# 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 2017

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1565898'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H64 Ca O6 P4, Cl14 Mo6, 2(C2 H3 N)'
_chemical_formula_sum            'C76 H70 Ca Cl14 Mo6 N2 O6 P4'
_chemical_formula_weight         2343.24

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   23.021(5)
_cell_length_b                   16.305(3)
_cell_length_c                   24.931(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.69(3)
_cell_angle_gamma                90.00
_cell_volume                     8864(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5765
_cell_measurement_theta_min      2.50
_cell_measurement_theta_max      31.94

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.17
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4632
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_T_max  0.7937
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           ?

_diffrn_ambient_temperature      150(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 Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            40747
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.56
_diffrn_reflns_theta_max         32.52
_reflns_number_total             15414
_reflns_number_gt                10680
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'

_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)+(0.0366P)²] 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         15414
_refine_ls_number_parameters     499
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0829
_refine_ls_wR_factor_gt          0.0757
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mo1 Mo 0.043348(9) 0.025546(12) 0.074033(7) 0.03230(5) Uani 1 1 d . . .
Mo2 Mo 0.036313(9) 0.086960(12) -0.024454(8) 0.03190(5) Uani 1 1 d . . .
Mo3 Mo 0.062604(9) -0.068081(12) -0.003586(8) 0.03197(5) Uani 1 1 d . . .
Ca1 Ca 0.5000 0.11151(4) 0.2500 0.02711(12) Uani 1 2 d S . .
Cl1 Cl 0.09871(3) 0.06148(5) 0.17145(3) 0.06011(19) Uani 1 1 d . . .
Cl2 Cl 0.08488(3) 0.20243(4) -0.05681(3) 0.05362(17) Uani 1 1 d . . .
Cl3 Cl 0.14275(3) -0.15996(4) -0.01113(3) 0.05125(16) Uani 1 1 d . . .
Cl4 Cl 0.01666(3) 0.17116(3) 0.05043(2) 0.04118(13) Uani 1 1 d . . .
Cl5 Cl 0.05315(3) -0.00579(4) -0.09666(2) 0.04134(13) Uani 1 1 d . . .
Cl6 Cl 0.06633(3) -0.12217(4) 0.09015(2) 0.04212(13) Uani 1 1 d . . .
Cl7 Cl 0.13488(3) 0.04214(4) 0.04389(2) 0.03964(13) Uani 1 1 d . . .
P1 P 0.33037(2) 0.10855(3) 0.23942(2) 0.03095(12) Uani 1 1 d . . .
P2 P 0.44545(3) -0.04138(4) 0.13315(2) 0.03660(13) Uani 1 1 d . . .
O1 O 0.39738(7) 0.10767(10) 0.24649(7) 0.0403(4) Uani 1 1 d . . .
O1W O 0.51118(9) 0.22434(12) 0.31491(8) 0.0582(5) Uani 1 1 d D . .
O2 O 0.47362(8) 0.02270(10) 0.17651(7) 0.0463(4) Uani 1 1 d . . .
N1 N 0.4351(3) 0.3563(3) 0.2712(2) 0.200(3) Uani 1 1 d . . .
C1 C 0.4077(3) 0.3994(4) 0.2436(3) 0.140(2) Uani 1 1 d . . .
C2 C 0.3705(3) 0.4670(4) 0.2028(2) 0.164(2) Uani 1 1 d . . .
H2A H 0.3925 0.5194 0.2118 0.246 Uiso 1 1 calc R . .
H2B H 0.3300 0.4726 0.2074 0.246 Uiso 1 1 calc R . .
H2C H 0.3658 0.4517 0.1636 0.246 Uiso 1 1 calc R . .
C111 C 0.28958(10) 0.18061(14) 0.18558(9) 0.0348(5) Uani 1 1 d . . .
C112 C 0.22663(11) 0.18083(16) 0.16312(10) 0.0464(6) Uani 1 1 d . . .
H112 H 0.2034 0.1421 0.1763 0.056 Uiso 1 1 calc R . .
C113 C 0.19661(13) 0.23658(19) 0.12170(12) 0.0603(8) Uani 1 1 d . . .
H113 H 0.1531 0.2365 0.1068 0.072 Uiso 1 1 calc R . .
C114 C 0.22986(15) 0.2917(2) 0.10235(12) 0.0674(9) Uani 1 1 d . . .
H114 H 0.2093 0.3298 0.0737 0.081 Uiso 1 1 calc R . .
C115 C 0.29300(15) 0.29258(19) 0.12394(13) 0.0694(9) Uani 1 1 d . . .
H115 H 0.3158 0.3311 0.1103 0.083 Uiso 1 1 calc R . .
C116 C 0.32287(12) 0.23719(16) 0.16556(11) 0.0506(6) Uani 1 1 d . . .
H116 H 0.3664 0.2378 0.1806 0.061 Uiso 1 1 calc R . .
C121 C 0.29217(10) 0.01117(13) 0.22001(9) 0.0324(4) Uani 1 1 d . . .
C122 C 0.28763(13) -0.04329(15) 0.26143(10) 0.0468(6) Uani 1 1 d . . .
H122 H 0.3046 -0.0293 0.3003 0.056 Uiso 1 1 calc R . .
C123 C 0.25875(15) -0.11691(17) 0.24618(12) 0.0610(8) Uani 1 1 d . . .
H123 H 0.2552 -0.1531 0.2748 0.073 Uiso 1 1 calc R . .
C124 C 0.23476(13) -0.13990(16) 0.19046(12) 0.0557(7) Uani 1 1 d . . .
H124 H 0.2146 -0.1912 0.1806 0.067 Uiso 1 1 calc R . .
C125 C 0.24045(12) -0.08738(16) 0.14905(11) 0.0499(6) Uani 1 1 d . . .
H125 H 0.2247 -0.1030 0.1104 0.060 Uiso 1 1 calc R . .
C126 C 0.26890(11) -0.01231(15) 0.16347(9) 0.0397(5) Uani 1 1 d . . .
H126 H 0.2726 0.0235 0.1347 0.048 Uiso 1 1 calc R . .
C131 C 0.31715(10) 0.13712(13) 0.30468(9) 0.0352(5) Uani 1 1 d . . .
C132 C 0.36545(12) 0.16333(15) 0.34997(9) 0.0430(6) Uani 1 1 d . . .
H132 H 0.4055 0.1661 0.3469 0.052 Uiso 1 1 calc R . .
C133 C 0.35595(14) 0.18582(17) 0.40022(10) 0.0551(7) Uani 1 1 d . . .
H133 H 0.3893 0.2052 0.4311 0.066 Uiso 1 1 calc R . .
C134 C 0.29907(16) 0.18021(18) 0.40540(11) 0.0632(8) Uani 1 1 d . . .
H134 H 0.2931 0.1945 0.4402 0.076 Uiso 1 1 calc R . .
C135 C 0.25011(15) 0.1540(2) 0.36080(12) 0.0660(8) Uani 1 1 d . . .
H135 H 0.2104 0.1505 0.3646 0.079 Uiso 1 1 calc R . .
C136 C 0.25901(12) 0.13296(18) 0.31045(11) 0.0524(7) Uani 1 1 d . . .
H136 H 0.2251 0.1154 0.2794 0.063 Uiso 1 1 calc R . .
C211 C 0.37379(11) -0.00662(15) 0.08451(9) 0.0396(5) Uani 1 1 d . . .
C212 C 0.33068(12) -0.05947(18) 0.05043(11) 0.0531(7) Uani 1 1 d . . .
H212 H 0.3379 -0.1169 0.0529 0.064 Uiso 1 1 calc R . .
C213 C 0.27686(13) -0.0287(2) 0.01252(12) 0.0653(9) Uani 1 1 d . . .
H213 H 0.2475 -0.0649 -0.0114 0.078 Uiso 1 1 calc R . .
C214 C 0.26619(14) 0.0543(2) 0.00969(12) 0.0673(9) Uani 1 1 d . . .
H214 H 0.2292 0.0750 -0.0161 0.081 Uiso 1 1 calc R . .
C215 C 0.30829(14) 0.1079(2) 0.04360(12) 0.0602(8) Uani 1 1 d . . .
H215 H 0.3006 0.1653 0.0414 0.072 Uiso 1 1 calc R . .
C216 C 0.36207(12) 0.07699(17) 0.08098(11) 0.0474(6) Uani 1 1 d . . .
H216 H 0.3914 0.1136 0.1046 0.057 Uiso 1 1 calc R . .
C221 C 0.43169(11) -0.13445(15) 0.16534(9) 0.0406(5) Uani 1 1 d . . .
C222 C 0.43507(17) -0.21068(19) 0.14311(13) 0.0726(10) Uani 1 1 d . . .
H222 H 0.4438 -0.2156 0.1085 0.087 Uiso 1 1 calc R . .
C223 C 0.4258(2) -0.2804(2) 0.17095(15) 0.0953(13) Uani 1 1 d . . .
H223 H 0.4287 -0.3330 0.1556 0.114 Uiso 1 1 calc R . .
C224 C 0.41260(17) -0.2737(2) 0.22034(15) 0.0805(10) Uani 1 1 d . . .
H224 H 0.4058 -0.3217 0.2391 0.097 Uiso 1 1 calc R . .
C225 C 0.40911(15) -0.1984(2) 0.24299(13) 0.0694(9) Uani 1 1 d . . .
H225 H 0.4006 -0.1941 0.2777 0.083 Uiso 1 1 calc R . .
C226 C 0.41805(13) -0.12822(18) 0.21523(11) 0.0536(7) Uani 1 1 d . . .
H226 H 0.4148 -0.0757 0.2306 0.064 Uiso 1 1 calc R . .
C231 C 0.49503(11) -0.06440(15) 0.09230(9) 0.0381(5) Uani 1 1 d . . .
C232 C 0.55594(13) -0.0441(2) 0.11532(11) 0.0635(9) Uani 1 1 d . . .
H232 H 0.5703 -0.0190 0.1516 0.076 Uiso 1 1 calc R . .
C233 C 0.59641(14) -0.0603(3) 0.08570(13) 0.0873(12) Uani 1 1 d . . .
H233 H 0.6383 -0.0452 0.1013 0.105 Uiso 1 1 calc R . .
C234 C 0.57577(14) -0.0981(2) 0.03365(12) 0.0692(9) Uani 1 1 d . . .
H234 H 0.6039 -0.1114 0.0142 0.083 Uiso 1 1 calc R . .
C235 C 0.51569(14) -0.11653(19) 0.01011(11) 0.0577(7) Uani 1 1 d . . .
H235 H 0.5016 -0.1410 -0.0264 0.069 Uiso 1 1 calc R . .
C236 C 0.47466(13) -0.10005(17) 0.03876(11) 0.0530(7) Uani 1 1 d . . .
H236 H 0.4325 -0.1131 0.0219 0.064 Uiso 1 1 calc R . .
H1W H 0.4856(10) 0.2624(13) 0.3012(9) 0.050 Uiso 1 1 d D . .
H2W H 0.5309(10) 0.2335(15) 0.3492(7) 0.050 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
Mo1 Cl1 2.4254(10) . ?
Mo1 Cl7 2.4684(8) . ?
Mo1 Cl6 2.4710(8) . ?
Mo1 Cl4 2.4756(8) . ?
Mo1 Cl5 2.4818(8) 5 ?
Mo1 Mo3 2.6018(9) 5 ?
Mo1 Mo2 2.6082(5) . ?
Mo1 Mo2 2.6083(6) 5 ?
Mo1 Mo3 2.6117(5) . ?
Mo2 Cl2 2.4542(7) . ?
Mo2 Cl7 2.4715(10) . ?
Mo2 Cl6 2.4729(11) 5 ?
Mo2 Cl4 2.4731(7) . ?
Mo2 Cl5 2.4747(7) . ?
Mo2 Mo3 2.6056(6) 5 ?
Mo2 Mo1 2.6083(6) 5 ?
Mo2 Mo3 2.6125(6) . ?
Mo3 Cl3 2.4302(7) . ?
Mo3 Cl6 2.4733(7) . ?
Mo3 Cl7 2.4773(8) . ?
Mo3 Cl5 2.4777(7) . ?
Mo3 Cl4 2.4804(8) 5 ?
Mo3 Mo1 2.6018(9) 5 ?
Mo3 Mo2 2.6056(6) 5 ?
Ca1 O2 2.2604(16) . ?
Ca1 O2 2.2604(16) 2_655 ?
Ca1 O1 2.3368(16) 2_655 ?
Ca1 O1 2.3368(16) . ?
Ca1 O1W 2.4087(18) . ?
Ca1 O1W 2.4087(18) 2_655 ?
Cl4 Mo3 2.4804(8) 5 ?
Cl5 Mo1 2.4818(8) 5 ?
Cl6 Mo2 2.4729(11) 5 ?
P1 O1 1.4955(16) . ?
P1 C111 1.804(2) . ?
P1 C121 1.804(2) . ?
P1 C131 1.809(2) . ?
P2 O2 1.4938(16) . ?
P2 C221 1.792(3) . ?
P2 C231 1.796(2) . ?
P2 C211 1.798(3) . ?
O1W H1W 0.849(15) . ?
O1W H2W 0.844(15) . ?
N1 C1 1.042(7) . ?
C1 C2 1.557(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C111 C112 1.376(3) . ?
C111 C116 1.390(3) . ?
C112 C113 1.383(3) . ?
C112 H112 0.9500 . ?
C113 C114 1.364(4) . ?
C113 H113 0.9500 . ?
C114 C115 1.379(4) . ?
C114 H114 0.9500 . ?
C115 C116 1.381(4) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C121 C122 1.391(3) . ?
C121 C126 1.392(3) . ?
C122 C123 1.366(4) . ?
C122 H122 0.9500 . ?
C123 C124 1.372(4) . ?
C123 H123 0.9500 . ?
C124 C125 1.380(4) . ?
C124 H124 0.9500 . ?
C125 C126 1.380(3) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C131 C132 1.374(3) . ?
C131 C136 1.393(3) . ?
C132 C133 1.388(3) . ?
C132 H132 0.9500 . ?
C133 C134 1.359(4) . ?
C133 H133 0.9500 . ?
C134 C135 1.373(4) . ?
C134 H134 0.9500 . ?
C135 C136 1.378(3) . ?
C135 H135 0.9500 . ?
C136 H136 0.9500 . ?
C211 C212 1.382(3) . ?
C211 C216 1.387(3) . ?
C212 C213 1.389(4) . ?
C212 H212 0.9500 . ?
C213 C214 1.372(5) . ?
C213 H213 0.9500 . ?
C214 C215 1.376(4) . ?
C214 H214 0.9500 . ?
C215 C216 1.384(4) . ?
C215 H215 0.9500 . ?
C216 H216 0.9500 . ?
C221 C222 1.373(4) . ?
C221 C226 1.381(3) . ?
C222 C223 1.383(4) . ?
C222 H222 0.9500 . ?
C223 C224 1.364(4) . ?
C223 H223 0.9500 . ?
C224 C225 1.363(5) . ?
C224 H224 0.9500 . ?
C225 C226 1.387(4) . ?
C225 H225 0.9500 . ?
C226 H226 0.9500 . ?
C231 C232 1.374(4) . ?
C231 C236 1.392(3) . ?
C232 C233 1.387(4) . ?
C232 H232 0.9500 . ?
C233 C234 1.377(4) . ?
C233 H233 0.9500 . ?
C234 C235 1.352(4) . ?
C234 H234 0.9500 . ?
C235 C236 1.381(3) . ?
C235 H235 0.9500 . ?
C236 H236 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Mo1 Cl7 93.01(3) . . ?
Cl1 Mo1 Cl6 93.22(3) . . ?
Cl7 Mo1 Cl6 89.84(2) . . ?
Cl1 Mo1 Cl4 90.98(3) . . ?
Cl7 Mo1 Cl4 89.63(2) . . ?
Cl6 Mo1 Cl4 175.79(2) . . ?
Cl1 Mo1 Cl5 91.44(3) . 5 ?
Cl7 Mo1 Cl5 175.548(19) . 5 ?
Cl6 Mo1 Cl5 89.84(2) . 5 ?
Cl4 Mo1 Cl5 90.37(2) . 5 ?
Cl1 Mo1 Mo3 133.61(3) . 5 ?
Cl7 Mo1 Mo3 118.19(2) . 5 ?
Cl6 Mo1 Mo3 118.367(16) . 5 ?
Cl4 Mo1 Mo3 58.424(15) . 5 ?
Cl5 Mo1 Mo3 58.28(2) 5 5 ?
Cl1 Mo1 Mo2 134.76(2) . . ?
Cl7 Mo1 Mo2 58.19(3) . . ?
Cl6 Mo1 Mo2 118.212(17) . . ?
Cl4 Mo1 Mo2 58.148(16) . . ?
Cl5 Mo1 Mo2 118.27(3) 5 . ?
Mo3 Mo1 Mo2 60.01(2) 5 . ?
Cl1 Mo1 Mo2 135.11(2) . 5 ?
Cl7 Mo1 Mo2 118.163(19) . 5 ?
Cl6 Mo1 Mo2 58.19(2) . 5 ?
Cl4 Mo1 Mo2 118.59(2) . 5 ?
Cl5 Mo1 Mo2 58.117(18) 5 5 ?
Mo3 Mo1 Mo2 60.19(2) 5 5 ?
Mo2 Mo1 Mo2 90.10(2) . 5 ?
Cl1 Mo1 Mo3 136.36(2) . . ?
Cl7 Mo1 Mo3 58.29(2) . . ?
Cl6 Mo1 Mo3 58.159(17) . . ?
Cl4 Mo1 Mo3 118.202(19) . . ?
Cl5 Mo1 Mo3 117.99(2) 5 . ?
Mo3 Mo1 Mo3 90.03(2) 5 . ?
Mo2 Mo1 Mo3 60.065(15) . . ?
Mo2 Mo1 Mo3 59.887(16) 5 . ?
Cl2 Mo2 Cl7 92.24(3) . . ?
Cl2 Mo2 Cl6 92.49(3) . 5 ?
Cl7 Mo2 Cl6 175.27(2) . 5 ?
Cl2 Mo2 Cl4 92.01(3) . . ?
Cl7 Mo2 Cl4 89.62(3) . . ?
Cl6 Mo2 Cl4 90.23(3) 5 . ?
Cl2 Mo2 Cl5 92.05(3) . . ?
Cl7 Mo2 Cl5 89.86(3) . . ?
Cl6 Mo2 Cl5 89.95(3) 5 . ?
Cl4 Mo2 Cl5 175.93(2) . . ?
Cl2 Mo2 Mo3 135.08(2) . 5 ?
Cl7 Mo2 Mo3 117.93(2) . 5 ?
Cl6 Mo2 Mo3 58.22(2) 5 5 ?
Cl4 Mo2 Mo3 58.40(2) . 5 ?
Cl5 Mo2 Mo3 118.49(2) . 5 ?
Cl2 Mo2 Mo1 134.95(2) . . ?
Cl7 Mo2 Mo1 58.07(2) . . ?
Cl6 Mo2 Mo1 118.07(3) 5 . ?
Cl4 Mo2 Mo1 58.24(2) . . ?
Cl5 Mo2 Mo1 118.24(2) . . ?
Mo3 Mo2 Mo1 59.87(2) 5 . ?
Cl2 Mo2 Mo1 135.15(2) . 5 ?
Cl7 Mo2 Mo1 118.01(2) . 5 ?
Cl6 Mo2 Mo1 58.12(2) 5 5 ?
Cl4 Mo2 Mo1 118.50(2) . 5 ?
Cl5 Mo2 Mo1 58.38(2) . 5 ?
Mo3 Mo2 Mo1 60.122(13) 5 5 ?
Mo1 Mo2 Mo1 89.90(2) . 5 ?
Cl2 Mo2 Mo3 134.98(2) . . ?
Cl7 Mo2 Mo3 58.244(15) . . ?
Cl6 Mo2 Mo3 117.887(16) 5 . ?
Cl4 Mo2 Mo3 118.262(19) . . ?
Cl5 Mo2 Mo3 58.217(18) . . ?
Mo3 Mo2 Mo3 89.936(10) 5 . ?
Mo1 Mo2 Mo3 60.034(10) . . ?
Mo1 Mo2 Mo3 59.783(19) 5 . ?
Cl3 Mo3 Cl6 93.21(3) . . ?
Cl3 Mo3 Cl7 94.23(3) . . ?
Cl6 Mo3 Cl7 89.58(3) . . ?
Cl3 Mo3 Cl5 91.22(3) . . ?
Cl6 Mo3 Cl5 175.55(2) . . ?
Cl7 Mo3 Cl5 89.66(3) . . ?
Cl3 Mo3 Cl4 90.46(3) . 5 ?
Cl6 Mo3 Cl4 90.05(3) . 5 ?
Cl7 Mo3 Cl4 175.30(2) . 5 ?
Cl5 Mo3 Cl4 90.35(3) . 5 ?
Cl3 Mo3 Mo1 133.06(2) . 5 ?
Cl6 Mo3 Mo1 118.30(3) . 5 ?
Cl7 Mo3 Mo1 118.03(2) . 5 ?
Cl5 Mo3 Mo1 58.43(3) . 5 ?
Cl4 Mo3 Mo1 58.24(2) 5 5 ?
Cl3 Mo3 Mo2 134.30(2) . 5 ?
Cl6 Mo3 Mo2 58.20(3) . 5 ?
Cl7 Mo3 Mo2 117.936(19) . 5 ?
Cl5 Mo3 Mo2 118.53(3) . 5 ?
Cl4 Mo3 Mo2 58.128(18) 5 5 ?
Mo1 Mo3 Mo2 60.115(16) 5 5 ?
Cl3 Mo3 Mo1 136.97(3) . . ?
Cl6 Mo3 Mo1 58.07(2) . . ?
Cl7 Mo3 Mo1 57.96(2) . . ?
Cl5 Mo3 Mo1 118.00(2) . . ?
Cl4 Mo3 Mo1 118.10(2) 5 . ?
Mo1 Mo3 Mo1 89.97(2) 5 . ?
Mo2 Mo3 Mo1 59.991(19) 5 . ?
Cl3 Mo3 Mo2 135.58(2) . . ?
Cl6 Mo3 Mo2 117.959(17) . . ?
Cl7 Mo3 Mo2 58.03(2) . . ?
Cl5 Mo3 Mo2 58.105(16) . . ?
Cl4 Mo3 Mo2 118.25(2) 5 . ?
Mo1 Mo3 Mo2 60.027(7) 5 . ?
Mo2 Mo3 Mo2 90.064(10) 5 . ?
Mo1 Mo3 Mo2 59.901(13) . . ?
O2 Ca1 O2 100.32(9) . 2_655 ?
O2 Ca1 O1 91.09(7) . 2_655 ?
O2 Ca1 O1 86.94(6) 2_655 2_655 ?
O2 Ca1 O1 86.94(6) . . ?
O2 Ca1 O1 91.09(6) 2_655 . ?
O1 Ca1 O1 176.93(8) 2_655 . ?
O2 Ca1 O1W 167.66(7) . . ?
O2 Ca1 O1W 90.09(7) 2_655 . ?
O1 Ca1 O1W 96.10(7) 2_655 . ?
O1 Ca1 O1W 86.26(7) . . ?
O2 Ca1 O1W 90.09(7) . 2_655 ?
O2 Ca1 O1W 167.66(7) 2_655 2_655 ?
O1 Ca1 O1W 86.26(7) 2_655 2_655 ?
O1 Ca1 O1W 96.10(7) . 2_655 ?
O1W Ca1 O1W 80.42(11) . 2_655 ?
Mo2 Cl4 Mo1 63.613(18) . . ?
Mo2 Cl4 Mo3 63.47(2) . 5 ?
Mo1 Cl4 Mo3 63.33(2) . 5 ?
Mo2 Cl5 Mo3 63.68(2) . . ?
Mo2 Cl5 Mo1 63.50(2) . 5 ?
Mo3 Cl5 Mo1 63.29(3) . 5 ?
Mo1 Cl6 Mo2 63.684(15) . 5 ?
Mo1 Cl6 Mo3 63.772(16) . . ?
Mo2 Cl6 Mo3 63.58(3) 5 . ?
Mo1 Cl7 Mo2 63.74(2) . . ?
Mo1 Cl7 Mo3 63.751(18) . . ?
Mo2 Cl7 Mo3 63.73(2) . . ?
O1 P1 C111 111.42(10) . . ?
O1 P1 C121 114.77(10) . . ?
C111 P1 C121 106.30(10) . . ?
O1 P1 C131 111.15(10) . . ?
C111 P1 C131 107.69(10) . . ?
C121 P1 C131 105.06(10) . . ?
O2 P2 C221 111.48(11) . . ?
O2 P2 C231 110.43(11) . . ?
C221 P2 C231 108.22(11) . . ?
O2 P2 C211 111.07(11) . . ?
C221 P2 C211 108.26(11) . . ?
C231 P2 C211 107.22(11) . . ?
P1 O1 Ca1 175.15(10) . . ?
Ca1 O1W H1W 112.2(16) . . ?
Ca1 O1W H2W 136.4(17) . . ?
H1W O1W H2W 111(2) . . ?
P2 O2 Ca1 167.48(11) . . ?
N1 C1 C2 176.3(9) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C112 C111 C116 118.8(2) . . ?
C112 C111 P1 122.25(18) . . ?
C116 C111 P1 118.93(18) . . ?
C111 C112 C113 121.0(2) . . ?
C111 C112 H112 119.5 . . ?
C113 C112 H112 119.5 . . ?
C114 C113 C112 119.6(3) . . ?
C114 C113 H113 120.2 . . ?
C112 C113 H113 120.2 . . ?
C113 C114 C115 120.6(3) . . ?
C113 C114 H114 119.7 . . ?
C115 C114 H114 119.7 . . ?
C114 C115 C116 119.7(3) . . ?
C114 C115 H115 120.2 . . ?
C116 C115 H115 120.2 . . ?
C115 C116 C111 120.3(3) . . ?
C115 C116 H116 119.8 . . ?
C111 C116 H116 119.8 . . ?
C122 C121 C126 118.7(2) . . ?
C122 C121 P1 120.58(17) . . ?
C126 C121 P1 120.67(17) . . ?
C123 C122 C121 120.0(2) . . ?
C123 C122 H122 120.0 . . ?
C121 C122 H122 120.0 . . ?
C122 C123 C124 121.6(2) . . ?
C122 C123 H123 119.2 . . ?
C124 C123 H123 119.2 . . ?
C123 C124 C125 119.0(2) . . ?
C123 C124 H124 120.5 . . ?
C125 C124 H124 120.5 . . ?
C124 C125 C126 120.4(2) . . ?
C124 C125 H125 119.8 . . ?
C126 C125 H125 119.8 . . ?
C125 C126 C121 120.3(2) . . ?
C125 C126 H126 119.9 . . ?
C121 C126 H126 119.9 . . ?
C132 C131 C136 118.8(2) . . ?
C132 C131 P1 119.60(19) . . ?
C136 C131 P1 121.63(18) . . ?
C131 C132 C133 120.2(3) . . ?
C131 C132 H132 119.9 . . ?
C133 C132 H132 119.9 . . ?
C134 C133 C132 120.2(3) . . ?
C134 C133 H133 119.9 . . ?
C132 C133 H133 119.9 . . ?
C133 C134 C135 120.6(3) . . ?
C133 C134 H134 119.7 . . ?
C135 C134 H134 119.7 . . ?
C134 C135 C136 119.5(3) . . ?
C134 C135 H135 120.3 . . ?
C136 C135 H135 120.3 . . ?
C135 C136 C131 120.7(3) . . ?
C135 C136 H136 119.7 . . ?
C131 C136 H136 119.7 . . ?
C212 C211 C216 119.2(2) . . ?
C212 C211 P2 122.8(2) . . ?
C216 C211 P2 118.07(19) . . ?
C211 C212 C213 120.1(3) . . ?
C211 C212 H212 120.0 . . ?
C213 C212 H212 120.0 . . ?
C214 C213 C212 119.8(3) . . ?
C214 C213 H213 120.1 . . ?
C212 C213 H213 120.1 . . ?
C213 C214 C215 121.0(3) . . ?
C213 C214 H214 119.5 . . ?
C215 C214 H214 119.5 . . ?
C214 C215 C216 118.9(3) . . ?
C214 C215 H215 120.5 . . ?
C216 C215 H215 120.5 . . ?
C215 C216 C211 121.0(3) . . ?
C215 C216 H216 119.5 . . ?
C211 C216 H216 119.5 . . ?
C222 C221 C226 119.3(3) . . ?
C222 C221 P2 123.0(2) . . ?
C226 C221 P2 117.7(2) . . ?
C221 C222 C223 120.2(3) . . ?
C221 C222 H222 119.9 . . ?
C223 C222 H222 119.9 . . ?
C224 C223 C222 120.1(3) . . ?
C224 C223 H223 119.9 . . ?
C222 C223 H223 119.9 . . ?
C225 C224 C223 120.4(3) . . ?
C225 C224 H224 119.8 . . ?
C223 C224 H224 119.8 . . ?
C224 C225 C226 119.9(3) . . ?
C224 C225 H225 120.1 . . ?
C226 C225 H225 120.1 . . ?
C221 C226 C225 120.1(3) . . ?
C221 C226 H226 119.9 . . ?
C225 C226 H226 119.9 . . ?
C232 C231 C236 119.1(2) . . ?
C232 C231 P2 117.48(19) . . ?
C236 C231 P2 123.42(19) . . ?
C231 C232 C233 120.1(3) . . ?
C231 C232 H232 120.0 . . ?
C233 C232 H232 120.0 . . ?
C234 C233 C232 119.9(3) . . ?
C234 C233 H233 120.0 . . ?
C232 C233 H233 120.0 . . ?
C235 C234 C233 120.3(3) . . ?
C235 C234 H234 119.8 . . ?
C233 C234 H234 119.8 . . ?
C234 C235 C236 120.4(3) . . ?
C234 C235 H235 119.8 . . ?
C236 C235 H235 119.8 . . ?
C235 C236 C231 120.1(3) . . ?
C235 C236 H236 120.0 . . ?
C231 C236 H236 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.959
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.085
####################################################################### 
# 
# 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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1565900'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Cl14 W6, C72 H60 Ca O4 P4'
_chemical_formula_sum            'C72 H60 Ca Cl14 O4 P4 W6'
_chemical_formula_weight         2752.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   25.3726(10)
_cell_length_b                   14.1362(6)
_cell_length_c                   24.2685(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 113.2120(10)
_cell_angle_gamma                90.00
_cell_volume                     7999.8(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6008
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      27.47

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5144
_exptl_absorpt_coefficient_mu    9.251
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2591
_exptl_absorpt_correction_T_max  0.3375
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            26998
_diffrn_reflns_av_R_equivalents  0.0496
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         27.51
_reflns_number_total             9037
_reflns_number_gt                6061
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'

_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)+(0.0309P)²] 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_number_reflns         9037
_refine_ls_number_parameters     458
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.0818
_refine_ls_wR_factor_gt          0.0739
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_restrained_S_all      0.980
_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
W1 W 0.0000 0.73811(3) 0.2500 0.01358(9) Uani 1 2 d S . .
W2 W 0.079232(11) 0.867669(19) 0.285619(11) 0.01382(7) Uani 1 1 d . . .
W3 W 0.002979(11) 0.869265(19) 0.175162(11) 0.01339(7) Uani 1 1 d . . .
W4 W 0.0000 0.99853(2) 0.2500 0.01265(9) Uani 1 2 d S . .
Ca1 Ca 0.0000 0.36781(12) 0.2500 0.0095(3) Uani 1 2 d S . .
Cl1 Cl 0.0000 0.56468(17) 0.2500 0.0351(7) Uani 1 2 d S . .
Cl2 Cl 0.18312(7) 0.86035(15) 0.33304(9) 0.0321(4) Uani 1 1 d . . .
Cl3 Cl 0.00728(9) 0.87922(14) 0.07815(8) 0.0333(5) Uani 1 1 d . . .
Cl5 Cl 0.07205(7) 0.74300(12) 0.35589(8) 0.0212(4) Uani 1 1 d . . .
Cl4 Cl 0.0000 1.17146(17) 0.2500 0.0323(7) Uani 1 2 d S . .
Cl6 Cl 0.07793(7) 0.74387(11) 0.21096(8) 0.0201(4) Uani 1 1 d . . .
Cl7 Cl 0.07343(7) 0.99365(12) 0.35456(8) 0.0202(4) Uani 1 1 d . . .
Cl8 Cl 0.07970(7) 0.99390(11) 0.21359(8) 0.0185(4) Uani 1 1 d . . .
P1 P 0.09562(7) 0.40051(12) 0.16897(8) 0.0149(4) Uani 1 1 d . . .
P2 P 0.13111(7) 0.32841(12) 0.38714(8) 0.0146(4) Uani 1 1 d . . .
O1 O 0.05697(18) 0.3624(3) 0.19744(19) 0.0167(10) Uani 1 1 d . . .
O2 O 0.07811(18) 0.3649(3) 0.33769(19) 0.0169(10) Uani 1 1 d . . .
C111 C 0.0612(3) 0.4944(4) 0.1170(3) 0.0149(14) Uani 1 1 d . . .
C112 C 0.0014(3) 0.5018(5) 0.0950(3) 0.0210(16) Uani 1 1 d . . .
H112 H -0.0203 0.4585 0.1075 0.025 Uiso 1 1 calc R . .
C113 C -0.0257(3) 0.5730(5) 0.0547(3) 0.0248(17) Uani 1 1 d . . .
H113 H -0.0662 0.5787 0.0399 0.030 Uiso 1 1 calc R . .
C114 C 0.0054(3) 0.6364(5) 0.0356(3) 0.0306(18) Uani 1 1 d . . .
H114 H -0.0139 0.6847 0.0077 0.037 Uiso 1 1 calc R . .
C115 C 0.0649(3) 0.6288(5) 0.0575(3) 0.0273(17) Uani 1 1 d . . .
H115 H 0.0865 0.6721 0.0447 0.033 Uiso 1 1 calc R . .
C116 C 0.0924(3) 0.5583(5) 0.0979(3) 0.0238(17) Uani 1 1 d . . .
H116 H 0.1329 0.5531 0.1129 0.029 Uiso 1 1 calc R . .
C121 C 0.1607(3) 0.4498(5) 0.2220(3) 0.0161(15) Uani 1 1 d . . .
C122 C 0.1551(3) 0.5286(5) 0.2546(3) 0.0233(17) Uani 1 1 d . . .
H122 H 0.1182 0.5528 0.2482 0.028 Uiso 1 1 calc R . .
C123 C 0.2043(4) 0.5707(6) 0.2965(3) 0.037(2) Uani 1 1 d . . .
H123 H 0.2010 0.6249 0.3180 0.044 Uiso 1 1 calc R . .
C124 C 0.2576(3) 0.5343(7) 0.3067(3) 0.037(2) Uani 1 1 d . . .
H124 H 0.2908 0.5629 0.3358 0.045 Uiso 1 1 calc R . .
C125 C 0.2631(3) 0.4572(6) 0.2754(4) 0.034(2) Uani 1 1 d . . .
H125 H 0.3002 0.4329 0.2826 0.040 Uiso 1 1 calc R . .
C126 C 0.2145(3) 0.4137(5) 0.2326(3) 0.0255(17) Uani 1 1 d . . .
H126 H 0.2185 0.3598 0.2112 0.031 Uiso 1 1 calc R . .
C131 C 0.1126(3) 0.3062(4) 0.1278(3) 0.0134(14) Uani 1 1 d . . .
C132 C 0.1386(3) 0.3249(5) 0.0884(3) 0.0279(18) Uani 1 1 d . . .
H132 H 0.1507 0.3874 0.0848 0.033 Uiso 1 1 calc R . .
C133 C 0.1471(3) 0.2520(6) 0.0539(4) 0.032(2) Uani 1 1 d . . .
H133 H 0.1656 0.2642 0.0273 0.039 Uiso 1 1 calc R . .
C134 C 0.1283(3) 0.1624(5) 0.0589(3) 0.0265(18) Uani 1 1 d . . .
H134 H 0.1324 0.1131 0.0343 0.032 Uiso 1 1 calc R . .
C135 C 0.1038(3) 0.1432(5) 0.0985(3) 0.0223(16) Uani 1 1 d . . .
H135 H 0.0924 0.0804 0.1025 0.027 Uiso 1 1 calc R . .
C136 C 0.0955(3) 0.2154(5) 0.1331(3) 0.0189(15) Uani 1 1 d . . .
H136 H 0.0780 0.2021 0.1604 0.023 Uiso 1 1 calc R . .
C211 C 0.1156(3) 0.2342(4) 0.4280(3) 0.0159(15) Uani 1 1 d . . .
C212 C 0.0611(3) 0.2276(5) 0.4286(3) 0.0185(15) Uani 1 1 d . . .
H212 H 0.0321 0.2715 0.4065 0.022 Uiso 1 1 calc R . .
C213 C 0.0492(3) 0.1565(5) 0.4616(3) 0.0217(16) Uani 1 1 d . . .
H213 H 0.0123 0.1529 0.4629 0.026 Uiso 1 1 calc R . .
C214 C 0.0910(3) 0.0908(5) 0.4927(3) 0.0237(17) Uani 1 1 d . . .
H214 H 0.0824 0.0417 0.5145 0.028 Uiso 1 1 calc R . .
C215 C 0.1449(3) 0.0964(5) 0.4920(3) 0.0248(17) Uani 1 1 d . . .
H215 H 0.1735 0.0519 0.5139 0.030 Uiso 1 1 calc R . .
C216 C 0.1574(3) 0.1680(5) 0.4590(3) 0.0217(16) Uani 1 1 d . . .
H216 H 0.1944 0.1713 0.4578 0.026 Uiso 1 1 calc R . .
C221 C 0.1818(3) 0.2804(5) 0.3603(3) 0.0164(15) Uani 1 1 d . . .
C222 C 0.1642(3) 0.2105(6) 0.3170(4) 0.0307(19) Uani 1 1 d . . .
H222 H 0.1250 0.1921 0.3005 0.037 Uiso 1 1 calc R . .
C223 C 0.2023(4) 0.1668(6) 0.2974(4) 0.040(2) Uani 1 1 d . . .
H223 H 0.1894 0.1193 0.2673 0.048 Uiso 1 1 calc R . .
C224 C 0.2590(3) 0.1926(6) 0.3214(4) 0.034(2) Uani 1 1 d . . .
H224 H 0.2854 0.1624 0.3082 0.041 Uiso 1 1 calc R . .
C225 C 0.2778(3) 0.2619(6) 0.3644(3) 0.032(2) Uani 1 1 d . . .
H225 H 0.3169 0.2806 0.3803 0.039 Uiso 1 1 calc R . .
C226 C 0.2395(3) 0.3044(5) 0.3847(3) 0.0214(16) Uani 1 1 d . . .
H226 H 0.2529 0.3504 0.4157 0.026 Uiso 1 1 calc R . .
C231 C 0.1671(3) 0.4224(5) 0.4395(3) 0.0163(15) Uani 1 1 d . . .
C232 C 0.1941(3) 0.4067(5) 0.5002(3) 0.0211(16) Uani 1 1 d . . .
H232 H 0.1920 0.3466 0.5166 0.025 Uiso 1 1 calc R . .
C233 C 0.2248(3) 0.4805(5) 0.5374(3) 0.0285(18) Uani 1 1 d . . .
H233 H 0.2442 0.4697 0.5793 0.034 Uiso 1 1 calc R . .
C234 C 0.2273(3) 0.5686(5) 0.5142(3) 0.0299(19) Uani 1 1 d . . .
H234 H 0.2488 0.6182 0.5395 0.036 Uiso 1 1 calc R . .
C235 C 0.1978(3) 0.5833(5) 0.4532(3) 0.0293(19) Uani 1 1 d . . .
H235 H 0.1981 0.6442 0.4368 0.035 Uiso 1 1 calc R . .
C236 C 0.1680(3) 0.5104(5) 0.4158(3) 0.0277(18) Uani 1 1 d . . .
H236 H 0.1482 0.5211 0.3740 0.033 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
W1 Cl1 2.452(2) . ?
W1 Cl5 2.4996(17) . ?
W1 Cl5 2.4996(17) 2 ?
W1 Cl6 2.5080(17) 2 ?
W1 Cl6 2.5080(17) . ?
W1 W2 2.6025(4) . ?
W1 W2 2.6025(4) 2 ?
W1 W3 2.6173(4) 2 ?
W1 W3 2.6173(4) . ?
W2 Cl2 2.4274(17) . ?
W2 Cl7 2.4873(17) . ?
W2 Cl8 2.5012(16) . ?
W2 Cl5 2.5085(17) . ?
W2 Cl6 2.5098(17) . ?
W2 W3 2.6120(4) 2 ?
W2 W4 2.6155(4) . ?
W2 W3 2.6156(4) . ?
W3 Cl3 2.4034(17) . ?
W3 Cl6 2.4922(17) . ?
W3 Cl5 2.4995(17) 2 ?
W3 Cl7 2.5036(17) 2 ?
W3 Cl8 2.5164(16) . ?
W3 W4 2.5984(4) . ?
W3 W2 2.6120(4) 2 ?
W4 Cl4 2.445(2) . ?
W4 Cl7 2.4876(17) . ?
W4 Cl7 2.4876(17) 2 ?
W4 Cl8 2.5065(16) 2 ?
W4 Cl8 2.5065(16) . ?
W4 W3 2.5984(4) 2 ?
W4 W2 2.6155(4) 2 ?
Ca1 O2 2.266(4) . ?
Ca1 O2 2.266(4) 2 ?
Ca1 O1 2.275(4) . ?
Ca1 O1 2.275(4) 2 ?
Ca1 Cl4 2.776(3) 1_545 ?
Ca1 Cl1 2.783(3) . ?
Cl5 W3 2.4995(17) 2 ?
Cl4 Ca1 2.776(3) 1_565 ?
Cl7 W3 2.5036(17) 2 ?
P1 O1 1.504(5) . ?
P1 C121 1.787(7) . ?
P1 C111 1.802(7) . ?
P1 C131 1.817(6) . ?
P2 O2 1.497(4) . ?
P2 C221 1.789(7) . ?
P2 C211 1.794(7) . ?
P2 C231 1.817(7) . ?
C111 C116 1.394(9) . ?
C111 C112 1.400(9) . ?
C112 C113 1.382(9) . ?
C112 H112 0.9500 . ?
C113 C114 1.388(10) . ?
C113 H113 0.9500 . ?
C114 C115 1.395(10) . ?
C114 H114 0.9500 . ?
C115 C116 1.379(10) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C121 C126 1.383(9) . ?
C121 C122 1.405(9) . ?
C122 C123 1.396(10) . ?
C122 H122 0.9500 . ?
C123 C124 1.374(11) . ?
C123 H123 0.9500 . ?
C124 C125 1.368(12) . ?
C124 H124 0.9500 . ?
C125 C126 1.403(10) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C131 C136 1.377(9) . ?
C131 C132 1.386(9) . ?
C132 C133 1.397(10) . ?
C132 H132 0.9500 . ?
C133 C134 1.377(10) . ?
C133 H133 0.9500 . ?
C134 C135 1.362(10) . ?
C134 H134 0.9500 . ?
C135 C136 1.390(9) . ?
C135 H135 0.9500 . ?
C136 H136 0.9500 . ?
C211 C216 1.392(9) . ?
C211 C212 1.392(9) . ?
C212 C213 1.390(9) . ?
C212 H212 0.9500 . ?
C213 C214 1.388(10) . ?
C213 H213 0.9500 . ?
C214 C215 1.375(10) . ?
C214 H214 0.9500 . ?
C215 C216 1.403(9) . ?
C215 H215 0.9500 . ?
C216 H216 0.9500 . ?
C221 C222 1.382(9) . ?
C221 C226 1.387(9) . ?
C222 C223 1.382(10) . ?
C222 H222 0.9500 . ?
C223 C224 1.370(11) . ?
C223 H223 0.9500 . ?
C224 C225 1.373(10) . ?
C224 H224 0.9500 . ?
C225 C226 1.388(10) . ?
C225 H225 0.9500 . ?
C226 H226 0.9500 . ?
C231 C232 1.375(9) . ?
C231 C236 1.375(9) . ?
C232 C233 1.398(10) . ?
C232 H232 0.9500 . ?
C233 C234 1.378(10) . ?
C233 H233 0.9500 . ?
C234 C235 1.388(10) . ?
C234 H234 0.9500 . ?
C235 C236 1.384(9) . ?
C235 H235 0.9500 . ?
C236 H236 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 W1 Cl5 91.58(4) . . ?
Cl1 W1 Cl5 91.58(4) . 2 ?
Cl5 W1 Cl5 176.83(8) . 2 ?
Cl1 W1 Cl6 91.86(4) . 2 ?
Cl5 W1 Cl6 88.67(6) . 2 ?
Cl5 W1 Cl6 91.23(6) 2 2 ?
Cl1 W1 Cl6 91.86(4) . . ?
Cl5 W1 Cl6 91.23(6) . . ?
Cl5 W1 Cl6 88.67(6) 2 . ?
Cl6 W1 Cl6 176.28(7) 2 . ?
Cl1 W1 W2 134.728(8) . . ?
Cl5 W1 W2 58.86(4) . . ?
Cl5 W1 W2 118.57(4) 2 . ?
Cl6 W1 W2 118.19(4) 2 . ?
Cl6 W1 W2 58.79(4) . . ?
Cl1 W1 W2 134.728(9) . 2 ?
Cl5 W1 W2 118.57(4) . 2 ?
Cl5 W1 W2 58.86(4) 2 2 ?
Cl6 W1 W2 58.79(4) 2 2 ?
Cl6 W1 W2 118.19(4) . 2 ?
W2 W1 W2 90.544(17) . 2 ?
Cl1 W1 W3 135.105(8) . 2 ?
Cl5 W1 W3 58.43(4) . 2 ?
Cl5 W1 W3 118.97(4) 2 2 ?
Cl6 W1 W3 58.14(4) 2 2 ?
Cl6 W1 W3 118.80(4) . 2 ?
W2 W1 W3 60.051(11) . 2 ?
W2 W1 W3 60.143(11) 2 2 ?
Cl1 W1 W3 135.105(8) . . ?
Cl5 W1 W3 118.97(4) . . ?
Cl5 W1 W3 58.43(4) 2 . ?
Cl6 W1 W3 118.80(4) 2 . ?
Cl6 W1 W3 58.14(4) . . ?
W2 W1 W3 60.143(11) . . ?
W2 W1 W3 60.051(11) 2 . ?
W3 W1 W3 89.790(17) 2 . ?
Cl2 W2 Cl7 93.02(6) . . ?
Cl2 W2 Cl8 93.35(6) . . ?
Cl7 W2 Cl8 88.69(6) . . ?
Cl2 W2 Cl5 90.23(6) . . ?
Cl7 W2 Cl5 90.36(6) . . ?
Cl8 W2 Cl5 176.35(6) . . ?
Cl2 W2 Cl6 90.88(6) . . ?
Cl7 W2 Cl6 175.87(6) . . ?
Cl8 W2 Cl6 89.73(5) . . ?
Cl5 W2 Cl6 90.98(6) . . ?
Cl2 W2 W1 132.83(5) . . ?
Cl7 W2 W1 118.98(4) . . ?
Cl8 W2 W1 119.06(4) . . ?
Cl5 W2 W1 58.52(4) . . ?
Cl6 W2 W1 58.72(4) . . ?
Cl2 W2 W3 134.55(5) . 2 ?
Cl7 W2 W3 58.75(4) . 2 ?
Cl8 W2 W3 118.23(4) . 2 ?
Cl5 W2 W3 58.39(4) . 2 ?
Cl6 W2 W3 118.94(4) . 2 ?
W1 W2 W3 60.254(9) . 2 ?
Cl2 W2 W4 137.43(5) . . ?
Cl7 W2 W4 58.29(4) . . ?
Cl8 W2 W4 58.61(4) . . ?
Cl5 W2 W4 117.99(4) . . ?
Cl6 W2 W4 117.70(4) . . ?
W1 W2 W4 89.741(11) . . ?
W3 W2 W4 59.612(9) 2 . ?
Cl2 W2 W3 135.45(5) . . ?
Cl7 W2 W3 117.85(4) . . ?
Cl8 W2 W3 58.87(4) . . ?
Cl5 W2 W3 118.70(4) . . ?
Cl6 W2 W3 58.14(4) . . ?
W1 W2 W3 60.208(9) . . ?
W3 W2 W3 89.943(11) 2 . ?
W4 W2 W3 59.566(9) . . ?
Cl3 W3 Cl6 93.45(6) . . ?
Cl3 W3 Cl5 93.99(6) . 2 ?
Cl6 W3 Cl5 89.03(6) . 2 ?
Cl3 W3 Cl7 90.32(6) . 2 ?
Cl6 W3 Cl7 176.19(6) . 2 ?
Cl5 W3 Cl7 90.19(6) 2 2 ?
Cl3 W3 Cl8 89.71(6) . . ?
Cl6 W3 Cl8 89.79(5) . . ?
Cl5 W3 Cl8 176.17(6) 2 . ?
Cl7 W3 Cl8 90.75(6) 2 . ?
Cl3 W3 W4 131.96(5) . . ?
Cl6 W3 W4 119.01(4) . . ?
Cl5 W3 W4 118.98(4) 2 . ?
Cl7 W3 W4 58.33(4) 2 . ?
Cl8 W3 W4 58.66(4) . . ?
Cl3 W3 W2 135.11(5) . 2 ?
Cl6 W3 W2 118.43(4) . 2 ?
Cl5 W3 W2 58.73(4) 2 2 ?
Cl7 W3 W2 58.14(4) 2 2 ?
Cl8 W3 W2 118.90(4) . 2 ?
W4 W3 W2 60.261(9) . 2 ?
Cl3 W3 W2 134.72(5) . . ?
Cl6 W3 W2 58.80(4) . . ?
Cl5 W3 W2 118.08(4) 2 . ?
Cl7 W3 W2 118.51(4) 2 . ?
Cl8 W3 W2 58.30(4) . . ?
W4 W3 W2 60.215(9) . . ?
W2 W3 W2 90.048(11) 2 . ?
Cl3 W3 W1 138.25(5) . . ?
Cl6 W3 W1 58.73(4) . . ?
Cl5 W3 W1 58.43(4) 2 . ?
Cl7 W3 W1 117.81(4) 2 . ?
Cl8 W3 W1 117.94(4) . . ?
W4 W3 W1 89.793(11) . . ?
W2 W3 W1 59.695(9) 2 . ?
W2 W3 W1 59.649(9) . . ?
Cl4 W4 Cl7 91.59(4) . . ?
Cl4 W4 Cl7 91.59(4) . 2 ?
Cl7 W4 Cl7 176.82(8) . 2 ?
Cl4 W4 Cl8 91.50(4) . 2 ?
Cl7 W4 Cl8 91.35(6) . 2 ?
Cl7 W4 Cl8 88.56(6) 2 2 ?
Cl4 W4 Cl8 91.50(4) . . ?
Cl7 W4 Cl8 88.56(6) . . ?
Cl7 W4 Cl8 91.35(6) 2 . ?
Cl8 W4 Cl8 177.01(7) 2 . ?
Cl4 W4 W3 134.688(8) . 2 ?
Cl7 W4 W3 58.93(4) . 2 ?
Cl7 W4 W3 118.50(4) 2 2 ?
Cl8 W4 W3 59.03(4) 2 2 ?
Cl8 W4 W3 118.54(4) . 2 ?
Cl4 W4 W3 134.688(8) . . ?
Cl7 W4 W3 118.50(4) . . ?
Cl7 W4 W3 58.93(4) 2 . ?
Cl8 W4 W3 118.54(4) 2 . ?
Cl8 W4 W3 59.03(4) . . ?
W3 W4 W3 90.624(17) 2 . ?
Cl4 W4 W2 135.013(8) . 2 ?
Cl7 W4 W2 119.12(4) . 2 ?
Cl7 W4 W2 58.28(4) 2 2 ?
Cl8 W4 W2 58.42(4) 2 2 ?
Cl8 W4 W2 119.13(4) . 2 ?
W3 W4 W2 60.219(11) 2 2 ?
W3 W4 W2 60.127(11) . 2 ?
Cl4 W4 W2 135.013(8) . . ?
Cl7 W4 W2 58.28(4) . . ?
Cl7 W4 W2 119.12(4) 2 . ?
Cl8 W4 W2 119.13(4) 2 . ?
Cl8 W4 W2 58.42(4) . . ?
W3 W4 W2 60.127(11) 2 . ?
W3 W4 W2 60.219(11) . . ?
W2 W4 W2 89.974(17) 2 . ?
O2 Ca1 O2 177.9(2) . 2 ?
O2 Ca1 O1 90.70(15) . . ?
O2 Ca1 O1 89.23(15) 2 . ?
O2 Ca1 O1 89.23(15) . 2 ?
O2 Ca1 O1 90.70(15) 2 2 ?
O1 Ca1 O1 176.2(2) . 2 ?
O2 Ca1 Cl4 88.95(12) . 1_545 ?
O2 Ca1 Cl4 88.95(12) 2 1_545 ?
O1 Ca1 Cl4 88.09(12) . 1_545 ?
O1 Ca1 Cl4 88.09(12) 2 1_545 ?
O2 Ca1 Cl1 91.05(12) . . ?
O2 Ca1 Cl1 91.05(12) 2 . ?
O1 Ca1 Cl1 91.91(12) . . ?
O1 Ca1 Cl1 91.91(12) 2 . ?
Cl4 Ca1 Cl1 180.0 1_545 . ?
W1 Cl1 Ca1 180.0 . . ?
W3 Cl5 W1 63.14(4) 2 . ?
W3 Cl5 W2 62.87(4) 2 . ?
W1 Cl5 W2 62.62(4) . . ?
W4 Cl4 Ca1 180.0 . 1_565 ?
W3 Cl6 W1 63.13(4) . . ?
W3 Cl6 W2 63.05(4) . . ?
W1 Cl6 W2 62.48(4) . . ?
W2 Cl7 W4 63.44(4) . . ?
W2 Cl7 W3 63.11(4) . 2 ?
W4 Cl7 W3 62.74(4) . 2 ?
W2 Cl8 W4 62.97(4) . . ?
W2 Cl8 W3 62.84(4) . . ?
W4 Cl8 W3 62.30(4) . . ?
O1 P1 C121 113.2(3) . . ?
O1 P1 C111 111.2(3) . . ?
C121 P1 C111 105.8(3) . . ?
O1 P1 C131 109.2(3) . . ?
C121 P1 C131 109.2(3) . . ?
C111 P1 C131 108.1(3) . . ?
O2 P2 C221 112.7(3) . . ?
O2 P2 C211 112.1(3) . . ?
C221 P2 C211 105.4(3) . . ?
O2 P2 C231 110.8(3) . . ?
C221 P2 C231 107.3(3) . . ?
C211 P2 C231 108.3(3) . . ?
P1 O1 Ca1 156.8(3) . . ?
P2 O2 Ca1 159.4(3) . . ?
C116 C111 C112 119.8(6) . . ?
C116 C111 P1 121.8(5) . . ?
C112 C111 P1 118.4(5) . . ?
C113 C112 C111 119.1(7) . . ?
C113 C112 H112 120.5 . . ?
C111 C112 H112 120.5 . . ?
C112 C113 C114 121.2(7) . . ?
C112 C113 H113 119.4 . . ?
C114 C113 H113 119.4 . . ?
C113 C114 C115 119.7(7) . . ?
C113 C114 H114 120.2 . . ?
C115 C114 H114 120.2 . . ?
C116 C115 C114 119.6(7) . . ?
C116 C115 H115 120.2 . . ?
C114 C115 H115 120.2 . . ?
C115 C116 C111 120.7(7) . . ?
C115 C116 H116 119.6 . . ?
C111 C116 H116 119.6 . . ?
C126 C121 C122 120.0(6) . . ?
C126 C121 P1 123.7(5) . . ?
C122 C121 P1 116.4(5) . . ?
C123 C122 C121 119.2(7) . . ?
C123 C122 H122 120.4 . . ?
C121 C122 H122 120.4 . . ?
C124 C123 C122 120.4(8) . . ?
C124 C123 H123 119.8 . . ?
C122 C123 H123 119.8 . . ?
C125 C124 C123 120.4(7) . . ?
C125 C124 H124 119.8 . . ?
C123 C124 H124 119.8 . . ?
C124 C125 C126 120.6(7) . . ?
C124 C125 H125 119.7 . . ?
C126 C125 H125 119.7 . . ?
C121 C126 C125 119.4(7) . . ?
C121 C126 H126 120.3 . . ?
C125 C126 H126 120.3 . . ?
C136 C131 C132 119.8(6) . . ?
C136 C131 P1 118.7(5) . . ?
C132 C131 P1 121.3(5) . . ?
C131 C132 C133 120.0(7) . . ?
C131 C132 H132 120.0 . . ?
C133 C132 H132 120.0 . . ?
C134 C133 C132 119.1(7) . . ?
C134 C133 H133 120.5 . . ?
C132 C133 H133 120.5 . . ?
C135 C134 C133 121.1(7) . . ?
C135 C134 H134 119.5 . . ?
C133 C134 H134 119.5 . . ?
C134 C135 C136 120.1(7) . . ?
C134 C135 H135 120.0 . . ?
C136 C135 H135 120.0 . . ?
C131 C136 C135 120.0(6) . . ?
C131 C136 H136 120.0 . . ?
C135 C136 H136 120.0 . . ?
C216 C211 C212 119.9(6) . . ?
C216 C211 P2 120.8(6) . . ?
C212 C211 P2 119.3(5) . . ?
C213 C212 C211 119.7(6) . . ?
C213 C212 H212 120.1 . . ?
C211 C212 H212 120.1 . . ?
C214 C213 C212 120.3(7) . . ?
C214 C213 H213 119.9 . . ?
C212 C213 H213 119.9 . . ?
C215 C214 C213 120.3(7) . . ?
C215 C214 H214 119.8 . . ?
C213 C214 H214 119.8 . . ?
C214 C215 C216 120.0(7) . . ?
C214 C215 H215 120.0 . . ?
C216 C215 H215 120.0 . . ?
C211 C216 C215 119.8(7) . . ?
C211 C216 H216 120.1 . . ?
C215 C216 H216 120.1 . . ?
C222 C221 C226 118.1(6) . . ?
C222 C221 P2 118.9(5) . . ?
C226 C221 P2 122.7(5) . . ?
C221 C222 C223 121.4(7) . . ?
C221 C222 H222 119.3 . . ?
C223 C222 H222 119.3 . . ?
C224 C223 C222 119.6(8) . . ?
C224 C223 H223 120.2 . . ?
C222 C223 H223 120.2 . . ?
C223 C224 C225 120.4(7) . . ?
C223 C224 H224 119.8 . . ?
C225 C224 H224 119.8 . . ?
C224 C225 C226 119.8(7) . . ?
C224 C225 H225 120.1 . . ?
C226 C225 H225 120.1 . . ?
C221 C226 C225 120.7(7) . . ?
C221 C226 H226 119.6 . . ?
C225 C226 H226 119.6 . . ?
C232 C231 C236 120.7(7) . . ?
C232 C231 P2 122.2(5) . . ?
C236 C231 P2 117.1(5) . . ?
C231 C232 C233 119.2(7) . . ?
C231 C232 H232 120.4 . . ?
C233 C232 H232 120.4 . . ?
C234 C233 C232 120.9(7) . . ?
C234 C233 H233 119.6 . . ?
C232 C233 H233 119.6 . . ?
C233 C234 C235 118.7(7) . . ?
C233 C234 H234 120.7 . . ?
C235 C234 H234 120.7 . . ?
C236 C235 C234 120.9(7) . . ?
C236 C235 H235 119.6 . . ?
C234 C235 H235 119.6 . . ?
C231 C236 C235 119.6(7) . . ?
C231 C236 H236 120.2 . . ?
C235 C236 H236 120.2 . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         1.522
_refine_diff_density_min         -2.081
_refine_diff_density_rms         0.235
####################################################################### 
# 
# 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_1_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1565899'
_audit_update_record             
;
2017-07-31 deposited with the CCDC.
2017-10-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H64 Ca O6 P4, Cl14 W6, 2(C2 H3 N)'
_chemical_formula_sum            'C76 H70 Ca Cl14 N2 O6 P4 W6'
_chemical_formula_weight         2870.70

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'

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                   22.955(5)
_cell_length_b                   16.219(3)
_cell_length_c                   24.818(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.58(3)
_cell_angle_gamma                90.00
_cell_volume                     8758(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6221
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5400
_exptl_absorpt_coefficient_mu    8.457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1012
_exptl_absorpt_correction_T_max  0.1330
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(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 Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        0
_diffrn_reflns_number            30487
_diffrn_reflns_av_R_equivalents  0.0740
_diffrn_reflns_av_sigmaI/netI    0.1487
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.48
_reflns_number_total             9576
_reflns_number_gt                6739
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'

_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)+(0.0454P)²] 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         9576
_refine_ls_number_parameters     499
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0616
_refine_ls_wR_factor_ref         0.1471
_refine_ls_wR_factor_gt          0.1328
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.985
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.043507(15) 0.02464(3) 0.075031(18) 0.01856(13) Uani 1 1 d . . .
W2 W 0.036997(15) 0.08780(3) -0.023920(18) 0.01799(13) Uani 1 1 d . . .
W3 W 0.062985(16) -0.06861(3) -0.003925(18) 0.01840(13) Uani 1 1 d . . .
Ca1 Ca 0.5000 0.11528(17) 0.2500 0.0159(6) Uani 1 2 d S . .
Cl1 Cl 0.09878(11) 0.0589(2) 0.17317(12) 0.0354(7) Uani 1 1 d . . .
Cl2 Cl 0.08668(10) 0.20354(17) -0.05525(13) 0.0310(7) Uani 1 1 d . . .
Cl3 Cl 0.14344(10) -0.16050(16) -0.01203(12) 0.0274(6) Uani 1 1 d . . .
Cl4 Cl 0.01733(10) 0.17338(16) 0.05282(11) 0.0230(6) Uani 1 1 d . . .
Cl5 Cl 0.05431(10) -0.00469(16) -0.09851(11) 0.0235(6) Uani 1 1 d . . .
Cl6 Cl 0.06676(10) -0.12506(16) 0.09090(11) 0.0231(6) Uani 1 1 d . . .
Cl7 Cl 0.13697(9) 0.04182(16) 0.04558(11) 0.0211(5) Uani 1 1 d . . .
P1 P 0.32969(10) 0.10883(16) 0.23960(12) 0.0176(6) Uani 1 1 d . . .
P2 P 0.44496(10) -0.03876(17) 0.13264(12) 0.0206(6) Uani 1 1 d . . .
O1 O 0.3976(2) 0.1087(4) 0.2475(3) 0.0232(17) Uani 1 1 d . . .
O1W O 0.5114(3) 0.2261(5) 0.3152(4) 0.036(2) Uani 1 1 d D . .
O2 O 0.4737(3) 0.0261(4) 0.1755(3) 0.0235(17) Uani 1 1 d . . .
N1 N 0.4362(7) 0.3633(12) 0.2690(7) 0.128(8) Uani 1 1 d . . .
C1 C 0.4032(8) 0.4079(13) 0.2393(9) 0.094(7) Uani 1 1 d . . .
C2 C 0.3639(8) 0.4705(10) 0.2003(7) 0.083(6) Uani 1 1 d . . .
H2A H 0.3881 0.5204 0.2005 0.125 Uiso 1 1 calc R . .
H2B H 0.3288 0.4843 0.2130 0.125 Uiso 1 1 calc R . .
H2C H 0.3490 0.4481 0.1616 0.125 Uiso 1 1 calc R . .
C111 C 0.2895(4) 0.1818(6) 0.1859(4) 0.021(2) Uani 1 1 d . . .
C112 C 0.2248(4) 0.1812(7) 0.1614(5) 0.030(3) Uani 1 1 d . . .
H112 H 0.2016 0.1411 0.1737 0.036 Uiso 1 1 calc R . .
C113 C 0.1948(4) 0.2365(7) 0.1206(5) 0.036(3) Uani 1 1 d . . .
H113 H 0.1512 0.2357 0.1052 0.043 Uiso 1 1 calc R . .
C114 C 0.2291(4) 0.2941(8) 0.1019(5) 0.038(3) Uani 1 1 d . . .
H114 H 0.2085 0.3331 0.0737 0.046 Uiso 1 1 calc R . .
C115 C 0.2925(5) 0.2958(8) 0.1234(5) 0.042(3) Uani 1 1 d . . .
H115 H 0.3154 0.3345 0.1095 0.050 Uiso 1 1 calc R . .
C116 C 0.3226(4) 0.2395(7) 0.1661(5) 0.029(3) Uani 1 1 d . . .
H116 H 0.3662 0.2407 0.1816 0.035 Uiso 1 1 calc R . .
C121 C 0.2913(4) 0.0089(6) 0.2202(4) 0.018(2) Uani 1 1 d . . .
C122 C 0.2873(4) -0.0431(7) 0.2603(5) 0.032(3) Uani 1 1 d . . .
H122 H 0.3043 -0.0279 0.2992 0.038 Uiso 1 1 calc R . .
C123 C 0.2583(4) -0.1196(7) 0.2464(6) 0.036(3) Uani 1 1 d . . .
H123 H 0.2547 -0.1558 0.2753 0.043 Uiso 1 1 calc R . .
C124 C 0.2352(4) -0.1411(7) 0.1902(5) 0.026(2) Uani 1 1 d . . .
H124 H 0.2153 -0.1929 0.1805 0.031 Uiso 1 1 calc R . .
C125 C 0.2398(4) -0.0898(6) 0.1471(5) 0.027(3) Uani 1 1 d . . .
H125 H 0.2239 -0.1056 0.1083 0.032 Uiso 1 1 calc R . .
C126 C 0.2693(4) -0.0126(6) 0.1633(5) 0.023(2) Uani 1 1 d . . .
H126 H 0.2739 0.0242 0.1352 0.027 Uiso 1 1 calc R . .
C131 C 0.3169(4) 0.1359(6) 0.3048(4) 0.016(2) Uani 1 1 d U . .
C132 C 0.3643(4) 0.1637(6) 0.3520(5) 0.027(3) Uani 1 1 d . . .
H132 H 0.4045 0.1686 0.3492 0.032 Uiso 1 1 calc R . .
C133 C 0.3550(4) 0.1843(7) 0.4026(4) 0.026(2) Uani 1 1 d . . .
H133 H 0.3887 0.2008 0.4344 0.032 Uiso 1 1 calc R . .
C134 C 0.2962(5) 0.1809(7) 0.4069(5) 0.032(3) Uani 1 1 d . . .
H134 H 0.2889 0.1968 0.4411 0.038 Uiso 1 1 calc R . .
C135 C 0.2483(5) 0.1540(8) 0.3605(6) 0.041(3) Uani 1 1 d . . .
H135 H 0.2082 0.1500 0.3635 0.049 Uiso 1 1 calc R . .
C136 C 0.2574(4) 0.1334(7) 0.3109(5) 0.032(3) Uani 1 1 d . . .
H136 H 0.2233 0.1169 0.2795 0.039 Uiso 1 1 calc R . .
C211 C 0.3722(4) -0.0034(6) 0.0835(4) 0.018(2) Uani 1 1 d . . .
C212 C 0.3297(4) -0.0585(7) 0.0497(5) 0.031(3) Uani 1 1 d . . .
H212 H 0.3369 -0.1163 0.0525 0.037 Uiso 1 1 calc R . .
C213 C 0.2753(4) -0.0256(8) 0.0111(5) 0.038(3) Uani 1 1 d . . .
H213 H 0.2461 -0.0615 -0.0136 0.045 Uiso 1 1 calc R . .
C214 C 0.2643(5) 0.0577(8) 0.0089(5) 0.036(3) Uani 1 1 d . . .
H214 H 0.2273 0.0784 -0.0172 0.043 Uiso 1 1 calc R . .
C215 C 0.3059(5) 0.1126(8) 0.0438(5) 0.038(3) Uani 1 1 d . . .
H215 H 0.2978 0.1702 0.0423 0.045 Uiso 1 1 calc R . .
C216 C 0.3605(4) 0.0798(7) 0.0813(4) 0.024(2) Uani 1 1 d . . .
H216 H 0.3899 0.1159 0.1056 0.029 Uiso 1 1 calc R . .
C221 C 0.4307(4) -0.1321(6) 0.1645(4) 0.021(2) Uani 1 1 d . . .
C222 C 0.4344(5) -0.2094(7) 0.1434(5) 0.031(3) Uani 1 1 d . . .
H222 H 0.4436 -0.2147 0.1089 0.037 Uiso 1 1 calc R . .
C223 C 0.4249(5) -0.2803(8) 0.1710(6) 0.052(4) Uani 1 1 d . . .
H223 H 0.4269 -0.3332 0.1552 0.062 Uiso 1 1 calc R . .
C224 C 0.4128(5) -0.2724(8) 0.2211(5) 0.042(3) Uani 1 1 d . . .
H224 H 0.4052 -0.3207 0.2395 0.050 Uiso 1 1 calc R . .
C225 C 0.4109(5) -0.1954(7) 0.2467(5) 0.031(3) Uani 1 1 d . . .
H225 H 0.4039 -0.1912 0.2823 0.037 Uiso 1 1 calc R . .
C226 C 0.4199(4) -0.1259(7) 0.2176(4) 0.024(2) Uani 1 1 d . . .
H226 H 0.4188 -0.0729 0.2336 0.029 Uiso 1 1 calc R . .
C231 C 0.4943(4) -0.0634(6) 0.0911(4) 0.021(2) Uani 1 1 d . . .
C232 C 0.5562(4) -0.0420(7) 0.1137(5) 0.034(3) Uani 1 1 d . . .
H232 H 0.5708 -0.0150 0.1495 0.041 Uiso 1 1 calc R . .
C233 C 0.5965(5) -0.0605(10) 0.0835(6) 0.057(4) Uani 1 1 d . . .
H233 H 0.6386 -0.0460 0.0990 0.069 Uiso 1 1 calc R . .
C234 C 0.5760(5) -0.0994(8) 0.0315(6) 0.046(4) Uani 1 1 d . . .
H234 H 0.6041 -0.1147 0.0123 0.055 Uiso 1 1 calc R . .
C235 C 0.5140(4) -0.1160(7) 0.0077(5) 0.031(3) Uani 1 1 d . . .
H235 H 0.4992 -0.1401 -0.0291 0.038 Uiso 1 1 calc R . .
C236 C 0.4735(5) -0.0979(7) 0.0366(5) 0.031(3) Uani 1 1 d . . .
H236 H 0.4310 -0.1091 0.0194 0.038 Uiso 1 1 calc R . .
H1W H 0.492(4) 0.269(4) 0.296(3) 0.050 Uiso 1 1 d D . .
H2W H 0.528(4) 0.245(6) 0.3507(16) 0.050 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
W1 Cl1 2.425(3) . ?
W1 Cl6 2.490(3) . ?
W1 Cl7 2.493(2) . ?
W1 Cl4 2.505(3) . ?
W1 Cl5 2.514(2) 5 ?
W1 W3 2.6172(10) 5 ?
W1 W2 2.6184(8) 5 ?
W1 W2 2.6208(8) . ?
W1 W3 2.6240(7) . ?
W2 Cl2 2.448(3) . ?
W2 Cl7 2.505(2) . ?
W2 Cl6 2.506(2) 5 ?
W2 Cl5 2.511(3) . ?
W2 Cl4 2.511(3) . ?
W2 W3 2.6170(8) . ?
W2 W3 2.6177(7) 5 ?
W2 W1 2.6184(8) 5 ?
W3 Cl3 2.431(2) . ?
W3 Cl6 2.501(3) . ?
W3 Cl7 2.504(2) . ?
W3 Cl5 2.515(3) . ?
W3 Cl4 2.517(2) 5 ?
W3 W1 2.6172(10) 5 ?
W3 W2 2.6177(7) 5 ?
Ca1 O2 2.273(7) . ?
Ca1 O2 2.273(7) 2_655 ?
Ca1 O1 2.335(6) 2_655 ?
Ca1 O1 2.335(6) . ?
Ca1 O1W 2.378(8) . ?
Ca1 O1W 2.378(8) 2_655 ?
Cl4 W3 2.517(2) 5 ?
Cl5 W1 2.514(2) 5 ?
Cl6 W2 2.506(2) 5 ?
P1 O1 1.507(6) . ?
P1 C131 1.788(10) . ?
P1 C111 1.801(10) . ?
P1 C121 1.835(9) . ?
P2 O2 1.492(7) . ?
P2 C221 1.786(11) . ?
P2 C231 1.803(10) . ?
P2 C211 1.819(9) . ?
O1W H1W 0.89(2) . ?
O1W H2W 0.89(2) . ?
N1 C1 1.13(2) . ?
C1 C2 1.49(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C111 C116 1.391(13) . ?
C111 C112 1.415(11) . ?
C112 C113 1.364(15) . ?
C112 H112 0.9500 . ?
C113 C114 1.395(15) . ?
C113 H113 0.9500 . ?
C114 C115 1.382(13) . ?
C114 H114 0.9500 . ?
C115 C116 1.404(15) . ?
C115 H115 0.9500 . ?
C116 H116 0.9500 . ?
C121 C122 1.330(15) . ?
C121 C126 1.384(14) . ?
C122 C123 1.398(14) . ?
C122 H122 0.9500 . ?
C123 C124 1.370(15) . ?
C123 H123 0.9500 . ?
C124 C125 1.387(15) . ?
C124 H124 0.9500 . ?
C125 C126 1.419(13) . ?
C125 H125 0.9500 . ?
C126 H126 0.9500 . ?
C131 C132 1.395(14) . ?
C131 C136 1.421(12) . ?
C132 C133 1.381(14) . ?
C132 H132 0.9500 . ?
C133 C134 1.390(13) . ?
C133 H133 0.9500 . ?
C134 C135 1.385(15) . ?
C134 H134 0.9500 . ?
C135 C136 1.356(16) . ?
C135 H135 0.9500 . ?
C136 H136 0.9500 . ?
C211 C216 1.375(14) . ?
C211 C212 1.389(13) . ?
C212 C213 1.415(14) . ?
C212 H212 0.9500 . ?
C213 C214 1.373(17) . ?
C213 H213 0.9500 . ?
C214 C215 1.388(16) . ?
C214 H214 0.9500 . ?
C215 C216 1.406(14) . ?
C215 H215 0.9500 . ?
C216 H216 0.9500 . ?
C221 C222 1.372(14) . ?
C221 C226 1.418(14) . ?
C222 C223 1.389(16) . ?
C222 H222 0.9500 . ?
C223 C224 1.366(17) . ?
C223 H223 0.9500 . ?
C224 C225 1.406(17) . ?
C224 H224 0.9500 . ?
C225 C226 1.390(15) . ?
C225 H225 0.9500 . ?
C226 H226 0.9500 . ?
C231 C232 1.394(13) . ?
C231 C236 1.400(15) . ?
C232 C233 1.397(15) . ?
C232 H232 0.9500 . ?
C233 C234 1.377(17) . ?
C233 H233 0.9500 . ?
C234 C235 1.382(14) . ?
C234 H234 0.9500 . ?
C235 C236 1.375(13) . ?
C235 H235 0.9500 . ?
C236 H236 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 W1 Cl6 92.73(10) . . ?
Cl1 W1 Cl7 92.59(9) . . ?
Cl6 W1 Cl7 89.67(8) . . ?
Cl1 W1 Cl4 90.69(10) . . ?
Cl6 W1 Cl4 176.55(9) . . ?
Cl7 W1 Cl4 89.79(8) . . ?
Cl1 W1 Cl5 90.97(9) . 5 ?
Cl6 W1 Cl5 90.00(8) . 5 ?
Cl7 W1 Cl5 176.44(8) . 5 ?
Cl4 W1 Cl5 90.32(8) . 5 ?
Cl1 W1 W3 133.79(7) . 5 ?
Cl6 W1 W3 118.64(6) . 5 ?
Cl7 W1 W3 118.56(6) . 5 ?
Cl4 W1 W3 58.81(5) . 5 ?
Cl5 W1 W3 58.67(6) 5 5 ?
Cl1 W1 W2 135.15(8) . 5 ?
Cl6 W1 W2 58.68(6) . 5 ?
Cl7 W1 W2 118.44(6) . 5 ?
Cl4 W1 W2 118.78(6) . 5 ?
Cl5 W1 W2 58.53(6) 5 5 ?
W3 W1 W2 59.98(2) 5 5 ?
Cl1 W1 W2 134.97(8) . . ?
Cl6 W1 W2 118.33(6) . . ?
Cl7 W1 W2 58.60(6) . . ?
Cl4 W1 W2 58.62(6) . . ?
Cl5 W1 W2 118.62(6) 5 . ?
W3 W1 W2 59.97(3) 5 . ?
W2 W1 W2 89.86(3) 5 . ?
Cl1 W1 W3 136.31(7) . . ?
Cl6 W1 W3 58.48(6) . . ?
Cl7 W1 W3 58.54(6) . . ?
Cl4 W1 W3 118.48(6) . . ?
Cl5 W1 W3 118.43(6) 5 . ?
W3 W1 W3 89.90(3) 5 . ?
W2 W1 W3 59.91(2) 5 . ?
W2 W1 W3 59.86(2) . . ?
Cl2 W2 Cl7 91.70(8) . . ?
Cl2 W2 Cl6 92.57(8) . 5 ?
Cl7 W2 Cl6 175.73(8) . 5 ?
Cl2 W2 Cl5 91.42(9) . . ?
Cl7 W2 Cl5 90.25(8) . . ?
Cl6 W2 Cl5 89.73(8) 5 . ?
Cl2 W2 Cl4 91.81(9) . . ?
Cl7 W2 Cl4 89.37(8) . . ?
Cl6 W2 Cl4 90.41(8) 5 . ?
Cl5 W2 Cl4 176.76(8) . . ?
Cl2 W2 W3 134.62(6) . . ?
Cl7 W2 W3 58.50(6) . . ?
Cl6 W2 W3 118.08(6) 5 . ?
Cl5 W2 W3 58.71(6) . . ?
Cl4 W2 W3 118.50(6) . . ?
Cl2 W2 W3 135.34(6) . 5 ?
Cl7 W2 W3 118.08(6) . 5 ?
Cl6 W2 W3 58.38(6) 5 5 ?
Cl5 W2 W3 118.79(5) . 5 ?
Cl4 W2 W3 58.73(5) . 5 ?
W3 W2 W3 90.044(18) . 5 ?
Cl2 W2 W1 135.10(7) . 5 ?
Cl7 W2 W1 118.46(6) . 5 ?
Cl6 W2 W1 58.11(6) 5 5 ?
Cl5 W2 W1 58.65(5) . 5 ?
Cl4 W2 W1 118.86(5) . 5 ?
W3 W2 W1 59.99(2) . 5 ?
W3 W2 W1 60.151(19) 5 5 ?
Cl2 W2 W1 134.75(7) . . ?
Cl7 W2 W1 58.15(6) . . ?
Cl6 W2 W1 118.31(6) 5 . ?
Cl5 W2 W1 118.83(6) . . ?
Cl4 W2 W1 58.38(6) . . ?
W3 W2 W1 60.130(17) . . ?
W3 W2 W1 59.95(3) 5 . ?
W1 W2 W1 90.14(3) 5 . ?
Cl3 W3 Cl6 93.09(9) . . ?
Cl3 W3 Cl7 93.71(8) . . ?
Cl6 W3 Cl7 89.17(8) . . ?
Cl3 W3 Cl5 90.68(9) . . ?
Cl6 W3 Cl5 176.20(8) . . ?
Cl7 W3 Cl5 90.16(8) . . ?
Cl3 W3 Cl4 90.30(8) . 5 ?
Cl6 W3 Cl4 90.40(9) . 5 ?
Cl7 W3 Cl4 175.98(7) . 5 ?
Cl5 W3 Cl4 90.02(9) . 5 ?
Cl3 W3 W2 135.39(6) . . ?
Cl6 W3 W2 118.09(6) . . ?
Cl7 W3 W2 58.52(6) . . ?
Cl5 W3 W2 58.53(6) . . ?
Cl4 W3 W2 118.38(6) 5 . ?
Cl3 W3 W1 133.02(7) . 5 ?
Cl6 W3 W1 118.63(5) . 5 ?
Cl7 W3 W1 118.53(6) . 5 ?
Cl5 W3 W1 58.61(5) . 5 ?
Cl4 W3 W1 58.36(6) 5 5 ?
W2 W3 W1 60.034(15) . 5 ?
Cl3 W3 W2 134.59(7) . 5 ?
Cl6 W3 W2 58.57(5) . 5 ?
Cl7 W3 W2 118.04(6) . 5 ?
Cl5 W3 W2 118.68(6) . 5 ?
Cl4 W3 W2 58.52(6) 5 5 ?
W2 W3 W2 89.956(18) . 5 ?
W1 W3 W2 60.08(2) 5 5 ?
Cl3 W3 W1 136.87(7) . . ?
Cl6 W3 W1 58.09(6) . . ?
Cl7 W3 W1 58.11(5) . . ?
Cl5 W3 W1 118.53(6) . . ?
Cl4 W3 W1 118.45(6) 5 . ?
W2 W3 W1 60.007(19) . . ?
W1 W3 W1 90.10(3) 5 . ?
W2 W3 W1 59.94(2) 5 . ?
O2 Ca1 O2 101.0(4) . 2_655 ?
O2 Ca1 O1 89.8(2) . 2_655 ?
O2 Ca1 O1 86.9(2) 2_655 2_655 ?
O2 Ca1 O1 86.9(2) . . ?
O2 Ca1 O1 89.8(2) 2_655 . ?
O1 Ca1 O1 174.8(4) 2_655 . ?
O2 Ca1 O1W 168.1(3) . . ?
O2 Ca1 O1W 89.1(3) 2_655 . ?
O1 Ca1 O1W 97.2(2) 2_655 . ?
O1 Ca1 O1W 86.8(3) . . ?
O2 Ca1 O1W 89.1(3) . 2_655 ?
O2 Ca1 O1W 168.1(3) 2_655 2_655 ?
O1 Ca1 O1W 86.8(3) 2_655 2_655 ?
O1 Ca1 O1W 97.2(2) . 2_655 ?
O1W Ca1 O1W 81.7(5) . 2_655 ?
W1 Cl4 W2 63.00(6) . . ?
W1 Cl4 W3 62.83(6) . 5 ?
W2 Cl4 W3 62.75(6) . 5 ?
W2 Cl5 W1 62.82(6) . 5 ?
W2 Cl5 W3 62.76(6) . . ?
W1 Cl5 W3 62.72(6) 5 . ?
W1 Cl6 W3 63.44(6) . . ?
W1 Cl6 W2 63.22(6) . 5 ?
W3 Cl6 W2 63.05(7) . 5 ?
W1 Cl7 W3 63.35(5) . . ?
W1 Cl7 W2 63.25(5) . . ?
W3 Cl7 W2 62.99(5) . . ?
O1 P1 C131 110.1(4) . . ?
O1 P1 C111 111.2(4) . . ?
C131 P1 C111 108.4(4) . . ?
O1 P1 C121 115.0(4) . . ?
C131 P1 C121 104.5(5) . . ?
C111 P1 C121 107.2(4) . . ?
O2 P2 C221 112.6(5) . . ?
O2 P2 C231 110.3(4) . . ?
C221 P2 C231 107.6(5) . . ?
O2 P2 C211 111.0(4) . . ?
C221 P2 C211 107.8(4) . . ?
C231 P2 C211 107.2(5) . . ?
P1 O1 Ca1 173.7(5) . . ?
Ca1 O1W H1W 108(6) . . ?
Ca1 O1W H2W 148(6) . . ?
H1W O1W H2W 104(7) . . ?
P2 O2 Ca1 166.2(4) . . ?
N1 C1 C2 176(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C116 C111 C112 118.1(10) . . ?
C116 C111 P1 119.7(7) . . ?
C112 C111 P1 122.3(8) . . ?
C113 C112 C111 121.9(10) . . ?
C113 C112 H112 119.1 . . ?
C111 C112 H112 119.1 . . ?
C112 C113 C114 118.8(9) . . ?
C112 C113 H113 120.6 . . ?
C114 C113 H113 120.6 . . ?
C115 C114 C113 121.6(11) . . ?
C115 C114 H114 119.2 . . ?
C113 C114 H114 119.2 . . ?
C114 C115 C116 118.9(10) . . ?
C114 C115 H115 120.6 . . ?
C116 C115 H115 120.6 . . ?
C111 C116 C115 120.8(9) . . ?
C111 C116 H116 119.6 . . ?
C115 C116 H116 119.6 . . ?
C122 C121 C126 121.0(10) . . ?
C122 C121 P1 120.3(8) . . ?
C126 C121 P1 118.6(8) . . ?
C121 C122 C123 121.2(11) . . ?
C121 C122 H122 119.4 . . ?
C123 C122 H122 119.4 . . ?
C124 C123 C122 118.5(11) . . ?
C124 C123 H123 120.7 . . ?
C122 C123 H123 120.7 . . ?
C123 C124 C125 122.2(10) . . ?
C123 C124 H124 118.9 . . ?
C125 C124 H124 118.9 . . ?
C124 C125 C126 117.2(10) . . ?
C124 C125 H125 121.4 . . ?
C126 C125 H125 121.4 . . ?
C121 C126 C125 119.8(10) . . ?
C121 C126 H126 120.1 . . ?
C125 C126 H126 120.1 . . ?
C132 C131 C136 115.9(10) . . ?
C132 C131 P1 122.1(7) . . ?
C136 C131 P1 122.0(8) . . ?
C133 C132 C131 122.5(9) . . ?
C133 C132 H132 118.7 . . ?
C131 C132 H132 118.7 . . ?
C132 C133 C134 119.8(9) . . ?
C132 C133 H133 120.1 . . ?
C134 C133 H133 120.1 . . ?
C135 C134 C133 118.7(11) . . ?
C135 C134 H134 120.6 . . ?
C133 C134 H134 120.6 . . ?
C136 C135 C134 121.5(10) . . ?
C136 C135 H135 119.2 . . ?
C134 C135 H135 119.2 . . ?
C135 C136 C131 121.4(10) . . ?
C135 C136 H136 119.3 . . ?
C131 C136 H136 119.3 . . ?
C216 C211 C212 121.1(9) . . ?
C216 C211 P2 117.5(7) . . ?
C212 C211 P2 121.4(8) . . ?
C211 C212 C213 117.7(11) . . ?
C211 C212 H212 121.1 . . ?
C213 C212 H212 121.1 . . ?
C214 C213 C212 120.6(11) . . ?
C214 C213 H213 119.7 . . ?
C212 C213 H213 119.7 . . ?
C213 C214 C215 121.7(11) . . ?
C213 C214 H214 119.1 . . ?
C215 C214 H214 119.1 . . ?
C214 C215 C216 117.4(11) . . ?
C214 C215 H215 121.3 . . ?
C216 C215 H215 121.3 . . ?
C211 C216 C215 121.3(10) . . ?
C211 C216 H216 119.3 . . ?
C215 C216 H216 119.3 . . ?
C222 C221 C226 118.0(10) . . ?
C222 C221 P2 124.3(9) . . ?
C226 C221 P2 117.5(8) . . ?
C221 C222 C223 122.0(12) . . ?
C221 C222 H222 119.0 . . ?
C223 C222 H222 119.0 . . ?
C224 C223 C222 118.7(13) . . ?
C224 C223 H223 120.6 . . ?
C222 C223 H223 120.6 . . ?
C223 C224 C225 122.5(12) . . ?
C223 C224 H224 118.7 . . ?
C225 C224 H224 118.7 . . ?
C226 C225 C224 117.1(11) . . ?
C226 C225 H225 121.4 . . ?
C224 C225 H225 121.4 . . ?
C225 C226 C221 121.5(10) . . ?
C225 C226 H226 119.2 . . ?
C221 C226 H226 119.2 . . ?
C232 C231 C236 118.6(9) . . ?
C232 C231 P2 117.4(8) . . ?
C236 C231 P2 123.9(7) . . ?
C231 C232 C233 119.6(11) . . ?
C231 C232 H232 120.2 . . ?
C233 C232 H232 120.2 . . ?
C234 C233 C232 120.9(11) . . ?
C234 C233 H233 119.5 . . ?
C232 C233 H233 119.5 . . ?
C233 C234 C235 119.2(10) . . ?
C233 C234 H234 120.4 . . ?
C235 C234 H234 120.4 . . ?
C236 C235 C234 120.7(11) . . ?
C236 C235 H235 119.7 . . ?
C234 C235 H235 119.7 . . ?
C235 C236 C231 120.7(10) . . ?
C235 C236 H236 119.7 . . ?
C231 C236 H236 119.7 . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         4.578
_refine_diff_density_min         -3.327
_refine_diff_density_rms         0.369
