# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_4216
_database_code_depnum_ccdc_archive 'CCDC 1470406'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2018-06-15 downloaded from the CCDC.
;
_audit_creation_date             2015-09-09
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        JF-163
_chemical_formula_moiety         'C18 H19 O6 P W'
_chemical_formula_sum            'C18 H19 O6 P W'
_chemical_formula_weight         546.15
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.7589(3)
_cell_length_b                   10.0633(2)
_cell_length_c                   10.9128(4)
_cell_angle_alpha                101.9656(17)
_cell_angle_beta                 90.9652(17)
_cell_angle_gamma                111.4234(17)
_cell_volume                     970.93(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3827
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    6.061
_exptl_absorpt_correction_T_max  0.8158
_exptl_absorpt_correction_T_min  0.3528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13184
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.998
_diffrn_reflns_theta_min         2.807
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4472
_reflns_number_total             4684
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.343
_refine_diff_density_min         -1.628
_refine_diff_density_rms         0.139
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         4684
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0233
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0222P)²+1.3122P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0548
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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
W W 0.90978(2) 0.79991(2) 0.67750(2) 0.01621(5) Uani 1 1 d . . . . .
P P 0.64800(8) 0.68520(8) 0.71704(7) 0.01477(15) Uani 1 1 d . . . . .
O1 O 0.5681(2) 0.5034(2) 0.6722(2) 0.0190(4) Uani 1 1 d . . . . .
O2 O 1.2323(3) 0.9401(3) 0.5996(3) 0.0427(7) Uani 1 1 d . . . . .
O3 O 1.0573(3) 0.8688(3) 0.9587(2) 0.0314(6) Uani 1 1 d . . . . .
O4 O 0.9287(3) 0.4830(3) 0.6300(3) 0.0330(6) Uani 1 1 d . . . . .
O5 O 0.8007(3) 0.7505(3) 0.3888(2) 0.0317(6) Uani 1 1 d . . . . .
O6 O 0.9012(3) 1.1193(3) 0.7328(3) 0.0295(6) Uani 1 1 d . . . . .
C1 C 0.5732(3) 0.5538(3) 0.8103(3) 0.0173(6) Uani 1 1 d . . . . .
H1 H 0.4762 0.5494 0.8414 0.021 Uiso 1 1 calc R . . . .
C2 C 0.6668(3) 0.5121(3) 0.8927(3) 0.0172(6) Uani 1 1 d . . . . .
C3 C 0.7334(3) 0.6107(3) 1.0082(3) 0.0184(6) Uani 1 1 d . . . . .
C4 C 0.8199(3) 0.5748(3) 1.0884(3) 0.0217(6) Uani 1 1 d . . . . .
H4 H 0.8660 0.6416 1.1661 0.026 Uiso 1 1 calc R . . . .
C5 C 0.8395(4) 0.4421(4) 1.0560(3) 0.0238(7) Uani 1 1 d . . . . .
H5 H 0.9000 0.4190 1.1105 0.029 Uiso 1 1 calc R . . . .
C6 C 0.7701(4) 0.3440(3) 0.9437(3) 0.0219(6) Uani 1 1 d . . . . .
H6 H 0.7820 0.2526 0.9229 0.026 Uiso 1 1 calc R . . . .
C7 C 0.6829(3) 0.3762(3) 0.8601(3) 0.0183(6) Uani 1 1 d . . . . .
C8 C 0.7093(4) 0.7527(3) 1.0483(3) 0.0234(7) Uani 1 1 d . . . . .
H8A H 0.7462 0.8131 0.9871 0.035 Uiso 1 1 calc GR . . . .
H8B H 0.7627 0.8057 1.1315 0.035 Uiso 1 1 calc GR . . . .
H8C H 0.6034 0.7316 1.0523 0.035 Uiso 1 1 calc GR . . . .
C9 C 0.6076(4) 0.2622(3) 0.7412(3) 0.0256(7) Uani 1 1 d . . . . .
H9A H 0.5055 0.2552 0.7275 0.038 Uiso 1 1 calc GR . . . .
H9B H 0.6076 0.1670 0.7492 0.038 Uiso 1 1 calc GR . . . .
H9C H 0.6610 0.2905 0.6696 0.038 Uiso 1 1 calc GR . . . .
C10 C 0.5041(3) 0.7592(3) 0.6891(3) 0.0175(6) Uani 1 1 d . . . . .
C11 C 0.5442(3) 0.8413(3) 0.5827(3) 0.0213(6) Uani 1 1 d . . . . .
H11A H 0.6395 0.9236 0.6076 0.032 Uiso 1 1 calc GR . . . .
H11B H 0.4674 0.8786 0.5665 0.032 Uiso 1 1 calc GR . . . .
H11C H 0.5511 0.7742 0.5061 0.032 Uiso 1 1 calc GR . . . .
C12 C 0.5027(4) 0.8650(4) 0.8130(3) 0.0263(7) Uani 1 1 d . . . . .
H12A H 0.4711 0.8099 0.8786 0.039 Uiso 1 1 calc GR . . . .
H12B H 0.4339 0.9126 0.8001 0.039 Uiso 1 1 calc GR . . . .
H12C H 0.6024 0.9397 0.8392 0.039 Uiso 1 1 calc GR . . . .
C13 C 0.3514(4) 0.6355(4) 0.6495(3) 0.0257(7) Uani 1 1 d . . . . .
H13A H 0.3550 0.5688 0.5713 0.039 Uiso 1 1 calc GR . . . .
H13B H 0.2778 0.6775 0.6360 0.039 Uiso 1 1 calc GR . . . .
H13C H 0.3239 0.5812 0.7160 0.039 Uiso 1 1 calc GR . . . .
C14 C 1.1161(4) 0.8879(4) 0.6295(3) 0.0251(7) Uani 1 1 d . . . . .
C15 C 0.9998(4) 0.8418(3) 0.8598(3) 0.0217(6) Uani 1 1 d . . . . .
C16 C 0.9198(4) 0.5943(3) 0.6460(3) 0.0223(6) Uani 1 1 d . . . . .
C17 C 0.8369(4) 0.7663(3) 0.4931(3) 0.0208(6) Uani 1 1 d . . . . .
C18 C 0.9017(3) 1.0039(3) 0.7135(3) 0.0205(6) Uani 1 1 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
W P 2.4768(8) . ?
W C14 2.009(3) . ?
W C15 2.057(3) . ?
W C16 2.065(3) . ?
W C17 2.040(3) . ?
W C18 2.040(3) . ?
P O1 1.664(2) . ?
P C1 1.788(3) . ?
P C10 1.861(3) . ?
O1 C1 1.481(4) . ?
O2 C14 1.147(4) . ?
O3 C15 1.140(4) . ?
O4 C16 1.133(4) . ?
O5 C17 1.148(4) . ?
O6 C18 1.138(4) . ?
C1 H1 1.0000 . ?
C1 C2 1.493(4) . ?
C2 C3 1.406(4) . ?
C2 C7 1.407(4) . ?
C3 C4 1.393(5) . ?
C3 C8 1.510(4) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(5) . ?
C5 H5 0.9500 . ?
C5 C6 1.384(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.400(5) . ?
C7 C9 1.508(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.537(4) . ?
C10 C12 1.541(4) . ?
C10 C13 1.536(4) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C14 W P 175.07(11) . . ?
C14 W C15 88.24(14) . . ?
C14 W C16 91.57(12) . . ?
C14 W C17 87.29(14) . . ?
C14 W C18 88.52(12) . . ?
C15 W P 96.66(9) . . ?
C15 W C16 89.14(13) . . ?
C16 W P 87.89(9) . . ?
C17 W P 87.82(9) . . ?
C17 W C15 175.51(12) . . ?
C17 W C16 91.23(13) . . ?
C18 W P 92.15(9) . . ?
C18 W C15 89.37(13) . . ?
C18 W C16 178.50(12) . . ?
C18 W C17 90.26(13) . . ?
O1 P W 117.27(8) . . ?
O1 P C1 50.65(12) . . ?
O1 P C10 106.91(13) . . ?
C1 P W 127.58(11) . . ?
C1 P C10 106.95(14) . . ?
C10 P W 123.69(10) . . ?
C1 O1 P 69.01(14) . . ?
P C1 H1 114.8 . . ?
O1 C1 P 60.34(13) . . ?
O1 C1 H1 114.8 . . ?
O1 C1 C2 118.0(2) . . ?
C2 C1 P 123.2(2) . . ?
C2 C1 H1 114.8 . . ?
C3 C2 C1 117.6(3) . . ?
C3 C2 C7 120.5(3) . . ?
C7 C2 C1 121.8(3) . . ?
C2 C3 C8 121.2(3) . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 C8 119.4(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.7(3) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 120.2 . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 H5 120.2 . . ?
C5 C6 H6 119.2 . . ?
C5 C6 C7 121.6(3) . . ?
C7 C6 H6 119.2 . . ?
C2 C7 C9 123.2(3) . . ?
C6 C7 C2 118.3(3) . . ?
C6 C7 C9 118.5(3) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 P 109.3(2) . . ?
C11 C10 C12 110.5(2) . . ?
C12 C10 P 107.0(2) . . ?
C13 C10 P 111.2(2) . . ?
C13 C10 C11 108.1(3) . . ?
C13 C10 C12 110.8(3) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O2 C14 W 177.8(3) . . ?
O3 C15 W 176.2(3) . . ?
O4 C16 W 178.4(3) . . ?
O5 C17 W 177.6(3) . . ?
O6 C18 W 178.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W P O1 C1 117.68(15) . . . . ?
W P C1 O1 -96.70(15) . . . . ?
W P C1 C2 9.1(3) . . . . ?
W P C10 C11 28.8(2) . . . . ?
W P C10 C12 -90.8(2) . . . . ?
W P C10 C13 148.11(19) . . . . ?
P O1 C1 C2 -114.3(3) . . . . ?
P C1 C2 C3 76.9(3) . . . . ?
P C1 C2 C7 -106.3(3) . . . . ?
O1 P C1 C2 105.8(3) . . . . ?
O1 P C10 C11 -112.3(2) . . . . ?
O1 P C10 C12 128.1(2) . . . . ?
O1 P C10 C13 7.0(3) . . . . ?
O1 C1 C2 C3 148.1(3) . . . . ?
O1 C1 C2 C7 -35.1(4) . . . . ?
C1 P C10 C11 -165.4(2) . . . . ?
C1 P C10 C12 75.0(2) . . . . ?
C1 P C10 C13 -46.1(3) . . . . ?
C1 C2 C3 C4 179.1(3) . . . . ?
C1 C2 C3 C8 0.8(4) . . . . ?
C1 C2 C7 C6 -178.6(3) . . . . ?
C1 C2 C7 C9 -0.2(4) . . . . ?
C2 C3 C4 C5 -0.8(4) . . . . ?
C3 C2 C7 C6 -1.9(4) . . . . ?
C3 C2 C7 C9 176.5(3) . . . . ?
C3 C4 C5 C6 -1.1(5) . . . . ?
C4 C5 C6 C7 1.4(5) . . . . ?
C5 C6 C7 C2 0.0(5) . . . . ?
C5 C6 C7 C9 -178.4(3) . . . . ?
C7 C2 C3 C4 2.2(4) . . . . ?
C7 C2 C3 C8 -176.1(3) . . . . ?
C8 C3 C4 C5 177.6(3) . . . . ?
C10 P O1 C1 -98.32(18) . . . . ?
C10 P C1 O1 98.24(16) . . . . ?
C10 P C1 C2 -155.9(2) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_3979
_database_code_depnum_ccdc_archive 'CCDC 1470409'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2018-06-15 downloaded from the CCDC.
;
_audit_creation_date             2015-03-23
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        JF-85
_chemical_formula_moiety         'C23 H11 F10 O7 P W'
_chemical_formula_sum            'C23 H11 F10 O7 P W'
_chemical_formula_weight         804.14
_chemical_melting_point          ?
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'
F F 0.0171 0.0103 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   11.2835(6)
_cell_length_b                   13.5886(5)
_cell_length_c                   17.7347(10)
_cell_angle_alpha                90
_cell_angle_beta                 108.059(4)
_cell_angle_gamma                90
_cell_volume                     2585.3(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8255
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      2.82
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.645
_exptl_absorpt_correction_T_max  0.9133
_exptl_absorpt_correction_T_min  0.5323
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plank
_exptl_crystal_F_000             1536
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1152
_diffrn_reflns_av_unetI/netI     0.1256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22564
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.843
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3693
_reflns_number_total             6227
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         2.338
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     382
_refine_ls_number_reflns         6227
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0505
_refine_ls_restrained_S_all      0.864
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0378P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1020
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
2.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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
W W 0.16539(3) 0.84762(3) 0.18104(2) 0.02870(9) Uani 1 1 d . . . . .
P P 0.01284(18) 0.83962(19) 0.25489(11) 0.0290(4) Uani 1 1 d . . . . .
F1 F -0.3302(5) 0.9197(4) 0.2977(3) 0.0405(12) Uani 1 1 d . . . . .
F2 F -0.5319(5) 1.0308(4) 0.2757(3) 0.0428(12) Uani 1 1 d . . . . .
F3 F -0.6213(4) 1.1404(4) 0.1407(3) 0.0424(12) Uani 1 1 d . . . . .
F4 F -0.5049(5) 1.1343(4) 0.0284(3) 0.0526(15) Uani 1 1 d . . . . .
F5 F -0.3037(5) 1.0181(4) 0.0483(3) 0.0483(14) Uani 1 1 d . . . . .
F6 F -0.4582(5) 0.7404(4) 0.2001(3) 0.0387(12) Uani 1 1 d . . . . .
F7 F -0.6228(4) 0.6415(5) 0.0826(3) 0.0485(13) Uani 1 1 d . . . . .
F8 F -0.5578(5) 0.5784(4) -0.0446(3) 0.0491(13) Uani 1 1 d . . . . .
F9 F -0.3247(5) 0.6140(4) -0.0513(3) 0.0546(15) Uani 1 1 d . . . . .
F10 F -0.1599(5) 0.7143(4) 0.0639(3) 0.0479(14) Uani 1 1 d . . . . .
O1 O -0.0892(5) 0.9306(4) 0.2361(3) 0.0318(13) Uani 1 1 d . . . . .
O2 O -0.0902(5) 0.7519(4) 0.2242(3) 0.0320(13) Uani 1 1 d . . . . .
O3 O 0.3570(5) 0.8637(5) 0.0844(3) 0.0416(15) Uani 1 1 d . . . . .
O4 O 0.1874(6) 1.0771(5) 0.2183(4) 0.0515(17) Uani 1 1 d . . . . .
O5 O -0.0497(6) 0.8991(5) 0.0206(4) 0.0509(17) Uani 1 1 d . . . . .
O6 O 0.1295(7) 0.6195(6) 0.1453(5) 0.056(2) Uani 1 1 d . . . . .
O7 O 0.4109(6) 0.7962(5) 0.3218(4) 0.0462(16) Uani 1 1 d . . . . .
C1 C -0.2021(7) 0.8969(6) 0.1779(5) 0.0294(18) Uani 1 1 d . . . . .
H1 H -0.1882 0.8965 0.1249 0.035 Uiso 1 1 calc R . . . .
C2 C -0.2168(7) 0.7893(6) 0.2018(5) 0.0297(18) Uani 1 1 d . . . . .
H2 H -0.2471 0.7888 0.2492 0.036 Uiso 1 1 calc R . . . .
C3 C -0.3106(7) 0.9634(6) 0.1732(5) 0.0286(17) Uani 1 1 d . . . . .
C4 C -0.3708(8) 0.9721(6) 0.2307(4) 0.0305(18) Uani 1 1 d . . . . .
C5 C -0.4749(8) 1.0297(6) 0.2196(5) 0.0342(19) Uani 1 1 d . . . . .
C6 C -0.5215(8) 1.0841(6) 0.1514(5) 0.0337(18) Uani 1 1 d . . . . .
C7 C -0.4617(8) 1.0796(7) 0.0947(5) 0.038(2) Uani 1 1 d . . . . .
C8 C -0.3604(8) 1.0209(7) 0.1054(5) 0.0349(19) Uani 1 1 d . . . . .
C9 C -0.3045(7) 0.7297(6) 0.1361(5) 0.0281(17) Uani 1 1 d . . . . .
C10 C -0.4231(8) 0.7093(7) 0.1381(5) 0.0335(19) Uani 1 1 d . . . . .
C11 C -0.5090(7) 0.6587(7) 0.0781(4) 0.0347(17) Uani 1 1 d . . . . .
C12 C -0.4743(8) 0.6289(6) 0.0147(5) 0.037(2) Uani 1 1 d . . . . .
C13 C -0.3550(8) 0.6470(8) 0.0104(4) 0.0382(18) Uani 1 1 d . . . . .
C14 C -0.2738(8) 0.6974(6) 0.0708(5) 0.0322(19) Uani 1 1 d . . . . .
C15 C 0.0632(7) 0.8368(8) 0.3652(4) 0.041(2) Uani 1 1 d . . . . .
C16 C 0.1360(9) 0.9311(8) 0.3940(5) 0.049(3) Uani 1 1 d . . . . .
H16A H 0.2080 0.9339 0.3743 0.073 Uiso 1 1 calc GR . . . .
H16B H 0.1649 0.9321 0.4521 0.073 Uiso 1 1 calc GR . . . .
H16C H 0.0821 0.9880 0.3742 0.073 Uiso 1 1 calc GR . . . .
C17 C -0.0521(9) 0.8309(10) 0.3949(5) 0.055(3) Uani 1 1 d . . . . .
H17A H -0.1023 0.8907 0.3793 0.083 Uiso 1 1 calc GR . . . .
H17B H -0.0245 0.8250 0.4529 0.083 Uiso 1 1 calc GR . . . .
H17C H -0.1024 0.7734 0.3715 0.083 Uiso 1 1 calc GR . . . .
C18 C 0.1391(11) 0.7422(9) 0.3926(6) 0.056(3) Uani 1 1 d . . . . .
H18A H 0.0905 0.6854 0.3659 0.084 Uiso 1 1 calc GR . . . .
H18B H 0.1582 0.7350 0.4501 0.084 Uiso 1 1 calc GR . . . .
H18C H 0.2169 0.7459 0.3791 0.084 Uiso 1 1 calc GR . . . .
C19 C 0.2854(8) 0.8572(7) 0.1187(5) 0.0349(18) Uani 1 1 d . . . . .
C20 C 0.1789(8) 0.9942(7) 0.2044(5) 0.035(2) Uani 1 1 d . . . . .
C21 C 0.0253(9) 0.8791(6) 0.0795(6) 0.037(2) Uani 1 1 d . . . . .
C22 C 0.1434(8) 0.7014(7) 0.1593(5) 0.0319(19) Uani 1 1 d . . . . .
C23 C 0.3200(9) 0.8163(6) 0.2748(5) 0.034(2) Uani 1 1 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
W P 2.4673(19) . ?
W C19 2.001(8) . ?
W C20 2.031(10) . ?
W C21 2.040(10) . ?
W C22 2.025(10) . ?
W C23 2.047(9) . ?
P O1 1.651(6) . ?
P O2 1.636(6) . ?
P C15 1.861(8) . ?
F1 C4 1.338(9) . ?
F2 C5 1.341(9) . ?
F3 C6 1.325(9) . ?
F4 C7 1.349(10) . ?
F5 C8 1.357(9) . ?
F6 C10 1.349(9) . ?
F7 C11 1.332(9) . ?
F8 C12 1.361(9) . ?
F9 C13 1.321(9) . ?
F10 C14 1.347(10) . ?
O1 C1 1.443(10) . ?
O2 C2 1.451(9) . ?
O3 C19 1.155(9) . ?
O4 C20 1.151(10) . ?
O5 C21 1.154(11) . ?
O6 C22 1.140(10) . ?
O7 C23 1.136(10) . ?
C1 H1 1.0000 . ?
C1 C2 1.546(11) . ?
C1 C3 1.503(11) . ?
C2 H2 1.0000 . ?
C2 C9 1.509(11) . ?
C3 C4 1.394(11) . ?
C3 C8 1.397(12) . ?
C4 C5 1.374(12) . ?
C5 C6 1.376(12) . ?
C6 C7 1.376(12) . ?
C7 C8 1.357(12) . ?
C9 C10 1.377(11) . ?
C9 C14 1.380(11) . ?
C10 C11 1.380(12) . ?
C11 C12 1.362(12) . ?
C12 C13 1.394(12) . ?
C13 C14 1.359(12) . ?
C15 C16 1.522(14) . ?
C15 C17 1.550(11) . ?
C15 C18 1.537(14) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 W P 178.1(3) . . ?
C19 W C20 91.6(3) . . ?
C19 W C21 88.3(3) . . ?
C19 W C22 91.3(3) . . ?
C19 W C23 84.9(3) . . ?
C20 W P 87.4(2) . . ?
C20 W C21 87.9(3) . . ?
C20 W C23 92.7(3) . . ?
C21 W P 90.0(2) . . ?
C21 W C23 173.1(3) . . ?
C22 W P 89.6(2) . . ?
C22 W C20 177.0(3) . . ?
C22 W C21 91.3(3) . . ?
C22 W C23 88.5(3) . . ?
C23 W P 96.8(2) . . ?
O1 P W 114.7(2) . . ?
O1 P C15 101.2(4) . . ?
O2 P W 113.4(2) . . ?
O2 P O1 95.7(3) . . ?
O2 P C15 106.8(4) . . ?
C15 P W 121.5(3) . . ?
C1 O1 P 108.2(5) . . ?
C2 O2 P 111.9(5) . . ?
O1 C1 H1 108.3 . . ?
O1 C1 C2 104.5(6) . . ?
O1 C1 C3 111.9(7) . . ?
C2 C1 H1 108.3 . . ?
C3 C1 H1 108.3 . . ?
C3 C1 C2 115.4(7) . . ?
O2 C2 C1 103.1(6) . . ?
O2 C2 H2 109.3 . . ?
O2 C2 C9 112.2(6) . . ?
C1 C2 H2 109.3 . . ?
C9 C2 C1 113.3(7) . . ?
C9 C2 H2 109.3 . . ?
C4 C3 C1 125.7(7) . . ?
C4 C3 C8 115.1(7) . . ?
C8 C3 C1 119.2(7) . . ?
F1 C4 C3 119.6(7) . . ?
F1 C4 C5 118.2(7) . . ?
C5 C4 C3 122.2(7) . . ?
F2 C5 C4 119.1(7) . . ?
F2 C5 C6 120.3(7) . . ?
C4 C5 C6 120.6(7) . . ?
F3 C6 C5 120.8(7) . . ?
F3 C6 C7 120.6(7) . . ?
C7 C6 C5 118.6(8) . . ?
F4 C7 C6 119.1(8) . . ?
F4 C7 C8 120.5(7) . . ?
C8 C7 C6 120.5(8) . . ?
F5 C8 C3 118.0(7) . . ?
F5 C8 C7 118.9(7) . . ?
C7 C8 C3 123.1(7) . . ?
C10 C9 C2 119.9(7) . . ?
C10 C9 C14 117.1(7) . . ?
C14 C9 C2 122.9(7) . . ?
F6 C10 C9 119.4(8) . . ?
F6 C10 C11 118.1(7) . . ?
C9 C10 C11 122.5(7) . . ?
F7 C11 C10 120.1(7) . . ?
F7 C11 C12 121.8(7) . . ?
C12 C11 C10 118.1(7) . . ?
F8 C12 C11 118.7(8) . . ?
F8 C12 C13 119.7(8) . . ?
C11 C12 C13 121.5(8) . . ?
F9 C13 C12 119.2(8) . . ?
F9 C13 C14 122.7(8) . . ?
C14 C13 C12 118.2(7) . . ?
F10 C14 C9 121.1(8) . . ?
F10 C14 C13 116.3(7) . . ?
C13 C14 C9 122.6(8) . . ?
C16 C15 P 107.0(6) . . ?
C16 C15 C17 110.6(9) . . ?
C16 C15 C18 114.1(7) . . ?
C17 C15 P 110.1(5) . . ?
C18 C15 P 107.9(7) . . ?
C18 C15 C17 107.1(9) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 H18A 109.5 . . ?
C15 C18 H18B 109.5 . . ?
C15 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O3 C19 W 178.2(8) . . ?
O4 C20 W 179.3(9) . . ?
O5 C21 W 176.7(7) . . ?
O6 C22 W 178.5(9) . . ?
O7 C23 W 173.6(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W P O1 C1 97.3(5) . . . . ?
W P O2 C2 -124.4(4) . . . . ?
W P C15 C16 60.2(7) . . . . ?
W P C15 C17 -179.5(6) . . . . ?
W P C15 C18 -63.0(8) . . . . ?
P O1 C1 C2 39.1(6) . . . . ?
P O1 C1 C3 164.6(5) . . . . ?
P O2 C2 C1 26.5(6) . . . . ?
P O2 C2 C9 148.8(6) . . . . ?
F1 C4 C5 F2 -0.3(12) . . . . ?
F1 C4 C5 C6 -179.2(8) . . . . ?
F2 C5 C6 F3 1.6(13) . . . . ?
F2 C5 C6 C7 -178.8(8) . . . . ?
F3 C6 C7 F4 1.0(13) . . . . ?
F3 C6 C7 C8 -179.2(8) . . . . ?
F4 C7 C8 F5 -0.2(13) . . . . ?
F4 C7 C8 C3 179.3(9) . . . . ?
F6 C10 C11 F7 -0.2(13) . . . . ?
F6 C10 C11 C12 178.8(8) . . . . ?
F7 C11 C12 F8 -1.5(13) . . . . ?
F7 C11 C12 C13 -179.9(9) . . . . ?
F8 C12 C13 F9 -0.4(13) . . . . ?
F8 C12 C13 C14 -179.8(8) . . . . ?
F9 C13 C14 F10 1.4(14) . . . . ?
F9 C13 C14 C9 -178.4(8) . . . . ?
O1 P O2 C2 -4.4(5) . . . . ?
O1 P C15 C16 -68.1(6) . . . . ?
O1 P C15 C17 52.1(9) . . . . ?
O1 P C15 C18 168.7(7) . . . . ?
O1 C1 C2 O2 -40.5(7) . . . . ?
O1 C1 C2 C9 -162.0(6) . . . . ?
O1 C1 C3 C4 -71.0(10) . . . . ?
O1 C1 C3 C8 110.7(9) . . . . ?
O2 P O1 C1 -21.6(5) . . . . ?
O2 P C15 C16 -167.6(6) . . . . ?
O2 P C15 C17 -47.4(9) . . . . ?
O2 P C15 C18 69.1(7) . . . . ?
O2 C2 C9 C10 140.1(8) . . . . ?
O2 C2 C9 C14 -42.9(11) . . . . ?
C1 C2 C9 C10 -103.7(9) . . . . ?
C1 C2 C9 C14 73.4(10) . . . . ?
C1 C3 C4 F1 1.4(13) . . . . ?
C1 C3 C4 C5 -175.4(8) . . . . ?
C1 C3 C8 F5 -3.5(12) . . . . ?
C1 C3 C8 C7 177.0(8) . . . . ?
C2 C1 C3 C4 48.3(11) . . . . ?
C2 C1 C3 C8 -130.0(8) . . . . ?
C2 C9 C10 F6 -2.0(12) . . . . ?
C2 C9 C10 C11 177.3(8) . . . . ?
C2 C9 C14 F10 2.8(13) . . . . ?
C2 C9 C14 C13 -177.4(9) . . . . ?
C3 C1 C2 O2 -163.8(6) . . . . ?
C3 C1 C2 C9 74.7(8) . . . . ?
C3 C4 C5 F2 176.6(8) . . . . ?
C3 C4 C5 C6 -2.3(13) . . . . ?
C4 C3 C8 F5 178.0(7) . . . . ?
C4 C3 C8 C7 -1.5(13) . . . . ?
C4 C5 C6 F3 -179.4(8) . . . . ?
C4 C5 C6 C7 0.1(13) . . . . ?
C5 C6 C7 F4 -178.6(8) . . . . ?
C5 C6 C7 C8 1.3(14) . . . . ?
C6 C7 C8 F5 180.0(8) . . . . ?
C6 C7 C8 C3 -0.6(15) . . . . ?
C8 C3 C4 F1 179.8(8) . . . . ?
C8 C3 C4 C5 2.9(13) . . . . ?
C9 C10 C11 F7 -179.5(8) . . . . ?
C9 C10 C11 C12 -0.5(14) . . . . ?
C10 C9 C14 F10 179.9(8) . . . . ?
C10 C9 C14 C13 -0.3(13) . . . . ?
C10 C11 C12 F8 179.6(8) . . . . ?
C10 C11 C12 C13 1.2(14) . . . . ?
C11 C12 C13 F9 178.0(9) . . . . ?
C11 C12 C13 C14 -1.4(14) . . . . ?
C12 C13 C14 F10 -179.3(8) . . . . ?
C12 C13 C14 C9 0.9(14) . . . . ?
C14 C9 C10 F6 -179.2(7) . . . . ?
C14 C9 C10 C11 0.1(13) . . . . ?
C15 P O1 C1 -130.0(5) . . . . ?
C15 P O2 C2 99.2(6) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
#END---------------------------------------------------------------------------

####################################################################### 
# 
# 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_4189
_database_code_depnum_ccdc_archive 'CCDC 1470407'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2018-06-15 downloaded from the CCDC.
;

_audit_creation_date             2015-07-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        JF-152
_chemical_formula_moiety         'C19 H21 O6 P W'
_chemical_formula_sum            'C19 H21 O6 P W'
_chemical_formula_weight         560.18
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9897(4)
_cell_length_b                   10.2207(4)
_cell_length_c                   11.3156(3)
_cell_angle_alpha                87.4885(19)
_cell_angle_beta                 74.0260(19)
_cell_angle_gamma                68.0590(16)
_cell_volume                     1028.02(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3684
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.727
_exptl_absorpt_correction_T_max  0.6211
_exptl_absorpt_correction_T_min  0.3541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.810
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             544
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.1
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.3852
_diffrn_reflns_av_unetI/netI     0.1889
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12583
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.993
_diffrn_reflns_theta_min         2.289
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3840
_reflns_number_total             4962
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         5.408
_refine_diff_density_min         -6.307
_refine_diff_density_rms         0.448
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4962
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1007
_refine_ls_R_factor_gt           0.0784
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1255P)²+4.0396P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2206
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C2) \\sim Ueq: with
sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C9) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of 0.08 and
sigma for terminal atoms of 0.16
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.004 and sigma for terminal atoms of 0.008
Uanis(C16) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
3.a Ternary CH refined with riding coordinates:
 C1(H1)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
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
W W 0.69580(3) 0.90033(3) 0.67864(3) 0.02289(18) Uani 1 1 d . . . . .
P P 0.8059(3) 0.6473(2) 0.7132(2) 0.0230(5) Uani 1 1 d . . . . .
O1 O 0.9934(8) 0.5691(7) 0.6738(6) 0.0283(14) Uani 1 1 d . . . . .
O2 O 0.5734(11) 1.2189(9) 0.6116(9) 0.048(2) Uani 1 1 d . . . . .
O3 O 0.6427(11) 1.0239(9) 0.9497(7) 0.041(2) Uani 1 1 d . . . . .
O4 O 1.0314(10) 0.8949(10) 0.6020(8) 0.0360(18) Uani 1 1 d . . . . .
O5 O 0.7308(13) 0.8251(12) 0.3982(8) 0.050(2) Uani 1 1 d . . . . .
O6 O 0.3656(10) 0.8969(10) 0.7572(9) 0.039(2) Uani 1 1 d . . . . .
C1 C 0.9298(11) 0.5675(9) 0.8081(8) 0.0254(18) Uani 1 1 d . . . . .
H1 H 0.9305 0.4735 0.8371 0.030 Uiso 1 1 calc R . . . .
C2 C 0.9631(11) 0.6513(9) 0.8918(9) 0.0274(18) Uani 1 1 d . U . . .
C3 C 0.8535(12) 0.7080(9) 1.0047(8) 0.027(2) Uani 1 1 d . U . . .
C4 C 0.8835(12) 0.7845(10) 1.0863(8) 0.030(2) Uani 1 1 d . U . . .
H4 H 0.8095 0.8238 1.1620 0.035 Uiso 1 1 calc R . . . .
C5 C 1.0209(13) 0.8053(10) 1.0597(10) 0.035(2) Uani 1 1 d . U . . .
C6 C 1.1244(14) 0.7464(10) 0.9511(10) 0.035(2) Uani 1 1 d . U . . .
H6 H 1.2173 0.7592 0.9323 0.042 Uiso 1 1 calc R . . . .
C7 C 1.1017(13) 0.6675(11) 0.8650(9) 0.031(2) Uani 1 1 d . U . . .
C8 C 0.7062(12) 0.6831(11) 1.0379(9) 0.035(2) Uani 1 1 d . . . . .
H8A H 0.6499 0.7266 0.9785 0.052 Uiso 1 1 calc GR . . . .
H8B H 0.6461 0.7254 1.1209 0.052 Uiso 1 1 calc GR . . . .
H8C H 0.7282 0.5813 1.0356 0.052 Uiso 1 1 calc GR . . . .
C9 C 1.0427(17) 0.8956(12) 1.1479(11) 0.045(3) Uani 1 1 d . U . . .
H9A H 1.0299 0.9887 1.1157 0.068 Uiso 1 1 calc GR . . . .
H9B H 1.1440 0.8505 1.1580 0.068 Uiso 1 1 calc GR . . . .
H9C H 0.9682 0.9065 1.2279 0.068 Uiso 1 1 calc GR . . . .
C10 C 1.2289(13) 0.6042(13) 0.7482(10) 0.037(2) Uani 1 1 d . . . . .
H10A H 1.2412 0.5064 0.7318 0.055 Uiso 1 1 calc GR . . . .
H10B H 1.3224 0.6057 0.7587 0.055 Uiso 1 1 calc GR . . . .
H10C H 1.2049 0.6597 0.6787 0.055 Uiso 1 1 calc GR . . . .
C11 C 0.7349(12) 0.5098(9) 0.6816(9) 0.029(2) Uani 1 1 d . U . . .
C12 C 0.6276(13) 0.4976(12) 0.8038(9) 0.036(2) Uani 1 1 d . U . . .
H12A H 0.6810 0.4732 0.8674 0.054 Uiso 1 1 calc GR . . . .
H12B H 0.5906 0.4237 0.7936 0.054 Uiso 1 1 calc GR . . . .
H12C H 0.5425 0.5881 0.8285 0.054 Uiso 1 1 calc GR . . . .
C13 C 0.8660(12) 0.3691(10) 0.6362(9) 0.0297(19) Uani 1 1 d . U . . .
H13A H 0.9312 0.3796 0.5571 0.044 Uiso 1 1 calc GR . . . .
H13B H 0.8270 0.2967 0.6257 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.9238 0.3405 0.6966 0.044 Uiso 1 1 calc GR . . . .
C14 C 0.6517(13) 0.5575(10) 0.5833(10) 0.035(2) Uani 1 1 d . U . . .
H14A H 0.5646 0.6455 0.6133 0.052 Uiso 1 1 calc GR . . . .
H14B H 0.6177 0.4842 0.5652 0.052 Uiso 1 1 calc GR . . . .
H14C H 0.7194 0.5735 0.5081 0.052 Uiso 1 1 calc GR . . . .
C15 C 0.6164(12) 1.1077(10) 0.6381(9) 0.0279(19) Uani 1 1 d . U . . .
C16 C 0.6649(10) 0.9732(9) 0.8501(8) 0.0181(15) Uani 1 1 d . U . . .
C17 C 0.9150(13) 0.8982(11) 0.6321(10) 0.029(2) Uani 1 1 d . U . . .
C18 C 0.7220(13) 0.8468(12) 0.5061(10) 0.026(2) Uani 1 1 d . U . . .
C19 C 0.4814(13) 0.8964(10) 0.7270(10) 0.030(2) Uani 1 1 d . 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
W P 2.464(2) . ?
W C15 2.048(9) . ?
W C16 2.009(9) . ?
W C17 2.099(12) . ?
W C18 1.971(11) . ?
W C19 2.075(12) . ?
P O1 1.673(7) . ?
P C1 1.803(10) . ?
P C11 1.879(11) . ?
O1 C1 1.479(10) . ?
O2 C15 1.114(12) . ?
O3 C16 1.190(13) . ?
O4 C17 1.106(15) . ?
O5 C18 1.224(14) . ?
O6 C19 1.110(16) . ?
C1 H1 1.0000 . ?
C1 C2 1.483(14) . ?
C2 C3 1.411(13) . ?
C2 C7 1.405(17) . ?
C3 C4 1.394(15) . ?
C3 C8 1.529(16) . ?
C4 H4 0.9500 . ?
C4 C5 1.417(17) . ?
C5 C6 1.356(16) . ?
C5 C9 1.499(17) . ?
C6 H6 0.9500 . ?
C6 C7 1.406(18) . ?
C7 C10 1.522(14) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.532(13) . ?
C11 C13 1.528(12) . ?
C11 C14 1.525(15) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 W P 175.8(3) . . ?
C15 W C17 90.1(4) . . ?
C15 W C19 91.6(4) . . ?
C16 W P 96.4(2) . . ?
C16 W C15 86.5(4) . . ?
C16 W C17 88.7(4) . . ?
C16 W C19 91.0(4) . . ?
C17 W P 87.0(3) . . ?
C18 W P 88.7(3) . . ?
C18 W C15 88.3(4) . . ?
C18 W C16 174.8(3) . . ?
C18 W C17 90.5(5) . . ?
C18 W C19 89.9(5) . . ?
C19 W P 91.2(3) . . ?
C19 W C17 178.2(3) . . ?
O1 P W 117.7(3) . . ?
O1 P C1 50.2(3) . . ?
O1 P C11 106.1(4) . . ?
C1 P W 127.1(3) . . ?
C1 P C11 106.0(4) . . ?
C11 P W 125.0(3) . . ?
C1 O1 P 69.5(5) . . ?
P C1 H1 114.8 . . ?
O1 C1 P 60.4(4) . . ?
O1 C1 H1 114.8 . . ?
O1 C1 C2 118.2(8) . . ?
C2 C1 P 122.9(6) . . ?
C2 C1 H1 114.8 . . ?
C3 C2 C1 117.5(9) . . ?
C7 C2 C1 122.2(9) . . ?
C7 C2 C3 120.2(10) . . ?
C2 C3 C8 120.5(9) . . ?
C4 C3 C2 118.7(10) . . ?
C4 C3 C8 120.8(9) . . ?
C3 C4 H4 119.0 . . ?
C3 C4 C5 122.0(9) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 C9 119.4(10) . . ?
C6 C5 C4 117.3(11) . . ?
C6 C5 C9 123.3(12) . . ?
C5 C6 H6 118.2 . . ?
C5 C6 C7 123.6(12) . . ?
C7 C6 H6 118.2 . . ?
C2 C7 C6 118.2(9) . . ?
C2 C7 C10 123.6(11) . . ?
C6 C7 C10 118.2(11) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P 105.9(7) . . ?
C13 C11 P 110.3(8) . . ?
C13 C11 C12 111.4(8) . . ?
C14 C11 P 109.8(6) . . ?
C14 C11 C12 110.5(10) . . ?
C14 C11 C13 109.0(8) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 W 177.3(10) . . ?
O3 C16 W 176.2(8) . . ?
O4 C17 W 176.7(10) . . ?
O5 C18 W 174.6(10) . . ?
O6 C19 W 177.3(11) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W P O1 C1 116.7(4) . . . . ?
W P C1 O1 -97.4(5) . . . . ?
W P C1 C2 8.9(9) . . . . ?
W P C11 C12 -94.2(7) . . . . ?
W P C11 C13 145.1(5) . . . . ?
W P C11 C14 25.0(8) . . . . ?
P O1 C1 C2 -113.8(7) . . . . ?
P C1 C2 C3 77.8(10) . . . . ?
P C1 C2 C7 -106.2(9) . . . . ?
O1 P C1 C2 106.3(9) . . . . ?
O1 P C11 C12 123.3(7) . . . . ?
O1 P C11 C13 2.6(7) . . . . ?
O1 P C11 C14 -117.5(7) . . . . ?
O1 C1 C2 C3 149.1(8) . . . . ?
O1 C1 C2 C7 -34.9(12) . . . . ?
C1 P C11 C12 70.9(8) . . . . ?
C1 P C11 C13 -49.8(7) . . . . ?
C1 P C11 C14 -169.8(7) . . . . ?
C1 C2 C3 C4 178.5(7) . . . . ?
C1 C2 C3 C8 -0.1(12) . . . . ?
C1 C2 C7 C6 -178.6(8) . . . . ?
C1 C2 C7 C10 1.2(14) . . . . ?
C2 C3 C4 C5 -0.8(13) . . . . ?
C3 C2 C7 C6 -2.7(13) . . . . ?
C3 C2 C7 C10 177.1(9) . . . . ?
C3 C4 C5 C6 -0.6(13) . . . . ?
C3 C4 C5 C9 176.5(9) . . . . ?
C4 C5 C6 C7 0.3(14) . . . . ?
C5 C6 C7 C2 1.4(14) . . . . ?
C5 C6 C7 C10 -178.5(9) . . . . ?
C7 C2 C3 C4 2.4(13) . . . . ?
C7 C2 C3 C8 -176.2(8) . . . . ?
C8 C3 C4 C5 177.9(8) . . . . ?
C9 C5 C6 C7 -176.7(10) . . . . ?
C11 P O1 C1 -97.6(5) . . . . ?
C11 P C1 O1 97.9(5) . . . . ?
C11 P C1 C2 -155.8(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_4319
_database_code_depnum_ccdc_archive 'CCDC 1470408'
_audit_update_record             
;
2016-03-24 deposited with the CCDC.
2018-06-15 downloaded from the CCDC.
;
_audit_creation_date             2015-11-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        JF-179
_chemical_formula_moiety         'C19 H21 Cr O6 P'
_chemical_formula_sum            'C19 H21 Cr O6 P'
_chemical_formula_weight         428.33
_chemical_melting_point          ?
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'
Cr Cr 0.3209 0.6236 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8816(4)
_cell_length_b                   15.0671(7)
_cell_length_c                   16.0872(5)
_cell_angle_alpha                110.802(3)
_cell_angle_beta                 95.641(3)
_cell_angle_gamma                108.864(2)
_cell_volume                     2056.39(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6931
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      1.00
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.665
_exptl_absorpt_correction_T_max  0.9541
_exptl_absorpt_correction_T_min  0.8525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.383
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             888
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.08
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23353
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         2.187
_diffrn_ambient_temperature      123.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'sealed tube'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7219
_reflns_number_total             9836
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.909
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         9836
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0959
_refine_ls_R_factor_gt           0.0650
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0737P)²+4.1708P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1587
_refine_ls_wR_factor_ref         0.1769
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C5', C6'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C1(H1), C1'(H1')
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C4'(H4'), C6'(H6')
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C8'(H8'A,H8'B,H8'C), C9'(H9'A,H9'B,
 H9'C), C10'(H10D,H10E,H10F), C12'(H12D,H12E,H12F), C13'(H13D,H13E,H13F),
 C14'(H14D,H14E,H14F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Cr Cr 0.81408(6) 0.28065(5) 0.21253(4) 0.02276(15) Uani 1 1 d . . . . .
P P 0.61465(10) 0.30527(8) 0.14603(6) 0.0230(2) Uani 1 1 d . . . . .
O1 O 0.6514(3) 0.40079(19) 0.11164(16) 0.0261(5) Uani 1 1 d . . . . .
O2 O 1.0816(3) 0.2582(3) 0.2961(2) 0.0392(7) Uani 1 1 d . . . . .
O3 O 0.6253(3) 0.1440(2) 0.2928(2) 0.0397(7) Uani 1 1 d . . . . .
O4 O 0.8852(4) 0.4679(2) 0.3914(2) 0.0449(8) Uani 1 1 d . . . . .
O5 O 1.0191(4) 0.4227(3) 0.1436(3) 0.0579(10) Uani 1 1 d . . . . .
O6 O 0.7868(4) 0.0932(2) 0.0444(2) 0.0417(7) Uani 1 1 d . . . . .
C1 C 0.5731(4) 0.3004(3) 0.0327(2) 0.0220(7) Uani 1 1 d . . . . .
H1 H 0.4673 0.2852 0.0084 0.026 Uiso 1 1 calc R . . . .
C2 C 0.6523(4) 0.2669(3) -0.0392(2) 0.0214(7) Uani 1 1 d . . . . .
C3 C 0.7582(4) 0.3371(3) -0.0612(2) 0.0230(7) Uani 1 1 d . . . . .
C4 C 0.8216(4) 0.2984(3) -0.1333(2) 0.0275(8) Uani 1 1 d . . . . .
H4 H 0.8969 0.3455 -0.1467 0.033 Uiso 1 1 calc R . . . .
C5 C 0.7780(4) 0.1940(3) -0.1854(2) 0.0291(8) Uani 1 1 d . . . . .
C6 C 0.6696(4) 0.1264(3) -0.1639(2) 0.0301(8) Uani 1 1 d . . . . .
H6 H 0.6383 0.0546 -0.1994 0.036 Uiso 1 1 calc R . . . .
C7 C 0.6053(4) 0.1600(3) -0.0926(2) 0.0258(8) Uani 1 1 d . . . . .
C8 C 0.8017(4) 0.4519(3) -0.0150(3) 0.0307(8) Uani 1 1 d . . . . .
H8A H 0.7129 0.4676 -0.0147 0.046 Uiso 1 1 calc GR . . . .
H8B H 0.8627 0.4850 -0.0483 0.046 Uiso 1 1 calc GR . . . .
H8C H 0.8577 0.4778 0.0482 0.046 Uiso 1 1 calc GR . . . .
C9 C 0.8432(5) 0.1555(4) -0.2656(3) 0.0410(11) Uani 1 1 d . . . . .
H9A H 0.8614 0.0949 -0.2666 0.061 Uiso 1 1 calc GR . . . .
H9B H 0.9362 0.2097 -0.2592 0.061 Uiso 1 1 calc GR . . . .
H9C H 0.7740 0.1368 -0.3227 0.061 Uiso 1 1 calc GR . . . .
C10 C 0.4843(4) 0.0845(3) -0.0730(3) 0.0317(9) Uani 1 1 d . . . . .
H10A H 0.5078 0.0988 -0.0078 0.048 Uiso 1 1 calc GR . . . .
H10B H 0.4755 0.0144 -0.1097 0.048 Uiso 1 1 calc GR . . . .
H10C H 0.3909 0.0913 -0.0887 0.048 Uiso 1 1 calc GR . . . .
C11 C 0.4462(4) 0.3010(3) 0.1906(2) 0.0311(9) Uani 1 1 d . . . . .
C12 C 0.4946(5) 0.3583(5) 0.2948(3) 0.0487(13) Uani 1 1 d . . . . .
H12A H 0.5517 0.3272 0.3199 0.073 Uiso 1 1 calc GR . . . .
H12B H 0.4074 0.3538 0.3200 0.073 Uiso 1 1 calc GR . . . .
H12C H 0.5556 0.4307 0.3115 0.073 Uiso 1 1 calc GR . . . .
C13 C 0.3587(5) 0.3506(5) 0.1529(3) 0.0467(12) Uani 1 1 d . . . . .
H13A H 0.4239 0.4202 0.1634 0.070 Uiso 1 1 calc GR . . . .
H13B H 0.2788 0.3540 0.1839 0.070 Uiso 1 1 calc GR . . . .
H13C H 0.3170 0.3095 0.0870 0.070 Uiso 1 1 calc GR . . . .
C14 C 0.3513(5) 0.1876(4) 0.1632(4) 0.0529(13) Uani 1 1 d . . . . .
H14A H 0.3238 0.1512 0.0962 0.079 Uiso 1 1 calc GR . . . .
H14B H 0.2620 0.1821 0.1862 0.079 Uiso 1 1 calc GR . . . .
H14C H 0.4073 0.1567 0.1895 0.079 Uiso 1 1 calc GR . . . .
C15 C 0.9792(4) 0.2668(3) 0.2651(3) 0.0286(8) Uani 1 1 d . . . . .
C16 C 0.6937(4) 0.1950(3) 0.2613(2) 0.0286(8) Uani 1 1 d . . . . .
C17 C 0.8540(4) 0.3979(3) 0.3235(3) 0.0309(8) Uani 1 1 d . . . . .
C18 C 0.9382(4) 0.3695(4) 0.1671(3) 0.0358(9) Uani 1 1 d . . . . .
C19 C 0.7913(4) 0.1634(3) 0.1052(3) 0.0298(8) Uani 1 1 d . . . . .
Cr' Cr 1.18804(6) 0.25871(4) 0.54895(4) 0.01991(14) Uani 1 1 d . . . . .
P' P 1.41197(11) 0.27204(8) 0.62625(6) 0.0253(2) Uani 1 1 d . . . . .
O1' O 1.4741(3) 0.3560(2) 0.7382(2) 0.0394(7) Uani 1 1 d . . . . .
O2' O 0.9070(3) 0.2580(2) 0.45613(19) 0.0358(7) Uani 1 1 d . . . . .
O3' O 1.3278(3) 0.4367(2) 0.4966(2) 0.0366(7) Uani 1 1 d . . . . .
O4' O 1.2100(3) 0.1132(2) 0.36683(18) 0.0378(7) Uani 1 1 d . . . . .
O5' O 0.9949(3) 0.0767(2) 0.58182(18) 0.0316(6) Uani 1 1 d . . . . .
O6' O 1.1507(3) 0.4013(2) 0.72661(18) 0.0376(7) Uani 1 1 d . . . . .
C1' C 1.4459(4) 0.2464(3) 0.7258(3) 0.0324(9) Uani 1 1 d . . . . .
H1' H 1.5367 0.2318 0.7349 0.039 Uiso 1 1 calc R . . . .
C2' C 1.3260(4) 0.1970(3) 0.7644(2) 0.0231(7) Uani 1 1 d . . . . .
C3' C 1.2599(5) 0.0905(3) 0.7259(3) 0.0360(9) Uani 1 1 d . . . . .
C4' C 1.1574(5) 0.0399(4) 0.7607(3) 0.0430(11) Uani 1 1 d . . . . .
H4' H 1.1139 -0.0331 0.7329 0.052 Uiso 1 1 calc R . . . .
C5' C 1.1164(5) 0.0916(4) 0.8340(3) 0.0451(10) Uani 1 1 d . U . . .
C6' C 1.1804(5) 0.1989(4) 0.8768(3) 0.0424(10) Uani 1 1 d . U . . .
H6' H 1.1505 0.2346 0.9285 0.051 Uiso 1 1 calc R . . . .
C7' C 1.2925(5) 0.2565(3) 0.8426(3) 0.0349(9) Uani 1 1 d . . . . .
C8' C 1.3046(6) 0.0286(4) 0.6419(3) 0.0446(11) Uani 1 1 d . . . . .
H8'A H 1.2952 0.0541 0.5943 0.067 Uiso 1 1 calc GR . . . .
H8'B H 1.2400 -0.0443 0.6180 0.067 Uiso 1 1 calc GR . . . .
H8'C H 1.4070 0.0367 0.6600 0.067 Uiso 1 1 calc GR . . . .
C9' C 1.0000(6) 0.0350(5) 0.8742(4) 0.0625(16) Uani 1 1 d . . . . .
H9'A H 1.0442 0.0055 0.9091 0.094 Uiso 1 1 calc GR . . . .
H9'B H 0.9173 -0.0201 0.8243 0.094 Uiso 1 1 calc GR . . . .
H9'C H 0.9643 0.0837 0.9147 0.094 Uiso 1 1 calc GR . . . .
C10' C 1.3649(6) 0.3693(4) 0.8947(3) 0.0461(11) Uani 1 1 d . . . . .
H10D H 1.4703 0.3915 0.8964 0.069 Uiso 1 1 calc GR . . . .
H10E H 1.3518 0.3879 0.9574 0.069 Uiso 1 1 calc GR . . . .
H10F H 1.3206 0.4032 0.8650 0.069 Uiso 1 1 calc GR . . . .
C11' C 1.5814(4) 0.2861(4) 0.5825(3) 0.0350(9) Uani 1 1 d . . . . .
C12' C 1.5794(5) 0.3261(5) 0.5093(3) 0.0495(13) Uani 1 1 d . . . . .
H12D H 1.4881 0.2826 0.4613 0.074 Uiso 1 1 calc GR . . . .
H12E H 1.6642 0.3247 0.4827 0.074 Uiso 1 1 calc GR . . . .
H12F H 1.5845 0.3969 0.5361 0.074 Uiso 1 1 calc GR . . . .
C13' C 1.5694(6) 0.1712(4) 0.5319(4) 0.0550(13) Uani 1 1 d . . . . .
H13D H 1.5807 0.1430 0.5773 0.083 Uiso 1 1 calc GR . . . .
H13E H 1.6472 0.1704 0.4987 0.083 Uiso 1 1 calc GR . . . .
H13F H 1.4729 0.1294 0.4887 0.083 Uiso 1 1 calc GR . . . .
C14' C 1.7215(5) 0.3436(5) 0.6545(4) 0.0596(16) Uani 1 1 d . . . . .
H14D H 1.7294 0.4140 0.6893 0.089 Uiso 1 1 calc GR . . . .
H14E H 1.8048 0.3456 0.6258 0.089 Uiso 1 1 calc GR . . . .
H14F H 1.7229 0.3093 0.6959 0.089 Uiso 1 1 calc GR . . . .
C15' C 1.0122(4) 0.2564(3) 0.4909(2) 0.0266(8) Uani 1 1 d . . . . .
C16' C 1.2817(4) 0.3713(3) 0.5192(2) 0.0255(8) Uani 1 1 d . . . . .
C17' C 1.2025(4) 0.1670(3) 0.4360(2) 0.0260(8) Uani 1 1 d . . . . .
C18' C 1.0726(4) 0.1441(3) 0.5714(2) 0.0234(7) Uani 1 1 d . . . . .
C19' C 1.1697(4) 0.3486(3) 0.6615(2) 0.0265(8) Uani 1 1 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
Cr P 2.3465(11) . ?
Cr C15 1.869(4) . ?
Cr C16 1.899(4) . ?
Cr C17 1.906(4) . ?
Cr C18 1.908(4) . ?
Cr C19 1.912(4) . ?
P O1 1.666(3) . ?
P C1 1.799(3) . ?
P C11 1.868(4) . ?
O1 C1 1.478(4) . ?
O2 C15 1.149(5) . ?
O3 C16 1.145(5) . ?
O4 C17 1.142(5) . ?
O5 C18 1.133(5) . ?
O6 C19 1.141(5) . ?
C1 H1 1.0000 . ?
C1 C2 1.491(5) . ?
C2 C3 1.401(5) . ?
C2 C7 1.415(5) . ?
C3 C4 1.405(5) . ?
C3 C8 1.508(5) . ?
C4 H4 0.9500 . ?
C4 C5 1.386(6) . ?
C5 C6 1.386(6) . ?
C5 C9 1.512(5) . ?
C6 H6 0.9500 . ?
C6 C7 1.385(5) . ?
C7 C10 1.507(5) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.527(5) . ?
C11 C13 1.520(6) . ?
C11 C14 1.530(7) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
Cr' P' 2.3404(11) . ?
Cr' C15' 1.874(4) . ?
Cr' C16' 1.900(4) . ?
Cr' C17' 1.904(4) . ?
Cr' C18' 1.914(4) . ?
Cr' C19' 1.905(4) . ?
P' O1' 1.698(3) . ?
P' C1' 1.801(4) . ?
P' C11' 1.858(4) . ?
O1' C1' 1.517(5) . ?
O2' C15' 1.143(5) . ?
O3' C16' 1.144(5) . ?
O4' C17' 1.147(4) . ?
O5' C18' 1.136(4) . ?
O6' C19' 1.143(4) . ?
C1' H1' 1.0000 . ?
C1' C2' 1.499(5) . ?
C2' C3' 1.386(6) . ?
C2' C7' 1.403(5) . ?
C3' C4' 1.355(6) . ?
C3' C8' 1.542(6) . ?
C4' H4' 0.9500 . ?
C4' C5' 1.344(7) . ?
C5' C6' 1.396(7) . ?
C5' C9' 1.540(6) . ?
C6' H6' 0.9500 . ?
C6' C7' 1.456(7) . ?
C7' C10' 1.479(6) . ?
C8' H8'A 0.9800 . ?
C8' H8'B 0.9800 . ?
C8' H8'C 0.9800 . ?
C9' H9'A 0.9800 . ?
C9' H9'B 0.9800 . ?
C9' H9'C 0.9800 . ?
C10' H10D 0.9800 . ?
C10' H10E 0.9800 . ?
C10' H10F 0.9800 . ?
C11' C12' 1.503(6) . ?
C11' C13' 1.587(7) . ?
C11' C14' 1.485(6) . ?
C12' H12D 0.9800 . ?
C12' H12E 0.9800 . ?
C12' H12F 0.9800 . ?
C13' H13D 0.9800 . ?
C13' H13E 0.9800 . ?
C13' H13F 0.9800 . ?
C14' H14D 0.9800 . ?
C14' H14E 0.9800 . ?
C14' H14F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 Cr P 177.18(13) . . ?
C15 Cr C16 89.80(17) . . ?
C15 Cr C17 87.36(17) . . ?
C15 Cr C18 89.35(17) . . ?
C15 Cr C19 87.53(17) . . ?
C16 Cr P 92.85(12) . . ?
C16 Cr C17 90.02(17) . . ?
C16 Cr C18 178.31(18) . . ?
C16 Cr C19 91.00(17) . . ?
C17 Cr P 91.68(12) . . ?
C17 Cr C18 88.48(19) . . ?
C17 Cr C19 174.79(17) . . ?
C18 Cr P 87.98(13) . . ?
C18 Cr C19 90.43(18) . . ?
C19 Cr P 93.37(12) . . ?
O1 P Cr 117.98(10) . . ?
O1 P C1 50.31(14) . . ?
O1 P C11 105.04(17) . . ?
C1 P Cr 127.19(12) . . ?
C1 P C11 106.60(17) . . ?
C11 P Cr 124.66(13) . . ?
C1 O1 P 69.52(17) . . ?
P C1 H1 114.4 . . ?
O1 C1 P 60.16(15) . . ?
O1 C1 H1 114.4 . . ?
O1 C1 C2 118.3(3) . . ?
C2 C1 P 124.3(3) . . ?
C2 C1 H1 114.4 . . ?
C3 C2 C1 122.3(3) . . ?
C3 C2 C7 119.9(3) . . ?
C7 C2 C1 117.4(3) . . ?
C2 C3 C4 118.4(3) . . ?
C2 C3 C8 123.3(3) . . ?
C4 C3 C8 118.2(3) . . ?
C3 C4 H4 118.9 . . ?
C5 C4 C3 122.2(3) . . ?
C5 C4 H4 118.9 . . ?
C4 C5 C6 118.1(3) . . ?
C4 C5 C9 120.7(4) . . ?
C6 C5 C9 121.2(4) . . ?
C5 C6 H6 118.9 . . ?
C7 C6 C5 122.2(4) . . ?
C7 C6 H6 118.9 . . ?
C2 C7 C10 120.1(3) . . ?
C6 C7 C2 119.1(3) . . ?
C6 C7 C10 120.8(3) . . ?
C3 C8 H8A 109.5 . . ?
C3 C8 H8B 109.5 . . ?
C3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 P 108.1(3) . . ?
C12 C11 C14 110.3(4) . . ?
C13 C11 P 112.7(3) . . ?
C13 C11 C12 108.8(4) . . ?
C13 C11 C14 110.0(4) . . ?
C14 C11 P 107.0(3) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O2 C15 Cr 178.8(3) . . ?
O3 C16 Cr 177.7(3) . . ?
O4 C17 Cr 176.3(4) . . ?
O5 C18 Cr 175.8(4) . . ?
O6 C19 Cr 174.9(4) . . ?
C15' Cr' P' 176.63(12) . . ?
C15' Cr' C16' 85.11(16) . . ?
C15' Cr' C17' 90.91(16) . . ?
C15' Cr' C18' 88.25(16) . . ?
C15' Cr' C19' 88.41(16) . . ?
C16' Cr' P' 92.63(12) . . ?
C16' Cr' C17' 89.60(15) . . ?
C16' Cr' C18' 173.35(16) . . ?
C16' Cr' C19' 91.26(16) . . ?
C17' Cr' P' 91.57(12) . . ?
C17' Cr' C18' 90.13(15) . . ?
C17' Cr' C19' 178.86(16) . . ?
C18' Cr' P' 94.02(11) . . ?
C19' Cr' P' 89.14(12) . . ?
C19' Cr' C18' 88.93(15) . . ?
O1' P' Cr' 116.16(12) . . ?
O1' P' C1' 51.30(17) . . ?
O1' P' C11' 104.17(18) . . ?
C1' P' Cr' 127.70(14) . . ?
C1' P' C11' 105.92(18) . . ?
C11' P' Cr' 125.38(13) . . ?
C1' O1' P' 67.86(19) . . ?
P' C1' H1' 114.8 . . ?
O1' C1' P' 60.84(18) . . ?
O1' C1' H1' 114.8 . . ?
C2' C1' P' 123.6(3) . . ?
C2' C1' O1' 117.2(3) . . ?
C2' C1' H1' 114.8 . . ?
C3' C2' C1' 117.8(4) . . ?
C3' C2' C7' 121.2(4) . . ?
C7' C2' C1' 120.6(4) . . ?
C2' C3' C8' 119.1(4) . . ?
C4' C3' C2' 121.4(4) . . ?
C4' C3' C8' 119.5(4) . . ?
C3' C4' H4' 119.5 . . ?
C5' C4' C3' 120.9(5) . . ?
C5' C4' H4' 119.5 . . ?
C4' C5' C6' 120.6(4) . . ?
C4' C5' C9' 121.4(5) . . ?
C6' C5' C9' 118.0(5) . . ?
C5' C6' H6' 119.8 . . ?
C5' C6' C7' 120.5(4) . . ?
C7' C6' H6' 119.8 . . ?
C2' C7' C6' 115.4(4) . . ?
C2' C7' C10' 126.3(4) . . ?
C6' C7' C10' 118.2(4) . . ?
C3' C8' H8'A 109.5 . . ?
C3' C8' H8'B 109.5 . . ?
C3' C8' H8'C 109.5 . . ?
H8'A C8' H8'B 109.5 . . ?
H8'A C8' H8'C 109.5 . . ?
H8'B C8' H8'C 109.5 . . ?
C5' C9' H9'A 109.5 . . ?
C5' C9' H9'B 109.5 . . ?
C5' C9' H9'C 109.5 . . ?
H9'A C9' H9'B 109.5 . . ?
H9'A C9' H9'C 109.5 . . ?
H9'B C9' H9'C 109.5 . . ?
C7' C10' H10D 109.5 . . ?
C7' C10' H10E 109.5 . . ?
C7' C10' H10F 109.5 . . ?
H10D C10' H10E 109.5 . . ?
H10D C10' H10F 109.5 . . ?
H10E C10' H10F 109.5 . . ?
C12' C11' P' 111.6(3) . . ?
C12' C11' C13' 105.4(4) . . ?
C13' C11' P' 103.9(3) . . ?
C14' C11' P' 114.8(3) . . ?
C14' C11' C12' 112.6(4) . . ?
C14' C11' C13' 107.6(4) . . ?
C11' C12' H12D 109.5 . . ?
C11' C12' H12E 109.5 . . ?
C11' C12' H12F 109.5 . . ?
H12D C12' H12E 109.5 . . ?
H12D C12' H12F 109.5 . . ?
H12E C12' H12F 109.5 . . ?
C11' C13' H13D 109.5 . . ?
C11' C13' H13E 109.5 . . ?
C11' C13' H13F 109.5 . . ?
H13D C13' H13E 109.5 . . ?
H13D C13' H13F 109.5 . . ?
H13E C13' H13F 109.5 . . ?
C11' C14' H14D 109.5 . . ?
C11' C14' H14E 109.5 . . ?
C11' C14' H14F 109.5 . . ?
H14D C14' H14E 109.5 . . ?
H14D C14' H14F 109.5 . . ?
H14E C14' H14F 109.5 . . ?
O2' C15' Cr' 178.0(4) . . ?
O3' C16' Cr' 174.6(3) . . ?
O4' C17' Cr' 178.1(3) . . ?
O5' C18' Cr' 174.8(3) . . ?
O6' C19' Cr' 176.1(3) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr P O1 C1 116.65(17) . . . . ?
Cr P C1 O1 -97.80(18) . . . . ?
Cr P C1 C2 7.8(4) . . . . ?
Cr P C11 C12 42.3(4) . . . . ?
Cr P C11 C13 162.6(3) . . . . ?
Cr P C11 C14 -76.5(3) . . . . ?
P O1 C1 C2 -115.4(3) . . . . ?
P C1 C2 C3 -102.9(4) . . . . ?
P C1 C2 C7 84.0(4) . . . . ?
O1 P C1 C2 105.6(3) . . . . ?
O1 P C11 C12 -98.6(3) . . . . ?
O1 P C11 C13 21.6(4) . . . . ?
O1 P C11 C14 142.6(3) . . . . ?
O1 C1 C2 C3 -31.4(5) . . . . ?
O1 C1 C2 C7 155.5(3) . . . . ?
C1 P C11 C12 -151.1(3) . . . . ?
C1 P C11 C13 -30.8(4) . . . . ?
C1 P C11 C14 90.2(3) . . . . ?
C1 C2 C3 C4 -176.6(3) . . . . ?
C1 C2 C3 C8 -0.1(5) . . . . ?
C1 C2 C7 C6 175.7(3) . . . . ?
C1 C2 C7 C10 -2.8(5) . . . . ?
C2 C3 C4 C5 3.0(5) . . . . ?
C3 C2 C7 C6 2.5(5) . . . . ?
C3 C2 C7 C10 -176.0(3) . . . . ?
C3 C4 C5 C6 -0.9(6) . . . . ?
C3 C4 C5 C9 176.8(4) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C5 C6 C7 C2 -0.4(6) . . . . ?
C5 C6 C7 C10 178.1(4) . . . . ?
C7 C2 C3 C4 -3.7(5) . . . . ?
C7 C2 C3 C8 172.8(3) . . . . ?
C8 C3 C4 C5 -173.7(4) . . . . ?
C9 C5 C6 C7 -178.0(4) . . . . ?
C11 P O1 C1 -99.3(2) . . . . ?
C11 P C1 O1 96.0(2) . . . . ?
C11 P C1 C2 -158.4(3) . . . . ?
Cr' P' O1' C1' 118.65(19) . . . . ?
Cr' P' C1' O1' -95.4(2) . . . . ?
Cr' P' C1' C2' 9.6(4) . . . . ?
Cr' P' C11' C12' 20.7(4) . . . . ?
Cr' P' C11' C13' -92.4(3) . . . . ?
Cr' P' C11' C14' 150.4(3) . . . . ?
P' O1' C1' C2' -115.1(3) . . . . ?
P' C1' C2' C3' 84.0(4) . . . . ?
P' C1' C2' C7' -102.1(4) . . . . ?
O1' P' C1' C2' 105.0(4) . . . . ?
O1' P' C11' C12' -116.7(4) . . . . ?
O1' P' C11' C13' 130.1(3) . . . . ?
O1' P' C11' C14' 12.9(4) . . . . ?
O1' C1' C2' C3' 155.6(3) . . . . ?
O1' C1' C2' C7' -30.6(5) . . . . ?
C1' P' C11' C12' -170.0(4) . . . . ?
C1' P' C11' C13' 76.9(3) . . . . ?
C1' P' C11' C14' -40.3(4) . . . . ?
C1' C2' C3' C4' 175.7(4) . . . . ?
C1' C2' C3' C8' -4.1(5) . . . . ?
C1' C2' C7' C6' -176.3(3) . . . . ?
C1' C2' C7' C10' 0.4(6) . . . . ?
C2' C3' C4' C5' 0.0(7) . . . . ?
C3' C2' C7' C6' -2.7(5) . . . . ?
C3' C2' C7' C10' 174.1(4) . . . . ?
C3' C4' C5' C6' -0.9(7) . . . . ?
C3' C4' C5' C9' 180.0(4) . . . . ?
C4' C5' C6' C7' 0.0(6) . . . . ?
C5' C6' C7' C2' 1.7(6) . . . . ?
C5' C6' C7' C10' -175.3(4) . . . . ?
C7' C2' C3' C4' 1.9(6) . . . . ?
C7' C2' C3' C8' -177.9(4) . . . . ?
C8' C3' C4' C5' 179.8(4) . . . . ?
C9' C5' C6' C7' 179.2(4) . . . . ?
C11' P' O1' C1' -99.2(2) . . . . ?
C11' P' C1' O1' 95.6(2) . . . . ?
C11' P' C1' C2' -159.4(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
