# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2302946'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2023-10-23
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number     2019/1
_chemical_name_common            ?
_chemical_name_systematic        DB-403
_chemical_formula_moiety         '2(C24 H17 O6 P W), C4 H8 O'
_chemical_formula_sum            'C52 H42 O13 P2 W2'
_chemical_formula_weight         1304.49
_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                   9.3995(9)
_cell_length_b                   11.6790(10)
_cell_length_c                   12.0501(11)
_cell_angle_alpha                97.985(3)
_cell_angle_beta                 91.166(4)
_cell_angle_gamma                109.171(3)
_cell_volume                     1234.3(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    9847
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.81
_cell_measurement_theta_min      2.33
_shelx_estimated_absorpt_T_max   0.448
_shelx_estimated_absorpt_T_min   0.251
_exptl_absorpt_coefficient_mu    4.786
_exptl_absorpt_correction_T_max  0.745472
_exptl_absorpt_correction_T_min  0.588614
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1118 before and 0.0676 after correction.
 The Ratio of minimum to maximum transmission is 0.79.

Final HKLF 4 output contains 96125 reflections, Rint = 0.1977
 (30273 with I > 3sig(I), Rint = 0.1238)
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0860
_diffrn_measured_fraction_theta_full 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.868
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4361
_reflns_number_total             4891
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         2.081
_refine_diff_density_min         -2.819
_refine_diff_density_rms         0.285
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     342
_refine_ls_number_reflns         4891
_refine_ls_number_restraints     117
_refine_ls_R_factor_all          0.0745
_refine_ls_R_factor_gt           0.0566
_refine_ls_restrained_S_all      1.104
_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)+(0.0125P)²+18.8775P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1321
_refine_special_details          
;
 Refined as a 5-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.592(6)
 0.093(3) 0.181(3) 0.109(3) 0.025(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All P(H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 O7-C28 = O7-C25
 1.44 with sigma of 0.02
 C28-C27 = C26-C25
 1.53 with sigma of 0.02
 C27-C26
 1.54 with sigma of 0.02
 O7-C27 = O7-C26 = C28-C26 = C27-C25
 2.38 with sigma of 0.04
 C27-C25 \\sim C28-C26
 with sigma of 0.04
 O7-C27 \\sim O7-C26
 with sigma of 0.04
 C28-C27 \\sim C27-C26 \\sim C26-C25
 with sigma of 0.02
 O7-C28 \\sim O7-C25
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O7 \\sim C25 \\sim C26 \\sim C27 \\sim C28: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08 within 2A
C27 \\sim C26 \\sim C28 \\sim O7: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.002 within 2A
Uanis(C25) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.01
Uanis(C24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C27) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 O7, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O7(0.5) C25(0.5) H25A(0.5) H25B(0.5) C26(0.5) H26A(0.5) H26B(0.5)
 C27(0.5) H27A(0.5) H27B(0.5) C28(0.5) H28A(0.5) H28B(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
7.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
7.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.25088(5) 0.10908(4) 0.35869(4) 0.01469(14) Uani 1 1 d . . . . .
P P 0.3567(3) 0.3341(3) 0.3412(2) 0.0163(6) Uani 1 1 d . . . . .
H H 0.241(12) 0.389(10) 0.368(9) 0.020 Uiso 1 1 d . U . . .
O1 O 0.4924(8) 0.4106(7) 0.4292(7) 0.0205(17) Uani 1 1 d . . . . .
H1 H 0.540679 0.365314 0.445490 0.031 Uiso 1 1 calc R U . . .
O2 O 0.5774(9) 0.0933(9) 0.4091(7) 0.033(2) Uani 1 1 d . . . . .
O3 O 0.2263(10) 0.1967(9) 0.6164(8) 0.037(2) Uani 1 1 d . . . . .
O4 O -0.0830(9) 0.1101(8) 0.3095(8) 0.032(2) Uani 1 1 d . . . . .
O5 O 0.2753(9) 0.0004(7) 0.1050(7) 0.0249(18) Uani 1 1 d . . . . .
O6 O 0.1069(9) -0.1599(8) 0.4103(8) 0.033(2) Uani 1 1 d . . . . .
C1 C 0.4080(11) 0.3948(10) 0.2021(9) 0.015(2) Uani 1 1 d . . . . .
C2 C 0.3097(11) 0.3022(9) 0.1059(9) 0.014(2) Uani 1 1 d . U . . .
C3 C 0.1527(11) 0.2577(10) 0.1139(10) 0.019(2) Uani 1 1 d . . . . .
H3 H 0.110467 0.282856 0.179976 0.023 Uiso 1 1 calc R U . . .
C4 C 0.0604(12) 0.1786(10) 0.0272(9) 0.022(2) Uani 1 1 d . . . . .
H4 H -0.045060 0.147281 0.035465 0.026 Uiso 1 1 calc R U . . .
C5 C 0.1163(13) 0.1425(11) -0.0728(10) 0.027(3) Uani 1 1 d . . . . .
H5 H 0.050466 0.089894 -0.133534 0.032 Uiso 1 1 calc R U . . .
C6 C 0.2717(12) 0.1858(11) -0.0810(9) 0.022(2) Uani 1 1 d . . . . .
H6 H 0.312360 0.160827 -0.147958 0.027 Uiso 1 1 calc R U . . .
C7 C 0.3686(12) 0.2646(9) 0.0061(8) 0.016(2) Uani 1 1 d . . . . .
H7 H 0.474366 0.293079 -0.001444 0.019 Uiso 1 1 calc R U . . .
C8 C 0.3818(12) 0.5185(9) 0.2067(9) 0.015(2) Uani 1 1 d . . . . .
C9 C 0.2960(12) 0.5398(10) 0.1203(10) 0.019(2) Uani 1 1 d . . . . .
H9 H 0.254778 0.476720 0.058136 0.023 Uiso 1 1 calc R U . . .
C10 C 0.2692(13) 0.6504(11) 0.1228(10) 0.023(3) Uani 1 1 d . . . . .
H10 H 0.212517 0.662204 0.061806 0.028 Uiso 1 1 calc R U . . .
C11 C 0.3240(14) 0.7426(11) 0.2123(10) 0.028(3) Uani 1 1 d . . . . .
H11 H 0.303573 0.817353 0.215177 0.034 Uiso 1 1 calc R U . . .
C12 C 0.4109(14) 0.7239(10) 0.2998(10) 0.027(3) Uani 1 1 d . . . . .
H12 H 0.451338 0.787124 0.362051 0.033 Uiso 1 1 calc R U . . .
C13 C 0.4381(13) 0.6130(10) 0.2958(10) 0.024(3) Uani 1 1 d . . . . .
H13 H 0.496865 0.601981 0.355862 0.028 Uiso 1 1 calc R U . . .
C14 C 0.5792(11) 0.4108(10) 0.1932(9) 0.015(2) Uani 1 1 d . . . . .
C15 C 0.6881(13) 0.5231(11) 0.1872(10) 0.024(3) Uani 1 1 d . . . . .
H15 H 0.659127 0.593672 0.186944 0.029 Uiso 1 1 calc R U . . .
C16 C 0.8391(13) 0.5334(12) 0.1817(11) 0.030(3) Uani 1 1 d . . . . .
H16 H 0.912957 0.611004 0.178526 0.035 Uiso 1 1 calc R U . . .
C17 C 0.8826(14) 0.4305(11) 0.1807(11) 0.029(3) Uani 1 1 d . . . . .
H17 H 0.986074 0.438153 0.176173 0.035 Uiso 1 1 calc R U . . .
C18 C 0.7770(12) 0.3175(12) 0.1861(11) 0.030(3) Uani 1 1 d . . . . .
H18 H 0.806284 0.246849 0.185048 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6258(12) 0.3091(11) 0.1932(9) 0.021(2) Uani 1 1 d . . . . .
H19 H 0.552517 0.231761 0.198125 0.026 Uiso 1 1 calc R U . . .
C20 C 0.4631(13) 0.1029(10) 0.3915(9) 0.023(2) Uani 1 1 d . . . . .
C21 C 0.2375(12) 0.1644(10) 0.5205(11) 0.024(3) Uani 1 1 d . . . . .
C22 C 0.0382(12) 0.1107(10) 0.3275(9) 0.021(2) Uani 1 1 d . . . . .
C23 C 0.2657(11) 0.0458(10) 0.1963(10) 0.018(2) Uani 1 1 d . . . . .
C24 C 0.1606(13) -0.0618(11) 0.3907(10) 0.024(2) Uani 1 1 d . U . . .
O7 O 0.8309(14) 0.3623(12) 0.4886(13) 0.022(2) Uani 0.5 1 d D U P A -1
C25 C 0.7841(18) 0.4490(14) 0.4496(18) 0.015(3) Uani 0.5 1 d D U P A -1
H25A H 0.703513 0.462899 0.495568 0.018 Uiso 0.5 1 calc R U P A -1
H25B H 0.740803 0.418462 0.371208 0.018 Uiso 0.5 1 calc R U P A -1
C26 C 0.9078(17) 0.5654(14) 0.4532(19) 0.022(2) Uani 0.5 1 d D U P A -1
H26A H 0.887867 0.632328 0.503333 0.026 Uiso 0.5 1 calc R U P A -1
H26B H 0.923540 0.588529 0.377202 0.026 Uiso 0.5 1 calc R U P A -1
C27 C 1.0387(17) 0.5389(14) 0.498(2) 0.021(2) Uani 0.5 1 d D U P A -1
H27A H 1.117335 0.550256 0.443056 0.026 Uiso 0.5 1 calc R U P A -1
H27B H 1.082711 0.595071 0.568641 0.026 Uiso 0.5 1 calc R U P A -1
C28 C 0.9857(18) 0.4120(14) 0.5185(19) 0.022(2) Uani 0.5 1 d D U P A -1
H28A H 1.039763 0.364187 0.473309 0.026 Uiso 0.5 1 calc R U P A -1
H28B H 1.005392 0.408989 0.598866 0.026 Uiso 0.5 1 calc R U P A -1


_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 2.527(3) . ?
W C20 2.052(12) . ?
W C21 1.987(13) . ?
W C22 2.033(11) . ?
W C23 2.017(12) . ?
W C24 1.991(12) . ?
P H 1.46(11) . ?
P O1 1.577(8) . ?
P C1 1.919(10) . ?
O1 H1 0.8400 . ?
O2 C20 1.135(13) . ?
O3 C21 1.183(14) . ?
O4 C22 1.153(13) . ?
O5 C23 1.172(13) . ?
O6 C24 1.150(14) . ?
C1 C2 1.523(14) . ?
C1 C8 1.537(14) . ?
C1 C14 1.566(14) . ?
C2 C3 1.405(14) . ?
C2 C7 1.409(14) . ?
C3 H3 0.9500 . ?
C3 C4 1.366(15) . ?
C4 H4 0.9500 . ?
C4 C5 1.392(16) . ?
C5 H5 0.9500 . ?
C5 C6 1.390(16) . ?
C6 H6 0.9500 . ?
C6 C7 1.386(15) . ?
C7 H7 0.9500 . ?
C8 C9 1.402(15) . ?
C8 C13 1.383(16) . ?
C9 H9 0.9500 . ?
C9 C10 1.392(15) . ?
C10 H10 0.9500 . ?
C10 C11 1.371(17) . ?
C11 H11 0.9500 . ?
C11 C12 1.404(17) . ?
C12 H12 0.9500 . ?
C12 C13 1.396(15) . ?
C13 H13 0.9500 . ?
C14 C15 1.385(16) . ?
C14 C19 1.394(15) . ?
C15 H15 0.9500 . ?
C15 C16 1.389(16) . ?
C16 H16 0.9500 . ?
C16 C17 1.389(17) . ?
C17 H17 0.9500 . ?
C17 C18 1.378(17) . ?
C18 H18 0.9500 . ?
C18 C19 1.397(15) . ?
C19 H19 0.9500 . ?
O7 C25 1.362(13) . ?
O7 C28 1.396(14) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.465(13) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.474(13) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.459(13) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?

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
C20 W P 91.5(3) . . ?
C21 W P 86.3(3) . . ?
C21 W C20 90.7(4) . . ?
C21 W C22 89.1(4) . . ?
C21 W C23 177.3(5) . . ?
C21 W C24 87.0(5) . . ?
C22 W P 90.0(3) . . ?
C22 W C20 178.4(5) . . ?
C23 W P 96.0(3) . . ?
C23 W C20 88.0(4) . . ?
C23 W C22 92.2(4) . . ?
C24 W P 173.1(3) . . ?
C24 W C20 90.0(4) . . ?
C24 W C22 88.4(4) . . ?
C24 W C23 90.7(4) . . ?
W P H 108(4) . . ?
O1 P W 114.0(3) . . ?
O1 P H 104(4) . . ?
O1 P C1 105.9(4) . . ?
C1 P W 124.1(4) . . ?
C1 P H 98(4) . . ?
P O1 H1 109.5 . . ?
C2 C1 P 109.2(7) . . ?
C2 C1 C8 110.3(8) . . ?
C2 C1 C14 111.8(9) . . ?
C8 C1 P 109.1(7) . . ?
C8 C1 C14 111.0(8) . . ?
C14 C1 P 105.3(6) . . ?
C3 C2 C1 118.8(9) . . ?
C3 C2 C7 118.4(10) . . ?
C7 C2 C1 122.7(9) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 C2 120.4(11) . . ?
C4 C3 H3 119.8 . . ?
C3 C4 H4 119.0 . . ?
C3 C4 C5 121.9(10) . . ?
C5 C4 H4 119.0 . . ?
C4 C5 H5 121.1 . . ?
C6 C5 C4 117.8(11) . . ?
C6 C5 H5 121.1 . . ?
C5 C6 H6 119.2 . . ?
C7 C6 C5 121.6(11) . . ?
C7 C6 H6 119.2 . . ?
C2 C7 H7 120.1 . . ?
C6 C7 C2 119.8(10) . . ?
C6 C7 H7 120.1 . . ?
C9 C8 C1 120.9(10) . . ?
C13 C8 C1 122.5(9) . . ?
C13 C8 C9 116.6(10) . . ?
C8 C9 H9 118.9 . . ?
C10 C9 C8 122.2(11) . . ?
C10 C9 H9 118.9 . . ?
C9 C10 H10 119.7 . . ?
C11 C10 C9 120.6(10) . . ?
C11 C10 H10 119.7 . . ?
C10 C11 H11 120.8 . . ?
C10 C11 C12 118.5(10) . . ?
C12 C11 H11 120.8 . . ?
C11 C12 H12 119.8 . . ?
C13 C12 C11 120.3(11) . . ?
C13 C12 H12 119.8 . . ?
C8 C13 C12 121.8(10) . . ?
C8 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C15 C14 C1 122.6(9) . . ?
C15 C14 C19 118.1(10) . . ?
C19 C14 C1 119.3(9) . . ?
C14 C15 H15 119.7 . . ?
C14 C15 C16 120.6(11) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.2(12) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.7 . . ?
C18 C17 C16 120.5(11) . . ?
C18 C17 H17 119.7 . . ?
C17 C18 H18 120.8 . . ?
C17 C18 C19 118.5(11) . . ?
C19 C18 H18 120.8 . . ?
C14 C19 C18 122.0(11) . . ?
C14 C19 H19 119.0 . . ?
C18 C19 H19 119.0 . . ?
O2 C20 W 176.6(10) . . ?
O3 C21 W 178.6(9) . . ?
O4 C22 W 179.2(10) . . ?
O5 C23 W 174.4(9) . . ?
O6 C24 W 178.9(11) . . ?
C25 O7 C28 109.0(13) . . ?
O7 C25 H25A 109.2 . . ?
O7 C25 H25B 109.2 . . ?
O7 C25 C26 112.1(12) . . ?
H25A C25 H25B 107.9 . . ?
C26 C25 H25A 109.2 . . ?
C26 C25 H25B 109.2 . . ?
C25 C26 H26A 111.2 . . ?
C25 C26 H26B 111.2 . . ?
C25 C26 C27 103.0(10) . . ?
H26A C26 H26B 109.1 . . ?
C27 C26 H26A 111.2 . . ?
C27 C26 H26B 111.2 . . ?
C26 C27 H27A 110.2 . . ?
C26 C27 H27B 110.2 . . ?
H27A C27 H27B 108.5 . . ?
C28 C27 C26 107.6(10) . . ?
C28 C27 H27A 110.2 . . ?
C28 C27 H27B 110.2 . . ?
O7 C28 C27 108.4(12) . . ?
O7 C28 H28A 110.0 . . ?
O7 C28 H28B 110.0 . . ?
C27 C28 H28A 110.0 . . ?
C27 C28 H28B 110.0 . . ?
H28A C28 H28B 108.4 . . ?

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
P C1 C2 C3 50.4(11) . . . . ?
P C1 C2 C7 -133.5(9) . . . . ?
P C1 C8 C9 -128.9(9) . . . . ?
P C1 C8 C13 49.8(12) . . . . ?
P C1 C14 C15 -119.6(10) . . . . ?
P C1 C14 C19 59.2(11) . . . . ?
C1 C2 C3 C4 177.2(9) . . . . ?
C1 C2 C7 C6 -176.0(10) . . . . ?
C1 C8 C9 C10 179.4(10) . . . . ?
C1 C8 C13 C12 -178.7(11) . . . . ?
C1 C14 C15 C16 178.7(11) . . . . ?
C1 C14 C19 C18 -179.6(10) . . . . ?
C2 C1 C8 C9 -9.1(13) . . . . ?
C2 C1 C8 C13 169.7(10) . . . . ?
C2 C1 C14 C15 121.9(11) . . . . ?
C2 C1 C14 C19 -59.2(12) . . . . ?
C2 C3 C4 C5 -2.3(17) . . . . ?
C3 C2 C7 C6 0.2(15) . . . . ?
C3 C4 C5 C6 2.5(17) . . . . ?
C4 C5 C6 C7 -1.4(17) . . . . ?
C5 C6 C7 C2 0.1(17) . . . . ?
C7 C2 C3 C4 0.9(15) . . . . ?
C8 C1 C2 C3 -69.4(12) . . . . ?
C8 C1 C2 C7 106.7(11) . . . . ?
C8 C1 C14 C15 -1.7(14) . . . . ?
C8 C1 C14 C19 177.2(9) . . . . ?
C8 C9 C10 C11 -1.5(17) . . . . ?
C9 C8 C13 C12 0.1(17) . . . . ?
C9 C10 C11 C12 1.7(18) . . . . ?
C10 C11 C12 C13 -1.1(18) . . . . ?
C11 C12 C13 C8 0.2(19) . . . . ?
C13 C8 C9 C10 0.6(16) . . . . ?
C14 C1 C2 C3 166.5(9) . . . . ?
C14 C1 C2 C7 -17.3(13) . . . . ?
C14 C1 C8 C9 115.4(11) . . . . ?
C14 C1 C8 C13 -65.8(13) . . . . ?
C14 C15 C16 C17 0.8(19) . . . . ?
C15 C14 C19 C18 -0.7(17) . . . . ?
C15 C16 C17 C18 -1(2) . . . . ?
C16 C17 C18 C19 0(2) . . . . ?
C17 C18 C19 C14 1.0(19) . . . . ?
C19 C14 C15 C16 -0.2(17) . . . . ?
O7 C25 C26 C27 1(3) . . . . ?
C25 O7 C28 C27 1(2) . . . . ?
C25 C26 C27 C28 0(2) . . . . ?
C26 C27 C28 O7 0(3) . . . . ?
C28 O7 C25 C26 -1(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C25^a H25A^a O1 0.99 1.99 2.629(17) 120.2 . yes


_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.592(6)
2 0.093(3)
3 0.181(3)
4 0.109(3)
5 0.025(2)
####################################################################### 
# 
# 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_10a
_database_code_depnum_ccdc_archive 'CCDC 2302947'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2022-08-19
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        DB-550
_chemical_formula_moiety         'C26 H16 F3 O7 P W'
_chemical_formula_sum            'C26 H16 F3 O7 P W'
_chemical_formula_weight         712.21
_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                   11.7247(3)
_cell_length_b                   11.0478(4)
_cell_length_c                   19.5690(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.179(2)
_cell_angle_gamma                90
_cell_volume                     2524.47(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    17241
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.53
_shelx_estimated_absorpt_T_max   0.705
_shelx_estimated_absorpt_T_min   0.602
_exptl_absorpt_coefficient_mu    4.706
_exptl_absorpt_correction_T_max  0.9140
_exptl_absorpt_correction_T_min  0.0215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1136
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18095
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.538
_diffrn_ambient_temperature      123
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details      
;
 359 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS2T'
_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                3493
_reflns_number_total             4366
_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       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area X-Red 2.3.0.0 (STOE, 2021) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.725
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.326
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4366
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0731
_refine_ls_restrained_S_all      1.063
_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)+(0.1137P)²+46.6193P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.2016
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 P-H
 1.5 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19)
;
_atom_sites_solution_hydrogens   mixed
_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
W W 0.59323(4) 0.86206(5) 0.61091(2) 0.0240(2) Uani 1 1 d . . . . .
P P 0.6694(3) 0.6552(3) 0.61381(15) 0.0242(7) Uani 1 1 d D . . . .
H H 0.595(8) 0.545(6) 0.606(5) 0.01(3) Uiso 1 1 d D . . . .
F1 F 0.7523(9) 0.6716(9) 0.8429(4) 0.051(2) Uani 1 1 d . . . . .
F2 F 0.7382(8) 0.4804(9) 0.8488(4) 0.045(2) Uani 1 1 d . . . . .
F3 F 0.8734(7) 0.5591(9) 0.7966(4) 0.047(2) Uani 1 1 d . . . . .
O1 O 0.7321(8) 0.6325(8) 0.6943(4) 0.030(2) Uani 1 1 d . . . . .
O2 O 0.5930(9) 0.5242(11) 0.7373(5) 0.043(3) Uani 1 1 d . . . . .
O3 O 0.4905(11) 1.1238(9) 0.6203(6) 0.043(3) Uani 1 1 d . . . . .
O4 O 0.3817(9) 0.7937(10) 0.5043(5) 0.041(2) Uani 1 1 d . . . . .
O5 O 0.4493(11) 0.7729(11) 0.7321(5) 0.052(3) Uani 1 1 d . . . . .
O6 O 0.7961(10) 0.9527(10) 0.7163(5) 0.047(3) Uani 1 1 d . . . . .
O7 O 0.7385(10) 0.9487(10) 0.4907(5) 0.043(3) Uani 1 1 d . . . . .
C1 C 0.7867(10) 0.5835(11) 0.5651(6) 0.022(2) Uani 1 1 d . . . . .
C2 C 0.8282(11) 0.4705(11) 0.6073(6) 0.025(3) Uani 1 1 d . . . . .
C3 C 0.7488(13) 0.3799(12) 0.6176(7) 0.033(3) Uani 1 1 d . . . . .
H3 H 0.672069 0.386641 0.597726 0.040 Uiso 1 1 calc R . . . .
C4 C 0.7837(13) 0.2777(13) 0.6580(7) 0.036(3) Uani 1 1 d . . . . .
H4 H 0.729522 0.216596 0.666147 0.044 Uiso 1 1 calc R . . . .
C5 C 0.8955(15) 0.2661(14) 0.6855(7) 0.042(4) Uani 1 1 d . . . . .
H5 H 0.917743 0.197034 0.712374 0.050 Uiso 1 1 calc R . . . .
C6 C 0.9752(13) 0.3537(14) 0.6744(7) 0.035(3) Uani 1 1 d . . . . .
H6 H 1.052433 0.344684 0.692957 0.042 Uiso 1 1 calc R . . . .
C7 C 0.9416(12) 0.4562(12) 0.6357(6) 0.029(3) Uani 1 1 d . . . . .
H7 H 0.996434 0.517138 0.628544 0.035 Uiso 1 1 calc R . . . .
C8 C 0.7320(10) 0.5426(13) 0.4936(5) 0.025(3) Uani 1 1 d . . . . .
C9 C 0.7755(12) 0.4432(14) 0.4631(6) 0.034(3) Uani 1 1 d . . . . .
H9 H 0.832620 0.395247 0.487700 0.040 Uiso 1 1 calc R . . . .
C10 C 0.7353(13) 0.4116(14) 0.3944(7) 0.036(3) Uani 1 1 d . . . . .
H10 H 0.766671 0.343736 0.372920 0.043 Uiso 1 1 calc R . . . .
C11 C 0.6500(13) 0.4802(13) 0.3591(6) 0.034(3) Uani 1 1 d . . . . .
H11 H 0.621130 0.458680 0.313833 0.041 Uiso 1 1 calc R . . . .
C12 C 0.6070(13) 0.5826(14) 0.3915(7) 0.036(3) Uani 1 1 d . . . . .
H12 H 0.549301 0.630709 0.367548 0.043 Uiso 1 1 calc R . . . .
C13 C 0.6477(11) 0.6135(13) 0.4574(6) 0.029(3) Uani 1 1 d . . . . .
H13 H 0.618474 0.683062 0.478452 0.034 Uiso 1 1 calc R . . . .
C14 C 0.8777(10) 0.6779(12) 0.5598(6) 0.026(3) Uani 1 1 d . . . . .
C15 C 0.9169(11) 0.7105(12) 0.4964(6) 0.027(3) Uani 1 1 d . . . . .
H15 H 0.886023 0.670733 0.455808 0.033 Uiso 1 1 calc R . . . .
C16 C 0.9996(11) 0.7996(13) 0.4917(8) 0.033(3) Uani 1 1 d . . . . .
H16 H 1.024365 0.820908 0.448409 0.039 Uiso 1 1 calc R . . . .
C17 C 1.0445(13) 0.8556(13) 0.5496(9) 0.041(4) Uani 1 1 d . . . . .
H17 H 1.100092 0.917271 0.546155 0.049 Uiso 1 1 calc R . . . .
C18 C 1.0119(12) 0.8256(14) 0.6137(8) 0.038(3) Uani 1 1 d . . . . .
H18 H 1.045928 0.864367 0.653777 0.046 Uiso 1 1 calc R . . . .
C19 C 0.9285(11) 0.7379(13) 0.6180(7) 0.031(3) Uani 1 1 d . . . . .
H19 H 0.904959 0.717614 0.661754 0.037 Uiso 1 1 calc R . . . .
C20 C 0.6843(11) 0.5678(14) 0.7427(6) 0.031(3) Uani 1 1 d . . . . .
C21 C 0.7630(12) 0.5678(16) 0.8085(7) 0.040(4) Uani 1 1 d . . . . .
C22 C 0.5278(12) 1.0287(13) 0.6161(7) 0.031(3) Uani 1 1 d . . . . .
C23 C 0.4574(13) 0.8142(12) 0.5426(7) 0.032(3) Uani 1 1 d . . . . .
C24 C 0.4992(13) 0.8054(13) 0.6896(7) 0.034(3) Uani 1 1 d . . . . .
C25 C 0.7258(13) 0.9195(13) 0.6780(7) 0.035(3) Uani 1 1 d . . . . .
C26 C 0.6875(11) 0.9171(13) 0.5324(6) 0.029(3) 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 2.452(3) . ?
W C22 2.001(14) . ?
W C23 2.054(14) . ?
W C24 2.070(14) . ?
W C25 2.043(16) . ?
W C26 2.064(13) . ?
P H 1.50(2) . ?
P O1 1.695(9) . ?
P C1 1.915(12) . ?
F1 C21 1.34(2) . ?
F2 C21 1.296(18) . ?
F3 C21 1.339(17) . ?
O1 C20 1.349(16) . ?
O2 C20 1.170(17) . ?
O3 C22 1.143(17) . ?
O4 C23 1.132(17) . ?
O5 C24 1.118(17) . ?
O6 C25 1.125(18) . ?
O7 C26 1.110(16) . ?
C1 C2 1.551(17) . ?
C1 C8 1.553(15) . ?
C1 C14 1.503(18) . ?
C2 C3 1.393(19) . ?
C2 C7 1.403(18) . ?
C3 H3 0.9500 . ?
C3 C4 1.42(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.38(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.38(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.40(2) . ?
C7 H7 0.9500 . ?
C8 C9 1.37(2) . ?
C8 C13 1.402(19) . ?
C9 H9 0.9500 . ?
C9 C10 1.427(18) . ?
C10 H10 0.9500 . ?
C10 C11 1.39(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.41(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.377(18) . ?
C13 H13 0.9500 . ?
C14 C15 1.408(17) . ?
C14 C19 1.403(18) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(19) . ?
C16 H16 0.9500 . ?
C16 C17 1.36(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.38(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.38(2) . ?
C19 H19 0.9500 . ?
C20 C21 1.515(18) . ?

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
C22 W P 175.5(4) . . ?
C22 W C23 89.5(5) . . ?
C22 W C24 90.4(6) . . ?
C22 W C25 87.4(5) . . ?
C22 W C26 90.0(5) . . ?
C23 W P 92.0(4) . . ?
C23 W C24 88.4(5) . . ?
C23 W C26 91.6(5) . . ?
C24 W P 85.3(4) . . ?
C25 W P 91.2(4) . . ?
C25 W C23 176.8(5) . . ?
C25 W C24 92.3(5) . . ?
C25 W C26 87.7(5) . . ?
C26 W P 94.2(4) . . ?
C26 W C24 179.5(5) . . ?
W P H 123(5) . . ?
O1 P W 106.6(3) . . ?
O1 P H 100(4) . . ?
O1 P C1 97.5(5) . . ?
C1 P W 130.6(4) . . ?
C1 P H 93(4) . . ?
C20 O1 P 124.0(9) . . ?
C2 C1 P 105.8(8) . . ?
C2 C1 C8 109.3(10) . . ?
C8 C1 P 108.2(8) . . ?
C14 C1 P 107.0(8) . . ?
C14 C1 C2 113.9(10) . . ?
C14 C1 C8 112.2(9) . . ?
C3 C2 C1 118.3(12) . . ?
C3 C2 C7 118.9(12) . . ?
C7 C2 C1 122.8(11) . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.3(13) . . ?
C4 C3 H3 120.3 . . ?
C3 C4 H4 119.7 . . ?
C5 C4 C3 120.6(13) . . ?
C5 C4 H4 119.7 . . ?
C4 C5 H5 119.7 . . ?
C6 C5 C4 120.6(14) . . ?
C6 C5 H5 119.7 . . ?
C5 C6 H6 120.3 . . ?
C5 C6 C7 119.5(14) . . ?
C7 C6 H6 120.3 . . ?
C2 C7 H7 119.5 . . ?
C6 C7 C2 121.0(13) . . ?
C6 C7 H7 119.5 . . ?
C9 C8 C1 119.0(11) . . ?
C9 C8 C13 120.1(11) . . ?
C13 C8 C1 120.5(12) . . ?
C8 C9 H9 120.0 . . ?
C8 C9 C10 120.1(13) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.1 . . ?
C11 C10 C9 119.8(13) . . ?
C11 C10 H10 120.1 . . ?
C10 C11 H11 120.5 . . ?
C10 C11 C12 119.0(12) . . ?
C12 C11 H11 120.5 . . ?
C11 C12 H12 119.6 . . ?
C13 C12 C11 120.8(13) . . ?
C13 C12 H12 119.6 . . ?
C8 C13 H13 119.9 . . ?
C12 C13 C8 120.2(13) . . ?
C12 C13 H13 119.9 . . ?
C15 C14 C1 121.9(11) . . ?
C19 C14 C1 121.6(11) . . ?
C19 C14 C15 116.5(13) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 C14 121.6(13) . . ?
C16 C15 H15 119.2 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.3(13) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 119.0 . . ?
C16 C17 C18 122.0(14) . . ?
C18 C17 H17 119.0 . . ?
C17 C18 H18 120.7 . . ?
C17 C18 C19 118.5(14) . . ?
C19 C18 H18 120.7 . . ?
C14 C19 H19 119.0 . . ?
C18 C19 C14 122.1(13) . . ?
C18 C19 H19 119.0 . . ?
O1 C20 C21 109.8(12) . . ?
O2 C20 O1 126.1(12) . . ?
O2 C20 C21 124.0(12) . . ?
F1 C21 C20 110.4(12) . . ?
F2 C21 F1 107.3(11) . . ?
F2 C21 F3 109.0(12) . . ?
F2 C21 C20 111.3(14) . . ?
F3 C21 F1 106.5(13) . . ?
F3 C21 C20 112.1(11) . . ?
O3 C22 W 178.8(12) . . ?
O4 C23 W 176.6(12) . . ?
O5 C24 W 178.8(13) . . ?
O6 C25 W 177.6(13) . . ?
O7 C26 W 178.7(13) . . ?

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 C20 102.8(10) . . . . ?
P O1 C20 O2 -4(2) . . . . ?
P O1 C20 C21 -179.2(9) . . . . ?
P C1 C2 C3 60.1(13) . . . . ?
P C1 C2 C7 -119.6(11) . . . . ?
P C1 C8 C9 -148.7(10) . . . . ?
P C1 C8 C13 38.1(13) . . . . ?
P C1 C14 C15 -126.6(11) . . . . ?
P C1 C14 C19 53.7(14) . . . . ?
O1 C20 C21 F1 79.9(14) . . . . ?
O1 C20 C21 F2 -161.1(12) . . . . ?
O1 C20 C21 F3 -38.7(18) . . . . ?
O2 C20 C21 F1 -95.6(19) . . . . ?
O2 C20 C21 F2 23(2) . . . . ?
O2 C20 C21 F3 145.8(15) . . . . ?
C1 P O1 C20 -120.7(11) . . . . ?
C1 C2 C3 C4 -177.9(12) . . . . ?
C1 C2 C7 C6 179.0(12) . . . . ?
C1 C8 C9 C10 -173.2(12) . . . . ?
C1 C8 C13 C12 174.1(12) . . . . ?
C1 C14 C15 C16 178.8(12) . . . . ?
C1 C14 C19 C18 -179.6(12) . . . . ?
C2 C1 C8 C9 -33.9(15) . . . . ?
C2 C1 C8 C13 152.8(11) . . . . ?
C2 C1 C14 C15 116.8(12) . . . . ?
C2 C1 C14 C19 -62.9(15) . . . . ?
C2 C3 C4 C5 -2(2) . . . . ?
C3 C2 C7 C6 -0.7(18) . . . . ?
C3 C4 C5 C6 0(2) . . . . ?
C4 C5 C6 C7 1(2) . . . . ?
C5 C6 C7 C2 -1(2) . . . . ?
C7 C2 C3 C4 1.8(19) . . . . ?
C8 C1 C2 C3 -56.2(14) . . . . ?
C8 C1 C2 C7 124.1(12) . . . . ?
C8 C1 C14 C15 -8.0(16) . . . . ?
C8 C1 C14 C19 172.3(12) . . . . ?
C8 C9 C10 C11 -1(2) . . . . ?
C9 C8 C13 C12 0.9(19) . . . . ?
C9 C10 C11 C12 2(2) . . . . ?
C10 C11 C12 C13 -1(2) . . . . ?
C11 C12 C13 C8 -1(2) . . . . ?
C13 C8 C9 C10 0.1(19) . . . . ?
C14 C1 C2 C3 177.4(11) . . . . ?
C14 C1 C2 C7 -2.3(16) . . . . ?
C14 C1 C8 C9 93.4(14) . . . . ?
C14 C1 C8 C13 -79.8(14) . . . . ?
C14 C15 C16 C17 1(2) . . . . ?
C15 C14 C19 C18 1(2) . . . . ?
C15 C16 C17 C18 1(2) . . . . ?
C16 C17 C18 C19 -2(2) . . . . ?
C17 C18 C19 C14 1(2) . . . . ?
C19 C14 C15 C16 -1.5(18) . . . . ?

_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_12
_database_code_depnum_ccdc_archive 'CCDC 2302952'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2022-05-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        DB-519
_chemical_formula_moiety         'C29 H24 N2 O5 P W, C F3 O3 S, C H2 Cl2'
_chemical_formula_sum            'C31 H26 Cl2 F3 N2 O8 P S W'
_chemical_formula_weight         929.32
_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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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                   9.1342(3)
_cell_length_b                   10.5960(4)
_cell_length_c                   18.7994(6)
_cell_angle_alpha                87.804(3)
_cell_angle_beta                 79.701(3)
_cell_angle_gamma                77.720(3)
_cell_volume                     1749.24(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    17803
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.812
_shelx_estimated_absorpt_T_min   0.670
_exptl_absorpt_coefficient_mu    3.627
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             912
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
15 1 0 0.1168
8 3 30 0.0816
5 -7 30 0.0912
9 -10 4 0.0975
11 8 -30 0.0763
7 30 0 0.1243
1 1 15 0.0507
-2 -4 15 0.0804
-30 -3 -11 0.1074
-30 -27 -11 0.1304
-6 1 -30 0.0722
-19 30 -8 0.1187
-12 -1 30 0.0799
-16 -11 30 0.0770
-3 -15 -2 0.1243
-2 -1 -30 0.0531

_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            44205
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.000
_diffrn_reflns_theta_min         1.967
_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 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
 359 frames, detector distance = 100 mm
;
_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                33570
_reflns_number_total             44205
_reflns_special_details          
;
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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    'XT  (Sheldrick, 2015)'
_refine_diff_density_max         1.454
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         44205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0586
_refine_ls_restrained_S_all      0.991
_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)+(0.1139P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1512
_refine_ls_wR_factor_ref         0.1631
_refine_special_details          
;
 Refined as a 5-component twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.3290(13)
 0.2918(9) 0.2145(8) 0.1205(5) 0.0442(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24)
3.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_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
W W 0.24349(3) 0.51065(3) 0.11148(2) 0.02279(11) Uani 1 1 d . . . . .
P P 0.1900(2) 0.37874(18) 0.22246(10) 0.0225(3) Uani 1 1 d . . . . .
O1 O 0.2815(7) 0.7072(6) -0.0162(3) 0.0355(13) Uani 1 1 d . . . . .
O2 O -0.0850(7) 0.5011(6) 0.0809(3) 0.0408(14) Uani 1 1 d . . . . .
O3 O 0.1001(8) 0.7518(6) 0.2141(4) 0.0457(15) Uani 1 1 d . . . . .
O4 O 0.5770(6) 0.5165(6) 0.1380(3) 0.0370(13) Uani 1 1 d . . . . .
O5 O 0.3789(7) 0.2866(6) -0.0054(3) 0.0346(12) Uani 1 1 d . . . . .
N1 N 0.2615(7) 0.4378(6) 0.2951(3) 0.0249(12) Uani 1 1 d . . . . .
N2 N 0.2673(7) 0.5626(6) 0.3834(3) 0.0284(13) Uani 1 1 d . . . . .
C1 C -0.0124(8) 0.4172(8) 0.2635(4) 0.0290(15) Uani 1 1 d . . . . .
H1A H -0.0256 0.3814 0.3125 0.044 Uiso 1 1 calc GR . . . .
H1B H -0.0710 0.3795 0.2343 0.044 Uiso 1 1 calc GR . . . .
H1C H -0.0487 0.5111 0.2656 0.044 Uiso 1 1 calc GR . . . .
C2 C 0.1779(9) 0.5212(7) 0.3456(4) 0.0270(15) Uani 1 1 d . . . . .
H2 H 0.0702 0.5471 0.3532 0.032 Uiso 1 1 calc R . . . .
C3 C 0.4156(9) 0.5020(7) 0.3574(4) 0.0290(15) Uani 1 1 d . . . . .
H3 H 0.5035 0.5119 0.3753 0.035 Uiso 1 1 calc R . . . .
C4 C 0.4126(8) 0.4263(8) 0.3021(4) 0.0295(15) Uani 1 1 d . . . . .
H4 H 0.4984 0.3743 0.2731 0.035 Uiso 1 1 calc R . . . .
C5 C 0.2182(10) 0.6543(9) 0.4430(4) 0.0385(19) Uani 1 1 d . . . . .
H5A H 0.2277 0.7408 0.4251 0.058 Uiso 1 1 calc GR . . . .
H5B H 0.2820 0.6287 0.4800 0.058 Uiso 1 1 calc GR . . . .
H5C H 0.1118 0.6552 0.4641 0.058 Uiso 1 1 calc GR . . . .
C6 C 0.2545(8) 0.1917(7) 0.2270(4) 0.0228(13) Uani 1 1 d . . . . .
C7 C 0.1589(8) 0.1341(7) 0.2907(4) 0.0244(14) Uani 1 1 d . . . . .
C8 C 0.1307(9) 0.1860(7) 0.3608(4) 0.0284(15) Uani 1 1 d . . . . .
H8 H 0.1717 0.2580 0.3694 0.034 Uiso 1 1 calc R . . . .
C9 C 0.0444(9) 0.1333(8) 0.4169(4) 0.0326(17) Uani 1 1 d . . . . .
H9 H 0.0253 0.1701 0.4638 0.039 Uiso 1 1 calc R . . . .
C10 C -0.0152(9) 0.0270(8) 0.4059(4) 0.0309(16) Uani 1 1 d . . . . .
H10 H -0.0767 -0.0076 0.4447 0.037 Uiso 1 1 calc R . . . .
C11 C 0.0158(9) -0.0280(8) 0.3379(4) 0.0303(16) Uani 1 1 d . . . . .
H11 H -0.0217 -0.1025 0.3303 0.036 Uiso 1 1 calc R . . . .
C12 C 0.1015(8) 0.0254(7) 0.2809(4) 0.0254(14) Uani 1 1 d . . . . .
H12 H 0.1214 -0.0128 0.2343 0.030 Uiso 1 1 calc R . . . .
C13 C 0.2348(8) 0.1398(7) 0.1544(4) 0.0227(13) Uani 1 1 d . . . . .
C14 C 0.3428(8) 0.0374(7) 0.1196(4) 0.0280(15) Uani 1 1 d . . . . .
H14 H 0.4319 0.0032 0.1393 0.034 Uiso 1 1 calc R . . . .
C15 C 0.3215(9) -0.0152(8) 0.0567(4) 0.0317(16) Uani 1 1 d . . . . .
H15 H 0.3958 -0.0853 0.0339 0.038 Uiso 1 1 calc R . . . .
C16 C 0.1926(9) 0.0336(8) 0.0268(4) 0.0340(17) Uani 1 1 d . . . . .
H16 H 0.1795 -0.0013 -0.0169 0.041 Uiso 1 1 calc R . . . .
C17 C 0.0835(9) 0.1338(8) 0.0613(4) 0.0308(16) Uani 1 1 d . . . . .
H17 H -0.0055 0.1678 0.0415 0.037 Uiso 1 1 calc R . . . .
C18 C 0.1042(8) 0.1847(7) 0.1248(4) 0.0265(14) Uani 1 1 d . . . . .
H18 H 0.0271 0.2519 0.1487 0.032 Uiso 1 1 calc R . . . .
C19 C 0.4238(8) 0.1664(7) 0.2342(4) 0.0234(14) Uani 1 1 d . . . . .
C20 C 0.4768(8) 0.1121(8) 0.2954(4) 0.0295(16) Uani 1 1 d . . . . .
H20 H 0.4082 0.0839 0.3337 0.035 Uiso 1 1 calc R . . . .
C21 C 0.6294(9) 0.0982(9) 0.3016(5) 0.0358(18) Uani 1 1 d . . . . .
H21 H 0.6638 0.0621 0.3442 0.043 Uiso 1 1 calc R . . . .
C22 C 0.7311(9) 0.1373(9) 0.2452(5) 0.0367(18) Uani 1 1 d . . . . .
H22 H 0.8347 0.1293 0.2496 0.044 Uiso 1 1 calc R . . . .
C23 C 0.6810(8) 0.1878(8) 0.1828(4) 0.0324(17) Uani 1 1 d . . . . .
H23 H 0.7505 0.2137 0.1440 0.039 Uiso 1 1 calc R . . . .
C24 C 0.5295(8) 0.2005(7) 0.1766(4) 0.0276(15) Uani 1 1 d . . . . .
H24 H 0.4966 0.2327 0.1330 0.033 Uiso 1 1 calc R . . . .
C25 C 0.2680(8) 0.6362(7) 0.0287(4) 0.0263(14) Uani 1 1 d . . . . .
C26 C 0.0309(8) 0.5060(8) 0.0921(4) 0.0287(15) Uani 1 1 d . . . . .
C27 C 0.1528(9) 0.6657(7) 0.1787(4) 0.0307(16) Uani 1 1 d . . . . .
C28 C 0.4600(8) 0.5131(7) 0.1290(4) 0.0276(15) Uani 1 1 d . . . . .
C29 C 0.3316(8) 0.3612(7) 0.0371(4) 0.0265(14) Uani 1 1 d . . . . .
S S 0.2436(2) 0.3403(2) 0.55545(11) 0.0330(4) Uani 1 1 d . . . . .
F1 F 0.4875(7) 0.2195(7) 0.4704(3) 0.0694(19) Uani 1 1 d . . . . .
F2 F 0.3360(7) 0.0979(6) 0.5161(4) 0.0653(18) Uani 1 1 d . . . . .
F3 F 0.4759(6) 0.1628(6) 0.5808(3) 0.0525(14) Uani 1 1 d . . . . .
O6 O 0.1661(7) 0.3623(6) 0.4945(3) 0.0403(14) Uani 1 1 d . . . . .
O7 O 0.3263(8) 0.4361(7) 0.5670(4) 0.0549(19) Uani 1 1 d . . . . .
O8 O 0.1548(7) 0.2993(7) 0.6204(4) 0.0495(17) Uani 1 1 d . . . . .
C30 C 0.3931(10) 0.1979(9) 0.5289(5) 0.0383(19) Uani 1 1 d . . . . .
Cl1 Cl 0.5572(3) 0.2145(2) 0.74435(14) 0.0504(6) Uani 1 1 d . . . . .
Cl2 Cl 0.2720(3) 0.1932(3) 0.83745(17) 0.0677(8) Uani 1 1 d . . . . .
C31 C 0.3566(13) 0.2568(13) 0.7571(7) 0.065(3) Uani 1 1 d . . . . .
H31A H 0.3237 0.3521 0.7581 0.078 Uiso 1 1 calc R . . . .
H31B H 0.3214 0.2243 0.7158 0.078 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W P 2.4996(19) . ?
W C25 2.022(7) . ?
W C26 2.050(7) . ?
W C27 2.046(8) . ?
W C28 2.068(7) . ?
W C29 2.083(7) . ?
P N1 1.801(6) . ?
P C1 1.837(7) . ?
P C6 1.947(7) . ?
O1 C25 1.117(9) . ?
O2 C26 1.128(9) . ?
O3 C27 1.119(10) . ?
O4 C28 1.120(9) . ?
O5 C29 1.108(9) . ?
N1 C2 1.335(9) . ?
N1 C4 1.389(9) . ?
N2 C2 1.321(9) . ?
N2 C3 1.380(10) . ?
N2 C5 1.457(10) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.344(11) . ?
C4 H4 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.538(9) . ?
C6 C13 1.544(9) . ?
C6 C19 1.542(9) . ?
C7 C8 1.406(10) . ?
C7 C12 1.394(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.375(10) . ?
C9 H9 0.9500 . ?
C9 C10 1.388(11) . ?
C10 H10 0.9500 . ?
C10 C11 1.382(11) . ?
C11 H11 0.9500 . ?
C11 C12 1.388(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(10) . ?
C13 C18 1.391(10) . ?
C14 H14 0.9500 . ?
C14 C15 1.388(10) . ?
C15 H15 0.9500 . ?
C15 C16 1.387(11) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(11) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(10) . ?
C19 C24 1.407(10) . ?
C20 H20 0.9500 . ?
C20 C21 1.395(11) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.383(11) . ?
C23 H23 0.9500 . ?
C23 C24 1.387(10) . ?
C24 H24 0.9500 . ?
S O6 1.437(6) . ?
S O7 1.432(7) . ?
S O8 1.447(7) . ?
S C30 1.824(10) . ?
F1 C30 1.315(10) . ?
F2 C30 1.324(11) . ?
F3 C30 1.334(10) . ?
Cl1 C31 1.766(12) . ?
Cl2 C31 1.748(13) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?

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
C25 W P 172.7(2) . . ?
C25 W C26 89.6(3) . . ?
C25 W C27 88.3(3) . . ?
C25 W C28 90.0(3) . . ?
C25 W C29 88.0(3) . . ?
C26 W P 88.2(2) . . ?
C26 W C28 178.8(3) . . ?
C26 W C29 88.3(3) . . ?
C27 W P 84.8(2) . . ?
C27 W C26 90.2(3) . . ?
C27 W C28 91.0(3) . . ?
C27 W C29 176.0(3) . . ?
C28 W P 92.3(2) . . ?
C28 W C29 90.5(3) . . ?
C29 W P 98.9(2) . . ?
N1 P W 109.4(2) . . ?
N1 P C1 97.1(3) . . ?
N1 P C6 104.6(3) . . ?
C1 P W 111.5(3) . . ?
C1 P C6 106.3(3) . . ?
C6 P W 124.3(2) . . ?
C2 N1 P 124.6(5) . . ?
C2 N1 C4 107.0(6) . . ?
C4 N1 P 127.4(5) . . ?
C2 N2 C3 108.2(6) . . ?
C2 N2 C5 126.2(7) . . ?
C3 N2 C5 125.7(7) . . ?
P C1 H1A 109.5 . . ?
P C1 H1B 109.5 . . ?
P C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2 125.0 . . ?
N2 C2 N1 110.0(7) . . ?
N2 C2 H2 125.0 . . ?
N2 C3 H3 126.4 . . ?
C4 C3 N2 107.2(7) . . ?
C4 C3 H3 126.4 . . ?
N1 C4 H4 126.2 . . ?
C3 C4 N1 107.7(7) . . ?
C3 C4 H4 126.2 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 P 111.7(5) . . ?
C7 C6 C13 110.6(6) . . ?
C7 C6 C19 111.8(6) . . ?
C13 C6 P 106.0(5) . . ?
C19 C6 P 105.3(5) . . ?
C19 C6 C13 111.1(6) . . ?
C8 C7 C6 121.6(6) . . ?
C12 C7 C6 120.5(6) . . ?
C12 C7 C8 117.9(7) . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.6(7) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 119.6 . . ?
C8 C9 C10 120.9(7) . . ?
C10 C9 H9 119.6 . . ?
C9 C10 H10 120.3 . . ?
C11 C10 C9 119.3(7) . . ?
C11 C10 H10 120.3 . . ?
C10 C11 H11 119.9 . . ?
C10 C11 C12 120.1(7) . . ?
C12 C11 H11 119.9 . . ?
C7 C12 H12 119.4 . . ?
C11 C12 C7 121.1(7) . . ?
C11 C12 H12 119.4 . . ?
C14 C13 C6 120.3(6) . . ?
C18 C13 C6 121.7(6) . . ?
C18 C13 C14 117.7(6) . . ?
C13 C14 H14 119.6 . . ?
C15 C14 C13 120.8(7) . . ?
C15 C14 H14 119.6 . . ?
C14 C15 H15 119.7 . . ?
C16 C15 C14 120.6(7) . . ?
C16 C15 H15 119.7 . . ?
C15 C16 H16 120.4 . . ?
C17 C16 C15 119.2(7) . . ?
C17 C16 H16 120.4 . . ?
C16 C17 H17 120.0 . . ?
C16 C17 C18 119.9(7) . . ?
C18 C17 H17 120.0 . . ?
C13 C18 H18 119.2 . . ?
C17 C18 C13 121.7(7) . . ?
C17 C18 H18 119.2 . . ?
C20 C19 C6 122.8(6) . . ?
C20 C19 C24 118.3(7) . . ?
C24 C19 C6 118.9(6) . . ?
C19 C20 H20 119.5 . . ?
C19 C20 C21 121.0(7) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 H21 120.1 . . ?
C22 C21 C20 119.9(7) . . ?
C22 C21 H21 120.1 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.9(7) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.1(7) . . ?
C24 C23 H23 120.0 . . ?
C19 C24 H24 119.6 . . ?
C23 C24 C19 120.8(7) . . ?
C23 C24 H24 119.6 . . ?
O1 C25 W 178.7(7) . . ?
O2 C26 W 178.6(7) . . ?
O3 C27 W 177.9(8) . . ?
O4 C28 W 178.7(7) . . ?
O5 C29 W 176.2(7) . . ?
O6 S O8 114.4(4) . . ?
O6 S C30 103.4(4) . . ?
O7 S O6 115.5(4) . . ?
O7 S O8 114.4(5) . . ?
O7 S C30 103.3(4) . . ?
O8 S C30 103.6(4) . . ?
F1 C30 S 111.7(7) . . ?
F1 C30 F2 108.1(8) . . ?
F1 C30 F3 107.0(7) . . ?
F2 C30 S 111.6(6) . . ?
F2 C30 F3 107.2(8) . . ?
F3 C30 S 111.1(6) . . ?
Cl1 C31 H31A 109.2 . . ?
Cl1 C31 H31B 109.2 . . ?
Cl2 C31 Cl1 112.0(6) . . ?
Cl2 C31 H31A 109.2 . . ?
Cl2 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?

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 N1 C2 96.0(6) . . . . ?
W P N1 C4 -71.1(7) . . . . ?
P N1 C2 N2 -169.2(5) . . . . ?
P N1 C4 C3 169.8(5) . . . . ?
P C6 C7 C8 -48.2(8) . . . . ?
P C6 C7 C12 133.9(6) . . . . ?
P C6 C13 C14 140.5(6) . . . . ?
P C6 C13 C18 -45.3(8) . . . . ?
P C6 C19 C20 114.3(7) . . . . ?
P C6 C19 C24 -65.2(7) . . . . ?
N2 C3 C4 N1 -1.4(9) . . . . ?
C1 P N1 C2 -19.8(7) . . . . ?
C1 P N1 C4 173.1(7) . . . . ?
C2 N1 C4 C3 0.8(9) . . . . ?
C2 N2 C3 C4 1.5(9) . . . . ?
C3 N2 C2 N1 -1.0(9) . . . . ?
C4 N1 C2 N2 0.1(8) . . . . ?
C5 N2 C2 N1 180.0(7) . . . . ?
C5 N2 C3 C4 -179.5(7) . . . . ?
C6 P N1 C2 -128.8(6) . . . . ?
C6 P N1 C4 64.1(7) . . . . ?
C6 C7 C8 C9 179.7(7) . . . . ?
C6 C7 C12 C11 179.6(6) . . . . ?
C6 C13 C14 C15 176.0(7) . . . . ?
C6 C13 C18 C17 -177.0(7) . . . . ?
C6 C19 C20 C21 -176.0(7) . . . . ?
C6 C19 C24 C23 175.5(7) . . . . ?
C7 C6 C13 C14 -98.2(8) . . . . ?
C7 C6 C13 C18 75.9(8) . . . . ?
C7 C6 C19 C20 -7.2(10) . . . . ?
C7 C6 C19 C24 173.2(6) . . . . ?
C7 C8 C9 C10 0.8(12) . . . . ?
C8 C7 C12 C11 1.7(11) . . . . ?
C8 C9 C10 C11 1.4(12) . . . . ?
C9 C10 C11 C12 -2.1(12) . . . . ?
C10 C11 C12 C7 0.5(11) . . . . ?
C12 C7 C8 C9 -2.4(11) . . . . ?
C13 C6 C7 C8 -166.0(7) . . . . ?
C13 C6 C7 C12 16.1(9) . . . . ?
C13 C6 C19 C20 -131.3(7) . . . . ?
C13 C6 C19 C24 49.1(9) . . . . ?
C13 C14 C15 C16 0.4(12) . . . . ?
C14 C13 C18 C17 -2.7(11) . . . . ?
C14 C15 C16 C17 -1.4(12) . . . . ?
C15 C16 C17 C18 0.4(12) . . . . ?
C16 C17 C18 C13 1.7(12) . . . . ?
C18 C13 C14 C15 1.6(11) . . . . ?
C19 C6 C7 C8 69.6(8) . . . . ?
C19 C6 C7 C12 -108.3(7) . . . . ?
C19 C6 C13 C14 26.5(9) . . . . ?
C19 C6 C13 C18 -159.3(6) . . . . ?
C19 C20 C21 C22 -1.1(13) . . . . ?
C20 C19 C24 C23 -4.0(11) . . . . ?
C20 C21 C22 C23 -1.1(14) . . . . ?
C21 C22 C23 C24 0.6(13) . . . . ?
C22 C23 C24 C19 2.0(12) . . . . ?
C24 C19 C20 C21 3.6(12) . . . . ?
O6 S C30 F1 61.5(7) . . . . ?
O6 S C30 F2 -59.5(7) . . . . ?
O6 S C30 F3 -179.1(6) . . . . ?
O7 S C30 F1 -59.2(7) . . . . ?
O7 S C30 F2 179.8(7) . . . . ?
O7 S C30 F3 60.2(7) . . . . ?
O8 S C30 F1 -178.8(7) . . . . ?
O8 S C30 F2 60.1(7) . . . . ?
O8 S C30 F3 -59.5(7) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.3290(13)
2 0.2918(9)
3 0.2145(8)
4 0.1205(5)
5 0.0442(3)
####################################################################### 
# 
# 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_10a-Cr
_database_code_depnum_ccdc_archive 'CCDC 2302948'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2022-06-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        DB-557
_chemical_formula_moiety         'C26 H16 Cr F3 O7 P'
_chemical_formula_sum            'C26 H16 Cr F3 O7 P'
_chemical_formula_weight         580.36
_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'
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'

_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                   11.7074(11)
_cell_length_b                   10.9879(9)
_cell_length_c                   19.4438(23)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.019(8)
_cell_angle_gamma                90.00
_cell_volume                     2491.7(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2476
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.13
_shelx_estimated_absorpt_T_max   0.922
_shelx_estimated_absorpt_T_min   0.843
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.9602
_exptl_absorpt_correction_T_min  0.8377
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   
'STOE X-Red32, absorption correction by Gaussian integration, analogous to P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12331
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.996
_diffrn_reflns_theta_min         2.103
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       'rotation method, ω scans'
_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                4537
_reflns_number_total             5000
_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>4u(I)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area WinXpose 2.0.22.0 (STOE, 2016)'
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5967
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0296
_refine_ls_restrained_S_all      1.013
_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)+(0.0500P)²]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0814
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All P(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.59537(2) 0.14121(2) 0.61072(2) 0.01510(7) Uani 1 1 d . . . . .
P P 0.66775(3) 0.33811(3) 0.61356(2) 0.01399(9) Uani 1 1 d . . . . .
H H 0.5918(13) 0.4254(16) 0.6099(8) 0.017 Uiso 1 1 d R . . . .
F1 F 0.74695(9) 0.32294(10) 0.84319(5) 0.0355(3) Uani 1 1 d . . . . .
F2 F 0.73867(9) 0.51891(10) 0.84975(5) 0.0315(2) Uani 1 1 d . . . . .
F3 F 0.87308(8) 0.43274(10) 0.79781(5) 0.0319(2) Uani 1 1 d . . . . .
O1 O 0.72920(9) 0.36098(9) 0.69511(5) 0.0166(2) Uani 1 1 d . . . . .
O2 O 0.59391(10) 0.48174(11) 0.73667(6) 0.0267(3) Uani 1 1 d . . . . .
O3 O 0.49578(10) -0.11232(11) 0.61969(6) 0.0287(3) Uani 1 1 d . . . . .
O4 O 0.46230(12) 0.22911(12) 0.72945(6) 0.0334(3) Uani 1 1 d . . . . .
O5 O 0.78960(11) 0.05020(12) 0.71207(7) 0.0339(3) Uani 1 1 d . . . . .
O6 O 0.73310(10) 0.05462(12) 0.49361(6) 0.0295(3) Uani 1 1 d . . . . .
O7 O 0.39066(10) 0.20683(12) 0.50976(6) 0.0310(3) Uani 1 1 d . . . . .
C1 C 0.68362(13) 0.42904(14) 0.74209(8) 0.0171(3) Uani 1 1 d . . . . .
C2 C 0.76228(14) 0.42638(15) 0.80958(8) 0.0221(3) Uani 1 1 d . . . . .
C3 C 0.78432(12) 0.41407(13) 0.56523(7) 0.0148(3) Uani 1 1 d . . . . .
C4 C 0.82557(13) 0.52677(14) 0.60821(7) 0.0167(3) Uani 1 1 d . . . . .
C5 C 0.74734(14) 0.61993(14) 0.61881(8) 0.0208(3) Uani 1 1 d . . . . .
H5 H 0.6709 0.6140 0.5982 0.025 Uiso 1 1 calc R . . . .
C6 C 0.77938(15) 0.72078(15) 0.65891(9) 0.0255(4) Uani 1 1 d . . . . .
H6 H 0.7248 0.7824 0.6661 0.031 Uiso 1 1 calc R . . . .
C7 C 0.89148(16) 0.73154(16) 0.68851(9) 0.0283(4) Uani 1 1 d . . . . .
H7 H 0.9137 0.8000 0.7164 0.034 Uiso 1 1 calc R . . . .
C8 C 0.96998(15) 0.64193(16) 0.67703(9) 0.0264(4) Uani 1 1 d . . . . .
H8 H 1.0469 0.6498 0.6965 0.032 Uiso 1 1 calc R . . . .
C9 C 0.93800(14) 0.53989(15) 0.63724(8) 0.0204(3) Uani 1 1 d . . . . .
H9 H 0.9932 0.4790 0.6299 0.024 Uiso 1 1 calc R . . . .
C10 C 0.87915(12) 0.31858(14) 0.55808(8) 0.0155(3) Uani 1 1 d . . . . .
C11 C 0.92838(13) 0.25755(15) 0.61656(8) 0.0208(3) Uani 1 1 d . . . . .
H11 H 0.9040 0.2766 0.6606 0.025 Uiso 1 1 calc R . . . .
C12 C 1.01211(14) 0.16988(16) 0.61119(9) 0.0258(4) Uani 1 1 d . . . . .
H12 H 1.0444 0.1294 0.6515 0.031 Uiso 1 1 calc R . . . .
C13 C 1.04921(15) 0.14081(16) 0.54710(9) 0.0269(4) Uani 1 1 d . . . . .
H13 H 1.1065 0.0806 0.5433 0.032 Uiso 1 1 calc R . . . .
C14 C 1.00149(14) 0.20085(15) 0.48914(9) 0.0242(4) Uani 1 1 d . . . . .
H14 H 1.0264 0.1818 0.4452 0.029 Uiso 1 1 calc R . . . .
C15 C 0.91733(13) 0.28884(15) 0.49437(8) 0.0194(3) Uani 1 1 d . . . . .
H15 H 0.8855 0.3292 0.4539 0.023 Uiso 1 1 calc R . . . .
C16 C 0.73103(12) 0.45375(14) 0.49354(7) 0.0158(3) Uani 1 1 d . . . . .
C17 C 0.77538(13) 0.55484(15) 0.46135(8) 0.0211(3) Uani 1 1 d . . . . .
H17 H 0.8331 0.6028 0.4857 0.025 Uiso 1 1 calc R . . . .
C18 C 0.73606(15) 0.58614(16) 0.39422(8) 0.0250(4) Uani 1 1 d . . . . .
H18 H 0.7675 0.6547 0.3729 0.030 Uiso 1 1 calc R . . . .
C19 C 0.65071(13) 0.51749(16) 0.35805(8) 0.0224(3) Uani 1 1 d . . . . .
H19 H 0.6236 0.5391 0.3122 0.027 Uiso 1 1 calc R . . . .
C20 C 0.60569(13) 0.41751(15) 0.38944(8) 0.0207(3) Uani 1 1 d . . . . .
H20 H 0.5471 0.3706 0.3651 0.025 Uiso 1 1 calc R . . . .
C21 C 0.64586(13) 0.38524(14) 0.45655(8) 0.0187(3) Uani 1 1 d . . . . .
H21 H 0.6150 0.3158 0.4774 0.022 Uiso 1 1 calc R . . . .
C22 C 0.53216(13) -0.01620(15) 0.61619(8) 0.0205(3) Uani 1 1 d . . . . .
C23 C 0.51118(14) 0.19458(14) 0.68494(8) 0.0210(3) Uani 1 1 d . . . . .
C24 C 0.71837(14) 0.08760(15) 0.67429(8) 0.0222(3) Uani 1 1 d . . . . .
C25 C 0.68249(13) 0.08935(14) 0.53708(8) 0.0192(3) Uani 1 1 d . . . . .
C26 C 0.46821(14) 0.18506(15) 0.54716(8) 0.0206(3) 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 2.3224(5) . ?
Cr C22 1.8880(17) . ?
Cr C23 1.9096(17) . ?
Cr C24 1.9071(17) . ?
Cr C25 1.9158(17) . ?
Cr C26 1.9115(16) . ?
P H 1.305(17) . ?
P O1 1.7017(10) . ?
P C3 1.9148(16) . ?
F1 C2 1.3311(19) . ?
F2 C2 1.3259(19) . ?
F3 C2 1.3385(19) . ?
O1 C1 1.3280(18) . ?
O2 C1 1.1958(19) . ?
O3 C22 1.143(2) . ?
O4 C23 1.143(2) . ?
O5 C24 1.1388(19) . ?
O6 C25 1.140(2) . ?
O7 C26 1.1378(19) . ?
C1 C2 1.536(2) . ?
C3 C4 1.548(2) . ?
C3 C10 1.543(2) . ?
C3 C16 1.5394(19) . ?
C4 C5 1.401(2) . ?
C4 C9 1.393(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.388(2) . ?
C6 H6 0.9500 . ?
C6 C7 1.391(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.378(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.395(2) . ?
C9 H9 0.9500 . ?
C10 C11 1.400(2) . ?
C10 C15 1.392(2) . ?
C11 H11 0.9500 . ?
C11 C12 1.385(2) . ?
C12 H12 0.9500 . ?
C12 C13 1.392(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.381(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.390(2) . ?
C15 H15 0.9500 . ?
C16 C17 1.397(2) . ?
C16 C21 1.397(2) . ?
C17 H17 0.9500 . ?
C17 C18 1.389(2) . ?
C18 H18 0.9500 . ?
C18 C19 1.393(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.383(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.393(2) . ?
C21 H21 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C22 Cr P 174.95(5) . . ?
C22 Cr C23 90.45(7) . . ?
C22 Cr C24 87.59(7) . . ?
C22 Cr C25 90.37(7) . . ?
C22 Cr C26 88.88(7) . . ?
C23 Cr P 84.68(5) . . ?
C23 Cr C25 178.85(7) . . ?
C23 Cr C26 89.25(7) . . ?
C24 Cr P 91.10(5) . . ?
C24 Cr C23 90.88(7) . . ?
C24 Cr C25 88.36(7) . . ?
C24 Cr C26 176.46(7) . . ?
C25 Cr P 94.47(5) . . ?
C26 Cr P 92.43(5) . . ?
C26 Cr C25 91.56(7) . . ?
Cr P H 116.0(7) . . ?
O1 P Cr 106.46(4) . . ?
O1 P H 99.9(7) . . ?
O1 P C3 97.56(6) . . ?
C3 P Cr 131.96(5) . . ?
C3 P H 99.5(7) . . ?
C1 O1 P 124.16(9) . . ?
O1 C1 C2 109.26(12) . . ?
O2 C1 O1 127.93(14) . . ?
O2 C1 C2 122.74(14) . . ?
F1 C2 F3 107.63(14) . . ?
F1 C2 C1 109.83(13) . . ?
F2 C2 F1 108.75(13) . . ?
F2 C2 F3 108.41(13) . . ?
F2 C2 C1 110.39(13) . . ?
F3 C2 C1 111.75(13) . . ?
C4 C3 P 106.61(10) . . ?
C10 C3 P 107.29(10) . . ?
C10 C3 C4 113.57(12) . . ?
C16 C3 P 108.54(10) . . ?
C16 C3 C4 110.18(12) . . ?
C16 C3 C10 110.43(12) . . ?
C5 C4 C3 119.15(13) . . ?
C9 C4 C3 122.72(14) . . ?
C9 C4 C5 118.13(14) . . ?
C4 C5 H5 119.4 . . ?
C6 C5 C4 121.21(15) . . ?
C6 C5 H5 119.4 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 119.95(16) . . ?
C7 C6 H6 120.0 . . ?
C6 C7 H7 120.3 . . ?
C8 C7 C6 119.37(15) . . ?
C8 C7 H7 120.3 . . ?
C7 C8 H8 119.5 . . ?
C7 C8 C9 120.91(15) . . ?
C9 C8 H8 119.5 . . ?
C4 C9 C8 120.40(15) . . ?
C4 C9 H9 119.8 . . ?
C8 C9 H9 119.8 . . ?
C11 C10 C3 120.07(13) . . ?
C15 C10 C3 121.96(13) . . ?
C15 C10 C11 117.96(14) . . ?
C10 C11 H11 119.5 . . ?
C12 C11 C10 121.05(15) . . ?
C12 C11 H11 119.5 . . ?
C11 C12 H12 119.8 . . ?
C11 C12 C13 120.36(16) . . ?
C13 C12 H12 119.8 . . ?
C12 C13 H13 120.5 . . ?
C14 C13 C12 119.03(15) . . ?
C14 C13 H13 120.5 . . ?
C13 C14 H14 119.6 . . ?
C13 C14 C15 120.73(16) . . ?
C15 C14 H14 119.6 . . ?
C10 C15 H15 119.6 . . ?
C14 C15 C10 120.87(15) . . ?
C14 C15 H15 119.6 . . ?
C17 C16 C3 119.58(13) . . ?
C17 C16 C21 118.30(13) . . ?
C21 C16 C3 121.86(14) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.82(14) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 H18 119.8 . . ?
C17 C18 C19 120.32(16) . . ?
C19 C18 H18 119.8 . . ?
C18 C19 H19 120.3 . . ?
C20 C19 C18 119.44(14) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 119.8 . . ?
C19 C20 C21 120.32(14) . . ?
C21 C20 H20 119.8 . . ?
C16 C21 H21 119.6 . . ?
C20 C21 C16 120.80(15) . . ?
C20 C21 H21 119.6 . . ?
O3 C22 Cr 178.80(14) . . ?
O4 C23 Cr 178.32(15) . . ?
O5 C24 Cr 176.75(15) . . ?
O6 C25 Cr 177.71(14) . . ?
O7 C26 Cr 177.31(15) . . ?

_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_11c
_database_code_depnum_ccdc_archive 'CCDC 2302951'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2022-12-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        DB-568
_chemical_formula_moiety         'C28 H22 N2 O5 P W'
_chemical_formula_sum            'C28 H22 N2 O5 P W'
_chemical_formula_weight         681.29
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.9563(5)
_cell_length_b                   34.958(2)
_cell_length_c                   16.3809(13)
_cell_angle_alpha                90
_cell_angle_beta                 97.490(2)
_cell_angle_gamma                90
_cell_volume                     5652.8(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9666
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.433
_cell_measurement_theta_min      2.575
_shelx_estimated_absorpt_T_max   0.903
_shelx_estimated_absorpt_T_min   0.787
_exptl_absorpt_coefficient_mu    2.091
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6491
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0931 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.8700. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.801
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1332
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0502
_diffrn_reflns_av_unetI/netI     0.0241
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            137230
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         2.144
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12411
_reflns_number_total             13629
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         2.265
_refine_diff_density_min         -1.883
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         13629
_refine_ls_number_restraints     268
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0824
_refine_ls_restrained_S_all      1.025
_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)+(0.1194P)²+96.5095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2406
_refine_ls_wR_factor_ref         0.2447
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P-H
 1.43 with sigma of 0.001
 W-H
 3 with sigma of 0.01
 H-N1
 3.3 with sigma of 0.1
 C5-H
 2.9 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C12 \\sim C12S \\sim C13 \\sim C13S \\sim C14 \\sim C14S \\sim C15 \\sim C15S
\\sim C16 \\sim C16S \\sim C17 \\sim C17S: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C28)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C14) \\sim Ueq, Uanis(C14S) \\sim Ueq, Uanis(C15S) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C16S) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Sof(C16S)=Sof(H16S)=Sof(C15S)=Sof(H15S)=Sof(C14S)=Sof(H14S)=Sof(C13S)=
 Sof(H13S)=Sof(C12S)=Sof(C17S)=Sof(H17S)=1-FVAR(1)
 Sof(C12)=Sof(C17)=Sof(H17)=Sof(C16)=Sof(H16)=Sof(C15)=Sof(H15)=Sof(C14)=
 Sof(H14)=Sof(C13)=Sof(H13)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C17(H17),
 C16(H16), C15(H15), C14(H14), C13(H13), C16S(H16S), C15S(H15S), C14S(H14S),
 C13S(H13S), C17S(H17S), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23)
5.b Fitted hexagon refined as free rotating group:
 C12(C17,C16,C15,C14,C13), C16S(C15S,C14S,C13S,C12S,C17S)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.50570(3) 0.44690(2) 0.64362(2) 0.03143(12) Uani 1 1 d D . . . .
P P 0.32121(16) 0.40887(5) 0.68971(10) 0.0175(3) Uani 1 1 d D . . . .
H H 0.390(2) 0.3987(14) 0.7688(14) 0.021 Uiso 1 1 d DR . . . .
O1 O 0.7644(8) 0.4880(2) 0.5892(5) 0.0572(19) Uani 1 1 d . U . . .
O2 O 0.6560(11) 0.3668(3) 0.6608(6) 0.074(3) Uani 1 1 d . U . . .
O3 O 0.6272(8) 0.4634(2) 0.8305(6) 0.056(2) Uani 1 1 d . . . . .
O4 O 0.3654(6) 0.52926(16) 0.6326(4) 0.0344(13) Uani 1 1 d . . . . .
O5 O 0.3895(10) 0.4327(3) 0.4560(6) 0.067(2) Uani 1 1 d . . . . .
N1 N 0.2855(6) 0.36723(16) 0.6277(4) 0.0209(11) Uani 1 1 d D . . . .
N2 N 0.2194(7) 0.32985(18) 0.5228(4) 0.0278(13) Uani 1 1 d . . . . .
C1 C 0.2213(7) 0.3658(2) 0.5497(5) 0.0245(14) Uani 1 1 d . . . . .
H1 H 0.183451 0.387143 0.518968 0.029 Uiso 1 1 calc R . . . .
C2 C 0.2871(9) 0.3069(2) 0.5860(5) 0.0322(17) Uani 1 1 d . . . . .
H2 H 0.302230 0.280157 0.583759 0.039 Uiso 1 1 calc R . . . .
C3 C 0.3258(8) 0.3299(2) 0.6492(5) 0.0297(16) Uani 1 1 d . . . . .
H3 H 0.373252 0.322148 0.700618 0.036 Uiso 1 1 calc R . . . .
C4 C 0.1576(13) 0.3181(3) 0.4416(6) 0.051(3) Uani 1 1 d . . . . .
H4A H 0.222788 0.303081 0.415002 0.076 Uiso 1 1 calc GR . . . .
H4B H 0.130859 0.340788 0.408285 0.076 Uiso 1 1 calc GR . . . .
H4C H 0.077372 0.302460 0.446650 0.076 Uiso 1 1 calc GR . . . .
C5 C 0.1476(7) 0.42698(19) 0.7126(4) 0.0185(12) Uani 1 1 d D . . . .
C6 C 0.0612(7) 0.42775(19) 0.6264(4) 0.0192(12) Uani 1 1 d . . . . .
C7 C 0.0957(7) 0.4523(2) 0.5642(4) 0.0207(13) Uani 1 1 d . . . . .
H7 H 0.167899 0.469984 0.576419 0.025 Uiso 1 1 calc R . . . .
C8 C 0.0259(8) 0.4510(2) 0.4855(5) 0.0260(14) Uani 1 1 d . . . . .
H8 H 0.051354 0.467550 0.444249 0.031 Uiso 1 1 calc R . . . .
C9 C -0.0818(8) 0.4254(2) 0.4661(5) 0.0298(16) Uani 1 1 d . . . . .
H9 H -0.128921 0.424874 0.411832 0.036 Uiso 1 1 calc R . . . .
C10 C -0.1202(8) 0.4010(2) 0.5256(6) 0.0316(16) Uani 1 1 d . . . . .
H10 H -0.192929 0.383461 0.512823 0.038 Uiso 1 1 calc R . . . .
C11 C -0.0478(7) 0.40279(19) 0.6063(4) 0.0202(12) Uani 1 1 d . . . . .
H11 H -0.074384 0.386547 0.647897 0.024 Uiso 1 1 calc R . . . .
C12 C 0.0818(12) 0.4021(3) 0.7735(6) 0.0279(9) Uani 0.506(14) 1 d . U P A 1
C17 C -0.0063(12) 0.4215(2) 0.8181(7) 0.0282(9) Uani 0.506(14) 1 d G U P A 1
H17 H -0.022223 0.448035 0.809150 0.034 Uiso 0.506(14) 1 calc R . P A 1
C16 C -0.0710(12) 0.4020(3) 0.8759(7) 0.0283(9) Uani 0.506(14) 1 d G U P A 1
H16 H -0.131220 0.415317 0.906421 0.034 Uiso 0.506(14) 1 calc R . P A 1
C15 C -0.0477(11) 0.3632(3) 0.8890(6) 0.0283(9) Uani 0.506(14) 1 d G U P A 1
H15 H -0.091951 0.349907 0.928520 0.034 Uiso 0.506(14) 1 calc R . P A 1
C14 C 0.0404(11) 0.3438(3) 0.8444(7) 0.0282(9) Uani 0.506(14) 1 d G U P A 1
H14 H 0.056315 0.317215 0.853346 0.034 Uiso 0.506(14) 1 calc R . P A 1
C13 C 0.1051(11) 0.3632(3) 0.7866(7) 0.0280(9) Uani 0.506(14) 1 d G U P A 1
H13 H 0.165314 0.349932 0.756074 0.034 Uiso 0.506(14) 1 calc R . P A 1
C16S C -0.0233(13) 0.3906(3) 0.8946(6) 0.0283(9) Uani 0.494(14) 1 d . U P A 2
H16S H -0.063275 0.401531 0.938769 0.034 Uiso 0.494(14) 1 calc R . P A 2
C15S C -0.0162(12) 0.3511(3) 0.8868(6) 0.0283(9) Uani 0.494(14) 1 d G U P A 2
H15S H -0.051287 0.335007 0.925623 0.034 Uiso 0.494(14) 1 calc R . P A 2
C14S C 0.0422(11) 0.3352(2) 0.8221(7) 0.0281(9) Uani 0.494(14) 1 d G U P A 2
H14S H 0.047066 0.308172 0.816739 0.034 Uiso 0.494(14) 1 calc R . P A 2
C13S C 0.0935(12) 0.3588(3) 0.7652(6) 0.0280(9) Uani 0.494(14) 1 d G U P A 2
H13S H 0.133432 0.347861 0.721000 0.034 Uiso 0.494(14) 1 calc R . P A 2
C12S C 0.0864(12) 0.3983(3) 0.7730(6) 0.0279(9) Uani 0.494(14) 1 d G U P A 2
C17S C 0.0280(13) 0.4142(3) 0.8377(7) 0.0282(9) Uani 0.494(14) 1 d G U P A 2
H17S H 0.023093 0.441221 0.843028 0.034 Uiso 0.494(14) 1 calc R . P A 2
C18 C 0.1779(7) 0.46571(19) 0.7501(4) 0.0198(12) Uani 1 1 d . . . . .
C19 C 0.1037(9) 0.4979(2) 0.7266(5) 0.0299(16) Uani 1 1 d . . . . .
H19 H 0.030570 0.496642 0.683164 0.036 Uiso 1 1 calc R . . . .
C20 C 0.1370(11) 0.5327(2) 0.7674(6) 0.040(2) Uani 1 1 d . . . . .
H20 H 0.086578 0.555084 0.750432 0.049 Uiso 1 1 calc R . . . .
C21 C 0.2393(11) 0.5351(2) 0.8305(6) 0.041(2) Uani 1 1 d . . . . .
H21 H 0.260527 0.558864 0.857274 0.050 Uiso 1 1 calc R . . . .
C22 C 0.3098(10) 0.5037(3) 0.8545(6) 0.041(2) Uani 1 1 d . U . . .
H22 H 0.380723 0.505652 0.899083 0.049 Uiso 1 1 calc R . . . .
C23 C 0.2836(8) 0.4678(2) 0.8165(5) 0.0283(15) Uani 1 1 d . . . . .
H23 H 0.335026 0.445826 0.834856 0.034 Uiso 1 1 calc R . . . .
C24 C 0.6697(9) 0.4732(3) 0.6083(7) 0.042(2) Uani 1 1 d . . . . .
C25 C 0.6037(11) 0.3965(3) 0.6552(7) 0.047(2) Uani 1 1 d . U . . .
C26 C 0.5818(9) 0.4576(3) 0.7680(7) 0.039(2) Uani 1 1 d . . . . .
C27 C 0.4133(7) 0.4994(2) 0.6380(5) 0.0264(15) Uani 1 1 d . . . . .
C28 C 0.4329(10) 0.4372(3) 0.5250(6) 0.0383(18) 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 2.4643(17) . ?
W C24 2.023(9) . ?
W C25 2.012(11) . ?
W C26 2.113(10) . ?
W C27 2.051(8) . ?
W C28 2.013(10) . ?
P H 1.4301(10) . ?
P N1 1.784(6) . ?
P C5 1.923(7) . ?
O1 C24 1.153(12) . ?
O2 C25 1.158(14) . ?
O3 C26 1.083(12) . ?
O4 C27 1.145(10) . ?
O5 C28 1.166(13) . ?
N1 C1 1.352(9) . ?
N1 C3 1.398(9) . ?
N2 C1 1.331(9) . ?
N2 C2 1.409(11) . ?
N2 C4 1.451(11) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.325(11) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.555(9) . ?
C5 C12 1.534(10) . ?
C5 C12S 1.586(10) . ?
C5 C18 1.501(9) . ?
C6 C7 1.409(9) . ?
C6 C11 1.398(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.382(10) . ?
C8 H8 0.9500 . ?
C8 C9 1.399(11) . ?
C9 H9 0.9500 . ?
C9 C10 1.388(12) . ?
C10 H10 0.9500 . ?
C10 C11 1.422(11) . ?
C11 H11 0.9500 . ?
C12 C17 1.3900 . ?
C12 C13 1.3900 . ?
C17 H17 0.9500 . ?
C17 C16 1.3900 . ?
C16 H16 0.9500 . ?
C16 C15 1.3900 . ?
C15 H15 0.9500 . ?
C15 C14 1.3900 . ?
C14 H14 0.9500 . ?
C14 C13 1.3900 . ?
C13 H13 0.9500 . ?
C16S H16S 0.9500 . ?
C16S C15S 1.3900 . ?
C16S C17S 1.3900 . ?
C15S H15S 0.9500 . ?
C15S C14S 1.3900 . ?
C14S H14S 0.9500 . ?
C14S C13S 1.3900 . ?
C13S H13S 0.9500 . ?
C13S C12S 1.3900 . ?
C12S C17S 1.3900 . ?
C17S H17S 0.9500 . ?
C18 C19 1.373(10) . ?
C18 C23 1.413(9) . ?
C19 H19 0.9500 . ?
C19 C20 1.409(12) . ?
C20 H20 0.9500 . ?
C20 C21 1.355(14) . ?
C21 H21 0.9500 . ?
C21 C22 1.334(13) . ?
C22 H22 0.9500 . ?
C22 C23 1.411(12) . ?
C23 H23 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C24 W P 174.0(3) . . ?
C24 W C26 89.7(4) . . ?
C24 W C27 87.4(3) . . ?
C25 W P 82.5(3) . . ?
C25 W C24 91.5(4) . . ?
C25 W C26 87.5(4) . . ?
C25 W C27 176.5(4) . . ?
C25 W C28 93.0(4) . . ?
C26 W P 89.3(2) . . ?
C27 W P 98.6(2) . . ?
C27 W C26 89.2(3) . . ?
C28 W P 90.9(3) . . ?
C28 W C24 90.1(4) . . ?
C28 W C26 179.5(4) . . ?
C28 W C27 90.3(4) . . ?
W P H 97.0(5) . . ?
N1 P W 111.5(2) . . ?
N1 P H 110(2) . . ?
N1 P C5 105.2(3) . . ?
C5 P W 127.4(2) . . ?
C5 P H 104.1(17) . . ?
C1 N1 P 127.0(5) . . ?
C1 N1 C3 106.8(6) . . ?
C3 N1 P 126.1(5) . . ?
C1 N2 C2 108.0(6) . . ?
C1 N2 C4 123.9(7) . . ?
C2 N2 C4 128.2(7) . . ?
N1 C1 H1 125.3 . . ?
N2 C1 N1 109.4(6) . . ?
N2 C1 H1 125.3 . . ?
N2 C2 H2 126.5 . . ?
C3 C2 N2 107.0(7) . . ?
C3 C2 H2 126.5 . . ?
N1 C3 H3 125.6 . . ?
C2 C3 N1 108.9(7) . . ?
C2 C3 H3 125.6 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P 103.5(4) . . ?
C6 C5 C12S 111.4(6) . . ?
C12 C5 P 114.3(6) . . ?
C12 C5 C6 111.5(7) . . ?
C12S C5 P 110.0(6) . . ?
C18 C5 P 103.9(4) . . ?
C18 C5 C6 114.4(5) . . ?
C18 C5 C12 109.0(6) . . ?
C18 C5 C12S 112.9(6) . . ?
C7 C6 C5 120.6(6) . . ?
C11 C6 C5 121.6(6) . . ?
C11 C6 C7 117.7(6) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 C6 120.9(6) . . ?
C8 C7 H7 119.5 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.7(7) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 119.8 . . ?
C10 C9 C8 120.4(7) . . ?
C10 C9 H9 119.8 . . ?
C9 C10 H10 120.9 . . ?
C9 C10 C11 118.2(7) . . ?
C11 C10 H10 120.9 . . ?
C6 C11 C10 122.0(6) . . ?
C6 C11 H11 119.0 . . ?
C10 C11 H11 119.0 . . ?
C17 C12 C5 114.6(7) . . ?
C17 C12 C13 120.0 . . ?
C13 C12 C5 125.4(7) . . ?
C12 C17 H17 120.0 . . ?
C12 C17 C16 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C16 H16 120.0 . . ?
C15 C16 C17 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C15 H15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C14 C15 H15 120.0 . . ?
C15 C14 H14 120.0 . . ?
C15 C14 C13 120.0 . . ?
C13 C14 H14 120.0 . . ?
C12 C13 H13 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15S C16S H16S 120.0 . . ?
C15S C16S C17S 120.0 . . ?
C17S C16S H16S 120.0 . . ?
C16S C15S H15S 120.0 . . ?
C14S C15S C16S 120.0 . . ?
C14S C15S H15S 120.0 . . ?
C15S C14S H14S 120.0 . . ?
C15S C14S C13S 120.0 . . ?
C13S C14S H14S 120.0 . . ?
C14S C13S H13S 120.0 . . ?
C12S C13S C14S 120.0 . . ?
C12S C13S H13S 120.0 . . ?
C13S C12S C5 122.9(7) . . ?
C13S C12S C17S 120.0 . . ?
C17S C12S C5 117.1(7) . . ?
C16S C17S H17S 120.0 . . ?
C12S C17S C16S 120.0 . . ?
C12S C17S H17S 120.0 . . ?
C19 C18 C5 123.5(6) . . ?
C19 C18 C23 119.6(7) . . ?
C23 C18 C5 116.8(6) . . ?
C18 C19 H19 120.3 . . ?
C18 C19 C20 119.4(8) . . ?
C20 C19 H19 120.3 . . ?
C19 C20 H20 119.3 . . ?
C21 C20 C19 121.4(8) . . ?
C21 C20 H20 119.3 . . ?
C20 C21 H21 120.4 . . ?
C22 C21 C20 119.3(8) . . ?
C22 C21 H21 120.4 . . ?
C21 C22 H22 118.6 . . ?
C21 C22 C23 122.8(9) . . ?
C23 C22 H22 118.6 . . ?
C18 C23 H23 121.3 . . ?
C22 C23 C18 117.5(7) . . ?
C22 C23 H23 121.3 . . ?
O1 C24 W 179.0(10) . . ?
O2 C25 W 177.7(10) . . ?
O3 C26 W 176.3(9) . . ?
O4 C27 W 177.1(7) . . ?
O5 C28 W 178.0(9) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.862 -0.166 -0.941 3490.7 303.8 ?

_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_12-Cr
_database_code_depnum_ccdc_archive 'CCDC 2302953'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2022-06-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-2
_chemical_name_common            ?
_chemical_name_systematic        DB-558
_chemical_formula_moiety         'C29 H24 Cr N2 O5 P, C H2 Cl2, C F3 O3 S'
_chemical_formula_sum            'C31 H26 Cl2 Cr F3 N2 O8 P S'
_chemical_formula_weight         797.47
_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 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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                   8.5285(6)
_cell_length_b                   12.2121(9)
_cell_length_c                   17.7662(12)
_cell_angle_alpha                69.997(5)
_cell_angle_beta                 78.901(5)
_cell_angle_gamma                79.928(6)
_cell_volume                     1694.3(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    32229
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      3.88
_shelx_estimated_absorpt_T_max   0.944
_shelx_estimated_absorpt_T_min   0.387
_exptl_absorpt_coefficient_mu    5.868
_exptl_absorpt_correction_T_max  0.9570
_exptl_absorpt_correction_T_min  0.4156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36949
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.748
_diffrn_reflns_theta_min         3.879
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
 4647 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Stadivari
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4434
_reflns_number_total             6088
_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       
;
X-Area Recipe 1.37.0.0 (STOE, 2021)
;
_computing_data_collection       
;
X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)
;
_computing_data_reduction        
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6088
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0714
_refine_ls_restrained_S_all      1.032
_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)+(0.1067P)²+5.7467P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.2061
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
  C23(H23), C24(H24)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C)
;
_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 0.77788(10) 0.79791(8) 0.60378(5) 0.0285(3) Uani 1 1 d . . . . .
P1 P 0.59467(14) 0.87599(11) 0.69891(8) 0.0229(3) Uani 1 1 d . . . . .
O1 O 1.0139(5) 0.7436(4) 0.4680(3) 0.0440(10) Uani 1 1 d . . . . .
O2 O 0.7654(5) 0.5360(4) 0.6870(3) 0.0454(11) Uani 1 1 d . . . . .
O3 O 1.0839(5) 0.7828(4) 0.6738(3) 0.0395(10) Uani 1 1 d . . . . .
O4 O 0.8103(5) 1.0509(4) 0.5035(3) 0.0431(10) Uani 1 1 d . . . . .
O5 O 0.5017(5) 0.7862(4) 0.5229(3) 0.0462(11) Uani 1 1 d . . . . .
N1 N 0.6748(5) 0.9995(4) 0.7014(2) 0.0242(9) Uani 1 1 d . . . . .
N2 N 0.7180(5) 1.1797(4) 0.6762(3) 0.0268(9) Uani 1 1 d . . . . .
C1 C 0.4101(6) 0.9525(5) 0.6581(3) 0.0262(11) Uani 1 1 d . . . . .
H1A H 0.4371 1.0019 0.6019 0.039 Uiso 1 1 calc GR . . . .
H1B H 0.3527 1.0018 0.6906 0.039 Uiso 1 1 calc GR . . . .
H1C H 0.3414 0.8949 0.6599 0.039 Uiso 1 1 calc GR . . . .
C2 C 0.6153(6) 1.1123(4) 0.6725(3) 0.0258(11) Uani 1 1 d . . . . .
H2 H 0.5153 1.1398 0.6524 0.031 Uiso 1 1 calc R . . . .
C3 C 0.8216(6) 0.9978(5) 0.7253(3) 0.0264(11) Uani 1 1 d . . . . .
H3 H 0.8909 0.9296 0.7489 0.032 Uiso 1 1 calc R . . . .
C4 C 0.8480(6) 1.1090(5) 0.7093(3) 0.0298(12) Uani 1 1 d . . . . .
H4 H 0.9394 1.1342 0.7190 0.036 Uiso 1 1 calc R . . . .
C5 C 0.6943(7) 1.3089(5) 0.6478(4) 0.0348(13) Uani 1 1 d . . . . .
H5A H 0.6646 1.3371 0.5932 0.052 Uiso 1 1 calc GR . . . .
H5B H 0.7943 1.3389 0.6468 0.052 Uiso 1 1 calc GR . . . .
H5C H 0.6082 1.3368 0.6845 0.052 Uiso 1 1 calc GR . . . .
C6 C 0.5209(6) 0.8066(4) 0.8130(3) 0.0223(10) Uani 1 1 d . . . . .
C7 C 0.4496(5) 0.6920(4) 0.8261(3) 0.0230(11) Uani 1 1 d . . . . .
C8 C 0.4205(6) 0.6566(4) 0.7644(3) 0.0261(11) Uani 1 1 d . . . . .
H8 H 0.4415 0.7050 0.7097 0.031 Uiso 1 1 calc R . . . .
C9 C 0.3602(6) 0.5494(5) 0.7823(4) 0.0304(12) Uani 1 1 d . . . . .
H9 H 0.3428 0.5253 0.7394 0.037 Uiso 1 1 calc R . . . .
C10 C 0.3264(6) 0.4795(5) 0.8601(4) 0.0310(12) Uani 1 1 d . . . . .
H10 H 0.2851 0.4072 0.8715 0.037 Uiso 1 1 calc R . . . .
C11 C 0.3523(6) 0.5141(5) 0.9226(4) 0.0317(12) Uani 1 1 d . . . . .
H11 H 0.3282 0.4660 0.9771 0.038 Uiso 1 1 calc R . . . .
C12 C 0.4138(6) 0.6195(5) 0.9054(3) 0.0293(12) Uani 1 1 d . . . . .
H12 H 0.4318 0.6425 0.9487 0.035 Uiso 1 1 calc R . . . .
C13 C 0.6695(6) 0.7694(4) 0.8585(3) 0.0228(10) Uani 1 1 d . . . . .
C14 C 0.7929(6) 0.6916(5) 0.8356(3) 0.0279(11) Uani 1 1 d . . . . .
H14 H 0.7848 0.6652 0.7922 0.033 Uiso 1 1 calc R . . . .
C15 C 0.9289(6) 0.6513(5) 0.8751(3) 0.0324(13) Uani 1 1 d . . . . .
H15 H 1.0138 0.6000 0.8574 0.039 Uiso 1 1 calc R . . . .
C16 C 0.9389(6) 0.6865(5) 0.9394(4) 0.0363(14) Uani 1 1 d . . . . .
H16 H 1.0313 0.6601 0.9663 0.044 Uiso 1 1 calc R . . . .
C17 C 0.8150(7) 0.7600(5) 0.9650(3) 0.0331(12) Uani 1 1 d . . . . .
H17 H 0.8217 0.7831 1.0101 0.040 Uiso 1 1 calc R . . . .
C18 C 0.6801(6) 0.8007(5) 0.9256(3) 0.0284(11) Uani 1 1 d . . . . .
H18 H 0.5946 0.8503 0.9446 0.034 Uiso 1 1 calc R . . . .
C19 C 0.3929(6) 0.8960(4) 0.8396(3) 0.0251(11) Uani 1 1 d . . . . .
C20 C 0.4335(6) 0.9964(5) 0.8494(3) 0.0260(11) Uani 1 1 d . . . . .
H20 H 0.5437 1.0076 0.8415 0.031 Uiso 1 1 calc R . . . .
C21 C 0.3165(7) 1.0798(5) 0.8704(3) 0.0327(12) Uani 1 1 d . . . . .
H21 H 0.3468 1.1475 0.8762 0.039 Uiso 1 1 calc R . . . .
C22 C 0.1550(6) 1.0636(5) 0.8829(4) 0.0338(13) Uani 1 1 d . . . . .
H22 H 0.0745 1.1197 0.8980 0.041 Uiso 1 1 calc R . . . .
C23 C 0.1120(6) 0.9660(5) 0.8733(3) 0.0336(13) Uani 1 1 d . . . . .
H23 H 0.0015 0.9556 0.8815 0.040 Uiso 1 1 calc R . . . .
C24 C 0.2282(6) 0.8827(5) 0.8519(3) 0.0287(11) Uani 1 1 d . . . . .
H24 H 0.1963 0.8161 0.8454 0.034 Uiso 1 1 calc R . . . .
C25 C 0.9216(7) 0.7616(5) 0.5192(4) 0.0358(13) Uani 1 1 d . . . . .
C26 C 0.7694(6) 0.6340(5) 0.6581(3) 0.0316(12) Uani 1 1 d . . . . .
C27 C 0.9665(7) 0.7904(5) 0.6498(3) 0.0318(12) Uani 1 1 d . . . . .
C28 C 0.7951(6) 0.9566(5) 0.5411(3) 0.0304(12) Uani 1 1 d . . . . .
C29 C 0.6002(7) 0.7937(5) 0.5519(4) 0.0354(13) Uani 1 1 d . . . . .
Cl1 Cl 0.1871(3) 0.6212(2) 0.10477(13) 0.0790(7) Uani 1 1 d . . . . .
Cl2 Cl 0.3016(2) 0.84183(17) 0.08255(12) 0.0588(5) Uani 1 1 d . . . . .
C31 C 0.2656(8) 0.7013(7) 0.1497(4) 0.0504(17) Uani 1 1 d . . . . .
H31A H 0.3677 0.6581 0.1685 0.060 Uiso 1 1 calc R . . . .
H31B H 0.1893 0.7096 0.1976 0.060 Uiso 1 1 calc R . . . .
S S 0.21102(15) 0.31343(12) 0.67936(9) 0.0328(3) Uani 1 1 d . . . . .
F1 F 0.3602(5) 0.4722(4) 0.5609(3) 0.0786(15) Uani 1 1 d . . . . .
F2 F 0.1532(5) 0.5425(3) 0.6263(3) 0.0615(11) Uani 1 1 d . . . . .
F3 F 0.1247(6) 0.4590(4) 0.5424(3) 0.0771(15) Uani 1 1 d . . . . .
O6 O 0.0435(5) 0.3094(4) 0.7125(3) 0.0479(11) Uani 1 1 d . . . . .
O7 O 0.2741(5) 0.2289(4) 0.6377(3) 0.0460(11) Uani 1 1 d . . . . .
O8 O 0.3138(5) 0.3247(4) 0.7305(3) 0.0405(10) Uani 1 1 d . . . . .
C30 C 0.2114(8) 0.4528(6) 0.5984(5) 0.0483(17) 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 P1 2.4024(15) . ?
Cr C25 1.875(6) . ?
Cr C26 1.909(6) . ?
Cr C27 1.915(6) . ?
Cr C28 1.891(6) . ?
Cr C29 1.935(6) . ?
P1 N1 1.778(4) . ?
P1 C1 1.828(5) . ?
P1 C6 1.935(5) . ?
O1 C25 1.138(7) . ?
O2 C26 1.134(7) . ?
O3 C27 1.140(7) . ?
O4 C28 1.133(7) . ?
O5 C29 1.098(7) . ?
N1 C2 1.338(7) . ?
N1 C3 1.392(6) . ?
N2 C2 1.328(7) . ?
N2 C4 1.375(7) . ?
N2 C5 1.472(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 H2 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.339(8) . ?
C4 H4 0.9500 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.551(7) . ?
C6 C13 1.552(7) . ?
C6 C19 1.531(7) . ?
C7 C8 1.385(8) . ?
C7 C12 1.392(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.402(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.360(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(8) . ?
C11 H11 0.9500 . ?
C11 C12 1.389(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(7) . ?
C13 C18 1.393(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.398(7) . ?
C15 H15 0.9500 . ?
C15 C16 1.374(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.375(8) . ?
C17 H17 0.9500 . ?
C17 C18 1.390(8) . ?
C18 H18 0.9500 . ?
C19 C20 1.403(7) . ?
C19 C24 1.409(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.390(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.391(8) . ?
C22 H22 0.9500 . ?
C22 C23 1.378(8) . ?
C23 H23 0.9500 . ?
C23 C24 1.389(8) . ?
C24 H24 0.9500 . ?
Cl1 C31 1.736(7) . ?
Cl2 C31 1.762(8) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
S O6 1.439(4) . ?
S O7 1.442(4) . ?
S O8 1.430(4) . ?
S C30 1.814(7) . ?
F1 C30 1.335(8) . ?
F2 C30 1.335(8) . ?
F3 C30 1.324(8) . ?

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
C25 Cr P1 170.99(19) . . ?
C25 Cr C26 89.1(2) . . ?
C25 Cr C27 85.4(2) . . ?
C25 Cr C28 85.7(2) . . ?
C25 Cr C29 89.3(2) . . ?
C26 Cr P1 99.85(17) . . ?
C26 Cr C27 90.1(2) . . ?
C26 Cr C29 86.9(2) . . ?
C27 Cr P1 95.43(17) . . ?
C27 Cr C29 173.9(2) . . ?
C28 Cr P1 85.30(17) . . ?
C28 Cr C26 174.7(2) . . ?
C28 Cr C27 90.8(2) . . ?
C28 Cr C29 91.6(2) . . ?
C29 Cr P1 90.31(17) . . ?
N1 P1 Cr 106.91(14) . . ?
N1 P1 C1 98.3(2) . . ?
N1 P1 C6 99.9(2) . . ?
C1 P1 Cr 111.61(18) . . ?
C1 P1 C6 103.2(2) . . ?
C6 P1 Cr 131.59(16) . . ?
C2 N1 P1 126.7(4) . . ?
C2 N1 C3 106.9(4) . . ?
C3 N1 P1 126.1(4) . . ?
C2 N2 C4 108.7(4) . . ?
C2 N2 C5 124.5(5) . . ?
C4 N2 C5 126.8(4) . . ?
P1 C1 H1A 109.5 . . ?
P1 C1 H1B 109.5 . . ?
P1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2 125.3 . . ?
N2 C2 N1 109.3(4) . . ?
N2 C2 H2 125.3 . . ?
N1 C3 H3 126.0 . . ?
C4 C3 N1 108.1(5) . . ?
C4 C3 H3 126.0 . . ?
N2 C4 H4 126.5 . . ?
C3 C4 N2 107.1(5) . . ?
C3 C4 H4 126.5 . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 P1 109.0(3) . . ?
C7 C6 C13 106.2(4) . . ?
C13 C6 P1 108.1(3) . . ?
C19 C6 P1 107.6(3) . . ?
C19 C6 C7 110.9(4) . . ?
C19 C6 C13 114.8(4) . . ?
C8 C7 C6 124.5(4) . . ?
C8 C7 C12 117.9(5) . . ?
C12 C7 C6 117.5(5) . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.2(5) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 119.5 . . ?
C10 C9 C8 121.1(5) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 120.2 . . ?
C9 C10 C11 119.6(5) . . ?
C11 C10 H10 120.2 . . ?
C10 C11 H11 120.1 . . ?
C10 C11 C12 119.8(5) . . ?
C12 C11 H11 120.1 . . ?
C7 C12 H12 119.3 . . ?
C11 C12 C7 121.4(5) . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C6 117.9(4) . . ?
C14 C13 C18 117.9(5) . . ?
C18 C13 C6 124.0(4) . . ?
C13 C14 H14 119.3 . . ?
C13 C14 C15 121.4(5) . . ?
C15 C14 H14 119.3 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.5(5) . . ?
C16 C15 H15 120.3 . . ?
C15 C16 H16 120.1 . . ?
C15 C16 C17 119.9(5) . . ?
C17 C16 H16 120.1 . . ?
C16 C17 H17 119.6 . . ?
C16 C17 C18 120.7(5) . . ?
C18 C17 H17 119.6 . . ?
C13 C18 H18 119.8 . . ?
C17 C18 C13 120.5(5) . . ?
C17 C18 H18 119.8 . . ?
C20 C19 C6 121.8(4) . . ?
C20 C19 C24 117.4(5) . . ?
C24 C19 C6 120.7(5) . . ?
C19 C20 H20 119.2 . . ?
C21 C20 C19 121.7(5) . . ?
C21 C20 H20 119.2 . . ?
C20 C21 H21 120.2 . . ?
C20 C21 C22 119.6(5) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 120.1 . . ?
C23 C22 C21 119.8(5) . . ?
C23 C22 H22 120.1 . . ?
C22 C23 H23 119.6 . . ?
C22 C23 C24 120.9(5) . . ?
C24 C23 H23 119.6 . . ?
C19 C24 H24 119.7 . . ?
C23 C24 C19 120.6(5) . . ?
C23 C24 H24 119.7 . . ?
O1 C25 Cr 176.4(5) . . ?
O2 C26 Cr 176.8(5) . . ?
O3 C27 Cr 175.8(5) . . ?
O4 C28 Cr 177.9(5) . . ?
O5 C29 Cr 176.9(6) . . ?
Cl1 C31 Cl2 112.1(4) . . ?
Cl1 C31 H31A 109.2 . . ?
Cl1 C31 H31B 109.2 . . ?
Cl2 C31 H31A 109.2 . . ?
Cl2 C31 H31B 109.2 . . ?
H31A C31 H31B 107.9 . . ?
O6 S O7 113.6(3) . . ?
O6 S C30 103.2(3) . . ?
O7 S C30 103.3(3) . . ?
O8 S O6 116.0(3) . . ?
O8 S O7 115.1(3) . . ?
O8 S C30 103.1(3) . . ?
F1 C30 S 111.5(4) . . ?
F2 C30 S 111.6(5) . . ?
F2 C30 F1 106.3(6) . . ?
F3 C30 S 112.7(5) . . ?
F3 C30 F1 107.1(6) . . ?
F3 C30 F2 107.3(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cr P1 N1 C2 109.8(4) . . . . ?
Cr P1 N1 C3 -62.1(4) . . . . ?
P1 N1 C2 N2 -172.3(3) . . . . ?
P1 N1 C3 C4 172.4(4) . . . . ?
P1 C6 C7 C8 -9.5(6) . . . . ?
P1 C6 C7 C12 169.9(4) . . . . ?
P1 C6 C13 C14 -57.7(5) . . . . ?
P1 C6 C13 C18 128.5(4) . . . . ?
P1 C6 C19 C20 -73.9(5) . . . . ?
P1 C6 C19 C24 103.4(5) . . . . ?
N1 C3 C4 N2 0.5(6) . . . . ?
C1 P1 N1 C2 -5.9(5) . . . . ?
C1 P1 N1 C3 -177.8(4) . . . . ?
C2 N1 C3 C4 -0.8(6) . . . . ?
C2 N2 C4 C3 0.0(6) . . . . ?
C3 N1 C2 N2 0.9(6) . . . . ?
C4 N2 C2 N1 -0.6(6) . . . . ?
C5 N2 C2 N1 178.5(5) . . . . ?
C5 N2 C4 C3 -179.0(5) . . . . ?
C6 P1 N1 C2 -111.0(4) . . . . ?
C6 P1 N1 C3 77.1(4) . . . . ?
C6 C7 C8 C9 178.0(4) . . . . ?
C6 C7 C12 C11 -178.8(5) . . . . ?
C6 C13 C14 C15 -178.2(4) . . . . ?
C6 C13 C18 C17 177.4(5) . . . . ?
C6 C19 C20 C21 177.4(5) . . . . ?
C6 C19 C24 C23 -177.8(5) . . . . ?
C7 C6 C13 C14 59.2(5) . . . . ?
C7 C6 C13 C18 -114.6(5) . . . . ?
C7 C6 C19 C20 166.9(5) . . . . ?
C7 C6 C19 C24 -15.8(7) . . . . ?
C7 C8 C9 C10 1.2(8) . . . . ?
C8 C7 C12 C11 0.6(7) . . . . ?
C8 C9 C10 C11 -0.3(8) . . . . ?
C9 C10 C11 C12 -0.5(8) . . . . ?
C10 C11 C12 C7 0.3(8) . . . . ?
C12 C7 C8 C9 -1.4(7) . . . . ?
C13 C6 C7 C8 -125.8(5) . . . . ?
C13 C6 C7 C12 53.6(5) . . . . ?
C13 C6 C19 C20 46.5(6) . . . . ?
C13 C6 C19 C24 -136.2(5) . . . . ?
C13 C14 C15 C16 2.0(8) . . . . ?
C14 C13 C18 C17 3.6(7) . . . . ?
C14 C15 C16 C17 0.6(8) . . . . ?
C15 C16 C17 C18 -1.0(8) . . . . ?
C16 C17 C18 C13 -1.1(8) . . . . ?
C18 C13 C14 C15 -4.0(7) . . . . ?
C19 C6 C7 C8 108.8(5) . . . . ?
C19 C6 C7 C12 -71.8(6) . . . . ?
C19 C6 C13 C14 -177.8(4) . . . . ?
C19 C6 C13 C18 8.3(7) . . . . ?
C19 C20 C21 C22 0.6(8) . . . . ?
C20 C19 C24 C23 -0.4(8) . . . . ?
C20 C21 C22 C23 -0.9(9) . . . . ?
C21 C22 C23 C24 0.5(9) . . . . ?
C22 C23 C24 C19 0.2(9) . . . . ?
C24 C19 C20 C21 0.0(8) . . . . ?
O6 S C30 F1 179.1(5) . . . . ?
O6 S C30 F2 60.4(5) . . . . ?
O6 S C30 F3 -60.4(6) . . . . ?
O7 S C30 F1 -62.3(6) . . . . ?
O7 S C30 F2 179.0(4) . . . . ?
O7 S C30 F3 58.2(6) . . . . ?
O8 S C30 F1 57.9(6) . . . . ?
O8 S C30 F2 -60.8(5) . . . . ?
O8 S C30 F3 178.4(5) . . . . ?

_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_11b
_database_code_depnum_ccdc_archive 'CCDC 2302950'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2022-12-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        DB-604
_chemical_formula_moiety         'C32 H12 B F24, C28 H22 N2 O5 P W, C H2 Cl2'
_chemical_formula_sum            'C61 H36 B Cl2 F24 N2 O5 P W'
_chemical_formula_weight         1629.45
_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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   11.3237(5)
_cell_length_b                   14.0365(6)
_cell_length_c                   20.5226(7)
_cell_angle_alpha                98.0490(10)
_cell_angle_beta                 104.5540(10)
_cell_angle_gamma                94.751(2)
_cell_volume                     3102.4(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    9850
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.484
_cell_measurement_theta_min      2.523
_shelx_estimated_absorpt_T_max   0.818
_shelx_estimated_absorpt_T_min   0.655
_exptl_absorpt_coefficient_mu    2.097
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0937 before and 0.0387 after correction. The Ratio of minimum to maximum transmission is 0.8483. The λ/2 correction factor is Not present.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            89491
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.942
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                14610
_reflns_number_total             14911
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         14911
_refine_ls_number_restraints     126
_refine_ls_R_factor_all          0.0192
_refine_ls_R_factor_gt           0.0188
_refine_ls_restrained_S_all      1.194
_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)+(0.0183P)²+2.9212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0473
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups, All P(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F15 \\sim F14S \\sim F14 \\sim F13S \\sim F13 \\sim F15S: within 2A with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F13S) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F14S) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F15S) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F24) \\sim Ueq,
Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl2S)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F24S) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F22S) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23S) \\sim Ueq, Uanis(F23) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(F15) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(F13S)=Sof(F14S)=Sof(F15S)=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(Cl2S)=Sof(H61C)=Sof(H61D)=1-FVAR(2)
 Sof(Cl2)=Sof(H61A)=Sof(H61B)=FVAR(2)
 Sof(F22S)=Sof(F23S)=Sof(F24S)=1-FVAR(3)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C61(H61A,H61B), C61(H61C,H61D)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C30(H30), C32(H32), C34(H34), C38(H38), C40(H40), C42(H42),
 C46(H46), C48(H48), C50(H50), C54(H54), C56(H56), C58(H58)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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 0.53043(2) 0.02782(2) 0.74212(2) 0.01462(2) Uani 1 1 d . . . . .
P P 0.74699(4) -0.00159(3) 0.77568(2) 0.01344(7) Uani 1 1 d . . . . .
H H 0.7655(18) -0.0884(14) 0.7537(10) 0.016 Uiso 1 1 d R . . . .
O1 O 0.25375(12) 0.06449(11) 0.68847(7) 0.0329(3) Uani 1 1 d . . . . .
O2 O 0.61465(12) 0.25101(9) 0.74598(7) 0.0261(3) Uani 1 1 d . . . . .
O3 O 0.52627(14) -0.03529(10) 0.58615(6) 0.0290(3) Uani 1 1 d . . . . .
O4 O 0.45635(14) -0.19497(10) 0.74714(8) 0.0346(3) Uani 1 1 d . . . . .
O5 O 0.49518(13) 0.06671(11) 0.89223(7) 0.0299(3) Uani 1 1 d . . . . .
N1 N 0.83764(12) 0.04993(10) 0.72719(7) 0.0157(2) Uani 1 1 d . . . . .
N2 N 0.94357(13) 0.15217(10) 0.68717(7) 0.0179(3) Uani 1 1 d . . . . .
C1 C 0.87630(15) 0.14397(12) 0.73095(8) 0.0177(3) Uani 1 1 d . . . . .
H1 H 0.858400 0.196224 0.760230 0.021 Uiso 1 1 calc R . . . .
C2 C 0.94746(16) 0.06102(12) 0.65300(9) 0.0215(3) Uani 1 1 d . . . . .
H2 H 0.988538 0.046043 0.618482 0.026 Uiso 1 1 calc R . . . .
C3 C 0.88193(16) -0.00286(12) 0.67784(8) 0.0205(3) Uani 1 1 d . . . . .
H3 H 0.868542 -0.071248 0.664123 0.025 Uiso 1 1 calc R . . . .
C4 C 1.00294(17) 0.24338(13) 0.67613(10) 0.0251(4) Uani 1 1 d . . . . .
H4A H 0.977992 0.248022 0.627477 0.038 Uiso 1 1 calc GR . . . .
H4B H 1.092437 0.244762 0.691064 0.038 Uiso 1 1 calc GR . . . .
H4C H 0.977992 0.298193 0.702470 0.038 Uiso 1 1 calc GR . . . .
C5 C 0.86069(14) 0.01391(11) 0.86468(8) 0.0145(3) Uani 1 1 d . . . . .
C6 C 0.96569(14) -0.04595(11) 0.85662(8) 0.0158(3) Uani 1 1 d . . . . .
C7 C 1.05147(15) -0.01463(12) 0.82285(8) 0.0187(3) Uani 1 1 d . . . . .
H7 H 1.048223 0.046503 0.808053 0.022 Uiso 1 1 calc R . . . .
C8 C 1.14094(16) -0.07125(13) 0.81066(9) 0.0234(3) Uani 1 1 d . . . . .
H8 H 1.197183 -0.049209 0.786977 0.028 Uiso 1 1 calc R . . . .
C9 C 1.14850(17) -0.16017(13) 0.83302(9) 0.0253(4) Uani 1 1 d . . . . .
H9 H 1.208125 -0.199922 0.823590 0.030 Uiso 1 1 calc R . . . .
C10 C 1.06812(16) -0.19019(12) 0.86920(9) 0.0227(3) Uani 1 1 d . . . . .
H10 H 1.074862 -0.249635 0.886193 0.027 Uiso 1 1 calc R . . . .
C11 C 0.97748(15) -0.13376(12) 0.88082(8) 0.0189(3) Uani 1 1 d . . . . .
H11 H 0.922889 -0.155381 0.905583 0.023 Uiso 1 1 calc R . . . .
C12 C 0.90571(15) 0.12168(11) 0.89239(8) 0.0162(3) Uani 1 1 d . . . . .
C13 C 1.02801(16) 0.15339(12) 0.92779(8) 0.0202(3) Uani 1 1 d . . . . .
H13 H 1.086177 0.108113 0.933237 0.024 Uiso 1 1 calc R . . . .
C14 C 1.06561(18) 0.25133(13) 0.95530(9) 0.0257(4) Uani 1 1 d . . . . .
H14 H 1.149131 0.272048 0.979373 0.031 Uiso 1 1 calc R . . . .
C15 C 0.98228(19) 0.31828(13) 0.94778(10) 0.0286(4) Uani 1 1 d . . . . .
H15 H 1.008697 0.384949 0.965713 0.034 Uiso 1 1 calc R . . . .
C16 C 0.86006(19) 0.28753(13) 0.91393(9) 0.0268(4) Uani 1 1 d . . . . .
H16 H 0.802265 0.333136 0.908976 0.032 Uiso 1 1 calc R . . . .
C17 C 0.82170(17) 0.18985(12) 0.88713(8) 0.0210(3) Uani 1 1 d . . . . .
H17 H 0.737327 0.169208 0.864964 0.025 Uiso 1 1 calc R . . . .
C18 C 0.78045(14) -0.02860(11) 0.90658(8) 0.0157(3) Uani 1 1 d . . . . .
C19 C 0.70643(15) -0.11751(12) 0.88087(8) 0.0177(3) Uani 1 1 d . . . . .
H19 H 0.709306 -0.152801 0.838389 0.021 Uiso 1 1 calc R . . . .
C20 C 0.62873(16) -0.15526(13) 0.91628(9) 0.0216(3) Uani 1 1 d . . . . .
H20 H 0.578039 -0.215162 0.897638 0.026 Uiso 1 1 calc R . . . .
C21 C 0.62553(17) -0.10495(14) 0.97909(9) 0.0248(4) Uani 1 1 d . . . . .
H21 H 0.572679 -0.130283 1.003556 0.030 Uiso 1 1 calc R . . . .
C22 C 0.69976(17) -0.01784(14) 1.00571(9) 0.0240(3) Uani 1 1 d . . . . .
H22 H 0.698547 0.016086 1.048925 0.029 Uiso 1 1 calc R . . . .
C23 C 0.77636(16) 0.02075(12) 0.96980(8) 0.0195(3) Uani 1 1 d . . . . .
H23 H 0.826120 0.081051 0.988489 0.023 Uiso 1 1 calc R . . . .
C24 C 0.35319(16) 0.04989(13) 0.70758(9) 0.0224(3) Uani 1 1 d . . . . .
C25 C 0.58322(15) 0.17090(13) 0.74364(8) 0.0192(3) Uani 1 1 d . . . . .
C26 C 0.53117(16) -0.01090(12) 0.64198(9) 0.0204(3) Uani 1 1 d . . . . .
C27 C 0.48150(16) -0.11591(13) 0.74428(9) 0.0226(3) Uani 1 1 d . . . . .
C28 C 0.51225(15) 0.05489(12) 0.83967(9) 0.0201(3) Uani 1 1 d . . . . .
Cl1 Cl 0.65341(6) 0.46004(4) 0.99633(3) 0.04028(12) Uani 1 1 d . . . . .
Cl2 Cl 0.65215(15) 0.27829(19) 1.0470(2) 0.0570(7) Uani 0.723(10) 1 d . U P A 1
Cl2S Cl 0.6632(4) 0.3024(4) 1.0776(4) 0.0498(11) Uani 0.277(10) 1 d . U P A 2
C61 C 0.5969(2) 0.39585(17) 1.05196(12) 0.0397(5) Uani 1 1 d . . . . .
H61A H 0.505892 0.387906 1.038546 0.048 Uiso 0.723(10) 1 calc R . P A 1
H61B H 0.626158 0.431729 1.099274 0.048 Uiso 0.723(10) 1 calc R . P A 1
H61C H 0.599750 0.442775 1.093270 0.048 Uiso 0.277(10) 1 calc R . P A 2
H61D H 0.509158 0.372532 1.029559 0.048 Uiso 0.277(10) 1 calc R . P A 2
F1 F 0.64719(11) 0.79856(7) 0.63873(6) 0.0272(2) Uani 1 1 d . . . . .
F2 F 0.68131(11) 0.67471(8) 0.57513(5) 0.0262(2) Uani 1 1 d . . . . .
F3 F 0.82371(10) 0.74709(8) 0.66327(6) 0.0288(2) Uani 1 1 d . . . . .
F4 F 0.67851(10) 0.61916(8) 0.90571(5) 0.0244(2) Uani 1 1 d . . . . .
F5 F 0.85095(10) 0.65164(8) 0.88254(5) 0.0270(2) Uani 1 1 d . . . . .
F6 F 0.77121(10) 0.50362(8) 0.87045(5) 0.0253(2) Uani 1 1 d . . . . .
F7 F 0.46195(11) 0.26700(9) 0.85587(6) 0.0328(3) Uani 1 1 d . . . . .
F8 F 0.28102(13) 0.18955(8) 0.83128(7) 0.0397(3) Uani 1 1 d . . . . .
F9 F 0.34372(12) 0.29768(9) 0.92111(6) 0.0347(3) Uani 1 1 d . . . . .
F10 F 0.05547(13) 0.53820(11) 0.87045(6) 0.0415(3) Uani 1 1 d . . . . .
F11 F -0.06174(11) 0.44773(10) 0.78096(8) 0.0435(3) Uani 1 1 d . . . . .
F12 F 0.01981(13) 0.58751(10) 0.77381(7) 0.0421(3) Uani 1 1 d . . . . .
F13 F 0.26470(17) 0.84144(11) 0.61338(9) 0.0460(4) Uani 0.858(2) 1 d . U P B 1
F13S F 0.2438(11) 0.8278(8) 0.6643(6) 0.0522(8) Uani 0.142(2) 1 d . U P B 2
F14 F 0.16491(19) 0.78958(12) 0.67709(9) 0.0484(4) Uani 0.858(2) 1 d . U P B 1
F14S F 0.0658(11) 0.7795(8) 0.6398(6) 0.0531(8) Uani 0.142(2) 1 d . U P B 2
F15 F 0.0691(2) 0.80620(15) 0.57641(11) 0.0619(5) Uani 0.858(2) 1 d . U P B 1
F15S F 0.1221(12) 0.8310(8) 0.5608(6) 0.0484(9) Uani 0.142(2) 1 d . U P B 2
F16 F 0.03698(11) 0.55990(9) 0.38357(6) 0.0333(3) Uani 1 1 d . . . . .
F17 F 0.21068(10) 0.50562(9) 0.38915(5) 0.0290(2) Uani 1 1 d . . . . .
F18 F 0.06222(11) 0.41606(8) 0.40547(5) 0.0300(2) Uani 1 1 d . . . . .
F19 F 0.09908(10) 0.13724(8) 0.55115(6) 0.0290(2) Uani 1 1 d . . . . .
F20 F 0.15526(11) 0.12653(9) 0.45848(5) 0.0333(3) Uani 1 1 d . . . . .
F21 F 0.22237(12) 0.03542(8) 0.53127(8) 0.0407(3) Uani 1 1 d . . . . .
F22 F 0.6493(3) 0.2218(4) 0.50898(18) 0.0429(9) Uani 0.614(12) 1 d . U P C 1
F22S F 0.6564(6) 0.2580(7) 0.5151(4) 0.0511(16) Uani 0.386(12) 1 d . U P C 2
F23 F 0.6724(3) 0.1492(2) 0.5976(3) 0.0306(8) Uani 0.614(12) 1 d . U P C 1
F23S F 0.6557(5) 0.1416(3) 0.5684(5) 0.0360(13) Uani 0.386(12) 1 d . U P C 2
F24 F 0.7317(4) 0.2994(3) 0.6070(3) 0.0304(8) Uani 0.614(12) 1 d . U P C 1
F24S F 0.7340(6) 0.2888(5) 0.6266(4) 0.0327(13) Uani 0.386(12) 1 d . U P C 2
C29 C 0.49254(14) 0.53733(11) 0.69544(8) 0.0149(3) Uani 1 1 d . . . . .
C30 C 0.54429(14) 0.59574(11) 0.65687(8) 0.0159(3) Uani 1 1 d . . . . .
H30 H 0.500413 0.596406 0.610970 0.019 Uiso 1 1 calc R . . . .
C31 C 0.65746(15) 0.65255(11) 0.68358(8) 0.0159(3) Uani 1 1 d . . . . .
C32 C 0.72568(14) 0.65385(11) 0.75024(8) 0.0159(3) Uani 1 1 d . . . . .
H32 H 0.803174 0.692401 0.768463 0.019 Uiso 1 1 calc R . . . .
C33 C 0.67632(14) 0.59668(11) 0.78925(8) 0.0153(3) Uani 1 1 d . . . . .
C34 C 0.56232(14) 0.54029(11) 0.76250(8) 0.0156(3) Uani 1 1 d . . . . .
H34 H 0.531079 0.502602 0.790859 0.019 Uiso 1 1 calc R . . . .
C35 C 0.70246(15) 0.71653(12) 0.64011(8) 0.0191(3) Uani 1 1 d . . . . .
C36 C 0.74468(15) 0.59307(12) 0.86118(8) 0.0173(3) Uani 1 1 d . . . . .
C37 C 0.29647(14) 0.44243(11) 0.72078(8) 0.0151(3) Uani 1 1 d . . . . .
C38 C 0.34175(14) 0.37352(11) 0.76114(8) 0.0160(3) Uani 1 1 d . . . . .
H38 H 0.406583 0.340123 0.751449 0.019 Uiso 1 1 calc R . . . .
C39 C 0.29501(15) 0.35252(11) 0.81474(8) 0.0176(3) Uani 1 1 d . . . . .
C40 C 0.19815(16) 0.39766(12) 0.82994(8) 0.0202(3) Uani 1 1 d . . . . .
H40 H 0.165696 0.383178 0.866337 0.024 Uiso 1 1 calc R . . . .
C41 C 0.15058(15) 0.46480(12) 0.78986(8) 0.0191(3) Uani 1 1 d . . . . .
C42 C 0.19845(14) 0.48690(11) 0.73689(8) 0.0169(3) Uani 1 1 d . . . . .
H42 H 0.163809 0.533480 0.710818 0.020 Uiso 1 1 calc R . . . .
C43 C 0.34569(17) 0.27742(13) 0.85578(9) 0.0227(3) Uani 1 1 d . . . . .
C44 C 0.04214(17) 0.51029(14) 0.80380(10) 0.0255(4) Uani 1 1 d . . . . .
C45 C 0.27530(14) 0.52706(11) 0.60718(8) 0.0157(3) Uani 1 1 d . . . . .
C46 C 0.25433(15) 0.62216(12) 0.62969(8) 0.0185(3) Uani 1 1 d . . . . .
H46 H 0.288014 0.649973 0.676367 0.022 Uiso 1 1 calc R . . . .
C47 C 0.18616(15) 0.67649(12) 0.58597(9) 0.0200(3) Uani 1 1 d . . . . .
C48 C 0.13727(15) 0.63955(12) 0.51701(9) 0.0201(3) Uani 1 1 d . . . . .
H48 H 0.090102 0.676574 0.487103 0.024 Uiso 1 1 calc R . . . .
C49 C 0.15923(14) 0.54739(12) 0.49317(8) 0.0176(3) Uani 1 1 d . . . . .
C50 C 0.22627(14) 0.49194(12) 0.53745(8) 0.0166(3) Uani 1 1 d . . . . .
H50 H 0.238873 0.428526 0.519630 0.020 Uiso 1 1 calc R . . . .
C51 C 0.16801(19) 0.77772(14) 0.61250(10) 0.0290(4) Uani 1 1 d . . . . .
C52 C 0.11676(16) 0.50733(13) 0.41844(8) 0.0210(3) Uani 1 1 d . . . . .
C53 C 0.38578(14) 0.36483(11) 0.62082(7) 0.0150(3) Uani 1 1 d . . . . .
C54 C 0.28760(14) 0.29018(11) 0.59257(8) 0.0160(3) Uani 1 1 d . . . . .
H54 H 0.207913 0.301106 0.596692 0.019 Uiso 1 1 calc R . . . .
C55 C 0.30334(15) 0.20100(11) 0.55884(8) 0.0164(3) Uani 1 1 d . . . . .
C56 C 0.41866(15) 0.18165(12) 0.55230(8) 0.0179(3) Uani 1 1 d . . . . .
H56 H 0.429895 0.120740 0.529465 0.021 Uiso 1 1 calc R . . . .
C57 C 0.51674(15) 0.25395(12) 0.58012(8) 0.0182(3) Uani 1 1 d . . . . .
C58 C 0.50060(15) 0.34389(11) 0.61311(8) 0.0168(3) Uani 1 1 d . . . . .
H58 H 0.569528 0.392242 0.630838 0.020 Uiso 1 1 calc R . . . .
C59 C 0.19613(16) 0.12555(12) 0.52557(8) 0.0207(3) Uani 1 1 d . . . . .
C60 C 0.64083(17) 0.23329(13) 0.57316(11) 0.0266(4) Uani 1 1 d . . . . .
B02O B 0.36090(16) 0.46793(13) 0.66063(9) 0.0149(3) 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 2.4611(4) . ?
W C24 2.0189(18) . ?
W C25 2.0411(18) . ?
W C26 2.0532(17) . ?
W C27 2.0571(18) . ?
W C28 2.0499(17) . ?
P H 1.29(2) . ?
P N1 1.7773(14) . ?
P C5 1.9239(16) . ?
O1 C24 1.141(2) . ?
O2 C25 1.142(2) . ?
O3 C26 1.135(2) . ?
O4 C27 1.136(2) . ?
O5 C28 1.135(2) . ?
N1 C1 1.341(2) . ?
N1 C3 1.390(2) . ?
N2 C1 1.326(2) . ?
N2 C2 1.380(2) . ?
N2 C4 1.469(2) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.350(2) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.540(2) . ?
C5 C12 1.535(2) . ?
C5 C18 1.539(2) . ?
C6 C7 1.404(2) . ?
C6 C11 1.396(2) . ?
C7 H7 0.9500 . ?
C7 C8 1.388(2) . ?
C8 H8 0.9500 . ?
C8 C9 1.391(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(3) . ?
C10 H10 0.9500 . ?
C10 C11 1.394(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.395(2) . ?
C12 C17 1.400(2) . ?
C13 H13 0.9500 . ?
C13 C14 1.398(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.383(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.393(2) . ?
C17 H17 0.9500 . ?
C18 C19 1.399(2) . ?
C18 C23 1.396(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.391(2) . ?
C20 H20 0.9500 . ?
C20 C21 1.391(2) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.394(2) . ?
C23 H23 0.9500 . ?
Cl1 C61 1.756(2) . ?
Cl2 C61 1.811(3) . ?
Cl2S C61 1.649(4) . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C61 H61C 0.9900 . ?
C61 H61D 0.9900 . ?
F1 C35 1.3557(19) . ?
F2 C35 1.3333(19) . ?
F3 C35 1.346(2) . ?
F4 C36 1.3515(18) . ?
F5 C36 1.3365(19) . ?
F6 C36 1.3429(19) . ?
F7 C43 1.336(2) . ?
F8 C43 1.342(2) . ?
F9 C43 1.337(2) . ?
F10 C44 1.336(2) . ?
F11 C44 1.346(2) . ?
F12 C44 1.331(2) . ?
F13 C51 1.350(3) . ?
F13S C51 1.262(11) . ?
F14 C51 1.322(3) . ?
F14S C51 1.407(12) . ?
F15 C51 1.305(3) . ?
F15S C51 1.402(12) . ?
F16 C52 1.344(2) . ?
F17 C52 1.347(2) . ?
F18 C52 1.336(2) . ?
F19 C59 1.344(2) . ?
F20 C59 1.340(2) . ?
F21 C59 1.337(2) . ?
F22 C60 1.333(4) . ?
F22S C60 1.336(7) . ?
F23 C60 1.386(3) . ?
F23S C60 1.305(5) . ?
F24 C60 1.306(4) . ?
F24S C60 1.402(7) . ?
C29 C30 1.406(2) . ?
C29 C34 1.397(2) . ?
C29 B02O 1.646(2) . ?
C30 H30 0.9500 . ?
C30 C31 1.391(2) . ?
C31 C32 1.389(2) . ?
C31 C35 1.496(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.388(2) . ?
C33 C34 1.395(2) . ?
C33 C36 1.495(2) . ?
C34 H34 0.9500 . ?
C37 C38 1.406(2) . ?
C37 C42 1.404(2) . ?
C37 B02O 1.649(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.391(2) . ?
C39 C40 1.391(2) . ?
C39 C43 1.502(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.390(2) . ?
C41 C42 1.391(2) . ?
C41 C44 1.501(2) . ?
C42 H42 0.9500 . ?
C45 C46 1.409(2) . ?
C45 C50 1.399(2) . ?
C45 B02O 1.639(2) . ?
C46 H46 0.9500 . ?
C46 C47 1.387(2) . ?
C47 C48 1.390(2) . ?
C47 C51 1.499(2) . ?
C48 H48 0.9500 . ?
C48 C49 1.383(2) . ?
C49 C50 1.399(2) . ?
C49 C52 1.498(2) . ?
C50 H50 0.9500 . ?
C53 C54 1.408(2) . ?
C53 C58 1.398(2) . ?
C53 B02O 1.641(2) . ?
C54 H54 0.9500 . ?
C54 C55 1.391(2) . ?
C55 C56 1.391(2) . ?
C55 C59 1.493(2) . ?
C56 H56 0.9500 . ?
C56 C57 1.386(2) . ?
C57 C58 1.395(2) . ?
C57 C60 1.495(2) . ?
C58 H58 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C24 W P 175.92(5) . . ?
C24 W C25 89.46(7) . . ?
C24 W C26 87.50(7) . . ?
C24 W C27 91.99(7) . . ?
C24 W C28 88.56(7) . . ?
C25 W P 90.50(5) . . ?
C25 W C26 93.23(6) . . ?
C25 W C27 177.82(7) . . ?
C25 W C28 92.00(7) . . ?
C26 W P 88.43(5) . . ?
C26 W C27 88.46(7) . . ?
C27 W P 88.17(5) . . ?
C28 W P 95.52(5) . . ?
C28 W C26 173.42(7) . . ?
C28 W C27 86.41(7) . . ?
W P H 114.0(9) . . ?
N1 P W 113.30(5) . . ?
N1 P H 92.1(9) . . ?
N1 P C5 102.46(7) . . ?
C5 P W 130.29(5) . . ?
C5 P H 97.3(9) . . ?
C1 N1 P 127.59(11) . . ?
C1 N1 C3 107.73(13) . . ?
C3 N1 P 124.68(11) . . ?
C1 N2 C2 108.85(14) . . ?
C1 N2 C4 125.66(15) . . ?
C2 N2 C4 125.49(14) . . ?
N1 C1 H1 125.5 . . ?
N2 C1 N1 108.94(14) . . ?
N2 C1 H1 125.5 . . ?
N2 C2 H2 126.4 . . ?
C3 C2 N2 107.12(14) . . ?
C3 C2 H2 126.4 . . ?
N1 C3 H3 126.3 . . ?
C2 C3 N1 107.35(15) . . ?
C2 C3 H3 126.3 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P 106.51(10) . . ?
C12 C5 P 110.44(10) . . ?
C12 C5 C6 112.87(13) . . ?
C12 C5 C18 111.16(12) . . ?
C18 C5 P 102.01(10) . . ?
C18 C5 C6 113.18(12) . . ?
C7 C6 C5 120.60(14) . . ?
C11 C6 C5 121.70(14) . . ?
C11 C6 C7 117.68(14) . . ?
C6 C7 H7 119.4 . . ?
C8 C7 C6 121.27(16) . . ?
C8 C7 H7 119.4 . . ?
C7 C8 H8 119.9 . . ?
C7 C8 C9 120.18(16) . . ?
C9 C8 H8 119.9 . . ?
C8 C9 H9 120.3 . . ?
C10 C9 C8 119.30(16) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 119.8 . . ?
C9 C10 C11 120.46(16) . . ?
C11 C10 H10 119.8 . . ?
C6 C11 H11 119.5 . . ?
C10 C11 C6 121.00(16) . . ?
C10 C11 H11 119.5 . . ?
C13 C12 C5 121.53(14) . . ?
C13 C12 C17 118.24(15) . . ?
C17 C12 C5 120.05(15) . . ?
C12 C13 H13 119.8 . . ?
C12 C13 C14 120.48(16) . . ?
C14 C13 H13 119.8 . . ?
C13 C14 H14 119.7 . . ?
C15 C14 C13 120.57(17) . . ?
C15 C14 H14 119.7 . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.58(17) . . ?
C16 C15 H15 120.2 . . ?
C15 C16 H16 119.9 . . ?
C15 C16 C17 120.13(17) . . ?
C17 C16 H16 119.9 . . ?
C12 C17 H17 119.5 . . ?
C16 C17 C12 120.95(17) . . ?
C16 C17 H17 119.5 . . ?
C19 C18 C5 120.23(13) . . ?
C23 C18 C5 121.60(14) . . ?
C23 C18 C19 118.15(15) . . ?
C18 C19 H19 119.3 . . ?
C20 C19 C18 121.32(15) . . ?
C20 C19 H19 119.3 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 C19 119.74(16) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 120.2 . . ?
C22 C21 C20 119.59(16) . . ?
C22 C21 H21 120.2 . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.71(16) . . ?
C23 C22 H22 119.6 . . ?
C18 C23 H23 119.8 . . ?
C22 C23 C18 120.47(16) . . ?
C22 C23 H23 119.8 . . ?
O1 C24 W 178.51(17) . . ?
O2 C25 W 178.37(15) . . ?
O3 C26 W 176.56(16) . . ?
O4 C27 W 178.25(16) . . ?
O5 C28 W 175.77(16) . . ?
Cl1 C61 Cl2 108.03(16) . . ?
Cl1 C61 H61A 110.1 . . ?
Cl1 C61 H61B 110.1 . . ?
Cl1 C61 H61C 107.4 . . ?
Cl1 C61 H61D 107.4 . . ?
Cl2 C61 H61A 110.1 . . ?
Cl2 C61 H61B 110.1 . . ?
Cl2S C61 Cl1 119.7(2) . . ?
Cl2S C61 H61C 107.4 . . ?
Cl2S C61 H61D 107.4 . . ?
H61A C61 H61B 108.4 . . ?
H61C C61 H61D 106.9 . . ?
C30 C29 B02O 120.51(13) . . ?
C34 C29 C30 115.53(14) . . ?
C34 C29 B02O 123.91(13) . . ?
C29 C30 H30 118.9 . . ?
C31 C30 C29 122.30(14) . . ?
C31 C30 H30 118.9 . . ?
C30 C31 C35 118.70(14) . . ?
C32 C31 C30 121.20(14) . . ?
C32 C31 C35 120.04(14) . . ?
C31 C32 H32 121.3 . . ?
C33 C32 C31 117.47(14) . . ?
C33 C32 H32 121.3 . . ?
C32 C33 C34 121.23(14) . . ?
C32 C33 C36 120.78(14) . . ?
C34 C33 C36 117.99(14) . . ?
C29 C34 H34 118.9 . . ?
C33 C34 C29 122.27(14) . . ?
C33 C34 H34 118.9 . . ?
F1 C35 C31 111.67(13) . . ?
F2 C35 F1 105.88(13) . . ?
F2 C35 F3 107.22(13) . . ?
F2 C35 C31 113.47(13) . . ?
F3 C35 F1 105.18(13) . . ?
F3 C35 C31 112.83(14) . . ?
F4 C36 C33 111.94(13) . . ?
F5 C36 F4 106.30(13) . . ?
F5 C36 F6 106.78(13) . . ?
F5 C36 C33 113.31(13) . . ?
F6 C36 F4 105.35(13) . . ?
F6 C36 C33 112.59(13) . . ?
C38 C37 B02O 119.82(13) . . ?
C42 C37 C38 115.62(14) . . ?
C42 C37 B02O 124.54(14) . . ?
C37 C38 H38 118.8 . . ?
C39 C38 C37 122.34(14) . . ?
C39 C38 H38 118.8 . . ?
C38 C39 C43 120.23(14) . . ?
C40 C39 C38 121.06(15) . . ?
C40 C39 C43 118.67(14) . . ?
C39 C40 H40 121.3 . . ?
C41 C40 C39 117.50(15) . . ?
C41 C40 H40 121.3 . . ?
C40 C41 C42 121.49(15) . . ?
C40 C41 C44 117.80(15) . . ?
C42 C41 C44 120.68(15) . . ?
C37 C42 H42 119.0 . . ?
C41 C42 C37 121.97(15) . . ?
C41 C42 H42 119.0 . . ?
F7 C43 F8 106.27(15) . . ?
F7 C43 F9 106.78(15) . . ?
F7 C43 C39 112.62(14) . . ?
F8 C43 C39 111.84(15) . . ?
F9 C43 F8 106.11(14) . . ?
F9 C43 C39 112.75(14) . . ?
F10 C44 F11 106.07(15) . . ?
F10 C44 C41 112.31(15) . . ?
F11 C44 C41 111.48(15) . . ?
F12 C44 F10 107.16(15) . . ?
F12 C44 F11 106.05(16) . . ?
F12 C44 C41 113.30(15) . . ?
C46 C45 B02O 119.96(14) . . ?
C50 C45 C46 115.77(14) . . ?
C50 C45 B02O 124.13(14) . . ?
C45 C46 H46 118.9 . . ?
C47 C46 C45 122.20(15) . . ?
C47 C46 H46 118.9 . . ?
C46 C47 C48 120.92(15) . . ?
C46 C47 C51 119.93(15) . . ?
C48 C47 C51 119.12(15) . . ?
C47 C48 H48 120.9 . . ?
C49 C48 C47 118.11(15) . . ?
C49 C48 H48 120.9 . . ?
C48 C49 C50 120.99(15) . . ?
C48 C49 C52 120.11(15) . . ?
C50 C49 C52 118.82(15) . . ?
C45 C50 C49 121.98(15) . . ?
C45 C50 H50 119.0 . . ?
C49 C50 H50 119.0 . . ?
F13 C51 C47 110.90(17) . . ?
F13S C51 F14S 96.0(7) . . ?
F13S C51 F15S 113.7(7) . . ?
F13S C51 C47 121.4(5) . . ?
F14 C51 F13 103.25(17) . . ?
F14 C51 C47 112.85(16) . . ?
F14S C51 C47 111.9(5) . . ?
F15 C51 F13 107.7(2) . . ?
F15 C51 F14 108.6(2) . . ?
F15 C51 C47 113.04(17) . . ?
F15S C51 F14S 95.5(7) . . ?
F15S C51 C47 113.4(5) . . ?
F16 C52 F17 106.06(13) . . ?
F16 C52 C49 112.54(14) . . ?
F17 C52 C49 112.04(14) . . ?
F18 C52 F16 107.09(14) . . ?
F18 C52 F17 105.65(14) . . ?
F18 C52 C49 112.94(13) . . ?
C54 C53 B02O 119.65(13) . . ?
C58 C53 C54 115.96(14) . . ?
C58 C53 B02O 124.39(14) . . ?
C53 C54 H54 118.9 . . ?
C55 C54 C53 122.22(14) . . ?
C55 C54 H54 118.9 . . ?
C54 C55 C59 120.97(15) . . ?
C56 C55 C54 120.74(15) . . ?
C56 C55 C59 118.21(14) . . ?
C55 C56 H56 121.0 . . ?
C57 C56 C55 117.97(15) . . ?
C57 C56 H56 121.0 . . ?
C56 C57 C58 121.28(15) . . ?
C56 C57 C60 118.06(15) . . ?
C58 C57 C60 120.66(15) . . ?
C53 C58 H58 119.1 . . ?
C57 C58 C53 121.82(15) . . ?
C57 C58 H58 119.1 . . ?
F19 C59 C55 113.10(14) . . ?
F20 C59 F19 105.89(14) . . ?
F20 C59 C55 111.88(14) . . ?
F21 C59 F19 106.44(14) . . ?
F21 C59 F20 105.95(14) . . ?
F21 C59 C55 113.02(14) . . ?
F22 C60 F23 106.4(2) . . ?
F22 C60 C57 113.8(2) . . ?
F22S C60 F24S 107.1(4) . . ?
F22S C60 C57 109.5(3) . . ?
F23 C60 C57 111.27(17) . . ?
F23S C60 F22S 104.7(3) . . ?
F23S C60 F24S 110.5(4) . . ?
F23S C60 C57 113.8(2) . . ?
F24 C60 F22 104.9(2) . . ?
F24 C60 F23 104.4(2) . . ?
F24 C60 C57 115.3(2) . . ?
F24S C60 C57 110.8(3) . . ?
C29 B02O C37 109.71(12) . . ?
C45 B02O C29 107.09(12) . . ?
C45 B02O C37 112.21(13) . . ?
C45 B02O C53 110.96(12) . . ?
C53 B02O C29 109.59(12) . . ?
C53 B02O C37 107.28(12) . . ?

_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_11a
_database_code_depnum_ccdc_archive 'CCDC 2302949'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2023-10-23 deposited with the CCDC.	2024-01-05 downloaded from the CCDC.
;
_audit_creation_date             2022-11-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        DB-571-2
_chemical_formula_moiety         'C28 H22 N2 O5 P W, C F3 O3 S, 0.25(C5 H12)'
_chemical_formula_sum            'C30.25 H25 F3 N2 O8 P S W'
_chemical_formula_weight         848.40
_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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   54.221(3)
_cell_length_b                   8.9542(5)
_cell_length_c                   32.5364(19)
_cell_angle_alpha                90
_cell_angle_beta                 125.097(2)
_cell_angle_gamma                90
_cell_volume                     12924.5(13)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    9218
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.279
_cell_measurement_theta_min      2.538
_shelx_estimated_absorpt_T_max   0.806
_shelx_estimated_absorpt_T_min   0.466
_exptl_absorpt_coefficient_mu    3.758
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1062 before and 0.0628 after correction.
The Ratio of minimum to maximum transmission is 0.7830.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             6664
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0551
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       74
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            145150
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.250
_diffrn_reflns_theta_min         1.836
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                15648
_reflns_number_total             17600
_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       'SAINT V8.40B (?, 2016)'
_computing_data_collection       ?
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         2.908
_refine_diff_density_min         -1.676
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         17600
_refine_ls_number_restraints     942
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0452
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0411P)²+184.8187P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1104
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C29T-F1T = C29T-F3T = C29T-F2T
 1.33 with sigma of 0.02
 C29T-ST
 1.82 with sigma of 0.02
 ST-O6T = ST-O7T = ST-O8T
 1.44 with sigma of 0.02
 C29S-F3S = C29S-F2S = C29S-F1S
 1.33 with sigma of 0.02
 C29S-SS
 1.82 with sigma of 0.02
 SS-O7S = SS-O8S = SS-O6S
 1.44 with sigma of 0.02
 H-P
 1.5 with sigma of 0.02
 H'-P'
 1.5 with sigma of 0.02
 C34-C33 = C33-C32 = C32-C31 = C31-C30
 1.52 with sigma of 0.001
 C34-C32 = C33-C31 = C32-C30
 2.54 with sigma of 0.001
 C29T-O7T
 2.56 with sigma of 0.04
 C29T-O6T
 2.58 with sigma of 0.04
 C29T-O8T
 2.57 with sigma of 0.04
 C29S-O7S
 2.58 with sigma of 0.04
 C29S-O8S
 2.56 with sigma of 0.04
 C29S-O6S
 2.57 with sigma of 0.04
 F1T-F2T \\sim F2T-F3T \\sim F3T-F1T
 with sigma of 0.001
 O6S-O7S \\sim O7S-O8S \\sim O8S-O6S
 with sigma of 0.001
3. Rigid bond restraints
 P', N1'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(N1') \\sim Ueq, Uanis(C3') \\sim Ueq, Uanis(C2') \\sim Ueq, Uanis(N2')
\\sim Ueq, Uanis(C1') \\sim Ueq, Uanis(C4') \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C23') \\sim Ueq, Uanis(C21') \\sim Ueq, Uanis(C22') \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2T) \\sim Ueq, Uanis(C29T) \\sim Ueq, Uanis(F3T) \\sim Ueq, Uanis(F1T)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: SS(0.5) F1S(0.5) F2S(0.5) F3S(0.5) O6S(0.5) O7S(0.5) O8S(0.5)
 C29S(0.5) ST(0.5) F1T(0.5) F2T(0.5) F3T(0.5) O6T(0.5) O7T(0.5) O8T(0.5)
 C29T(0.5) C30(0.5) H30A(0.5) H30B(0.5) H30C(0.5) C31(0.5) H31A(0.5) H31B(0.5)
 C32(0.5) H32A(0.5) H32B(0.5) C33(0.5) H33A(0.5) H33B(0.5) C34(0.5) H34A(0.5)
 H34B(0.5) H34C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B)
7.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C1'(H1'), C2'(H2'), C3'(H3'), C7'(H7'), C8'(H8'), C9'(H9'),
 C10'(H10'), C11'(H11'), C13'(H13'), C14'(H14'), C15'(H15'), C16'(H16'),
 C17'(H17'), C19'(H19'), C20'(H20'), C21'(H21'), C22'(H22'), C23'(H23')
7.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C4'(H4'A,H4'B,H4'C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C)
;
_atom_sites_solution_hydrogens   mixed
_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
W W 0.55186(2) 0.67030(2) 0.53310(2) 0.02030(5) Uani 1 1 d . U . . .
P P 0.57748(3) 0.75018(13) 0.49351(5) 0.0224(2) Uani 1 1 d D U . . .
H H 0.5956(12) 0.887(4) 0.518(2) 0.039(17) Uiso 1 1 d D . . . .
O1 O 0.52520(8) 0.5934(4) 0.59524(14) 0.0297(7) Uani 1 1 d . U . . .
O2 O 0.55696(10) 1.0109(4) 0.56559(17) 0.0426(10) Uani 1 1 d . U . . .
O3 O 0.48419(8) 0.7303(4) 0.43917(13) 0.0275(7) Uani 1 1 d . U . . .
O4 O 0.54686(9) 0.3274(4) 0.50330(15) 0.0327(8) Uani 1 1 d . U . . .
O5 O 0.61743(9) 0.5943(6) 0.62961(15) 0.0444(10) Uani 1 1 d . U . . .
N1 N 0.60969(9) 0.6379(4) 0.51450(15) 0.0241(7) Uani 1 1 d . U . . .
N2 N 0.65584(10) 0.5619(5) 0.56335(17) 0.0307(8) Uani 1 1 d . U . . .
C1 C 0.63816(11) 0.6807(6) 0.54778(18) 0.0263(8) Uani 1 1 d . U . . .
H1 H 0.644674 0.780468 0.558541 0.032 Uiso 1 1 calc R . . . .
C2 C 0.63833(12) 0.4366(6) 0.5391(2) 0.0310(9) Uani 1 1 d . U . . .
H2 H 0.645348 0.336924 0.542927 0.037 Uiso 1 1 calc R . . . .
C3 C 0.60951(11) 0.4829(5) 0.5091(2) 0.0284(9) Uani 1 1 d . U . . .
H3 H 0.592307 0.421770 0.488267 0.034 Uiso 1 1 calc R . . . .
C4 C 0.68859(13) 0.5625(8) 0.5992(2) 0.0444(14) Uani 1 1 d . U . . .
H4A H 0.694777 0.478647 0.622529 0.067 Uiso 1 1 calc GR . . . .
H4B H 0.695003 0.656535 0.618005 0.067 Uiso 1 1 calc GR . . . .
H4C H 0.697977 0.552649 0.581037 0.067 Uiso 1 1 calc GR . . . .
C5 C 0.56003(10) 0.7774(5) 0.42418(18) 0.0224(6) Uani 1 1 d . U . . .
C6 C 0.53016(11) 0.8594(5) 0.40400(19) 0.0236(7) Uani 1 1 d . U . . .
C7 C 0.53039(12) 0.9802(5) 0.4315(2) 0.0285(9) Uani 1 1 d . U . . .
H7 H 0.548693 1.009184 0.461921 0.034 Uiso 1 1 calc R . . . .
C8 C 0.50381(12) 1.0586(5) 0.4144(2) 0.0317(9) Uani 1 1 d . U . . .
H8 H 0.503925 1.137173 0.434103 0.038 Uiso 1 1 calc R . . . .
C9 C 0.47757(12) 1.0228(6) 0.3692(2) 0.0328(9) Uani 1 1 d . U . . .
H9 H 0.459575 1.076627 0.357510 0.039 Uiso 1 1 calc R . . . .
C10 C 0.47756(12) 0.9069(6) 0.3407(2) 0.0330(9) Uani 1 1 d . U . . .
H10 H 0.459612 0.883783 0.308929 0.040 Uiso 1 1 calc R . . . .
C11 C 0.50378(11) 0.8240(6) 0.3586(2) 0.0288(9) Uani 1 1 d . U . . .
H11 H 0.503386 0.743127 0.339309 0.035 Uiso 1 1 calc R . . . .
C12 C 0.57758(11) 0.8750(5) 0.4100(2) 0.0258(8) Uani 1 1 d . U . . .
C13 C 0.56502(13) 0.8892(6) 0.3589(2) 0.0317(9) Uani 1 1 d . U . . .
H13 H 0.546647 0.839189 0.335302 0.038 Uiso 1 1 calc R . . . .
C14 C 0.57877(14) 0.9750(6) 0.3416(2) 0.0356(10) Uani 1 1 d . U . . .
H14 H 0.569839 0.982976 0.306621 0.043 Uiso 1 1 calc R . . . .
C15 C 0.60570(13) 1.0491(6) 0.3760(2) 0.0363(10) Uani 1 1 d . U . . .
H15 H 0.615438 1.106756 0.364727 0.044 Uiso 1 1 calc R . . . .
C16 C 0.61804(12) 1.0376(6) 0.4267(2) 0.0365(10) Uani 1 1 d . U . . .
H16 H 0.636219 1.089080 0.450233 0.044 Uiso 1 1 calc R . . . .
C17 C 0.60417(11) 0.9509(5) 0.4441(2) 0.0318(9) Uani 1 1 d . U . . .
H17 H 0.612959 0.944264 0.479035 0.038 Uiso 1 1 calc R . . . .
C18 C 0.55637(10) 0.6173(5) 0.40439(17) 0.0219(7) Uani 1 1 d . U . . .
C19 C 0.53476(10) 0.5214(5) 0.40038(17) 0.0228(8) Uani 1 1 d . U . . .
H19 H 0.520741 0.558190 0.406559 0.027 Uiso 1 1 calc R . . . .
C20 C 0.53364(12) 0.3719(5) 0.38736(19) 0.0274(9) Uani 1 1 d . U . . .
H20 H 0.518664 0.308258 0.384340 0.033 Uiso 1 1 calc R . . . .
C21 C 0.55412(13) 0.3147(6) 0.3787(2) 0.0311(9) Uani 1 1 d . U . . .
H21 H 0.553431 0.212399 0.370359 0.037 Uiso 1 1 calc R . . . .
C22 C 0.57565(12) 0.4099(5) 0.3826(2) 0.0307(10) Uani 1 1 d . U . . .
H22 H 0.589578 0.372597 0.376263 0.037 Uiso 1 1 calc R . . . .
C23 C 0.57696(11) 0.5593(5) 0.39556(19) 0.0266(9) Uani 1 1 d . U . . .
H23 H 0.591950 0.622614 0.398475 0.032 Uiso 1 1 calc R . . . .
C24 C 0.53502(10) 0.6207(5) 0.57293(17) 0.0239(8) Uani 1 1 d . U . . .
C25 C 0.55533(11) 0.8890(6) 0.5546(2) 0.0290(9) Uani 1 1 d . U . . .
C26 C 0.50866(10) 0.7109(5) 0.47187(17) 0.0219(7) Uani 1 1 d . U . . .
C27 C 0.54840(10) 0.4510(5) 0.51285(17) 0.0230(8) Uani 1 1 d . U . . .
C28 C 0.59390(11) 0.6247(6) 0.59539(19) 0.0293(9) Uani 1 1 d . U . . .
W' W 0.32592(2) 0.65446(2) 0.09662(2) 0.02030(5) Uani 1 1 d . U . . .
P' P 0.31983(3) 0.58147(14) 0.16430(5) 0.0280(3) Uani 1 1 d D U . . .
H' H 0.3362(14) 0.439(5) 0.187(2) 0.06(2) Uiso 1 1 d D . . . .
O1' O 0.33866(12) 0.7199(6) 0.01546(18) 0.0526(12) Uani 1 1 d . U . . .
O2' O 0.34242(10) 0.3162(5) 0.0937(2) 0.0580(14) Uani 1 1 d . U . . .
O3' O 0.25893(8) 0.5879(4) 0.00288(12) 0.0260(6) Uani 1 1 d . U . . .
O4' O 0.31188(9) 1.0017(4) 0.09465(14) 0.0313(7) Uani 1 1 d . U . . .
O5' O 0.39404(10) 0.7153(6) 0.18804(19) 0.0575(13) Uani 1 1 d . U . . .
N1' N 0.34247(12) 0.6953(6) 0.21832(19) 0.0400(8) Uani 1 1 d . U . . .
N2' N 0.38217(15) 0.7697(8) 0.2881(3) 0.0603(11) Uani 1 1 d . U . . .
C1' C 0.36830(16) 0.6431(8) 0.2613(3) 0.0502(10) Uani 1 1 d . U . . .
H1' H 0.374940 0.542656 0.270201 0.060 Uiso 1 1 calc R . . . .
C2' C 0.36738(19) 0.8893(10) 0.2647(3) 0.0623(12) Uani 1 1 d . U . . .
H2' H 0.373836 0.987991 0.277031 0.075 Uiso 1 1 calc R . . . .
C3' C 0.34082(18) 0.8537(8) 0.2193(3) 0.0545(11) Uani 1 1 d . U . . .
H3' H 0.325394 0.918562 0.194983 0.065 Uiso 1 1 calc R . . . .
C4' C 0.4124(2) 0.7504(12) 0.3390(3) 0.0742(17) Uani 1 1 d . U . . .
H4'A H 0.419382 0.647305 0.342466 0.111 Uiso 1 1 calc GR . . . .
H4'B H 0.409868 0.772592 0.365940 0.111 Uiso 1 1 calc GR . . . .
H4'C H 0.427230 0.818930 0.341390 0.111 Uiso 1 1 calc GR . . . .
C5' C 0.28363(11) 0.5619(5) 0.15970(17) 0.0255(7) Uani 1 1 d . U . . .
C6' C 0.26159(10) 0.4821(5) 0.10985(16) 0.0201(7) Uani 1 1 d . U . . .
C7' C 0.27125(12) 0.3566(5) 0.09743(17) 0.0239(8) Uani 1 1 d . U . . .
H7' H 0.291520 0.323837 0.119573 0.029 Uiso 1 1 calc R . . . .
C8' C 0.25170(14) 0.2787(6) 0.05324(18) 0.0332(10) Uani 1 1 d . U . . .
H8' H 0.258861 0.195701 0.044766 0.040 Uiso 1 1 calc R . . . .
C9' C 0.22205(15) 0.3212(7) 0.0217(2) 0.0417(11) Uani 1 1 d . U . . .
H9' H 0.208615 0.267529 -0.008480 0.050 Uiso 1 1 calc R . . . .
C10' C 0.21189(13) 0.4435(7) 0.0343(2) 0.0382(10) Uani 1 1 d . U . . .
H10' H 0.191284 0.471829 0.013042 0.046 Uiso 1 1 calc R . . . .
C11' C 0.23147(11) 0.5246(6) 0.07769(18) 0.0283(8) Uani 1 1 d . U . . .
H11' H 0.224334 0.609326 0.085483 0.034 Uiso 1 1 calc R . . . .
C12' C 0.28527(13) 0.4667(5) 0.20089(17) 0.0299(9) Uani 1 1 d . U . . .
C13' C 0.25802(14) 0.4392(6) 0.1948(2) 0.0341(10) Uani 1 1 d . U . . .
H13' H 0.240037 0.482742 0.167227 0.041 Uiso 1 1 calc R . . . .
C14' C 0.25660(16) 0.3496(6) 0.2282(2) 0.0399(11) Uani 1 1 d . U . . .
H14' H 0.237727 0.330700 0.222885 0.048 Uiso 1 1 calc R . . . .
C15' C 0.28244(16) 0.2884(7) 0.2688(2) 0.0454(12) Uani 1 1 d . U . . .
H15' H 0.281570 0.228847 0.292129 0.054 Uiso 1 1 calc R . . . .
C16' C 0.30928(18) 0.3131(9) 0.2756(2) 0.0625(19) Uani 1 1 d . U . . .
H16' H 0.327163 0.269887 0.303568 0.075 Uiso 1 1 calc R . . . .
C17' C 0.31074(15) 0.4033(9) 0.2412(2) 0.0570(18) Uani 1 1 d . U . . .
H17' H 0.329602 0.419612 0.246155 0.068 Uiso 1 1 calc R . . . .
C18' C 0.27481(13) 0.7245(5) 0.1606(2) 0.0337(9) Uani 1 1 d . U . . .
C19' C 0.26518(12) 0.8169(5) 0.1195(2) 0.0304(9) Uani 1 1 d . U . . .
H19' H 0.262328 0.776312 0.090055 0.036 Uiso 1 1 calc R . . . .
C20' C 0.25970(15) 0.9677(6) 0.1210(3) 0.0396(11) Uani 1 1 d . U . . .
H20' H 0.252955 1.029099 0.092629 0.048 Uiso 1 1 calc R . . . .
C21' C 0.26400(15) 1.0284(8) 0.1636(3) 0.0476(11) Uani 1 1 d . U . . .
H21' H 0.261244 1.132549 0.164990 0.057 Uiso 1 1 calc R . . . .
C22' C 0.27206(16) 0.9416(8) 0.2030(3) 0.0495(11) Uani 1 1 d . U . . .
H22' H 0.273944 0.983231 0.231534 0.059 Uiso 1 1 calc R . . . .
C23' C 0.27773(15) 0.7885(7) 0.2021(2) 0.0442(10) Uani 1 1 d . U . . .
H23' H 0.283663 0.727939 0.230324 0.053 Uiso 1 1 calc R . . . .
C24' C 0.33459(12) 0.6978(6) 0.0457(2) 0.0335(10) Uani 1 1 d . U . . .
C25' C 0.33645(11) 0.4361(6) 0.0958(2) 0.0349(10) Uani 1 1 d . U . . .
C26' C 0.28246(10) 0.6121(5) 0.03767(16) 0.0188(7) Uani 1 1 d . U . . .
C27' C 0.31645(10) 0.8782(5) 0.09600(17) 0.0223(8) Uani 1 1 d . U . . .
C28' C 0.36986(12) 0.6945(6) 0.1551(2) 0.0353(10) Uani 1 1 d . U . . .
S S 0.33161(3) 0.93279(16) 0.39265(5) 0.0376(3) Uani 1 1 d . U . . .
F1 F 0.3311(2) 0.8998(10) 0.3137(2) 0.136(2) Uani 1 1 d . U . . .
F2 F 0.36895(14) 1.0242(7) 0.3729(3) 0.0950(16) Uani 1 1 d . U . . .
F3 F 0.36760(18) 0.7862(8) 0.3799(3) 0.118(2) Uani 1 1 d . U . . .
O6 O 0.31583(11) 1.0731(5) 0.3730(2) 0.0608(13) Uani 1 1 d . U . . .
O7 O 0.31383(11) 0.8007(6) 0.3791(2) 0.0663(15) Uani 1 1 d . U . . .
O8 O 0.35599(13) 0.9401(6) 0.44482(17) 0.0586(12) Uani 1 1 d . U . . .
C29 C 0.3506(2) 0.9075(11) 0.3634(3) 0.0730(15) Uani 1 1 d . U . . .
SS S 0.40238(7) 0.2472(4) 0.25462(12) 0.0406(6) Uani 0.5 1 d D U P A 2
F1S F 0.45795(17) 0.3142(8) 0.3006(3) 0.0467(15) Uani 0.5 1 d D U P A 2
F2S F 0.4336(2) 0.3422(11) 0.2222(3) 0.065(2) Uani 0.5 1 d D U P A 2
F3S F 0.4291(2) 0.5000(9) 0.2683(4) 0.066(2) Uani 0.5 1 d D U P A 2
O6S O 0.41188(18) 0.0993(9) 0.2527(3) 0.053(2) Uani 0.5 1 d D U P A 2
O7S O 0.4038(3) 0.2880(15) 0.2973(3) 0.044(3) Uani 0.5 1 d D U P A 2
O8S O 0.3764(2) 0.3006(11) 0.2067(3) 0.066(3) Uani 0.5 1 d D U P A 2
C29S C 0.4327(2) 0.3562(12) 0.2618(4) 0.0437(15) Uani 0.5 1 d D U P A 2
ST S 0.60075(11) 0.7121(4) 0.71401(12) 0.0276(6) Uani 0.5 1 d D U P B 1
F1T F 0.59794(17) 0.6652(8) 0.7909(3) 0.0579(15) Uani 0.5 1 d D U P B 1
F2T F 0.55837(16) 0.7732(9) 0.7281(3) 0.0672(16) Uani 0.5 1 d D U P B 1
F3T F 0.59989(18) 0.8973(8) 0.7746(3) 0.0648(17) Uani 0.5 1 d D U P B 1
O6T O 0.5867(2) 0.5698(9) 0.6925(3) 0.0469(18) Uani 0.5 1 d D U P B 1
O7T O 0.63237(16) 0.7079(9) 0.7503(3) 0.0371(15) Uani 0.5 1 d D U P B 1
O8T O 0.58934(15) 0.8342(7) 0.6788(3) 0.0280(13) Uani 0.5 1 d D U P B 1
C29T C 0.5875(3) 0.7636(13) 0.7536(4) 0.0516(13) Uani 0.5 1 d D U P B 1
C30 C 0.5375(2) 0.5711(19) 0.2490(5) 0.068(2) Uani 0.5 1 d D U P C -1
H30A H 0.547279 0.482202 0.269740 0.101 Uiso 0.5 1 calc GR . P C -1
H30B H 0.552752 0.646574 0.257172 0.101 Uiso 0.5 1 calc GR . P C -1
H30C H 0.526554 0.544119 0.213408 0.101 Uiso 0.5 1 calc GR . P C -1
C31 C 0.5155(2) 0.6339(12) 0.2592(5) 0.068(2) Uani 0.5 1 d D U P C -1
H31A H 0.505644 0.723572 0.238051 0.082 Uiso 0.5 1 calc R . P C -1
H31B H 0.526816 0.665697 0.294781 0.082 Uiso 0.5 1 calc R . P C -1
C32 C 0.4912(2) 0.5234(10) 0.2489(5) 0.072(2) Uani 0.5 1 d D U P C -1
H32A H 0.500065 0.450917 0.276904 0.086 Uiso 0.5 1 calc R . P C -1
H32B H 0.484470 0.467059 0.217871 0.086 Uiso 0.5 1 calc R . P C -1
C33 C 0.4640(2) 0.5971(15) 0.2427(5) 0.074(2) Uani 0.5 1 d D U P C -1
H33A H 0.448204 0.611451 0.206488 0.089 Uiso 0.5 1 calc R . P C -1
H33B H 0.469987 0.696954 0.258663 0.089 Uiso 0.5 1 calc R . P C -1
C34 C 0.4510(3) 0.5073(19) 0.2657(5) 0.079(2) Uani 0.5 1 d D U P C -1
H34A H 0.430297 0.477624 0.239228 0.118 Uiso 0.5 1 calc GR . P C -1
H34B H 0.450988 0.568504 0.290641 0.118 Uiso 0.5 1 calc GR . P C -1
H34C H 0.463305 0.417891 0.281970 0.118 Uiso 0.5 1 calc GR . P C -1


_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 2.4815(12) . ?
W C24 2.018(5) . ?
W C25 2.051(5) . ?
W C26 2.055(5) . ?
W C27 2.046(5) . ?
W C28 2.039(5) . ?
P H 1.48(2) . ?
P N1 1.776(4) . ?
P C5 1.894(5) . ?
O1 C24 1.147(6) . ?
O2 C25 1.136(6) . ?
O3 C26 1.140(6) . ?
O4 C27 1.140(6) . ?
O5 C28 1.143(6) . ?
N1 C1 1.334(6) . ?
N1 C3 1.398(6) . ?
N2 C1 1.322(6) . ?
N2 C2 1.386(7) . ?
N2 C4 1.460(7) . ?
C1 H1 0.9500 . ?
C2 H2 0.9500 . ?
C2 C3 1.346(7) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.540(6) . ?
C5 C12 1.545(6) . ?
C5 C18 1.537(6) . ?
C6 C7 1.399(7) . ?
C6 C11 1.378(7) . ?
C7 H7 0.9500 . ?
C7 C8 1.399(7) . ?
C8 H8 0.9500 . ?
C8 C9 1.371(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.391(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.400(7) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(7) . ?
C12 C17 1.390(7) . ?
C13 H13 0.9500 . ?
C13 C14 1.395(7) . ?
C14 H14 0.9500 . ?
C14 C15 1.395(8) . ?
C15 H15 0.9500 . ?
C15 C16 1.382(9) . ?
C16 H16 0.9500 . ?
C16 C17 1.405(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.397(6) . ?
C18 C23 1.402(6) . ?
C19 H19 0.9500 . ?
C19 C20 1.394(6) . ?
C20 H20 0.9500 . ?
C20 C21 1.390(7) . ?
C21 H21 0.9500 . ?
C21 C22 1.392(7) . ?
C22 H22 0.9500 . ?
C22 C23 1.393(6) . ?
C23 H23 0.9500 . ?
W' P' 2.4947(13) . ?
W' C24' 2.002(5) . ?
W' C25' 2.041(5) . ?
W' C26' 2.044(4) . ?
W' C27' 2.065(5) . ?
W' C28' 2.052(5) . ?
P' H' 1.48(2) . ?
P' N1' 1.776(5) . ?
P' C5' 1.889(5) . ?
O1' C24' 1.144(6) . ?
O2' C25' 1.135(7) . ?
O3' C26' 1.138(5) . ?
O4' C27' 1.129(6) . ?
O5' C28' 1.135(7) . ?
N1' C1' 1.372(9) . ?
N1' C3' 1.423(9) . ?
N2' C1' 1.363(10) . ?
N2' C2' 1.291(11) . ?
N2' C4' 1.529(11) . ?
C1' H1' 0.9500 . ?
C2' H2' 0.9500 . ?
C2' C3' 1.382(11) . ?
C3' H3' 0.9500 . ?
C4' H4'A 0.9800 . ?
C4' H4'B 0.9800 . ?
C4' H4'C 0.9800 . ?
C5' C6' 1.530(6) . ?
C5' C12' 1.547(6) . ?
C5' C18' 1.538(7) . ?
C6' C7' 1.394(6) . ?
C6' C11' 1.394(7) . ?
C7' H7' 0.9500 . ?
C7' C8' 1.387(6) . ?
C8' H8' 0.9500 . ?
C8' C9' 1.373(9) . ?
C9' H9' 0.9500 . ?
C9' C10' 1.391(9) . ?
C10' H10' 0.9500 . ?
C10' C11' 1.386(7) . ?
C11' H11' 0.9500 . ?
C12' C13' 1.395(8) . ?
C12' C17' 1.366(8) . ?
C13' H13' 0.9500 . ?
C13' C14' 1.386(7) . ?
C14' H14' 0.9500 . ?
C14' C15' 1.372(9) . ?
C15' H15' 0.9500 . ?
C15' C16' 1.359(10) . ?
C16' H16' 0.9500 . ?
C16' C17' 1.420(8) . ?
C17' H17' 0.9500 . ?
C18' C19' 1.394(7) . ?
C18' C23' 1.388(8) . ?
C19' H19' 0.9500 . ?
C19' C20' 1.389(7) . ?
C20' H20' 0.9500 . ?
C20' C21' 1.376(9) . ?
C21' H21' 0.9500 . ?
C21' C22' 1.340(10) . ?
C22' H22' 0.9500 . ?
C22' C23' 1.409(9) . ?
C23' H23' 0.9500 . ?
S O6 1.446(5) . ?
S O7 1.426(5) . ?
S O8 1.433(5) . ?
S C29 1.775(8) . ?
F1 C29 1.330(11) . ?
F2 C29 1.349(11) . ?
F3 C29 1.322(11) . ?
SS O6S 1.435(8) . ?
SS O7S 1.394(9) . ?
SS O8S 1.455(8) . ?
SS C29S 1.806(11) . ?
F1S C29S 1.275(12) . ?
F2S C29S 1.326(11) . ?
F3S C29S 1.337(12) . ?
ST O6T 1.442(9) . ?
ST O7T 1.417(8) . ?
ST O8T 1.441(7) . ?
ST C29T 1.859(12) . ?
F1T C29T 1.334(12) . ?
F2T C29T 1.297(13) . ?
F3T C29T 1.350(13) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C30 C31 1.5191(10) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.5200(10) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.5204(10) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.5201(10) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 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
C24 W P 172.72(14) . . ?
C24 W C25 88.8(2) . . ?
C24 W C26 88.69(18) . . ?
C24 W C27 90.23(18) . . ?
C24 W C28 88.73(19) . . ?
C25 W P 86.12(14) . . ?
C25 W C26 89.52(19) . . ?
C26 W P 96.43(13) . . ?
C27 W P 94.85(13) . . ?
C27 W C25 178.9(2) . . ?
C27 W C26 90.87(18) . . ?
C28 W P 86.22(15) . . ?
C28 W C25 91.2(2) . . ?
C28 W C26 177.29(19) . . ?
C28 W C27 88.3(2) . . ?
W P H 111(2) . . ?
N1 P W 110.94(14) . . ?
N1 P H 93(2) . . ?
N1 P C5 103.78(19) . . ?
C5 P W 127.57(15) . . ?
C5 P H 105(2) . . ?
C1 N1 P 124.9(3) . . ?
C1 N1 C3 107.9(4) . . ?
C3 N1 P 125.4(3) . . ?
C1 N2 C2 109.0(4) . . ?
C1 N2 C4 125.7(5) . . ?
C2 N2 C4 125.3(5) . . ?
N1 C1 H1 125.5 . . ?
N2 C1 N1 109.0(5) . . ?
N2 C1 H1 125.5 . . ?
N2 C2 H2 126.5 . . ?
C3 C2 N2 107.0(5) . . ?
C3 C2 H2 126.5 . . ?
N1 C3 H3 126.5 . . ?
C2 C3 N1 107.1(5) . . ?
C2 C3 H3 126.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C6 C5 P 104.6(3) . . ?
C6 C5 C12 106.3(4) . . ?
C12 C5 P 117.2(3) . . ?
C18 C5 P 103.6(3) . . ?
C18 C5 C6 114.5(4) . . ?
C18 C5 C12 110.8(4) . . ?
C7 C6 C5 118.4(4) . . ?
C11 C6 C5 122.4(4) . . ?
C11 C6 C7 119.1(4) . . ?
C6 C7 H7 119.8 . . ?
C6 C7 C8 120.3(5) . . ?
C8 C7 H7 119.8 . . ?
C7 C8 H8 119.8 . . ?
C9 C8 C7 120.4(5) . . ?
C9 C8 H8 119.8 . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.4(5) . . ?
C10 C9 H9 120.3 . . ?
C9 C10 H10 119.7 . . ?
C9 C10 C11 120.5(5) . . ?
C11 C10 H10 119.7 . . ?
C6 C11 C10 120.2(5) . . ?
C6 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C13 C12 C5 116.4(4) . . ?
C17 C12 C5 125.0(5) . . ?
C17 C12 C13 118.6(5) . . ?
C12 C13 H13 119.2 . . ?
C12 C13 C14 121.5(5) . . ?
C14 C13 H13 119.2 . . ?
C13 C14 H14 120.2 . . ?
C15 C14 C13 119.6(6) . . ?
C15 C14 H14 120.2 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.1(5) . . ?
C16 C15 H15 120.4 . . ?
C15 C16 H16 119.4 . . ?
C15 C16 C17 121.1(5) . . ?
C17 C16 H16 119.4 . . ?
C12 C17 C16 120.0(5) . . ?
C12 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C19 C18 C5 120.8(4) . . ?
C19 C18 C23 118.5(4) . . ?
C23 C18 C5 120.3(4) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 C18 120.4(4) . . ?
C20 C19 H19 119.8 . . ?
C19 C20 H20 119.5 . . ?
C21 C20 C19 121.0(5) . . ?
C21 C20 H20 119.5 . . ?
C20 C21 H21 120.6 . . ?
C20 C21 C22 118.8(5) . . ?
C22 C21 H21 120.6 . . ?
C21 C22 H22 119.7 . . ?
C21 C22 C23 120.6(5) . . ?
C23 C22 H22 119.7 . . ?
C18 C23 H23 119.7 . . ?
C22 C23 C18 120.7(5) . . ?
C22 C23 H23 119.7 . . ?
O1 C24 W 179.3(4) . . ?
O2 C25 W 178.8(7) . . ?
O3 C26 W 176.6(4) . . ?
O4 C27 W 177.5(4) . . ?
O5 C28 W 177.6(5) . . ?
C24' W' P' 173.81(17) . . ?
C24' W' C25' 88.5(2) . . ?
C24' W' C26' 87.3(2) . . ?
C24' W' C27' 88.8(2) . . ?
C24' W' C28' 91.9(2) . . ?
C25' W' P' 86.61(18) . . ?
C25' W' C26' 89.44(19) . . ?
C25' W' C27' 177.2(2) . . ?
C25' W' C28' 89.7(2) . . ?
C26' W' P' 96.50(12) . . ?
C26' W' C27' 91.40(17) . . ?
C26' W' C28' 178.8(2) . . ?
C27' W' P' 95.98(13) . . ?
C28' W' P' 84.25(17) . . ?
C28' W' C27' 89.4(2) . . ?
W' P' H' 109(3) . . ?
N1' P' W' 110.87(17) . . ?
N1' P' H' 97(3) . . ?
N1' P' C5' 103.1(2) . . ?
C5' P' W' 127.84(15) . . ?
C5' P' H' 105(3) . . ?
C1' N1' P' 122.2(5) . . ?
C1' N1' C3' 110.9(6) . . ?
C3' N1' P' 125.3(5) . . ?
C1' N2' C4' 116.9(7) . . ?
C2' N2' C1' 112.7(7) . . ?
C2' N2' C4' 130.4(8) . . ?
N1' C1' H1' 128.3 . . ?
N2' C1' N1' 103.5(6) . . ?
N2' C1' H1' 128.3 . . ?
N2' C2' H2' 124.7 . . ?
N2' C2' C3' 110.5(8) . . ?
C3' C2' H2' 124.7 . . ?
N1' C3' H3' 128.8 . . ?
C2' C3' N1' 102.4(7) . . ?
C2' C3' H3' 128.8 . . ?
N2' C4' H4'A 109.5 . . ?
N2' C4' H4'B 109.5 . . ?
N2' C4' H4'C 109.5 . . ?
H4'A C4' H4'B 109.5 . . ?
H4'A C4' H4'C 109.5 . . ?
H4'B C4' H4'C 109.5 . . ?
C6' C5' P' 105.7(3) . . ?
C6' C5' C12' 106.4(3) . . ?
C6' C5' C18' 113.6(4) . . ?
C12' C5' P' 116.3(4) . . ?
C18' C5' P' 103.4(3) . . ?
C18' C5' C12' 111.6(4) . . ?
C7' C6' C5' 119.3(4) . . ?
C11' C6' C5' 122.2(4) . . ?
C11' C6' C7' 118.4(4) . . ?
C6' C7' H7' 119.5 . . ?
C8' C7' C6' 121.0(5) . . ?
C8' C7' H7' 119.5 . . ?
C7' C8' H8' 119.9 . . ?
C9' C8' C7' 120.3(5) . . ?
C9' C8' H8' 119.9 . . ?
C8' C9' H9' 120.3 . . ?
C8' C9' C10' 119.3(5) . . ?
C10' C9' H9' 120.3 . . ?
C9' C10' H10' 119.6 . . ?
C11' C10' C9' 120.8(5) . . ?
C11' C10' H10' 119.6 . . ?
C6' C11' H11' 119.9 . . ?
C10' C11' C6' 120.2(5) . . ?
C10' C11' H11' 119.9 . . ?
C13' C12' C5' 116.5(5) . . ?
C17' C12' C5' 125.6(5) . . ?
C17' C12' C13' 117.8(5) . . ?
C12' C13' H13' 119.3 . . ?
C14' C13' C12' 121.5(6) . . ?
C14' C13' H13' 119.3 . . ?
C13' C14' H14' 120.0 . . ?
C15' C14' C13' 120.0(6) . . ?
C15' C14' H14' 120.0 . . ?
C14' C15' H15' 120.1 . . ?
C16' C15' C14' 119.8(5) . . ?
C16' C15' H15' 120.1 . . ?
C15' C16' H16' 119.8 . . ?
C15' C16' C17' 120.3(7) . . ?
C17' C16' H16' 119.8 . . ?
C12' C17' C16' 120.6(7) . . ?
C12' C17' H17' 119.7 . . ?
C16' C17' H17' 119.7 . . ?
C19' C18' C5' 119.5(5) . . ?
C23' C18' C5' 123.1(5) . . ?
C23' C18' C19' 117.3(5) . . ?
C18' C19' H19' 119.6 . . ?
C20' C19' C18' 120.7(5) . . ?
C20' C19' H19' 119.6 . . ?
C19' C20' H20' 119.8 . . ?
C21' C20' C19' 120.3(6) . . ?
C21' C20' H20' 119.8 . . ?
C20' C21' H21' 119.8 . . ?
C22' C21' C20' 120.5(7) . . ?
C22' C21' H21' 119.8 . . ?
C21' C22' H22' 120.0 . . ?
C21' C22' C23' 119.9(7) . . ?
C23' C22' H22' 120.0 . . ?
C18' C23' C22' 121.2(6) . . ?
C18' C23' H23' 119.4 . . ?
C22' C23' H23' 119.4 . . ?
O1' C24' W' 177.6(5) . . ?
O2' C25' W' 177.1(6) . . ?
O3' C26' W' 175.4(4) . . ?
O4' C27' W' 177.0(4) . . ?
O5' C28' W' 178.6(6) . . ?
O6 S C29 104.6(4) . . ?
O7 S O6 117.4(3) . . ?
O7 S O8 113.8(3) . . ?
O7 S C29 103.0(4) . . ?
O8 S O6 113.1(3) . . ?
O8 S C29 102.5(4) . . ?
F1 C29 S 110.9(8) . . ?
F1 C29 F2 106.6(8) . . ?
F2 C29 S 110.8(6) . . ?
F3 C29 S 111.8(6) . . ?
F3 C29 F1 109.4(8) . . ?
F3 C29 F2 107.1(9) . . ?
O6S SS O8S 114.0(5) . . ?
O6S SS C29S 100.5(5) . . ?
O7S SS O6S 117.9(5) . . ?
O7S SS O8S 116.6(5) . . ?
O7S SS C29S 101.8(8) . . ?
O8S SS C29S 102.0(6) . . ?
F1S C29S SS 110.4(7) . . ?
F1S C29S F2S 108.3(9) . . ?
F1S C29S F3S 107.3(10) . . ?
F2S C29S SS 111.4(8) . . ?
F2S C29S F3S 109.6(9) . . ?
F3S C29S SS 109.7(8) . . ?
O6T ST C29T 104.4(6) . . ?
O7T ST O6T 115.4(5) . . ?
O7T ST O8T 116.3(6) . . ?
O7T ST C29T 101.2(5) . . ?
O8T ST O6T 114.8(5) . . ?
O8T ST C29T 101.7(5) . . ?
F1T C29T ST 109.6(8) . . ?
F1T C29T F3T 107.4(8) . . ?
F2T C29T ST 112.7(9) . . ?
F2T C29T F1T 110.5(9) . . ?
F2T C29T F3T 109.5(9) . . ?
F3T C29T ST 107.0(8) . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
C30 C31 H31A 108.9 . . ?
C30 C31 H31B 108.9 . . ?
C30 C31 C32 113.45(11) . . ?
H31A C31 H31B 107.7 . . ?
C32 C31 H31A 108.9 . . ?
C32 C31 H31B 108.9 . . ?
C31 C32 H32A 108.9 . . ?
C31 C32 H32B 108.9 . . ?
C31 C32 C33 113.30(11) . . ?
H32A C32 H32B 107.7 . . ?
C33 C32 H32A 108.9 . . ?
C33 C32 H32B 108.9 . . ?
C32 C33 H33A 108.9 . . ?
C32 C33 H33B 108.9 . . ?
C32 C33 C34 113.32(11) . . ?
H33A C33 H33B 107.7 . . ?
C34 C33 H33A 108.9 . . ?
C34 C33 H33B 108.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
W P N1 C1 -104.3(4) . . . . ?
W P N1 C3 58.9(4) . . . . ?
W P C5 C6 43.1(3) . . . . ?
W P C5 C12 160.4(2) . . . . ?
W P C5 C18 -77.2(3) . . . . ?
P N1 C1 N2 165.9(3) . . . . ?
P N1 C3 C2 -166.5(4) . . . . ?
P C5 C6 C7 45.6(5) . . . . ?
P C5 C6 C11 -138.5(4) . . . . ?
P C5 C12 C13 177.6(3) . . . . ?
P C5 C12 C17 -4.0(6) . . . . ?
P C5 C18 C19 71.1(5) . . . . ?
P C5 C18 C23 -101.4(4) . . . . ?
N1 P C5 C6 173.8(3) . . . . ?
N1 P C5 C12 -68.8(3) . . . . ?
N1 P C5 C18 53.5(3) . . . . ?
N2 C2 C3 N1 1.3(6) . . . . ?
C1 N1 C3 C2 -1.0(6) . . . . ?
C1 N2 C2 C3 -1.1(6) . . . . ?
C2 N2 C1 N1 0.4(6) . . . . ?
C3 N1 C1 N2 0.3(5) . . . . ?
C4 N2 C1 N1 178.8(5) . . . . ?
C4 N2 C2 C3 -179.5(5) . . . . ?
C5 P N1 C1 115.7(4) . . . . ?
C5 P N1 C3 -81.2(4) . . . . ?
C5 C6 C7 C8 179.5(4) . . . . ?
C5 C6 C11 C10 -176.8(4) . . . . ?
C5 C12 C13 C14 179.7(4) . . . . ?
C5 C12 C17 C16 -179.5(4) . . . . ?
C5 C18 C19 C20 -173.4(4) . . . . ?
C5 C18 C23 C22 173.4(5) . . . . ?
C6 C5 C12 C13 -66.0(5) . . . . ?
C6 C5 C12 C17 112.5(5) . . . . ?
C6 C5 C18 C19 -42.1(6) . . . . ?
C6 C5 C18 C23 145.3(4) . . . . ?
C6 C7 C8 C9 -3.3(7) . . . . ?
C7 C6 C11 C10 -0.9(7) . . . . ?
C7 C8 C9 C10 0.5(7) . . . . ?
C8 C9 C10 C11 2.1(8) . . . . ?
C9 C10 C11 C6 -1.9(8) . . . . ?
C11 C6 C7 C8 3.5(7) . . . . ?
C12 C5 C6 C7 -79.0(5) . . . . ?
C12 C5 C6 C11 96.9(5) . . . . ?
C12 C5 C18 C19 -162.4(4) . . . . ?
C12 C5 C18 C23 25.0(6) . . . . ?
C12 C13 C14 C15 -0.2(8) . . . . ?
C13 C12 C17 C16 -1.1(7) . . . . ?
C13 C14 C15 C16 -0.9(8) . . . . ?
C14 C15 C16 C17 1.0(8) . . . . ?
C15 C16 C17 C12 0.0(8) . . . . ?
C17 C12 C13 C14 1.2(7) . . . . ?
C18 C5 C6 C7 158.2(4) . . . . ?
C18 C5 C6 C11 -25.9(6) . . . . ?
C18 C5 C12 C13 59.1(5) . . . . ?
C18 C5 C12 C17 -122.5(5) . . . . ?
C18 C19 C20 C21 0.8(7) . . . . ?
C19 C18 C23 C22 0.7(7) . . . . ?
C19 C20 C21 C22 -0.9(8) . . . . ?
C20 C21 C22 C23 1.0(8) . . . . ?
C21 C22 C23 C18 -0.8(8) . . . . ?
C23 C18 C19 C20 -0.7(7) . . . . ?
W' P' N1' C1' -106.4(5) . . . . ?
W' P' N1' C3' 57.9(6) . . . . ?
W' P' C5' C6' 42.6(4) . . . . ?
W' P' C5' C12' 160.3(3) . . . . ?
W' P' C5' C18' -77.0(3) . . . . ?
P' N1' C1' N2' 166.3(4) . . . . ?
P' N1' C3' C2' -164.7(5) . . . . ?
P' C5' C6' C7' 46.3(5) . . . . ?
P' C5' C6' C11' -138.1(4) . . . . ?
P' C5' C12' C13' -173.6(4) . . . . ?
P' C5' C12' C17' 3.6(7) . . . . ?
P' C5' C18' C19' 69.7(5) . . . . ?
P' C5' C18' C23' -106.1(5) . . . . ?
N1' P' C5' C6' 172.7(3) . . . . ?
N1' P' C5' C12' -69.6(4) . . . . ?
N1' P' C5' C18' 53.1(4) . . . . ?
N2' C2' C3' N1' -1.9(9) . . . . ?
C1' N1' C3' C2' 1.1(8) . . . . ?
C1' N2' C2' C3' 2.1(10) . . . . ?
C2' N2' C1' N1' -1.3(8) . . . . ?
C3' N1' C1' N2' 0.0(8) . . . . ?
C4' N2' C1' N1' -179.7(6) . . . . ?
C4' N2' C2' C3' -179.8(8) . . . . ?
C5' P' N1' C1' 113.9(5) . . . . ?
C5' P' N1' C3' -81.8(6) . . . . ?
C5' C6' C7' C8' 178.2(4) . . . . ?
C5' C6' C11' C10' -176.1(4) . . . . ?
C5' C12' C13' C14' 177.0(5) . . . . ?
C5' C12' C17' C16' -177.6(6) . . . . ?
C5' C18' C19' C20' -174.1(5) . . . . ?
C5' C18' C23' C22' 174.0(6) . . . . ?
C6' C5' C12' C13' -56.3(6) . . . . ?
C6' C5' C12' C17' 120.9(6) . . . . ?
C6' C5' C18' C19' -44.3(6) . . . . ?
C6' C5' C18' C23' 139.9(5) . . . . ?
C6' C7' C8' C9' -2.4(7) . . . . ?
C7' C6' C11' C10' -0.4(7) . . . . ?
C7' C8' C9' C10' 0.4(8) . . . . ?
C8' C9' C10' C11' 1.5(8) . . . . ?
C9' C10' C11' C6' -1.5(8) . . . . ?
C11' C6' C7' C8' 2.4(6) . . . . ?
C12' C5' C6' C7' -77.9(5) . . . . ?
C12' C5' C6' C11' 97.7(5) . . . . ?
C12' C5' C18' C19' -164.6(5) . . . . ?
C12' C5' C18' C23' 19.7(7) . . . . ?
C12' C13' C14' C15' 1.4(8) . . . . ?
C13' C12' C17' C16' -0.3(10) . . . . ?
C13' C14' C15' C16' -1.4(9) . . . . ?
C14' C15' C16' C17' 0.6(12) . . . . ?
C15' C16' C17' C12' 0.3(13) . . . . ?
C17' C12' C13' C14' -0.4(8) . . . . ?
C18' C5' C6' C7' 158.9(4) . . . . ?
C18' C5' C6' C11' -25.5(6) . . . . ?
C18' C5' C12' C13' 68.1(6) . . . . ?
C18' C5' C12' C17' -114.6(7) . . . . ?
C18' C19' C20' C21' 0.6(9) . . . . ?
C19' C18' C23' C22' -1.9(9) . . . . ?
C19' C20' C21' C22' -3.3(10) . . . . ?
C20' C21' C22' C23' 3.4(11) . . . . ?
C21' C22' C23' C18' -0.7(10) . . . . ?
C23' C18' C19' C20' 1.9(8) . . . . ?
O6 S C29 F1 -61.1(8) . . . . ?
O6 S C29 F2 57.2(8) . . . . ?
O6 S C29 F3 176.6(7) . . . . ?
O7 S C29 F1 62.2(8) . . . . ?
O7 S C29 F2 -179.5(6) . . . . ?
O7 S C29 F3 -60.2(8) . . . . ?
O8 S C29 F1 -179.3(7) . . . . ?
O8 S C29 F2 -61.1(7) . . . . ?
O8 S C29 F3 58.3(8) . . . . ?
O6S SS C29S F1S -57.1(9) . . . . ?
O6S SS C29S F2S 63.3(9) . . . . ?
O6S SS C29S F3S -175.1(8) . . . . ?
O7S SS C29S F1S 64.6(9) . . . . ?
O7S SS C29S F2S -175.0(8) . . . . ?
O7S SS C29S F3S -53.4(9) . . . . ?
O8S SS C29S F1S -174.6(8) . . . . ?
O8S SS C29S F2S -54.2(9) . . . . ?
O8S SS C29S F3S 67.3(9) . . . . ?
O6T ST C29T F1T 64.3(9) . . . . ?
O6T ST C29T F2T -59.2(9) . . . . ?
O6T ST C29T F3T -179.6(7) . . . . ?
O7T ST C29T F1T -55.9(9) . . . . ?
O7T ST C29T F2T -179.4(8) . . . . ?
O7T ST C29T F3T 60.2(8) . . . . ?
O8T ST C29T F1T -176.1(7) . . . . ?
O8T ST C29T F2T 60.4(9) . . . . ?
O8T ST C29T F3T -60.0(8) . . . . ?
C30 C31 C32 C33 -161.6(12) . . . . ?
C31 C32 C33 C34 -142.1(11) . . . . ?

