .
C67 C 1.2496(15) 1.0265(11) 0.3122(5) 0.045(4) Uani 1 1 d . . . . .
H67 H 1.3564 1.0475 0.3060 0.054 Uiso 1 1 calc R U . . .
C78 C 0.4978(15) 0.3136(9) 0.3898(4) 0.037(3) Uani 1 1 d . . . . .
H78 H 0.3955 0.3286 0.4014 0.044 Uiso 1 1 calc R U . . .
C6 C -0.1353(17) 0.3995(11) 0.0076(4) 0.045(4) Uani 1 1 d . . . . .
H6 H -0.2233 0.3734 -0.0078 0.054 Uiso 1 1 calc R U . . .
C16 C 0.5755(15) 0.7320(9) -0.0192(4) 0.033(3) Uani 1 1 d . . . . .
H16 H 0.6225 0.7939 -0.0247 0.039 Uiso 1 1 calc R U . . .
C29 C 0.471(2) 0.9996(11) 0.1559(5) 0.052(4) Uani 1 1 d . . . . .
H29 H 0.5551 1.0317 0.1708 0.063 Uiso 1 1 calc R U . . .
C23 C 0.0814(16) 0.8692(11) 0.0945(4) 0.045(4) Uani 1 1 d . . . . .
H23 H 0.0905 0.8082 0.0808 0.054 Uiso 1 1 calc R U . . .
C26 C 0.0389(19) 1.0419(11) 0.1355(5) 0.048(4) Uani 1 1 d . U . . .
H26 H 0.0193 1.1010 0.1499 0.057 Uiso 1 1 calc R U . . .
C30 C 0.506(2) 0.9069(10) 0.1322(4) 0.050(4) Uani 1 1 d . . . . .
H30 H 0.6119 0.8800 0.1308 0.060 Uiso 1 1 calc R U . . .
C27 C 0.195(2) 1.0015(12) 0.1373(5) 0.062(5) Uani 1 1 d . . . . .
C84 C 0.355(2) 0.8407(14) 0.2277(5) 0.077(5) Uani 1 1 d D . . . .
H84A H 0.3340 0.9063 0.2385 0.116 Uiso 1 1 calc R U . . .
H84B H 0.2597 0.8173 0.2127 0.116 Uiso 1 1 calc R U . . .
H84C H 0.4482 0.8430 0.2091 0.116 Uiso 1 1 calc R U . . .
C28 C 0.326(2) 1.0343(13) 0.1555(5) 0.059(4) Uani 1 1 d . . . . .
H28 H 0.3117 1.0928 0.1708 0.071 Uiso 1 1 calc R U . . .
C83 C 0.862(2) 0.7760(13) 0.1800(5) 0.069(5) Uani 1 1 d D . . . .
H83A H 0.8344 0.8452 0.1768 0.104 Uiso 1 1 calc R U . . .
H83B H 0.8041 0.7374 0.1593 0.104 Uiso 1 1 calc DR U . . .
H83C H 0.9790 0.7674 0.1764 0.104 Uiso 1 1 calc DR U . . .
C25 C -0.089(2) 0.9998(13) 0.1136(5) 0.072(5) Uani 1 1 d . U . . .
H25 H -0.1919 1.0304 0.1127 0.087 Uiso 1 1 calc R U . . .
C24 C -0.063(2) 0.9150(13) 0.0939(5) 0.065(5) Uani 1 1 d . . . . .
H24 H -0.1501 0.8863 0.0790 0.078 Uiso 1 1 calc R U . . .
O14 O 0.3002(11) 0.5969(9) 0.3607(3) 0.064(3) Uani 1 1 d D . . . .
C85 C 0.338(3) 0.650(2) 0.3954(7) 0.061(7) Uani 0.65 1 d D . P A 2
H85A H 0.3797 0.7143 0.3873 0.091 Uiso 0.65 1 calc R U P A 2
H85B H 0.4213 0.6153 0.4113 0.091 Uiso 0.65 1 calc R U P A 2
H85C H 0.2412 0.6583 0.4122 0.091 Uiso 0.65 1 calc R U P A 2
C86 C 0.339(7) 0.702(3) 0.3744(18) 0.069(17) Uiso 0.35 1 d D . P A 1
H86A H 0.4411 0.7020 0.3900 0.103 Uiso 0.35 1 calc R U P A 1
H86B H 0.2517 0.7262 0.3918 0.103 Uiso 0.35 1 calc R U P A 1
H86C H 0.3501 0.7436 0.3502 0.103 Uiso 0.35 1 calc R U P A 1
H9 H 0.394(19) 0.566(8) 0.315(3) 0.103 Uiso 1 1 d D U . . .
H11 H 0.292(7) 0.752(6) 0.2694(17) 0.103 Uiso 1 1 d D U . . .
H1 H 0.895(8) 0.716(12) 0.235(2) 0.103 Uiso 1 1 d D U . . .
H10 H 0.810(6) 0.5172(13) 0.2165(8) 0.103 Uiso 1 1 d D U . . .
H15A H 1.1382 0.6579 0.2307 0.103 Uiso 1 1 d DR U . . .
H15B H 1.0729 0.6386 0.2695 0.103 Uiso 1 1 d DR U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O5 2.277(7) . ?
Ca1 O4 2.311(7) . ?
Ca1 O10 2.332(8) . ?
Ca1 O9 2.349(8) . ?
Ca1 O12 2.354(8) . ?
Ca1 O11 2.393(9) . ?
Ca1 P1 3.546(3) . ?
Ca1 H1 2.60(9) . ?
P2 O5 1.471(7) . ?
P2 O8 1.476(8) . ?
P2 O6 1.607(7) . ?
P2 O7 1.610(7) . ?
P1 O3 1.476(8) . ?
P1 O4 1.480(7) . ?
P1 O1 1.612(7) . ?
P1 O2 1.621(7) . ?
O1 C1 1.373(12) . ?
O6 C41 1.396(11) . ?
O2 C12 1.379(12) . ?
O7 C52 1.401(12) . ?
O15 H15A 0.8760 . ?
O15 H15B 0.8892 . ?
O10 C82 1.440(15) . ?
O10 H10 0.894(19) . ?
O9 C81 1.425(14) . ?
O9 H9 0.92(3) . ?
O13 C087 1.462(17) . ?
O13 H13 0.8400 . ?
O12 C83 1.412(17) . ?
O12 H1 0.89(3) . ?
C9 C8 1.416(16) . ?
C9 C10 1.424(15) . ?
C9 C4 1.449(16) . ?
C49 C48 1.404(15) . ?
C49 C50 1.445(14) . ?
C49 C44 1.451(15) . ?
C41 C50 1.365(14) . ?
C41 C42 1.428(14) . ?
C40 C31 1.426(15) . ?
C40 C35 1.427(16) . ?
C40 C39 1.443(16) . ?
O11 C84 1.415(19) . ?
O11 H11 0.92(3) . ?
C45 C46 1.366(16) . ?
C45 C44 1.410(14) . ?
C45 H45 0.9500 . ?
C42 C43 1.369(14) . ?
C42 C71 1.479(14) . ?
C46 C47 1.416(16) . ?
C46 H46 0.9500 . ?
C15 C16 1.395(16) . ?
C15 C14 1.404(14) . ?
C15 C20 1.452(14) . ?
C12 C13 1.389(14) . ?
C12 C11 1.399(14) . ?
C52 C51 1.363(15) . ?
C52 C53 1.397(15) . ?
C53 C54 1.382(16) . ?
C53 C61 1.497(16) . ?
C2 C3 1.390(15) . ?
C2 C1 1.419(15) . ?
C2 C31 1.463(15) . ?
C35 C36 1.372(16) . ?
C35 C34 1.446(16) . ?
C11 C20 1.444(15) . ?
C11 C10 1.461(15) . ?
C38 C39 1.325(16) . ?
C38 C37 1.426(16) . ?
C38 H38 0.9500 . ?
C48 C47 1.369(15) . ?
C48 H48 0.9500 . ?
C55 C60 1.406(16) . ?
C55 C54 1.409(17) . ?
C55 C56 1.443(17) . ?
C51 C60 1.443(15) . ?
C51 C50 1.502(15) . ?
C4 C3 1.370(16) . ?
C4 C5 1.436(17) . ?
C17 C16 1.326(17) . ?
C17 C18 1.425(18) . ?
C17 H17 0.9500 . ?
C5 C6 1.345(19) . ?
C5 H5 0.9500 . ?
C65 C64 1.403(17) . ?
C65 C70 1.420(16) . ?
C65 C66 1.429(18) . ?
C14 C13 1.383(15) . ?
C14 H14 0.9500 . ?
C43 C44 1.408(15) . ?
C43 H43 0.9500 . ?
C71 C72 1.386(16) . ?
C71 C80 1.428(15) . ?
C61 C62 1.387(15) . ?
C61 C70 1.415(16) . ?
C60 C59 1.434(16) . ?
C13 C21 1.513(15) . ?
C33 C34 1.366(16) . ?
C33 C32 1.393(17) . ?
C33 H33 0.9500 . ?
C70 C69 1.442(16) . ?
C80 C79 1.420(17) . ?
C80 C75 1.448(16) . ?
C20 C19 1.419(15) . ?
C19 C18 1.375(17) . ?
C19 H19 0.9500 . ?
C76 C77 1.303(19) . ?
C76 C75 1.427(17) . ?
C76 H76 0.9500 . ?
C62 C63 1.394(17) . ?
C62 H62 0.9500 . ?
C1 C10 1.404(15) . ?
C79 C78 1.375(17) . ?
C79 H79 0.9500 . ?
C18 H18 0.9500 . ?
C68 C69 1.380(17) . ?
C68 C67 1.384(18) . ?
C68 H68 0.9500 . ?
C54 H54 0.9500 . ?
C34 H34 0.9500 . ?
C59 C58 1.354(17) . ?
C59 H59 0.9500 . ?
C3 H3 0.9500 . ?
C32 C31 1.373(16) . ?
C32 H32 0.9500 . ?
C47 H47 0.9500 . ?
C75 C74 1.377(18) . ?
C72 C73 1.409(16) . ?
C72 H72 0.9500 . ?
C66 C67 1.355(19) . ?
C66 H66 0.9500 . ?
C7 C8 1.345(16) . ?
C7 C6 1.404(19) . ?
C7 H7 0.9500 . ?
C37 C36 1.335(17) . ?
C37 H37 0.9500 . ?
C39 H39 0.9500 . ?
C73 C74 1.378(18) . ?
C73 H73 0.9500 . ?
C63 C64 1.353(18) . ?
C63 H63 0.9500 . ?
C69 H69 0.9500 . ?
C22 C23 1.41(2) . ?
C22 C21 1.433(18) . ?
C22 C27 1.51(2) . ?
C36 H36 0.9500 . ?
C77 C78 1.412(19) . ?
C77 H77 0.9500 . ?
C21 C30 1.365(18) . ?
C57 C56 1.35(2) . ?
C57 C58 1.39(2) . ?
C57 H57 0.9500 . ?
C8 H8 0.9500 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C64 H64 0.9500 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C74 H74 0.9500 . ?
C087 H08A 0.9800 . ?
C087 H08B 0.9800 . ?
C087 H08C 0.9800 . ?
C56 H56 0.9500 . ?
C58 H58 0.9500 . ?
C67 H67 0.9500 . ?
C78 H78 0.9500 . ?
C6 H6 0.9500 . ?
C16 H16 0.9500 . ?
C29 C28 1.29(2) . ?
C29 C30 1.51(2) . ?
C29 H29 0.9500 . ?
C23 C24 1.349(19) . ?
C23 H23 0.9500 . ?
C26 C25 1.39(2) . ?
C26 C27 1.40(2) . ?
C26 H26 0.9500 . ?
C30 H30 0.9500 . ?
C27 C28 1.31(2) . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C28 H28 0.9500 . ?
C83 H83A 0.9800 . ?
C83 H83B 0.9800 . ?
C83 H83C 0.9800 . ?
C25 C24 1.34(2) . ?
C25 H25 0.9500 . ?
C24 H24 0.9500 . ?
O14 C85 1.38(2) . ?
O14 C86 1.54(4) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 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
O5 Ca1 O4 170.9(3) . . ?
O5 Ca1 O10 93.5(3) . . ?
O4 Ca1 O10 88.3(3) . . ?
O5 Ca1 O9 85.4(3) . . ?
O4 Ca1 O9 103.6(3) . . ?
O10 Ca1 O9 82.4(3) . . ?
O5 Ca1 O12 83.4(3) . . ?
O4 Ca1 O12 87.8(3) . . ?
O10 Ca1 O12 88.2(3) . . ?
O9 Ca1 O12 165.0(3) . . ?
O5 Ca1 O11 95.6(3) . . ?
O4 Ca1 O11 84.9(3) . . ?
O10 Ca1 O11 163.3(3) . . ?
O9 Ca1 O11 84.3(3) . . ?
O12 Ca1 O11 106.8(3) . . ?
O5 Ca1 P1 172.4(2) . . ?
O4 Ca1 P1 16.37(19) . . ?
O10 Ca1 P1 88.2(2) . . ?
O9 Ca1 P1 87.4(2) . . ?
O12 Ca1 P1 104.1(2) . . ?
O11 Ca1 P1 81.0(3) . . ?
O5 Ca1 H1 69(2) . . ?
O4 Ca1 H1 102.8(19) . . ?
O10 Ca1 H1 76(3) . . ?
O9 Ca1 H1 145.0(10) . . ?
O12 Ca1 H1 19.9(10) . . ?
O11 Ca1 H1 121(3) . . ?
P1 Ca1 H1 119(2) . . ?
O5 P2 O8 120.1(4) . . ?
O5 P2 O6 106.3(4) . . ?
O8 P2 O6 110.9(4) . . ?
O5 P2 O7 111.2(4) . . ?
O8 P2 O7 105.0(4) . . ?
O6 P2 O7 101.9(3) . . ?
O3 P1 O4 119.5(4) . . ?
O3 P1 O1 111.1(4) . . ?
O4 P1 O1 106.1(4) . . ?
O3 P1 O2 104.8(4) . . ?
O4 P1 O2 111.9(4) . . ?
O1 P1 O2 102.0(3) . . ?
O3 P1 Ca1 94.2(3) . . ?
O4 P1 Ca1 26.1(3) . . ?
O1 P1 Ca1 113.7(3) . . ?
O2 P1 Ca1 129.8(3) . . ?
C1 O1 P1 117.8(6) . . ?
C41 O6 P2 118.0(6) . . ?
C12 O2 P1 119.8(6) . . ?
C52 O7 P2 117.4(6) . . ?
P1 O4 Ca1 137.5(5) . . ?
P2 O5 Ca1 149.2(5) . . ?
H15A O15 H15B 104.9 . . ?
C82 O10 Ca1 128.8(8) . . ?
C82 O10 H10 107(3) . . ?
Ca1 O10 H10 114.5(17) . . ?
C81 O9 Ca1 128.5(7) . . ?
C81 O9 H9 102(5) . . ?
Ca1 O9 H9 130(5) . . ?
C087 O13 H13 109.5 . . ?
C83 O12 Ca1 137.1(9) . . ?
C83 O12 H1 117(4) . . ?
Ca1 O12 H1 96(7) . . ?
C8 C9 C10 122.9(10) . . ?
C8 C9 C4 118.2(10) . . ?
C10 C9 C4 118.8(9) . . ?
C48 C49 C50 124.2(10) . . ?
C48 C49 C44 117.6(9) . . ?
C50 C49 C44 118.3(9) . . ?
C50 C41 O6 118.9(8) . . ?
C50 C41 C42 124.0(9) . . ?
O6 C41 C42 117.1(8) . . ?
C31 C40 C35 121.9(10) . . ?
C31 C40 C39 122.8(10) . . ?
C35 C40 C39 115.3(10) . . ?
C84 O11 Ca1 116.3(9) . . ?
C84 O11 H11 107(5) . . ?
Ca1 O11 H11 116(6) . . ?
C46 C45 C44 121.2(11) . . ?
C46 C45 H45 119.4 . . ?
C44 C45 H45 119.4 . . ?
C43 C42 C41 117.0(9) . . ?
C43 C42 C71 120.5(9) . . ?
C41 C42 C71 122.4(9) . . ?
C45 C46 C47 119.4(10) . . ?
C45 C46 H46 120.3 . . ?
C47 C46 H46 120.3 . . ?
C16 C15 C14 123.5(10) . . ?
C16 C15 C20 118.1(10) . . ?
C14 C15 C20 118.4(9) . . ?
O2 C12 C13 118.6(9) . . ?
O2 C12 C11 118.3(8) . . ?
C13 C12 C11 122.9(9) . . ?
C51 C52 C53 124.3(9) . . ?
C51 C52 O7 118.8(9) . . ?
C53 C52 O7 116.9(9) . . ?
C54 C53 C52 116.9(10) . . ?
C54 C53 C61 121.7(10) . . ?
C52 C53 C61 121.0(10) . . ?
C3 C2 C1 116.5(10) . . ?
C3 C2 C31 120.8(9) . . ?
C1 C2 C31 122.5(9) . . ?
C36 C35 C40 121.2(10) . . ?
C36 C35 C34 121.7(11) . . ?
C40 C35 C34 117.1(10) . . ?
C12 C11 C20 117.7(9) . . ?
C12 C11 C10 119.8(9) . . ?
C20 C11 C10 122.5(9) . . ?
C39 C38 C37 120.8(11) . . ?
C39 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C47 C48 C49 121.4(10) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 H48 119.3 . . ?
C60 C55 C54 120.2(10) . . ?
C60 C55 C56 118.4(11) . . ?
C54 C55 C56 120.9(11) . . ?
C52 C51 C60 118.3(9) . . ?
C52 C51 C50 119.5(9) . . ?
C60 C51 C50 121.9(9) . . ?
C41 C50 C49 118.7(9) . . ?
C41 C50 C51 119.6(8) . . ?
C49 C50 C51 121.5(9) . . ?
C3 C4 C5 122.8(11) . . ?
C3 C4 C9 120.1(10) . . ?
C5 C4 C9 116.6(11) . . ?
C16 C17 C18 119.2(11) . . ?
C16 C17 H17 120.4 . . ?
C18 C17 H17 120.4 . . ?
C6 C5 C4 122.8(13) . . ?
C6 C5 H5 118.6 . . ?
C4 C5 H5 118.6 . . ?
C64 C65 C70 118.6(11) . . ?
C64 C65 C66 123.0(11) . . ?
C70 C65 C66 118.5(11) . . ?
C13 C14 C15 122.1(9) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C42 C43 C44 123.0(10) . . ?
C42 C43 H43 118.5 . . ?
C44 C43 H43 118.5 . . ?
C72 C71 C80 118.7(10) . . ?
C72 C71 C42 119.5(10) . . ?
C80 C71 C42 121.5(10) . . ?
C62 C61 C70 119.2(10) . . ?
C62 C61 C53 118.5(10) . . ?
C70 C61 C53 122.3(10) . . ?
C55 C60 C59 118.9(10) . . ?
C55 C60 C51 117.9(10) . . ?
C59 C60 C51 123.1(10) . . ?
C14 C13 C12 119.2(9) . . ?
C14 C13 C21 118.7(9) . . ?
C12 C13 C21 121.9(9) . . ?
C34 C33 C32 121.1(11) . . ?
C34 C33 H33 119.4 . . ?
C32 C33 H33 119.4 . . ?
C61 C70 C65 119.4(10) . . ?
C61 C70 C69 121.4(10) . . ?
C65 C70 C69 119.1(11) . . ?
C79 C80 C71 122.2(10) . . ?
C79 C80 C75 119.6(10) . . ?
C71 C80 C75 118.2(10) . . ?
C19 C20 C11 122.4(9) . . ?
C19 C20 C15 118.2(9) . . ?
C11 C20 C15 119.4(9) . . ?
C18 C19 C20 119.9(11) . . ?
C18 C19 H19 120.0 . . ?
C20 C19 H19 120.0 . . ?
C43 C44 C45 121.7(10) . . ?
C43 C44 C49 118.9(9) . . ?
C45 C44 C49 119.4(9) . . ?
C77 C76 C75 123.2(11) . . ?
C77 C76 H76 118.4 . . ?
C75 C76 H76 118.4 . . ?
C61 C62 C63 120.9(12) . . ?
C61 C62 H62 119.5 . . ?
C63 C62 H62 119.5 . . ?
O1 C1 C10 118.1(9) . . ?
O1 C1 C2 117.9(9) . . ?
C10 C1 C2 123.9(9) . . ?
C78 C79 C80 120.0(12) . . ?
C78 C79 H79 120.0 . . ?
C80 C79 H79 120.0 . . ?
C19 C18 C17 121.0(11) . . ?
C19 C18 H18 119.5 . . ?
C17 C18 H18 119.5 . . ?
C1 C10 C9 117.4(9) . . ?
C1 C10 C11 119.2(9) . . ?
C9 C10 C11 123.3(9) . . ?
C69 C68 C67 122.6(12) . . ?
C69 C68 H68 118.7 . . ?
C67 C68 H68 118.7 . . ?
C53 C54 C55 121.7(11) . . ?
C53 C54 H54 119.2 . . ?
C55 C54 H54 119.2 . . ?
C33 C34 C35 119.9(11) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C58 C59 C60 120.5(12) . . ?
C58 C59 H59 119.8 . . ?
C60 C59 H59 119.8 . . ?
C4 C3 C2 122.9(11) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C31 C32 C33 122.7(12) . . ?
C31 C32 H32 118.6 . . ?
C33 C32 H32 118.6 . . ?
C48 C47 C46 121.0(10) . . ?
C48 C47 H47 119.5 . . ?
C46 C47 H47 119.5 . . ?
C74 C75 C76 123.6(11) . . ?
C74 C75 C80 120.4(11) . . ?
C76 C75 C80 116.0(11) . . ?
C71 C72 C73 122.2(11) . . ?
C71 C72 H72 118.9 . . ?
C73 C72 H72 118.9 . . ?
C67 C66 C65 121.4(12) . . ?
C67 C66 H66 119.3 . . ?
C65 C66 H66 119.3 . . ?
C8 C7 C6 120.9(12) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C36 C37 C38 119.2(11) . . ?
C36 C37 H37 120.4 . . ?
C38 C37 H37 120.4 . . ?
C38 C39 C40 121.7(11) . . ?
C38 C39 H39 119.1 . . ?
C40 C39 H39 119.1 . . ?
C74 C73 C72 119.2(11) . . ?
C74 C73 H73 120.4 . . ?
C72 C73 H73 120.4 . . ?
C64 C63 C62 120.1(12) . . ?
C64 C63 H63 119.9 . . ?
C62 C63 H63 119.9 . . ?
C68 C69 C70 118.4(12) . . ?
C68 C69 H69 120.8 . . ?
C70 C69 H69 120.8 . . ?
C23 C22 C21 124.6(11) . . ?
C23 C22 C27 115.6(13) . . ?
C21 C22 C27 119.7(13) . . ?
C37 C36 C35 121.8(11) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C76 C77 C78 121.6(12) . . ?
C76 C77 H77 119.2 . . ?
C78 C77 H77 119.2 . . ?
C32 C31 C40 117.2(10) . . ?
C32 C31 C2 120.0(10) . . ?
C40 C31 C2 122.8(10) . . ?
C30 C21 C22 120.9(12) . . ?
C30 C21 C13 119.5(12) . . ?
C22 C21 C13 119.0(10) . . ?
C56 C57 C58 121.1(12) . . ?
C56 C57 H57 119.5 . . ?
C58 C57 H57 119.5 . . ?
C7 C8 C9 121.9(12) . . ?
C7 C8 H8 119.1 . . ?
C9 C8 H8 119.1 . . ?
O9 C81 H81A 109.5 . . ?
O9 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
O9 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C63 C64 C65 121.7(11) . . ?
C63 C64 H64 119.1 . . ?
C65 C64 H64 119.1 . . ?
O10 C82 H82A 109.5 . . ?
O10 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
O10 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
C75 C74 C73 121.2(11) . . ?
C75 C74 H74 119.4 . . ?
C73 C74 H74 119.4 . . ?
O13 C087 H08A 109.5 . . ?
O13 C087 H08B 109.5 . . ?
H08A C087 H08B 109.5 . . ?
O13 C087 H08C 109.5 . . ?
H08A C087 H08C 109.5 . . ?
H08B C087 H08C 109.5 . . ?
C57 C56 C55 120.3(12) . . ?
C57 C56 H56 119.9 . . ?
C55 C56 H56 119.9 . . ?
C59 C58 C57 120.8(13) . . ?
C59 C58 H58 119.6 . . ?
C57 C58 H58 119.6 . . ?
C66 C67 C68 119.9(12) . . ?
C66 C67 H67 120.0 . . ?
C68 C67 H67 120.0 . . ?
C79 C78 C77 119.6(12) . . ?
C79 C78 H78 120.2 . . ?
C77 C78 H78 120.2 . . ?
C5 C6 C7 119.5(12) . . ?
C5 C6 H6 120.2 . . ?
C7 C6 H6 120.2 . . ?
C17 C16 C15 123.5(11) . . ?
C17 C16 H16 118.2 . . ?
C15 C16 H16 118.2 . . ?
C28 C29 C30 118.7(14) . . ?
C28 C29 H29 120.6 . . ?
C30 C29 H29 120.6 . . ?
C24 C23 C22 123.4(16) . . ?
C24 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
C25 C26 C27 123.4(15) . . ?
C25 C26 H26 118.3 . . ?
C27 C26 H26 118.3 . . ?
C21 C30 C29 116.5(14) . . ?
C21 C30 H30 121.7 . . ?
C29 C30 H30 121.7 . . ?
C28 C27 C26 129.8(17) . . ?
C28 C27 C22 113.8(17) . . ?
C26 C27 C22 116.4(15) . . ?
O11 C84 H84A 109.5 . . ?
O11 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
O11 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
C29 C28 C27 130.2(17) . . ?
C29 C28 H28 114.9 . . ?
C27 C28 H28 114.9 . . ?
O12 C83 H83A 109.5 . . ?
O12 C83 H83B 109.5 . . ?
H83A C83 H83B 109.5 . . ?
O12 C83 H83C 109.5 . . ?
H83A C83 H83C 109.5 . . ?
H83B C83 H83C 109.5 . . ?
C24 C25 C26 118.7(17) . . ?
C24 C25 H25 120.6 . . ?
C26 C25 H25 120.6 . . ?
C25 C24 C23 122.4(19) . . ?
C25 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
O14 C85 H85A 109.5 . . ?
O14 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
O14 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
O14 C86 H86A 109.5 . . ?
O14 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
O14 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 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 P1 O1 C1 58.8(8) . . . . ?
O4 P1 O1 C1 -169.8(7) . . . . ?
O2 P1 O1 C1 -52.5(7) . . . . ?
Ca1 P1 O1 C1 163.6(6) . . . . ?
O5 P2 O6 C41 -161.3(7) . . . . ?
O8 P2 O6 C41 66.6(7) . . . . ?
O7 P2 O6 C41 -44.7(7) . . . . ?
O3 P1 O2 C12 -156.7(7) . . . . ?
O4 P1 O2 C12 72.3(8) . . . . ?
O1 P1 O2 C12 -40.8(7) . . . . ?
Ca1 P1 O2 C12 94.6(7) . . . . ?
O5 P2 O7 C52 64.4(8) . . . . ?
O8 P2 O7 C52 -164.2(7) . . . . ?
O6 P2 O7 C52 -48.5(7) . . . . ?
O3 P1 O4 Ca1 15.4(9) . . . . ?
O1 P1 O4 Ca1 -111.0(6) . . . . ?
O2 P1 O4 Ca1 138.5(6) . . . . ?
O8 P2 O5 Ca1 38.2(10) . . . . ?
O6 P2 O5 Ca1 -88.6(9) . . . . ?
O7 P2 O5 Ca1 161.4(7) . . . . ?
P2 O6 C41 C50 76.2(10) . . . . ?
P2 O6 C41 C42 -101.7(9) . . . . ?
C50 C41 C42 C43 -1.7(15) . . . . ?
O6 C41 C42 C43 176.1(9) . . . . ?
C50 C41 C42 C71 178.3(10) . . . . ?
O6 C41 C42 C71 -3.9(14) . . . . ?
C44 C45 C46 C47 -2.9(18) . . . . ?
P1 O2 C12 C13 -111.4(9) . . . . ?
P1 O2 C12 C11 72.9(10) . . . . ?
P2 O7 C52 C51 75.7(10) . . . . ?
P2 O7 C52 C53 -104.4(9) . . . . ?
C51 C52 C53 C54 -1.5(16) . . . . ?
O7 C52 C53 C54 178.5(9) . . . . ?
C51 C52 C53 C61 -175.1(10) . . . . ?
O7 C52 C53 C61 4.9(14) . . . . ?
C31 C40 C35 C36 178.8(11) . . . . ?
C39 C40 C35 C36 0.0(16) . . . . ?
C31 C40 C35 C34 0.7(16) . . . . ?
C39 C40 C35 C34 -178.1(10) . . . . ?
O2 C12 C11 C20 -177.9(8) . . . . ?
C13 C12 C11 C20 6.5(15) . . . . ?
O2 C12 C11 C10 -0.1(14) . . . . ?
C13 C12 C11 C10 -175.6(9) . . . . ?
C50 C49 C48 C47 179.2(11) . . . . ?
C44 C49 C48 C47 -2.0(17) . . . . ?
C53 C52 C51 C60 7.4(15) . . . . ?
O7 C52 C51 C60 -172.6(9) . . . . ?
C53 C52 C51 C50 -178.6(10) . . . . ?
O7 C52 C51 C50 1.3(14) . . . . ?
O6 C41 C50 C49 -176.8(9) . . . . ?
C42 C41 C50 C49 1.0(15) . . . . ?
O6 C41 C50 C51 -1.8(14) . . . . ?
C42 C41 C50 C51 176.0(9) . . . . ?
C48 C49 C50 C41 178.1(10) . . . . ?
C44 C49 C50 C41 -0.7(15) . . . . ?
C48 C49 C50 C51 3.1(16) . . . . ?
C44 C49 C50 C51 -175.6(9) . . . . ?
C52 C51 C50 C41 -51.7(14) . . . . ?
C60 C51 C50 C41 122.1(11) . . . . ?
C52 C51 C50 C49 123.2(11) . . . . ?
C60 C51 C50 C49 -63.0(14) . . . . ?
C8 C9 C4 C3 -173.3(11) . . . . ?
C10 C9 C4 C3 2.5(16) . . . . ?
C8 C9 C4 C5 -0.8(15) . . . . ?
C10 C9 C4 C5 175.0(10) . . . . ?
C3 C4 C5 C6 172.7(13) . . . . ?
C9 C4 C5 C6 0.5(18) . . . . ?
C16 C15 C14 C13 177.4(11) . . . . ?
C20 C15 C14 C13 -0.8(15) . . . . ?
C41 C42 C43 C44 2.2(15) . . . . ?
C71 C42 C43 C44 -177.8(10) . . . . ?
C43 C42 C71 C72 -66.0(14) . . . . ?
C41 C42 C71 C72 114.0(12) . . . . ?
C43 C42 C71 C80 106.8(12) . . . . ?
C41 C42 C71 C80 -73.2(13) . . . . ?
C54 C53 C61 C62 -61.4(15) . . . . ?
C52 C53 C61 C62 111.9(12) . . . . ?
C54 C53 C61 C70 120.5(12) . . . . ?
C52 C53 C61 C70 -66.1(14) . . . . ?
C54 C55 C60 C59 -173.1(10) . . . . ?
C56 C55 C60 C59 -0.3(15) . . . . ?
C54 C55 C60 C51 5.5(15) . . . . ?
C56 C55 C60 C51 178.3(10) . . . . ?
C52 C51 C60 C55 -9.2(14) . . . . ?
C50 C51 C60 C55 177.0(9) . . . . ?
C52 C51 C60 C59 169.3(10) . . . . ?
C50 C51 C60 C59 -4.5(16) . . . . ?
C15 C14 C13 C12 3.4(15) . . . . ?
C15 C14 C13 C21 -171.7(10) . . . . ?
O2 C12 C13 C14 178.0(9) . . . . ?
C11 C12 C13 C14 -6.4(15) . . . . ?
O2 C12 C13 C21 -7.1(15) . . . . ?
C11 C12 C13 C21 168.5(10) . . . . ?
C62 C61 C70 C65 0.0(16) . . . . ?
C53 C61 C70 C65 178.0(10) . . . . ?
C62 C61 C70 C69 177.1(10) . . . . ?
C53 C61 C70 C69 -4.8(16) . . . . ?
C64 C65 C70 C61 -0.1(15) . . . . ?
C66 C65 C70 C61 179.8(10) . . . . ?
C64 C65 C70 C69 -177.3(10) . . . . ?
C66 C65 C70 C69 2.6(15) . . . . ?
C72 C71 C80 C79 -179.2(10) . . . . ?
C42 C71 C80 C79 7.9(16) . . . . ?
C72 C71 C80 C75 2.3(15) . . . . ?
C42 C71 C80 C75 -170.6(9) . . . . ?
C12 C11 C20 C19 177.6(10) . . . . ?
C10 C11 C20 C19 -0.2(16) . . . . ?
C12 C11 C20 C15 -3.6(14) . . . . ?
C10 C11 C20 C15 178.6(10) . . . . ?
C16 C15 C20 C19 1.5(16) . . . . ?
C14 C15 C20 C19 179.8(10) . . . . ?
C16 C15 C20 C11 -177.4(10) . . . . ?
C14 C15 C20 C11 0.9(15) . . . . ?
C11 C20 C19 C18 178.8(12) . . . . ?
C15 C20 C19 C18 0.0(18) . . . . ?
C42 C43 C44 C45 -179.8(10) . . . . ?
C42 C43 C44 C49 -2.0(16) . . . . ?
C46 C45 C44 C43 -180.0(11) . . . . ?
C46 C45 C44 C49 2.3(17) . . . . ?
C48 C49 C44 C43 -177.7(10) . . . . ?
C50 C49 C44 C43 1.2(15) . . . . ?
C48 C49 C44 C45 0.2(15) . . . . ?
C50 C49 C44 C45 179.0(10) . . . . ?
C70 C61 C62 C63 -0.4(17) . . . . ?
C53 C61 C62 C63 -178.5(11) . . . . ?
P1 O1 C1 C10 73.9(10) . . . . ?
P1 O1 C1 C2 -102.7(9) . . . . ?
C3 C2 C1 O1 176.2(9) . . . . ?
C31 C2 C1 O1 0.9(15) . . . . ?
C3 C2 C1 C10 -0.1(15) . . . . ?
C31 C2 C1 C10 -175.4(10) . . . . ?
C71 C80 C79 C78 -177.2(10) . . . . ?
C75 C80 C79 C78 1.3(16) . . . . ?
C20 C19 C18 C17 -2(2) . . . . ?
C16 C17 C18 C19 3(2) . . . . ?
O1 C1 C10 C9 -171.4(9) . . . . ?
C2 C1 C10 C9 4.9(15) . . . . ?
O1 C1 C10 C11 6.5(14) . . . . ?
C2 C1 C10 C11 -177.2(10) . . . . ?
C8 C9 C10 C1 169.6(10) . . . . ?
C4 C9 C10 C1 -6.0(15) . . . . ?
C8 C9 C10 C11 -8.2(17) . . . . ?
C4 C9 C10 C11 176.2(10) . . . . ?
C12 C11 C10 C1 -55.6(14) . . . . ?
C20 C11 C10 C1 122.2(11) . . . . ?
C12 C11 C10 C9 122.1(11) . . . . ?
C20 C11 C10 C9 -60.1(14) . . . . ?
C52 C53 C54 C55 -2.6(16) . . . . ?
C61 C53 C54 C55 171.0(10) . . . . ?
C60 C55 C54 C53 0.4(17) . . . . ?
C56 C55 C54 C53 -172.3(11) . . . . ?
C32 C33 C34 C35 -0.7(18) . . . . ?
C36 C35 C34 C33 -178.0(12) . . . . ?
C40 C35 C34 C33 0.1(17) . . . . ?
C55 C60 C59 C58 0.1(17) . . . . ?
C51 C60 C59 C58 -178.4(12) . . . . ?
C5 C4 C3 C2 -169.4(11) . . . . ?
C9 C4 C3 C2 2.6(17) . . . . ?
C1 C2 C3 C4 -3.8(16) . . . . ?
C31 C2 C3 C4 171.6(10) . . . . ?
C34 C33 C32 C31 0.5(18) . . . . ?
C49 C48 C47 C46 1.4(19) . . . . ?
C45 C46 C47 C48 1.0(19) . . . . ?
C77 C76 C75 C74 179.1(12) . . . . ?
C77 C76 C75 C80 -0.5(17) . . . . ?
C79 C80 C75 C74 179.0(11) . . . . ?
C71 C80 C75 C74 -2.5(15) . . . . ?
C79 C80 C75 C76 -1.4(14) . . . . ?
C71 C80 C75 C76 177.1(10) . . . . ?
C80 C71 C72 C73 0.3(16) . . . . ?
C42 C71 C72 C73 173.3(10) . . . . ?
C64 C65 C66 C67 179.1(12) . . . . ?
C70 C65 C66 C67 -0.9(18) . . . . ?
C39 C38 C37 C36 -0.2(17) . . . . ?
C37 C38 C39 C40 -0.3(17) . . . . ?
C31 C40 C39 C38 -178.4(10) . . . . ?
C35 C40 C39 C38 0.4(16) . . . . ?
C71 C72 C73 C74 -2.9(17) . . . . ?
C61 C62 C63 C64 1.1(19) . . . . ?
C67 C68 C69 C70 0.9(19) . . . . ?
C61 C70 C69 C68 -179.8(11) . . . . ?
C65 C70 C69 C68 -2.6(16) . . . . ?
C38 C37 C36 C35 0.5(17) . . . . ?
C40 C35 C36 C37 -0.4(18) . . . . ?
C34 C35 C36 C37 177.6(11) . . . . ?
C75 C76 C77 C78 2.5(19) . . . . ?
C33 C32 C31 C40 0.2(16) . . . . ?
C33 C32 C31 C2 -179.2(10) . . . . ?
C35 C40 C31 C32 -0.9(16) . . . . ?
C39 C40 C31 C32 177.9(10) . . . . ?
C35 C40 C31 C2 178.5(10) . . . . ?
C39 C40 C31 C2 -2.7(16) . . . . ?
C3 C2 C31 C32 -60.7(14) . . . . ?
C1 C2 C31 C32 114.4(12) . . . . ?
C3 C2 C31 C40 119.9(12) . . . . ?
C1 C2 C31 C40 -65.0(15) . . . . ?
C23 C22 C21 C30 178.0(12) . . . . ?
C27 C22 C21 C30 0.0(18) . . . . ?
C23 C22 C21 C13 6.6(18) . . . . ?
C27 C22 C21 C13 -171.4(10) . . . . ?
C14 C13 C21 C30 -67.8(15) . . . . ?
C12 C13 C21 C30 117.3(12) . . . . ?
C14 C13 C21 C22 103.7(12) . . . . ?
C12 C13 C21 C22 -71.2(14) . . . . ?
C6 C7 C8 C9 -5(2) . . . . ?
C10 C9 C8 C7 -172.4(12) . . . . ?
C4 C9 C8 C7 3.2(18) . . . . ?
C62 C63 C64 C65 -1(2) . . . . ?
C70 C65 C64 C63 0.7(18) . . . . ?
C66 C65 C64 C63 -179.2(12) . . . . ?
C76 C75 C74 C73 -179.6(11) . . . . ?
C80 C75 C74 C73 0.0(17) . . . . ?
C72 C73 C74 C75 2.7(17) . . . . ?
C58 C57 C56 C55 0(2) . . . . ?
C60 C55 C56 C57 0.4(18) . . . . ?
C54 C55 C56 C57 173.2(13) . . . . ?
C60 C59 C58 C57 0(2) . . . . ?
C56 C57 C58 C59 0(2) . . . . ?
C65 C66 C67 C68 -1(2) . . . . ?
C69 C68 C67 C66 1(2) . . . . ?
C80 C79 C78 C77 0.6(17) . . . . ?
C76 C77 C78 C79 -2.6(19) . . . . ?
C4 C5 C6 C7 -2(2) . . . . ?
C8 C7 C6 C5 5(2) . . . . ?
C18 C17 C16 C15 -1(2) . . . . ?
C14 C15 C16 C17 -179.1(12) . . . . ?
C20 C15 C16 C17 -0.8(18) . . . . ?
C21 C22 C23 C24 -175.2(13) . . . . ?
C27 C22 C23 C24 3(2) . . . . ?
C22 C21 C30 C29 2.1(18) . . . . ?
C13 C21 C30 C29 173.5(11) . . . . ?
C28 C29 C30 C21 -2(2) . . . . ?
C25 C26 C27 C28 177.8(16) . . . . ?
C25 C26 C27 C22 -1(2) . . . . ?
C23 C22 C27 C28 179.8(13) . . . . ?
C21 C22 C27 C28 -2.0(18) . . . . ?
C23 C22 C27 C26 -1.4(18) . . . . ?
C21 C22 C27 C26 176.8(12) . . . . ?
C30 C29 C28 C27 0(3) . . . . ?
C26 C27 C28 C29 -176.8(17) . . . . ?
C22 C27 C28 C29 2(2) . . . . ?
C27 C26 C25 C24 1(2) . . . . ?
C26 C25 C24 C23 0(2) . . . . ?
C22 C23 C24 C25 -2(2) . . . . ?

_refine_diff_density_max         0.758
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.083

_shelxl_version_number           2012-9
_database_code_depnum_ccdc_archive 'CCDC 1009078'
