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

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

data_compound1
_database_code_depnum_ccdc_archive 'CCDC 1547968'
_audit_update_record             
;
2017-05-04 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;

_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C25 H20 Mo2 N O4 P'
_chemical_formula_sum            'C25 H20 Mo2 N O4 P'
_chemical_formula_weight         621.27
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/a'
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'1/2-x, 1/2+y, -z'
'-x, -y, -z'
'1/2+x, 1/2-y, z'

_cell_length_a                   17.296(3)
_cell_length_b                   16.028(5)
_cell_length_c                   8.760(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.46(2)
_cell_angle_gamma                90
_cell_volume                     2380(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    291
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      1
_cell_measurement_theta_max      25
_cell_measurement_wavelength     0.71069

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232.0
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Difabs
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  1.07

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      291(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_source         'Philips PW1100 X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       2θ/ω
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_av_unetI/netI     0.032
_diffrn_reflns_number            4251
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_reflns_number_total             4207
_reflns_number_gt                2522
_reflns_threshold_expression     >3σ(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_structure_solution    'SHELXS (Sheldrick, 1986)'
_computing_structure_refinement  'SHELXS (Sheldrick, 1986)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_ls_structure_factor_coef F
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         4207
_refine_ls_number_parameters     300
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          ?
_refine_ls_R_factor_gt           0.032
_refine_ls_wR_factor_ref         ?
_refine_ls_wR_factor_gt          0.033
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.40

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 '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'

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 0.14883(3) 0.98905(3) 0.29627(6) 0.0291 Uani 1 1 d . . .
Mo2 Mo 0.27418(3) 1.00917(4) 0.60681(6) 0.0353 Uani 1 1 d . . .
P1 P 0.28905(8) 0.99976(9) 0.3359(2) 0.0289 Uani 1 1 d . . .
O1 O 0.0786(4) 1.1531(3) 0.3981(8) 0.0807 Uani 1 1 d . . .
O2 O 0.1542(3) 1.1018(4) 0.0131(6) 0.0676 Uani 1 1 d . . .
O3 O 0.1087(3) 0.9702(4) 0.6775(6) 0.0725 Uani 1 1 d . . .
O4 O 0.3122(4) 0.8293(3) 0.6771(7) 0.0731 Uani 1 1 d . . .
N1 N 0.2971(3) 0.9012(4) 0.6468(6) 0.0455 Uani 1 1 d . . .
C1 C 0.1068(4) 1.0924(4) 0.3652(8) 0.0463 Uani 1 1 d . . .
C2 C 0.1542(4) 1.0615(4) 0.1243(8) 0.0396 Uani 1 1 d . . .
C3 C 0.1645(4) 0.9847(4) 0.6293(8) 0.0449 Uani 1 1 d . . .
C10 C 0.0932(5) 0.8911(5) 0.1138(9) 0.0635 Uani 1 1 d . . .
H(101) H 0.0971 0.8984 0.0091 0.066(5) Uiso 1 1 calc R . .
C11 C 0.0331(4) 0.9265(4) 0.181(1) 0.0552 Uani 1 1 d . . .
H(111) H -0.0103 0.9629 0.1283 0.066(5) Uiso 1 1 calc R . .
C12 C 0.0469(4) 0.9029(4) 0.3373(9) 0.0476 Uani 1 1 d . . .
H(121) H 0.0135 0.9154 0.4134 0.066(5) Uiso 1 1 calc R . .
C13 C 0.1133(4) 0.8535(4) 0.3687(9) 0.0505 Uani 1 1 d . . .
H(131) H 0.1371 0.8305 0.4634 0.066(5) Uiso 1 1 calc R . .
C14 C 0.1438(5) 0.8451(4) 0.230(1) 0.0565 Uani 1 1 d . . .
H(141) H 0.1895 0.8180 0.2259 0.066(5) Uiso 1 1 calc R . .
C20 C 0.2912(8) 1.1562(6) 0.619(1) 0.0813 Uani 1 1 d . . .
H(201) H 0.2674 1.1954 0.5225 0.066(5) Uiso 1 1 calc R . .
C21 C 0.2586(5) 1.1341(5) 0.740(1) 0.0653 Uani 1 1 d . . .
H(211) H 0.2021 1.1486 0.7537 0.066(5) Uiso 1 1 calc R . .
C22 C 0.3083(6) 1.0817(6) 0.8406(9) 0.0691 Uani 1 1 d . . .
H(221) H 0.2984 1.0537 0.9321 0.066(5) Uiso 1 1 calc R . .
C23 C 0.3769(6) 1.0743(7) 0.776(1) 0.0890 Uani 1 1 d . . .
H(231) H 0.4164 1.0430 0.8190 0.066(5) Uiso 1 1 calc R . .
C24 C 0.3650(7) 1.1200(7) 0.637(1) 0.0869 Uani 1 1 d . . .
H(241) H 0.4017 1.1244 0.5730 0.066(5) Uiso 1 1 calc R . .
C30 C 0.3430(4) 1.0869(4) 0.2686(7) 0.0335 Uani 1 1 d . . .
C31 C 0.4198(4) 1.0770(4) 0.2492(8) 0.0453 Uani 1 1 d . . .
H(311) H 0.4443 1.0265 0.2659 0.066(5) Uiso 1 1 calc R . .
C32 C 0.4633(4) 1.1424(6) 0.2075(9) 0.0613 Uani 1 1 d . . .
H(321) H 0.5164 1.1325 0.2000 0.066(5) Uiso 1 1 calc R . .
C33 C 0.4286(5) 1.2208(5) 0.183(1) 0.0679 Uani 1 1 d . . .
H(331) H 0.4581 1.2691 0.1481 0.066(5) Uiso 1 1 calc R . .
C34 C 0.3514(5) 1.2319(5) 0.1987(9) 0.0593 Uani 1 1 d . . .
H(341) H 0.3241 1.2839 0.1841 0.066(5) Uiso 1 1 calc R . .
C35 C 0.3092(4) 1.1655(4) 0.2419(8) 0.0422 Uani 1 1 d . . .
H(351) H 0.2550 1.1708 0.2550 0.066(5) Uiso 1 1 calc R . .
C40 C 0.3424(4) 0.9102(4) 0.2797(8) 0.0333 Uani 1 1 d . . .
C41 C 0.3995(4) 0.8676(4) 0.3848(7) 0.0406 Uani 1 1 d . . .
H(411) H 0.4096 0.8891 0.4954 0.066(5) Uiso 1 1 calc R . .
C42 C 0.4396(4) 0.7999(4) 0.337(1) 0.0494 Uani 1 1 d . . .
H(421) H 0.4760 0.7698 0.4150 0.066(5) Uiso 1 1 calc R . .
C43 C 0.4234(5) 0.7763(5) 0.183(1) 0.0579 Uani 1 1 d . . .
H(431) H 0.4516 0.7298 0.1527 0.066(5) Uiso 1 1 calc R . .
C44 C 0.3670(5) 0.8175(5) 0.0763(8) 0.0546 Uani 1 1 d . . .
H(441) H 0.3540 0.8007 -0.0282 0.066(5) Uiso 1 1 calc R . .
C45 C 0.3274(4) 0.8833(4) 0.1260(8) 0.0476 Uani 1 1 d . . .
H(451) H 0.2876 0.9104 0.0497 0.066(5) Uiso 1 1 calc R . .


#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 Mo2 3.1400(7) . ?
Mo1 P1 2.387(1) . ?
Mo1 C1 1.951(7) . ?
Mo1 C2 1.919(7) . ?
Mo1 C10 2.309(7) . ?
Mo1 C11 2.287(6) . ?
Mo1 C12 2.323(7) . ?
Mo1 C13 2.378(7) . ?
Mo1 C14 2.376(7) . ?
Mo2 P1 2.442(1) . ?
Mo2 N1 1.794(6) . ?
Mo2 C3 1.984(7) . ?
Mo2 C20 2.375(8) . ?
Mo2 C21 2.362(7) . ?
Mo2 C22 2.326(7) . ?
Mo2 C23 2.324(9) . ?
Mo2 C24 2.350(8) . ?
P1 C30 1.841(6) . ?
P1 C40 1.827(6) . ?
O1 c1 1.151(8) . ?
O2 C2 1.170(7) . ?
O3 C3 1.152(7) . ?
O4 N1 1.201(7) . ?
C10 C11 1.41(1) . ?
C10 C14 1.41(1) . ?
C11 C12 1.40(1) . ?
C12 C13 1.38(1) . ?
C13 C14 1.42(1) . ?
C20 C21 1.34(1) . ?
C20 C24 1.38(1) . ?
C21 C22 1.38(1) . ?
C22 C23 1.42(1) . ?
C23 C24 1.40(1) . ?
C30 C31 1.382(9) . ?
C30 C35 1.388(9) . ?
C31 C32 1.381(9) . ?
C32 C33 1.39(1) . ?
C33 C34 1.38(1) . ?
C34 C35 1.385(9) . ?
C40 C41 1.388(8) . ?
C40 C45 1.387(9) . ?
C41 C42 1.395(9) . ?
C42 C43 1.38(1) . ?
C43 C44 1.38(1) . ?
C44 C45 1.375(9) . ?

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
Mo2 Mo1 P1 50.21(4) . . ?
Mo2 Mo1 C1 83.1(2) . . ?
P1 Mo1 C1 108.9(2) . . ?
Mo2 Mo1 C2 119.0(2) . . ?
P1 Mo1 C2 82.2(2) . . ?
C1 Mo1 C2 79.0(3) . . ?
Mo1 Mo2 P1 48.68(3) . . ?
Mo1 Mo2 N1 99.1(2) . . ?
P1 Mo2 N1 93.9(2) . . ?
Mo1 Mo2 C3 63.7(2) . . ?
P1 Mo2 C3 111.8(2) . . ?
N1 Mo2 C3 88.2(3) . . ?
Mo1 P1 Mo2 81.11(5) . . ?
Mo1 P1 C30 124.9(2) . . ?
Mo2 P1 C30 115.0(2) . . ?
Mo1 P1 C40 117.2(2) . . ?
Mo2 P1 C40 117.8(2) . . ?
C30 P1 C40 101.2(3) . . ?
Mo2 N1 O4 178.4(5) . . ?
Mo1 C1 O1 175.9(7) . . ?
Mo1 C2 O2 175.4(6) . . ?
Mo2 C3 O3 164.5(6) . . ?
C11 C10 C14 108.2(7) . . ?
C10 C11 C12 107.6(7) . . ?
C11 C12 C13 109.0(7) . . ?
C12 C13 C14 108.7(7) . . ?
C10 C14 C13 106.6(7) . . ?
C21 C20 C24 108.6(9) . . ?
C20 C21 C22 110.9(9) . . ?
C21 C22 C23 105.2(8) . . ?
C22 C23 C24 108.1(9) . . ?
C20 C24 C23 107.2(8) . . ?
P1 C30 C31 120.8(5) . . ?
P1 C30 C35 121.3(5) . . ?
C31 C30 C35 117.8(6) . . ?
C30 C31 C32 122.2(7) . . ?
C31 C32 C33 119.1(7) . . ?
C32 C33 C34 119.8(7) . . ?
C33 C34 C35 120.1(7) . . ?
C30 C35 C34 121.0(7) . . ?
P1 C40 C41 122.6(5) . . ?
P1 C40 C45 119.9(5) . . ?
C41 C40 C45 117.6(6) . . ?
C40 C41 C42 121.1(6) . . ?
C41 C42 C43 119.2(7) . . ?
C42 C43 C44 120.8(6) . . ?
C43 C44 C45 118.9(7) . . ?
C40 C45 C44 122.4(6) . . ?
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_compound4b
_database_code_depnum_ccdc_archive 'CCDC 1547969'
_audit_update_record             
;
2017-05-04 deposited with the CCDC.
2017-07-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H41 N O6 P2 W2'
_chemical_formula_sum            'C27 H41 N O6 P2 W2'
_chemical_formula_weight         905.23

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'
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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -5.4734 5.5774 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   12.0125(3)
_cell_length_b                   15.8531(5)
_cell_length_c                   18.6734(6)
_cell_angle_alpha                90
_cell_angle_beta                 93.514(3)
_cell_angle_gamma                90
_cell_volume                     3549.39(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    8165
_cell_measurement_theta_min      3.6572
_cell_measurement_theta_max      69.1663

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             1744.0
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    12.939
_shelx_estimated_absorpt_T_min   0.324
_shelx_estimated_absorpt_T_max   0.499
_exptl_absorpt_correction_T_min  0.81194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'ONYX CCD'
_diffrn_measurement_method       CCD
_diffrn_radiation_probe          x-ray
_diffrn_reflns_number            15594
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.660
_diffrn_reflns_theta_max         69.291
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6502
_reflns_number_gt                5907
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
;
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0884P)²+66.1530P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6502
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0414
_refine_ls_wR_factor_ref         0.1344
_refine_ls_wR_factor_gt          0.1309
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_restrained_S_all      0.832
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         1.204
_refine_diff_density_min         -1.267
_refine_diff_density_rms         0.162

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 385 123 ' '
2 0.000 0.500 0.000 385 123 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
;

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
W1 W 0.70741(3) 0.96427(2) 0.20723(2) 0.03123(13) Uani 1 1 d . . . . .
W2 W 0.57166(3) 0.83990(2) 0.11536(2) 0.02640(12) Uani 1 1 d . . . . .
P1 P 0.76542(16) 0.82812(13) 0.16656(10) 0.0277(4) Uani 1 1 d . . . . .
P2 P 0.61491(17) 0.71225(14) 0.05546(11) 0.0315(4) Uani 1 1 d . . . . .
N1 N 0.6052(5) 0.8969(4) 0.0375(3) 0.0303(14) Uani 1 1 d . . . . .
O1 O 0.5670(6) 0.9197(5) 0.3353(3) 0.0503(17) Uani 1 1 d . . . . .
O2 O 0.8981(6) 0.9178(5) 0.3204(4) 0.0533(18) Uani 1 1 d . . . . .
O3 O 0.7283(5) 0.7125(4) 0.0182(3) 0.0422(15) Uani 1 1 d . . . . .
O4 O 0.5246(5) 0.6846(4) -0.0079(3) 0.0416(14) Uani 1 1 d . . . . .
O5 O 0.6103(6) 0.6304(4) 0.1033(3) 0.0434(15) Uani 1 1 d . . . . .
O6 O 0.6135(5) 0.9377(4) -0.0174(3) 0.0381(13) Uani 1 1 d . . . . .
C1 C 0.6210(7) 0.9319(6) 0.2855(5) 0.0374(19) Uani 1 1 d . . . . .
C2 C 0.8296(8) 0.9341(6) 0.2774(5) 0.042(2) Uani 1 1 d . . . . .
C3 C 0.7657(8) 0.6505(8) -0.0325(6) 0.055(3) Uani 1 1 d . . . . .
H3A H 0.802813 0.605120 -0.006808 0.082 Uiso 1 1 calc R U . . .
H3B H 0.816386 0.676740 -0.063501 0.082 Uiso 1 1 calc R U . . .
H3C H 0.702520 0.628901 -0.060697 0.082 Uiso 1 1 calc R U . . .
C4 C 0.5046(10) 0.7415(7) -0.0682(5) 0.053(3) Uani 1 1 d . . . . .
H4A H 0.453455 0.784820 -0.055673 0.079 Uiso 1 1 calc R U . . .
H4B H 0.473365 0.710556 -0.108828 0.079 Uiso 1 1 calc R U . . .
H4C H 0.573740 0.766783 -0.080059 0.079 Uiso 1 1 calc R U . . .
C5 C 0.6090(16) 0.5452(8) 0.0791(8) 0.086(5) Uani 1 1 d . . . . .
H5A H 0.535381 0.530962 0.060042 0.128 Uiso 1 1 calc R U . . .
H5B H 0.629878 0.508550 0.118581 0.128 Uiso 1 1 calc R U . . .
H5C H 0.660878 0.538791 0.042391 0.128 Uiso 1 1 calc R U . . .
C6 C 0.7244(8) 1.0552(6) 0.1071(5) 0.0390(19) Uani 1 1 d . . . . .
H6 H 0.742747 1.034030 0.062910 0.047 Uiso 1 1 calc R U . . .
C7 C 0.6147(8) 1.0659(6) 0.1308(5) 0.040(2) Uani 1 1 d . . . . .
H7 H 0.549141 1.052995 0.103980 0.048 Uiso 1 1 calc R U . . .
C8 C 0.6207(8) 1.0986(6) 0.2003(5) 0.043(2) Uani 1 1 d . . . . .
H8 H 0.560699 1.111673 0.227478 0.052 Uiso 1 1 calc R U . . .
C9 C 0.7372(10) 1.1084(6) 0.2219(6) 0.052(3) Uani 1 1 d . . . . .
H9 H 0.766243 1.127914 0.266120 0.063 Uiso 1 1 calc R U . . .
C10 C 0.7999(8) 1.0827(6) 0.1632(6) 0.049(2) Uani 1 1 d . . . . .
H10 H 0.877164 1.083858 0.162068 0.059 Uiso 1 1 calc R U . . .
C11 C 0.3851(6) 0.8050(6) 0.0911(5) 0.0366(19) Uani 1 1 d . . . . .
H11 H 0.365410 0.782485 0.046111 0.044 Uiso 1 1 calc R U . . .
C12 C 0.4178(7) 0.7582(6) 0.1530(5) 0.039(2) Uani 1 1 d . . . . .
H12 H 0.421854 0.699756 0.156325 0.046 Uiso 1 1 calc R U . . .
C13 C 0.4429(7) 0.8150(6) 0.2082(5) 0.0389(19) Uani 1 1 d . . . . .
H13 H 0.467605 0.801269 0.254895 0.047 Uiso 1 1 calc R U . . .
C14 C 0.4241(7) 0.8985(6) 0.1807(5) 0.0369(19) Uani 1 1 d . . . . .
H14 H 0.434488 0.948715 0.206008 0.044 Uiso 1 1 calc R U . . .
C15 C 0.3872(6) 0.8902(6) 0.1083(5) 0.0358(19) Uani 1 1 d . . . . .
H15 H 0.367487 0.934185 0.077158 0.043 Uiso 1 1 calc R U . . .
C16 C 0.8025(7) 0.7425(6) 0.2334(4) 0.0334(17) Uani 1 1 d . . . . .
H16 H 0.856022 0.766891 0.269332 0.040 Uiso 1 1 calc R U . . .
C17 C 0.7004(7) 0.7160(6) 0.2730(5) 0.038(2) Uani 1 1 d . . . . .
H17A H 0.643670 0.694236 0.238588 0.046 Uiso 1 1 calc R U . . .
H17B H 0.669880 0.764933 0.295945 0.046 Uiso 1 1 calc R U . . .
C18 C 0.7297(8) 0.6474(7) 0.3305(5) 0.048(2) Uani 1 1 d . . . . .
H18A H 0.778816 0.671553 0.368260 0.058 Uiso 1 1 calc R U . . .
H18B H 0.662024 0.629245 0.351656 0.058 Uiso 1 1 calc R U . . .
C19 C 0.7857(9) 0.5723(7) 0.2990(6) 0.050(2) Uani 1 1 d . . . . .
H19A H 0.807144 0.532644 0.336986 0.060 Uiso 1 1 calc R U . . .
H19B H 0.733676 0.544125 0.265190 0.060 Uiso 1 1 calc R U . . .
C20 C 0.8883(8) 0.5987(7) 0.2611(6) 0.051(2) Uani 1 1 d . . . . .
H20A H 0.920499 0.549820 0.238960 0.061 Uiso 1 1 calc R U . . .
H20B H 0.943618 0.621692 0.295828 0.061 Uiso 1 1 calc R U . . .
C21 C 0.8575(7) 0.6653(6) 0.2036(5) 0.0357(18) Uani 1 1 d . . . . .
H21A H 0.924544 0.682398 0.181022 0.043 Uiso 1 1 calc R U . . .
H21B H 0.807298 0.640151 0.166867 0.043 Uiso 1 1 calc R U . . .
C22 C 0.8894(7) 0.8272(6) 0.1112(4) 0.0370(19) Uani 1 1 d . . . . .
H22 H 0.897475 0.768821 0.095128 0.044 Uiso 1 1 calc R U . . .
C23 C 0.8815(6) 0.8803(6) 0.0441(4) 0.0336(18) Uani 1 1 d . . . . .
H23A H 0.877534 0.939425 0.056962 0.040 Uiso 1 1 calc R U . . .
H23B H 0.813966 0.865946 0.015506 0.040 Uiso 1 1 calc R U . . .
C24 C 0.9829(7) 0.8654(6) 0.0001(5) 0.041(2) Uani 1 1 d . . . . .
H24A H 0.977857 0.901385 -0.041969 0.049 Uiso 1 1 calc R U . . .
H24B H 0.983127 0.807214 -0.016087 0.049 Uiso 1 1 calc R U . . .
C25 C 1.0912(7) 0.8837(7) 0.0438(5) 0.048(2) Uani 1 1 d . . . . .
H25A H 1.153647 0.868763 0.015799 0.058 Uiso 1 1 calc R U . . .
H25B H 1.095784 0.943726 0.053794 0.058 Uiso 1 1 calc R U . . .
C26 C 1.0999(8) 0.8355(7) 0.1140(5) 0.048(2) Uani 1 1 d . . . . .
H26A H 1.164726 0.854962 0.142894 0.057 Uiso 1 1 calc R U . . .
H26B H 1.109958 0.775987 0.104259 0.057 Uiso 1 1 calc R U . . .
C27 C 0.9950(7) 0.8475(6) 0.1562(5) 0.040(2) Uani 1 1 d . . . . .
H27A H 0.999875 0.811131 0.198052 0.047 Uiso 1 1 calc R U . . .
H27B H 0.991802 0.905368 0.172677 0.047 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C1 1.914(9) . ?
W1 C2 1.966(10) . ?
W1 C9 2.326(9) . ?
W1 C10 2.355(10) . ?
W1 C8 2.371(9) . ?
W1 C6 2.379(9) . ?
W1 C7 2.383(8) . ?
W1 P1 2.405(2) . ?
W1 W2 3.0243(5) . ?
W2 N1 1.779(7) . ?
W2 C11 2.325(7) . ?
W2 C15 2.351(7) . ?
W2 P2 2.385(2) . ?
W2 C12 2.397(8) . ?
W2 C14 2.399(8) . ?
W2 C13 2.425(9) . ?
W2 P1 2.4685(19) . ?
P1 C22 1.864(9) . ?
P1 C16 1.879(8) . ?
P2 O3 1.567(6) . ?
P2 O5 1.579(7) . ?
P2 O4 1.616(6) . ?
N1 O6 1.221(9) . ?
O1 C1 1.182(11) . ?
O2 C2 1.144(11) . ?
O3 C3 1.455(11) . ?
O4 C4 1.451(12) . ?
O5 C5 1.423(13) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C10 1.412(14) . ?
C6 C7 1.425(13) . ?
C6 H6 0.9300 . ?
C7 C8 1.395(13) . ?
C7 H7 0.9300 . ?
C8 C9 1.441(15) . ?
C8 H8 0.9300 . ?
C9 C10 1.427(16) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C15 1.388(13) . ?
C11 C12 1.409(13) . ?
C11 H11 0.9300 . ?
C12 C13 1.387(14) . ?
C12 H12 0.9300 . ?
C13 C14 1.433(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.403(12) . ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C21 1.513(12) . ?
C16 C17 1.530(11) . ?
C16 H16 0.9800 . ?
C17 C18 1.553(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.505(15) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.517(14) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.536(12) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 C23 1.507(11) . ?
C22 C27 1.512(13) . ?
C22 H22 0.9800 . ?
C23 C24 1.530(11) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.520(13) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 C26 1.516(13) . ?
C25 H25A 0.9700 . ?
C25 H25B 0.9700 . ?
C26 C27 1.538(13) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?

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
C1 W1 C2 81.0(4) . . ?
C1 W1 C9 105.1(4) . . ?
C2 W1 C9 93.3(4) . . ?
C1 W1 C10 140.3(4) . . ?
C2 W1 C10 94.5(4) . . ?
C9 W1 C10 35.5(4) . . ?
C1 W1 C8 91.5(4) . . ?
C2 W1 C8 124.2(4) . . ?
C9 W1 C8 35.7(4) . . ?
C10 W1 C8 58.7(4) . . ?
C1 W1 C6 147.0(3) . . ?
C2 W1 C6 125.1(4) . . ?
C9 W1 C6 58.5(4) . . ?
C10 W1 C6 34.7(3) . . ?
C8 W1 C6 58.1(3) . . ?
C1 W1 C7 112.5(4) . . ?
C2 W1 C7 150.0(4) . . ?
C9 W1 C7 57.9(3) . . ?
C10 W1 C7 57.6(3) . . ?
C8 W1 C7 34.1(3) . . ?
C6 W1 C7 34.8(3) . . ?
C1 W1 P1 100.5(3) . . ?
C2 W1 P1 76.9(3) . . ?
C9 W1 P1 150.8(3) . . ?
C10 W1 P1 116.9(3) . . ?
C8 W1 P1 157.4(2) . . ?
C6 W1 P1 104.8(2) . . ?
C7 W1 P1 123.5(2) . . ?
C1 W1 W2 87.7(3) . . ?
C2 W1 W2 125.0(3) . . ?
C9 W1 W2 141.3(3) . . ?
C10 W1 W2 124.8(3) . . ?
C8 W1 W2 109.5(2) . . ?
C6 W1 W2 91.1(2) . . ?
C7 W1 W2 83.4(2) . . ?
P1 W1 W2 52.59(5) . . ?
N1 W2 C11 103.0(3) . . ?
N1 W2 C15 92.4(3) . . ?
C11 W2 C15 34.5(3) . . ?
N1 W2 P2 88.9(2) . . ?
C11 W2 P2 86.7(2) . . ?
C15 W2 P2 119.5(2) . . ?
N1 W2 C12 137.0(3) . . ?
C11 W2 C12 34.7(3) . . ?
C15 W2 C12 57.2(3) . . ?
P2 W2 C12 82.7(2) . . ?
N1 W2 C14 115.5(3) . . ?
C11 W2 C14 57.2(3) . . ?
C15 W2 C14 34.3(3) . . ?
P2 W2 C14 139.1(2) . . ?
C12 W2 C14 56.9(3) . . ?
N1 W2 C13 148.6(3) . . ?
C11 W2 C13 56.7(3) . . ?
C15 W2 C13 57.0(3) . . ?
P2 W2 C13 111.3(2) . . ?
C12 W2 C13 33.4(3) . . ?
C14 W2 C13 34.5(3) . . ?
N1 W2 P1 95.7(2) . . ?
C11 W2 P1 158.7(2) . . ?
C15 W2 P1 155.6(2) . . ?
P2 W2 P1 83.69(7) . . ?
C12 W2 P1 124.8(2) . . ?
C14 W2 P1 122.7(2) . . ?
C13 W2 P1 109.8(2) . . ?
N1 W2 W1 89.5(2) . . ?
C11 W2 W1 138.2(2) . . ?
C15 W2 W1 106.5(2) . . ?
P2 W2 W1 133.93(5) . . ?
C12 W2 W1 125.8(2) . . ?
C14 W2 W1 81.3(2) . . ?
C13 W2 W1 92.6(2) . . ?
P1 W2 W1 50.71(5) . . ?
C22 P1 C16 101.4(4) . . ?
C22 P1 W1 116.0(3) . . ?
C16 P1 W1 120.0(3) . . ?
C22 P1 W2 123.5(3) . . ?
C16 P1 W2 119.5(3) . . ?
W1 P1 W2 76.70(6) . . ?
O3 P2 O5 108.4(4) . . ?
O3 P2 O4 103.8(3) . . ?
O5 P2 O4 98.4(4) . . ?
O3 P2 W2 115.2(3) . . ?
O5 P2 W2 114.6(3) . . ?
O4 P2 W2 114.7(3) . . ?
O6 N1 W2 171.6(6) . . ?
C3 O3 P2 126.8(6) . . ?
C4 O4 P2 118.2(6) . . ?
C5 O5 P2 126.8(8) . . ?
O1 C1 W1 173.8(8) . . ?
O2 C2 W1 177.2(9) . . ?
O3 C3 H3A 109.5 . . ?
O3 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
O3 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O4 C4 H4A 109.5 . . ?
O4 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
O4 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 H5A 109.5 . . ?
O5 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
O5 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C10 C6 C7 107.3(9) . . ?
C10 C6 W1 71.7(5) . . ?
C7 C6 W1 72.7(5) . . ?
C10 C6 H6 126.4 . . ?
C7 C6 H6 126.4 . . ?
W1 C6 H6 121.0 . . ?
C8 C7 C6 109.7(8) . . ?
C8 C7 W1 72.5(5) . . ?
C6 C7 W1 72.5(5) . . ?
C8 C7 H7 125.1 . . ?
C6 C7 H7 125.1 . . ?
W1 C7 H7 121.5 . . ?
C7 C8 C9 107.1(9) . . ?
C7 C8 W1 73.4(5) . . ?
C9 C8 W1 70.4(5) . . ?
C7 C8 H8 126.5 . . ?
C9 C8 H8 126.5 . . ?
W1 C8 H8 121.5 . . ?
C10 C9 C8 107.7(9) . . ?
C10 C9 W1 73.4(5) . . ?
C8 C9 W1 73.9(5) . . ?
C10 C9 H9 126.2 . . ?
C8 C9 H9 126.2 . . ?
W1 C9 H9 118.6 . . ?
C6 C10 C9 108.2(9) . . ?
C6 C10 W1 73.6(5) . . ?
C9 C10 W1 71.1(5) . . ?
C6 C10 H10 125.9 . . ?
C9 C10 H10 125.9 . . ?
W1 C10 H10 121.1 . . ?
C15 C11 C12 108.8(8) . . ?
C15 C11 W2 73.7(4) . . ?
C12 C11 W2 75.4(5) . . ?
C15 C11 H11 125.6 . . ?
C12 C11 H11 125.6 . . ?
W2 C11 H11 117.2 . . ?
C13 C12 C11 107.7(8) . . ?
C13 C12 W2 74.4(5) . . ?
C11 C12 W2 69.9(4) . . ?
C13 C12 H12 126.1 . . ?
C11 C12 H12 126.1 . . ?
W2 C12 H12 121.3 . . ?
C12 C13 C14 108.2(8) . . ?
C12 C13 W2 72.2(5) . . ?
C14 C13 W2 71.7(5) . . ?
C12 C13 H13 125.9 . . ?
C14 C13 H13 125.9 . . ?
W2 C13 H13 121.9 . . ?
C15 C14 C13 106.9(8) . . ?
C15 C14 W2 70.9(5) . . ?
C13 C14 W2 73.7(5) . . ?
C15 C14 H14 126.5 . . ?
C13 C14 H14 126.5 . . ?
W2 C14 H14 120.7 . . ?
C11 C15 C14 108.4(8) . . ?
C11 C15 W2 71.7(4) . . ?
C14 C15 W2 74.7(5) . . ?
C11 C15 H15 125.8 . . ?
C14 C15 H15 125.8 . . ?
W2 C15 H15 119.5 . . ?
C21 C16 C17 109.6(7) . . ?
C21 C16 P1 115.6(6) . . ?
C17 C16 P1 110.8(6) . . ?
C21 C16 H16 106.8 . . ?
C17 C16 H16 106.8 . . ?
P1 C16 H16 106.8 . . ?
C16 C17 C18 111.8(7) . . ?
C16 C17 H17A 109.3 . . ?
C18 C17 H17A 109.3 . . ?
C16 C17 H17B 109.3 . . ?
C18 C17 H17B 109.3 . . ?
H17A C17 H17B 107.9 . . ?
C19 C18 C17 111.8(8) . . ?
C19 C18 H18A 109.2 . . ?
C17 C18 H18A 109.2 . . ?
C19 C18 H18B 109.2 . . ?
C17 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
C20 C19 C18 111.0(9) . . ?
C20 C19 H19A 109.4 . . ?
C18 C19 H19A 109.4 . . ?
C20 C19 H19B 109.4 . . ?
C18 C19 H19B 109.4 . . ?
H19A C19 H19B 108.0 . . ?
C19 C20 C21 110.4(8) . . ?
C19 C20 H20A 109.6 . . ?
C21 C20 H20A 109.6 . . ?
C19 C20 H20B 109.6 . . ?
C21 C20 H20B 109.6 . . ?
H20A C20 H20B 108.1 . . ?
C16 C21 C20 113.0(8) . . ?
C16 C21 H21A 109.0 . . ?
C20 C21 H21A 109.0 . . ?
C16 C21 H21B 109.0 . . ?
C20 C21 H21B 109.0 . . ?
H21A C21 H21B 107.8 . . ?
C23 C22 C27 110.6(8) . . ?
C23 C22 P1 116.4(6) . . ?
C27 C22 P1 111.2(6) . . ?
C23 C22 H22 105.9 . . ?
C27 C22 H22 105.9 . . ?
P1 C22 H22 105.9 . . ?
C22 C23 C24 110.4(7) . . ?
C22 C23 H23A 109.6 . . ?
C24 C23 H23A 109.6 . . ?
C22 C23 H23B 109.6 . . ?
C24 C23 H23B 109.6 . . ?
H23A C23 H23B 108.1 . . ?
C23 C24 C25 111.4(8) . . ?
C23 C24 H24A 109.3 . . ?
C25 C24 H24A 109.3 . . ?
C23 C24 H24B 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 108.0 . . ?
C26 C25 C24 112.3(8) . . ?
C26 C25 H25A 109.1 . . ?
C24 C25 H25A 109.1 . . ?
C26 C25 H25B 109.1 . . ?
C24 C25 H25B 109.1 . . ?
H25A C25 H25B 107.9 . . ?
C25 C26 C27 111.4(8) . . ?
C25 C26 H26A 109.3 . . ?
C27 C26 H26A 109.3 . . ?
C25 C26 H26B 109.3 . . ?
C27 C26 H26B 109.3 . . ?
H26A C26 H26B 108.0 . . ?
C22 C27 C26 112.1(8) . . ?
C22 C27 H27A 109.2 . . ?
C26 C27 H27A 109.2 . . ?
C22 C27 H27B 109.2 . . ?
C26 C27 H27B 109.2 . . ?
H27A C27 H27B 107.9 . . ?





_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene and petroleum ether'
