# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 2132109'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_audit_creation_date             2020-09-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        AMF-38
_chemical_formula_moiety         'C13 H19 N2 O5 P W'
_chemical_formula_sum            'C13 H19 N2 O5 P W'
_chemical_formula_weight         498.12
_chemical_absolute_configuration ?
_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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   8.3463(4)
_cell_length_b                   9.9319(5)
_cell_length_c                   21.1509(13)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1753.30(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4604
_cell_measurement_temperature    123.0
_cell_measurement_theta_max      28.66
_cell_measurement_theta_min      2.62
_shelx_estimated_absorpt_T_max   0.689
_shelx_estimated_absorpt_T_min   0.500
_exptl_absorpt_coefficient_mu    6.701
_exptl_absorpt_correction_T_max  0.5198
_exptl_absorpt_correction_T_min  0.3226
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9246
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         2.623
_diffrn_ambient_temperature      123.0
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_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         0.719
_reflns_Friedel_fraction_full    0.974
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                3130
_reflns_number_total             3768
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 
;
 Flack x determined using 1142 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.641
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0230
_refine_ls_restrained_S_all      0.641
_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)] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0314
_refine_ls_wR_factor_ref         0.0327
_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 Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_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 0.58325(3) 0.55719(3) 0.66262(2) 0.01486(6) Uani 1 1 d . . . . .
P P 0.8533(2) 0.59519(17) 0.61939(10) 0.0194(4) Uani 1 1 d . . . . .
H H 0.966(6) 0.529(5) 0.663(4) 0.031(17) Uiso 1 1 d . . . . .
O1 O 0.2440(5) 0.4857(5) 0.7202(3) 0.0304(14) Uani 1 1 d . . . . .
O2 O 0.7176(6) 0.6343(5) 0.7993(3) 0.0322(14) Uani 1 1 d . . . . .
O3 O 0.4887(5) 0.8666(4) 0.6532(3) 0.0298(13) Uani 1 1 d . . . . .
O4 O 0.4461(7) 0.5015(4) 0.5248(2) 0.0338(14) Uani 1 1 d . . . . .
O5 O 0.6641(6) 0.2453(5) 0.6791(3) 0.0381(17) Uani 1 1 d . . . . .
N1 N 0.9005(6) 0.5485(6) 0.5450(2) 0.0179(11) Uani 1 1 d . . . . .
N2 N 0.9268(8) 0.7502(4) 0.6088(2) 0.0201(12) Uani 1 1 d . . . . .
C1 C 1.0264(8) 0.6371(7) 0.5182(4) 0.0236(17) Uani 1 1 d . . . . .
H1A H 0.9847 0.6859 0.4809 0.028 Uiso 1 1 calc R . . . .
H1B H 1.1202 0.5830 0.5050 0.028 Uiso 1 1 calc R . . . .
C2 C 1.0743(10) 0.7366(6) 0.5700(3) 0.0216(14) Uani 1 1 d . . . . .
H2A H 1.1642 0.7011 0.5956 0.026 Uiso 1 1 calc R . . . .
H2B H 1.1060 0.8244 0.5517 0.026 Uiso 1 1 calc R . . . .
C3 C 0.8976(10) 0.4046(6) 0.5275(3) 0.0204(18) Uani 1 1 d . . . . .
H3 H 0.7984 0.3638 0.5458 0.024 Uiso 1 1 calc R . . . .
C4 C 1.0396(9) 0.3253(7) 0.5513(4) 0.038(2) Uani 1 1 d . . . . .
H4A H 1.1379 0.3603 0.5320 0.057 Uiso 1 1 calc GR . . . .
H4B H 1.0264 0.2303 0.5400 0.057 Uiso 1 1 calc GR . . . .
H4C H 1.0466 0.3339 0.5974 0.057 Uiso 1 1 calc GR . . . .
C5 C 0.8873(10) 0.3937(6) 0.4547(3) 0.0285(19) Uani 1 1 d . . . . .
H5A H 0.7991 0.4500 0.4393 0.043 Uiso 1 1 calc GR . . . .
H5B H 0.8680 0.2998 0.4428 0.043 Uiso 1 1 calc GR . . . .
H5C H 0.9882 0.4244 0.4360 0.043 Uiso 1 1 calc GR . . . .
C6 C 0.9297(8) 0.8474(5) 0.6622(4) 0.0189(12) Uani 1 1 d . . . . .
H6 H 0.8264 0.8358 0.6855 0.023 Uiso 1 1 calc R . . . .
C7 C 1.0634(9) 0.8224(7) 0.7098(3) 0.0258(17) Uani 1 1 d . . . . .
H7A H 1.0606 0.7282 0.7235 0.039 Uiso 1 1 calc GR . . . .
H7B H 1.0485 0.8813 0.7465 0.039 Uiso 1 1 calc GR . . . .
H7C H 1.1670 0.8417 0.6900 0.039 Uiso 1 1 calc GR . . . .
C8 C 0.9296(10) 0.9904(5) 0.6360(3) 0.0261(16) Uani 1 1 d . . . . .
H8A H 1.0301 1.0069 0.6133 0.039 Uiso 1 1 calc GR . . . .
H8B H 0.9197 1.0547 0.6709 0.039 Uiso 1 1 calc GR . . . .
H8C H 0.8391 1.0016 0.6070 0.039 Uiso 1 1 calc GR . . . .
C9 C 0.3668(8) 0.5136(6) 0.6996(3) 0.0224(17) Uani 1 1 d . . . . .
C10 C 0.6698(8) 0.6027(6) 0.7510(4) 0.0208(17) Uani 1 1 d . . . . .
C11 C 0.5228(7) 0.7552(7) 0.6553(4) 0.0205(16) Uani 1 1 d . . . . .
C12 C 0.4969(8) 0.5224(6) 0.5746(4) 0.0215(17) Uani 1 1 d . . . . .
C13 C 0.6391(7) 0.3575(7) 0.6727(4) 0.025(2) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W P 2.4611(18) . ?
W C9 2.015(7) . ?
W C10 2.055(8) . ?
W C11 2.036(7) . ?
W C12 2.025(8) . ?
W C13 2.048(7) . ?
P H 1.47(7) . ?
P N1 1.687(5) . ?
P N2 1.673(5) . ?
O1 C9 1.148(7) . ?
O2 C10 1.140(9) . ?
O3 C11 1.143(7) . ?
O4 C12 1.154(8) . ?
O5 C13 1.142(8) . ?
N1 C1 1.483(8) . ?
N1 C3 1.476(9) . ?
N2 C2 1.485(9) . ?
N2 C6 1.486(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.529(9) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3 1.0000 . ?
C3 C4 1.509(10) . ?
C3 C5 1.546(10) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6 1.0000 . ?
C6 C7 1.523(10) . ?
C6 C8 1.525(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 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
C9 W P 176.19(18) . . ?
C9 W C10 90.5(3) . . ?
C9 W C11 90.8(2) . . ?
C9 W C12 90.1(3) . . ?
C9 W C13 87.5(3) . . ?
C10 W P 88.99(19) . . ?
C11 W P 92.90(18) . . ?
C11 W C10 86.8(3) . . ?
C11 W C13 178.0(3) . . ?
C12 W P 90.60(19) . . ?
C12 W C10 177.1(3) . . ?
C12 W C11 90.4(3) . . ?
C12 W C13 90.7(3) . . ?
C13 W P 88.79(19) . . ?
C13 W C10 92.2(3) . . ?
W P H 107(2) . . ?
N1 P W 121.2(2) . . ?
N1 P H 108(3) . . ?
N2 P W 121.8(2) . . ?
N2 P H 105(2) . . ?
N2 P N1 92.5(3) . . ?
C1 N1 P 111.0(4) . . ?
C3 N1 P 119.8(5) . . ?
C3 N1 C1 119.3(5) . . ?
C2 N2 P 107.1(4) . . ?
C2 N2 C6 117.8(5) . . ?
C6 N2 P 120.2(4) . . ?
N1 C1 H1A 110.3 . . ?
N1 C1 H1B 110.3 . . ?
N1 C1 C2 107.2(6) . . ?
H1A C1 H1B 108.5 . . ?
C2 C1 H1A 110.3 . . ?
C2 C1 H1B 110.3 . . ?
N2 C2 C1 103.8(6) . . ?
N2 C2 H2A 111.0 . . ?
N2 C2 H2B 111.0 . . ?
C1 C2 H2A 111.0 . . ?
C1 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
N1 C3 H3 108.0 . . ?
N1 C3 C4 114.1(6) . . ?
N1 C3 C5 108.6(5) . . ?
C4 C3 H3 108.0 . . ?
C4 C3 C5 109.8(6) . . ?
C5 C3 H3 108.0 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6 106.7 . . ?
N2 C6 C7 114.1(5) . . ?
N2 C6 C8 109.2(6) . . ?
C7 C6 H6 106.7 . . ?
C7 C6 C8 113.1(6) . . ?
C8 C6 H6 106.7 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O1 C9 W 178.4(6) . . ?
O2 C10 W 176.7(6) . . ?
O3 C11 W 177.9(8) . . ?
O4 C12 W 179.1(6) . . ?
O5 C13 W 177.3(6) . . ?

_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_4
_database_code_depnum_ccdc_archive 'CCDC 2132110'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_audit_creation_date             2020-11-26
_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        AMF-42
_chemical_formula_moiety         'C22 H36 N3 O6 P W'
_chemical_formula_sum            'C22 H36 N3 O6 P W'
_chemical_formula_weight         653.36
_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'
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                   12.1269(3)
_cell_length_b                   10.9786(2)
_cell_length_c                   20.1204(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.575(2)
_cell_angle_gamma                90
_cell_volume                     2614.50(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    31046
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.78
_shelx_estimated_absorpt_T_max   0.661
_shelx_estimated_absorpt_T_min   0.398
_exptl_absorpt_coefficient_mu    4.519
_exptl_absorpt_correction_T_max  0.6122
_exptl_absorpt_correction_T_min  0.3373
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.660
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36816
_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         27.997
_diffrn_reflns_theta_min         2.783
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5552
_reflns_number_total             6301
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.998
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         6301
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0240
_refine_ls_R_factor_gt           0.0185
_refine_ls_restrained_S_all      0.986
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0173P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0380
_refine_ls_wR_factor_ref         0.0391
_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. Rigid bond restraints
 W, P
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 W, C21
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_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 0.51027(2) 0.84196(2) 0.72653(2) 0.01354(3) Uani 1 1 d . U . . .
P P 0.48633(4) 0.67391(4) 0.63825(3) 0.01056(9) Uani 1 1 d . U . . .
O1 O 0.37029(11) 0.66381(11) 0.57706(7) 0.0128(3) Uani 1 1 d . . . . .
O2 O 0.58977(14) 1.02834(17) 0.84555(10) 0.0353(4) Uani 1 1 d . . . . .
O3 O 0.41576(17) 0.69847(17) 0.83974(10) 0.0367(4) Uani 1 1 d . . . . .
O4 O 0.75539(13) 0.72436(14) 0.76446(9) 0.0257(3) Uani 1 1 d . . . . .
O5 O 0.59099(16) 1.04689(14) 0.63619(10) 0.0342(4) Uani 1 1 d . . . . .
O6 O 0.26517(14) 0.96300(16) 0.68839(9) 0.0308(4) Uani 1 1 d . . . . .
N1 N 0.50894(13) 0.52990(14) 0.66681(9) 0.0145(3) Uani 1 1 d . . . . .
N2 N 0.59078(13) 0.66390(13) 0.59606(9) 0.0126(3) Uani 1 1 d . . . . .
N3 N 0.27148(13) 0.74201(13) 0.57783(9) 0.0122(3) Uani 1 1 d . . . . .
C1 C 0.60805(16) 0.47290(18) 0.64886(11) 0.0159(4) Uani 1 1 d . . . . .
H1A H 0.595136 0.384739 0.640136 0.019 Uiso 1 1 calc R . . . .
H1B H 0.675846 0.483548 0.685984 0.019 Uiso 1 1 calc R . . . .
C2 C 0.62249(16) 0.53772(16) 0.58523(10) 0.0139(4) Uani 1 1 d . . . . .
H2A H 0.701697 0.532827 0.580043 0.017 Uiso 1 1 calc R . . . .
H2B H 0.572315 0.502537 0.544278 0.017 Uiso 1 1 calc R . . . .
C3 C 0.47192(17) 0.47816(19) 0.72632(11) 0.0178(4) Uani 1 1 d . . . . .
H3 H 0.413351 0.533744 0.737699 0.021 Uiso 1 1 calc R . . . .
C4 C 0.56830(19) 0.4681(2) 0.78935(12) 0.0260(5) Uani 1 1 d . . . . .
H4A H 0.623026 0.407325 0.781204 0.039 Uiso 1 1 calc GR . . . .
H4B H 0.537811 0.443333 0.828565 0.039 Uiso 1 1 calc GR . . . .
H4C H 0.605786 0.547318 0.798652 0.039 Uiso 1 1 calc GR . . . .
C5 C 0.4170(2) 0.35332(18) 0.70818(14) 0.0260(5) Uani 1 1 d . . . . .
H5A H 0.353808 0.361519 0.668726 0.039 Uiso 1 1 calc GR . . . .
H5B H 0.389057 0.321818 0.747020 0.039 Uiso 1 1 calc GR . . . .
H5C H 0.472984 0.296801 0.697185 0.039 Uiso 1 1 calc GR . . . .
C6 C 0.62677(16) 0.75844(16) 0.55382(11) 0.0137(4) Uani 1 1 d . . . . .
H6 H 0.592063 0.837079 0.563831 0.016 Uiso 1 1 calc R . . . .
C7 C 0.75491(17) 0.77402(19) 0.57283(13) 0.0224(5) Uani 1 1 d . . . . .
H7A H 0.779021 0.787342 0.622022 0.034 Uiso 1 1 calc GR . . . .
H7B H 0.776688 0.844273 0.548508 0.034 Uiso 1 1 calc GR . . . .
H7C H 0.791254 0.700459 0.560169 0.034 Uiso 1 1 calc GR . . . .
C8 C 0.58717(18) 0.73344(18) 0.47790(11) 0.0192(4) Uani 1 1 d . . . . .
H8A H 0.622329 0.658343 0.466221 0.029 Uiso 1 1 calc GR . . . .
H8B H 0.608881 0.801578 0.451990 0.029 Uiso 1 1 calc GR . . . .
H8C H 0.504804 0.724320 0.466631 0.029 Uiso 1 1 calc GR . . . .
C9 C 0.25198(16) 0.81652(16) 0.51418(11) 0.0131(4) Uani 1 1 d . . . . .
C10 C 0.14165(17) 0.88848(18) 0.51020(12) 0.0189(4) Uani 1 1 d . . . . .
H10A H 0.153513 0.948978 0.547572 0.023 Uiso 1 1 calc R . . . .
H10B H 0.123734 0.933675 0.466599 0.023 Uiso 1 1 calc R . . . .
C11 C 0.04131(17) 0.8084(2) 0.51519(13) 0.0236(5) Uani 1 1 d . . . . .
H11A H -0.026084 0.859458 0.514871 0.028 Uiso 1 1 calc R . . . .
H11B H 0.023843 0.752077 0.475865 0.028 Uiso 1 1 calc R . . . .
C12 C 0.07168(17) 0.7368(2) 0.58096(13) 0.0230(5) Uani 1 1 d . . . . .
H12A H 0.007274 0.683561 0.584463 0.028 Uiso 1 1 calc R . . . .
H12B H 0.083725 0.794352 0.619733 0.028 Uiso 1 1 calc R . . . .
C13 C 0.17775(16) 0.65788(17) 0.58680(12) 0.0165(4) Uani 1 1 d . . . . .
C14 C 0.34747(17) 0.90958(17) 0.52211(12) 0.0176(4) Uani 1 1 d . . . . .
H14A H 0.351044 0.956637 0.563915 0.026 Uiso 1 1 calc GR . . . .
H14B H 0.333314 0.964708 0.482861 0.026 Uiso 1 1 calc GR . . . .
H14C H 0.419365 0.867144 0.524647 0.026 Uiso 1 1 calc GR . . . .
C15 C 0.24696(17) 0.74593(18) 0.44764(11) 0.0178(4) Uani 1 1 d . . . . .
H15A H 0.307756 0.685375 0.454508 0.027 Uiso 1 1 calc GR . . . .
H15B H 0.256096 0.802744 0.411654 0.027 Uiso 1 1 calc GR . . . .
H15C H 0.173811 0.704669 0.434315 0.027 Uiso 1 1 calc GR . . . .
C16 C 0.20909(18) 0.6088(2) 0.65950(13) 0.0239(5) Uani 1 1 d . . . . .
H16A H 0.267716 0.546293 0.662570 0.036 Uiso 1 1 calc GR . . . .
H16B H 0.142098 0.572999 0.671647 0.036 Uiso 1 1 calc GR . . . .
H16C H 0.237575 0.675470 0.690923 0.036 Uiso 1 1 calc GR . . . .
C17 C 0.15603(18) 0.54846(18) 0.53802(13) 0.0241(5) Uani 1 1 d . . . . .
H17A H 0.118573 0.576377 0.492423 0.036 Uiso 1 1 calc GR . . . .
H17B H 0.107565 0.489390 0.554473 0.036 Uiso 1 1 calc GR . . . .
H17C H 0.228122 0.509858 0.536056 0.036 Uiso 1 1 calc GR . . . .
C18 C 0.55809(17) 0.9619(2) 0.80149(12) 0.0208(4) Uani 1 1 d . U . . .
C19 C 0.4507(2) 0.7429(2) 0.79755(13) 0.0239(5) Uani 1 1 d . . . . .
C20 C 0.66744(17) 0.76560(17) 0.75131(11) 0.0171(4) Uani 1 1 d . U . . .
C21 C 0.56302(18) 0.96870(19) 0.66610(12) 0.0204(4) Uani 1 1 d . U . . .
C22 C 0.35111(18) 0.91679(18) 0.69942(12) 0.0192(4) 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 2.5335(5) . ?
W C18 1.991(2) . ?
W C19 2.048(2) . ?
W C20 2.042(2) . ?
W C21 2.040(2) . ?
W C22 2.059(2) . ?
P O1 1.6595(15) . ?
P N1 1.6842(16) . ?
P N2 1.6749(16) . ?
O1 N3 1.4770(18) . ?
O2 C18 1.148(3) . ?
O3 C19 1.138(3) . ?
O4 C20 1.136(3) . ?
O5 C21 1.141(3) . ?
O6 C22 1.137(3) . ?
N1 C1 1.468(2) . ?
N1 C3 1.481(3) . ?
N2 C2 1.467(2) . ?
N2 C6 1.467(2) . ?
N3 C9 1.494(3) . ?
N3 C13 1.506(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.508(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3 1.0000 . ?
C3 C4 1.530(3) . ?
C3 C5 1.533(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6 1.0000 . ?
C6 C7 1.527(3) . ?
C6 C8 1.523(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.541(3) . ?
C9 C14 1.526(3) . ?
C9 C15 1.537(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.522(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.514(3) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C12 C13 1.534(3) . ?
C13 C16 1.527(3) . ?
C13 C17 1.537(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 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
C18 W P 169.33(6) . . ?
C18 W C19 84.92(9) . . ?
C18 W C20 89.09(8) . . ?
C18 W C21 85.58(9) . . ?
C18 W C22 92.20(8) . . ?
C19 W P 95.65(7) . . ?
C19 W C22 86.81(9) . . ?
C20 W P 80.25(6) . . ?
C20 W C19 93.65(9) . . ?
C20 W C22 178.67(8) . . ?
C21 W P 94.69(6) . . ?
C21 W C19 169.05(9) . . ?
C21 W C20 91.62(8) . . ?
C21 W C22 88.14(9) . . ?
C22 W P 98.46(6) . . ?
O1 P W 121.20(5) . . ?
O1 P N1 103.84(7) . . ?
O1 P N2 103.43(8) . . ?
N1 P W 117.33(6) . . ?
N2 P W 114.79(6) . . ?
N2 P N1 91.52(8) . . ?
N3 O1 P 120.81(11) . . ?
C1 N1 P 113.41(12) . . ?
C1 N1 C3 116.36(15) . . ?
C3 N1 P 125.49(13) . . ?
C2 N2 P 112.88(12) . . ?
C2 N2 C6 117.49(15) . . ?
C6 N2 P 126.91(12) . . ?
O1 N3 C9 106.65(13) . . ?
O1 N3 C13 106.26(13) . . ?
C9 N3 C13 117.12(16) . . ?
N1 C1 H1A 110.7 . . ?
N1 C1 H1B 110.7 . . ?
N1 C1 C2 105.08(15) . . ?
H1A C1 H1B 108.8 . . ?
C2 C1 H1A 110.7 . . ?
C2 C1 H1B 110.7 . . ?
N2 C2 C1 103.71(15) . . ?
N2 C2 H2A 111.0 . . ?
N2 C2 H2B 111.0 . . ?
C1 C2 H2A 111.0 . . ?
C1 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
N1 C3 H3 107.9 . . ?
N1 C3 C4 112.74(16) . . ?
N1 C3 C5 110.06(18) . . ?
C4 C3 H3 107.9 . . ?
C4 C3 C5 110.30(18) . . ?
C5 C3 H3 107.9 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6 107.6 . . ?
N2 C6 C7 110.43(17) . . ?
N2 C6 C8 112.64(16) . . ?
C7 C6 H6 107.6 . . ?
C8 C6 H6 107.6 . . ?
C8 C6 C7 110.67(18) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 107.38(15) . . ?
N3 C9 C14 107.58(16) . . ?
N3 C9 C15 116.07(15) . . ?
C14 C9 C10 107.02(15) . . ?
C14 C9 C15 108.30(16) . . ?
C15 C9 C10 110.12(17) . . ?
C9 C10 H10A 108.9 . . ?
C9 C10 H10B 108.9 . . ?
H10A C10 H10B 107.7 . . ?
C11 C10 C9 113.45(16) . . ?
C11 C10 H10A 108.9 . . ?
C11 C10 H10B 108.9 . . ?
C10 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
C12 C11 C10 108.16(18) . . ?
C12 C11 H11A 110.1 . . ?
C12 C11 H11B 110.1 . . ?
C11 C12 H12A 108.8 . . ?
C11 C12 H12B 108.8 . . ?
C11 C12 C13 113.61(18) . . ?
H12A C12 H12B 107.7 . . ?
C13 C12 H12A 108.8 . . ?
C13 C12 H12B 108.8 . . ?
N3 C13 C12 106.67(15) . . ?
N3 C13 C16 107.12(17) . . ?
N3 C13 C17 115.58(17) . . ?
C12 C13 C17 111.60(18) . . ?
C16 C13 C12 107.60(18) . . ?
C16 C13 C17 107.93(17) . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C9 C15 H15A 109.5 . . ?
C9 C15 H15B 109.5 . . ?
C9 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O2 C18 W 177.14(19) . . ?
O3 C19 W 173.3(2) . . ?
O4 C20 W 179.0(2) . . ?
O5 C21 W 174.16(19) . . ?
O6 C22 W 175.25(19) . . ?

_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_6b
_database_code_depnum_ccdc_archive 'CCDC 2132112'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_audit_creation_date             2021-08-10
_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        PB-213
_chemical_formula_moiety         'C11 H13 O7 P W'
_chemical_formula_sum            'C11 H13 O7 P W'
_chemical_formula_weight         472.03
_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                   7.0371(3)
_cell_length_b                   10.1674(4)
_cell_length_c                   10.6647(4)
_cell_angle_alpha                99.282(3)
_cell_angle_beta                 101.783(3)
_cell_angle_gamma                91.016(3)
_cell_volume                     736.17(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    33982
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.60
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   0.448
_shelx_estimated_absorpt_T_min   0.401
_exptl_absorpt_coefficient_mu    7.980
_exptl_absorpt_correction_T_max  0.3962
_exptl_absorpt_correction_T_min  0.1271
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             448
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25605
_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         27.994
_diffrn_reflns_theta_min         2.961
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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                3474
_reflns_number_total             3563
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.470
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.0082(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.167
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3563
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0147
_refine_ls_restrained_S_all      1.167
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0101P)²+0.4086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0347
_refine_ls_wR_factor_ref         0.0350
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_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 0.28740(2) 0.26397(2) 0.87609(2) 0.01180(4) Uani 1 1 d . . . . .
P P 0.12936(7) 0.22776(5) 0.64791(5) 0.01264(10) Uani 1 1 d . . . . .
H H -0.061(5) 0.200(3) 0.616(3) 0.031(8) Uiso 1 1 d . . . . .
O1 O 0.2052(2) 0.11674(15) 0.54472(15) 0.0158(3) Uani 1 1 d . . . . .
O2 O 0.1477(2) 0.35212(15) 0.57355(15) 0.0142(3) Uani 1 1 d . . . . .
O3 O 0.5149(3) 0.33163(18) 1.16897(17) 0.0229(3) Uani 1 1 d . . . . .
O4 O 0.4351(3) -0.03099(19) 0.8429(2) 0.0322(4) Uani 1 1 d . . . . .
O5 O 0.6681(3) 0.3672(2) 0.79609(19) 0.0281(4) Uani 1 1 d . . . . .
O6 O 0.1105(3) 0.55118(17) 0.89807(19) 0.0245(4) Uani 1 1 d . . . . .
O7 O -0.0812(3) 0.15079(19) 0.9639(2) 0.0298(4) Uani 1 1 d . . . . .
C1 C 0.2491(3) 0.1733(2) 0.4342(2) 0.0134(4) Uani 1 1 d . . . . .
C2 C 0.1319(3) 0.3026(2) 0.4339(2) 0.0137(4) Uani 1 1 d . . . . .
C3 C 0.4678(3) 0.2018(2) 0.4621(2) 0.0190(4) Uani 1 1 d . . . . .
H3A H 0.506437 0.270073 0.539989 0.028 Uiso 1 1 calc GR . . . .
H3B H 0.504182 0.233913 0.387964 0.028 Uiso 1 1 calc GR . . . .
H3C H 0.533902 0.119803 0.476430 0.028 Uiso 1 1 calc GR . . . .
C4 C 0.1840(4) 0.0697(2) 0.3132(2) 0.0204(4) Uani 1 1 d . . . . .
H4A H 0.264252 -0.007730 0.319148 0.031 Uiso 1 1 calc GR . . . .
H4B H 0.198077 0.108021 0.236702 0.031 Uiso 1 1 calc GR . . . .
H4C H 0.047468 0.041741 0.305214 0.031 Uiso 1 1 calc GR . . . .
C5 C 0.2204(3) 0.4125(2) 0.3799(2) 0.0184(4) Uani 1 1 d . . . . .
H5A H 0.139766 0.490011 0.384294 0.028 Uiso 1 1 calc GR . . . .
H5B H 0.226921 0.380330 0.289232 0.028 Uiso 1 1 calc GR . . . .
H5C H 0.351715 0.438160 0.431212 0.028 Uiso 1 1 calc GR . . . .
C6 C -0.0814(3) 0.2759(2) 0.3688(2) 0.0203(4) Uani 1 1 d . . . . .
H6A H -0.135804 0.202311 0.401802 0.030 Uiso 1 1 calc GR . . . .
H6B H -0.093847 0.251999 0.274631 0.030 Uiso 1 1 calc GR . . . .
H6C H -0.152187 0.356339 0.388037 0.030 Uiso 1 1 calc GR . . . .
C7 C 0.4312(3) 0.3055(2) 1.0641(2) 0.0158(4) Uani 1 1 d . . . . .
C8 C 0.3845(3) 0.0752(2) 0.8562(2) 0.0196(4) Uani 1 1 d . . . . .
C9 C 0.5306(3) 0.3319(2) 0.8235(2) 0.0181(4) Uani 1 1 d . . . . .
C10 C 0.1758(3) 0.4494(2) 0.8904(2) 0.0164(4) Uani 1 1 d . . . . .
C11 C 0.0481(3) 0.1921(2) 0.9314(2) 0.0184(4) 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 2.4260(6) . ?
W C7 2.026(2) . ?
W C8 2.042(2) . ?
W C9 2.048(2) . ?
W C10 2.050(2) . ?
W C11 2.054(2) . ?
P O1 1.6217(16) . ?
P O2 1.6136(15) . ?
O1 C1 1.476(2) . ?
O2 C2 1.474(3) . ?
O3 C7 1.139(3) . ?
O4 C8 1.140(3) . ?
O5 C9 1.134(3) . ?
O6 C10 1.137(3) . ?
O7 C11 1.135(3) . ?
C1 C2 1.564(3) . ?
C1 C3 1.520(3) . ?
C1 C4 1.513(3) . ?
C2 C5 1.516(3) . ?
C2 C6 1.519(3) . ?

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
C7 W P 175.76(6) . . ?
C7 W C8 91.60(9) . . ?
C7 W C9 88.57(9) . . ?
C7 W C10 90.70(9) . . ?
C7 W C11 90.57(9) . . ?
C8 W P 90.52(7) . . ?
C8 W C9 89.79(9) . . ?
C8 W C10 176.96(9) . . ?
C8 W C11 88.88(9) . . ?
C9 W P 87.77(7) . . ?
C9 W C10 92.25(9) . . ?
C9 W C11 178.40(8) . . ?
C10 W P 87.31(7) . . ?
C10 W C11 89.11(9) . . ?
C11 W P 93.14(7) . . ?
O1 P W 120.36(6) . . ?
O2 P W 115.41(6) . . ?
O2 P O1 96.57(8) . . ?
C1 O1 P 112.07(12) . . ?
C2 O2 P 109.49(12) . . ?
O1 C1 C2 103.97(15) . . ?
O1 C1 C3 106.93(17) . . ?
O1 C1 C4 107.61(16) . . ?
C3 C1 C2 113.11(17) . . ?
C4 C1 C2 113.73(19) . . ?
C4 C1 C3 110.88(18) . . ?
O2 C2 C1 102.70(16) . . ?
O2 C2 C5 106.41(17) . . ?
O2 C2 C6 109.01(16) . . ?
C5 C2 C1 114.54(16) . . ?
C5 C2 C6 110.13(18) . . ?
C6 C2 C1 113.43(18) . . ?
O3 C7 W 178.12(19) . . ?
O4 C8 W 178.5(2) . . ?
O5 C9 W 178.2(2) . . ?
O6 C10 W 178.67(19) . . ?
O7 C11 W 178.3(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_7a
_database_code_depnum_ccdc_archive 'CCDC 2132113'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_audit_creation_date             2020-12-17
_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        PB-211
_chemical_formula_moiety         'C19 H29 N2 O7 P W'
_chemical_formula_sum            'C19 H29 N2 O7 P W'
_chemical_formula_weight         612.26
_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      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                   8.2932(3)
_cell_length_b                   10.1104(3)
_cell_length_c                   15.3182(5)
_cell_angle_alpha                73.319(2)
_cell_angle_beta                 74.659(3)
_cell_angle_gamma                71.740(3)
_cell_volume                     1146.66(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    23979
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.74
_shelx_estimated_absorpt_T_max   0.577
_shelx_estimated_absorpt_T_min   0.307
_exptl_absorpt_coefficient_mu    5.148
_exptl_absorpt_correction_T_max  0.6833
_exptl_absorpt_correction_T_min  0.3164
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0643
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19824
_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         27.998
_diffrn_reflns_theta_min         2.741
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5246
_reflns_number_total             5540
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         1.105
_refine_diff_density_min         -1.899
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         5540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0197
_refine_ls_R_factor_gt           0.0175
_refine_ls_restrained_S_all      1.018
_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)+(0.0200P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0418
_refine_ls_wR_factor_ref         0.0423
_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 Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_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 0.34334(2) 0.49816(2) 0.33214(2) 0.01077(3) Uani 1 1 d . . . . .
P P 0.32708(7) 0.69278(5) 0.19188(3) 0.00987(10) Uani 1 1 d . . . . .
O1 O 0.22134(19) 0.66576(16) 0.12576(10) 0.0133(3) Uani 1 1 d . . . . .
O2 O 0.24596(19) 0.86184(15) 0.19325(10) 0.0118(3) Uani 1 1 d . . . . .
O3 O 0.3872(3) 0.2114(2) 0.48647(14) 0.0360(5) Uani 1 1 d . . . . .
O4 O 0.5826(3) 0.3213(2) 0.18416(14) 0.0286(4) Uani 1 1 d . . . . .
O5 O 0.6556(2) 0.5597(2) 0.38474(14) 0.0291(4) Uani 1 1 d . . . . .
O6 O 0.0830(2) 0.6684(2) 0.48254(12) 0.0269(4) Uani 1 1 d . . . . .
O7 O 0.0178(2) 0.44546(19) 0.28689(14) 0.0255(4) Uani 1 1 d . . . . .
N1 N 0.5001(2) 0.70368(19) 0.10778(12) 0.0132(3) Uani 1 1 d . . . . .
N2 N 0.1338(2) 0.90297(18) 0.27854(11) 0.0108(3) Uani 1 1 d . . . . .
C1 C 0.2807(3) 0.7274(2) 0.02924(14) 0.0183(4) Uani 1 1 d . . . . .
H1A H 0.225368 0.831206 0.014206 0.022 Uiso 1 1 calc R . . . .
H1B H 0.252779 0.681381 -0.011895 0.022 Uiso 1 1 calc R . . . .
C2 C 0.4757(3) 0.7002(3) 0.01728(15) 0.0182(4) Uani 1 1 d . . . . .
H2A H 0.536622 0.606002 0.002013 0.022 Uiso 1 1 calc R . . . .
H2B H 0.518825 0.775407 -0.032444 0.022 Uiso 1 1 calc R . . . .
C3 C 0.6645(3) 0.7167(2) 0.11827(15) 0.0164(4) Uani 1 1 d . . . . .
H3 H 0.659605 0.703529 0.186080 0.020 Uiso 1 1 calc R . . . .
C4 C 0.8169(3) 0.6009(3) 0.0837(2) 0.0315(6) Uani 1 1 d . . . . .
H4A H 0.798773 0.506684 0.117066 0.047 Uiso 1 1 calc GR . . . .
H4B H 0.923769 0.609688 0.094817 0.047 Uiso 1 1 calc GR . . . .
H4C H 0.826097 0.611813 0.017040 0.047 Uiso 1 1 calc GR . . . .
C5 C 0.6916(3) 0.8652(3) 0.06996(16) 0.0232(5) Uani 1 1 d . . . . .
H5A H 0.695405 0.881830 0.003270 0.035 Uiso 1 1 calc GR . . . .
H5B H 0.800824 0.871388 0.079750 0.035 Uiso 1 1 calc GR . . . .
H5C H 0.595738 0.937605 0.095896 0.035 Uiso 1 1 calc GR . . . .
C6 C 0.2111(3) 1.0071(2) 0.29601(14) 0.0133(4) Uani 1 1 d . . . . .
C7 C 0.0882(3) 1.0692(2) 0.37618(15) 0.0167(4) Uani 1 1 d . . . . .
H7A H 0.087596 0.992458 0.433378 0.020 Uiso 1 1 calc R . . . .
H7B H 0.132416 1.142931 0.386247 0.020 Uiso 1 1 calc R . . . .
C8 C -0.0964(3) 1.1357(2) 0.36044(16) 0.0182(4) Uani 1 1 d . . . . .
H8A H -0.170775 1.171557 0.415376 0.022 Uiso 1 1 calc R . . . .
H8B H -0.099587 1.217040 0.305810 0.022 Uiso 1 1 calc R . . . .
C9 C -0.1613(3) 1.0216(2) 0.34427(16) 0.0179(4) Uani 1 1 d . . . . .
H9A H -0.280662 1.064337 0.332520 0.022 Uiso 1 1 calc R . . . .
H9B H -0.166068 0.945107 0.401493 0.022 Uiso 1 1 calc R . . . .
C10 C -0.0493(3) 0.9548(2) 0.26279(15) 0.0134(4) Uani 1 1 d . . . . .
C11 C 0.3812(3) 0.9192(3) 0.32779(17) 0.0204(5) Uani 1 1 d . . . . .
H11A H 0.359626 0.838965 0.379267 0.031 Uiso 1 1 calc GR . . . .
H11B H 0.428729 0.979799 0.348450 0.031 Uiso 1 1 calc GR . . . .
H11C H 0.464051 0.882470 0.275976 0.031 Uiso 1 1 calc GR . . . .
C12 C 0.2496(3) 1.1272(2) 0.21149(16) 0.0207(5) Uani 1 1 d . . . . .
H12A H 0.306124 1.086616 0.156737 0.031 Uiso 1 1 calc GR . . . .
H12B H 0.326138 1.173481 0.223983 0.031 Uiso 1 1 calc GR . . . .
H12C H 0.141055 1.197850 0.200001 0.031 Uiso 1 1 calc GR . . . .
C13 C -0.1084(3) 0.8226(2) 0.26860(16) 0.0171(4) Uani 1 1 d . . . . .
H13A H -0.042020 0.778910 0.216192 0.026 Uiso 1 1 calc GR . . . .
H13B H -0.231786 0.851007 0.266340 0.026 Uiso 1 1 calc GR . . . .
H13C H -0.089019 0.753583 0.326990 0.026 Uiso 1 1 calc GR . . . .
C14 C -0.0737(3) 1.0586(2) 0.16891(16) 0.0193(4) Uani 1 1 d . . . . .
H14A H -0.055254 1.150010 0.168304 0.029 Uiso 1 1 calc GR . . . .
H14B H -0.191339 1.073930 0.159829 0.029 Uiso 1 1 calc GR . . . .
H14C H 0.010046 1.017994 0.118786 0.029 Uiso 1 1 calc GR . . . .
C15 C 0.3691(3) 0.3167(3) 0.43249(16) 0.0214(5) Uani 1 1 d . . . . .
C16 C 0.4993(3) 0.3839(2) 0.23877(17) 0.0174(4) Uani 1 1 d . . . . .
C17 C 0.5459(3) 0.5385(2) 0.36372(16) 0.0188(4) Uani 1 1 d . . . . .
C18 C 0.1757(3) 0.6133(2) 0.42696(16) 0.0172(4) Uani 1 1 d . . . . .
C19 C 0.1333(3) 0.4631(2) 0.30396(16) 0.0170(4) 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 2.4629(5) . ?
W C15 2.021(2) . ?
W C16 2.021(3) . ?
W C17 2.048(2) . ?
W C18 2.070(3) . ?
W C19 2.054(2) . ?
P O1 1.6274(14) . ?
P O2 1.6331(15) . ?
P N1 1.6647(18) . ?
O1 C1 1.447(2) . ?
O2 N2 1.473(2) . ?
O3 C15 1.140(3) . ?
O4 C16 1.141(3) . ?
O5 C17 1.137(3) . ?
O6 C18 1.134(3) . ?
O7 C19 1.133(3) . ?
N1 C2 1.465(3) . ?
N1 C3 1.464(3) . ?
N2 C6 1.505(2) . ?
N2 C10 1.504(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.523(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3 1.0000 . ?
C3 C4 1.524(4) . ?
C3 C5 1.529(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.524(3) . ?
C6 C11 1.532(3) . ?
C6 C12 1.541(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.520(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C8 C9 1.518(3) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C9 C10 1.535(3) . ?
C10 C13 1.533(3) . ?
C10 C14 1.538(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C15 W P 170.50(8) . . ?
C15 W C16 89.09(10) . . ?
C15 W C17 89.28(9) . . ?
C15 W C18 90.78(10) . . ?
C15 W C19 90.96(9) . . ?
C16 W P 82.01(6) . . ?
C16 W C17 93.18(9) . . ?
C16 W C18 177.84(8) . . ?
C16 W C19 89.17(9) . . ?
C17 W P 94.50(6) . . ?
C17 W C18 88.97(9) . . ?
C17 W C19 177.64(9) . . ?
C18 W P 97.98(6) . . ?
C19 W P 85.62(6) . . ?
C19 W C18 88.68(9) . . ?
O1 P W 109.81(5) . . ?
O1 P O2 103.79(8) . . ?
O1 P N1 93.25(8) . . ?
O2 P W 124.21(6) . . ?
O2 P N1 99.59(8) . . ?
N1 P W 120.91(6) . . ?
C1 O1 P 110.59(12) . . ?
N2 O2 P 119.47(11) . . ?
C2 N1 P 113.71(13) . . ?
C3 N1 P 125.75(15) . . ?
C3 N1 C2 120.54(17) . . ?
O2 N2 C6 104.38(14) . . ?
O2 N2 C10 107.51(14) . . ?
C10 N2 C6 118.01(16) . . ?
O1 C1 H1A 110.6 . . ?
O1 C1 H1B 110.6 . . ?
O1 C1 C2 105.69(16) . . ?
H1A C1 H1B 108.7 . . ?
C2 C1 H1A 110.6 . . ?
C2 C1 H1B 110.6 . . ?
N1 C2 C1 103.91(17) . . ?
N1 C2 H2A 111.0 . . ?
N1 C2 H2B 111.0 . . ?
C1 C2 H2A 111.0 . . ?
C1 C2 H2B 111.0 . . ?
H2A C2 H2B 109.0 . . ?
N1 C3 H3 107.5 . . ?
N1 C3 C4 111.69(19) . . ?
N1 C3 C5 111.46(18) . . ?
C4 C3 H3 107.5 . . ?
C4 C3 C5 110.8(2) . . ?
C5 C3 H3 107.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 C7 107.34(16) . . ?
N2 C6 C11 106.29(17) . . ?
N2 C6 C12 115.29(17) . . ?
C7 C6 C11 108.36(17) . . ?
C7 C6 C12 110.69(18) . . ?
C11 C6 C12 108.60(18) . . ?
C6 C7 H7A 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C8 C7 C6 113.71(17) . . ?
C8 C7 H7A 108.8 . . ?
C8 C7 H7B 108.8 . . ?
C7 C8 H8A 110.1 . . ?
C7 C8 H8B 110.1 . . ?
H8A C8 H8B 108.4 . . ?
C9 C8 C7 108.06(18) . . ?
C9 C8 H8A 110.1 . . ?
C9 C8 H8B 110.1 . . ?
C8 C9 H9A 108.8 . . ?
C8 C9 H9B 108.8 . . ?
C8 C9 C10 113.92(18) . . ?
H9A C9 H9B 107.7 . . ?
C10 C9 H9A 108.8 . . ?
C10 C9 H9B 108.8 . . ?
N2 C10 C9 107.37(16) . . ?
N2 C10 C13 107.14(16) . . ?
N2 C10 C14 114.88(17) . . ?
C9 C10 C14 111.42(18) . . ?
C13 C10 C9 107.21(17) . . ?
C13 C10 C14 108.48(17) . . ?
C6 C11 H11A 109.5 . . ?
C6 C11 H11B 109.5 . . ?
C6 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C6 C12 H12A 109.5 . . ?
C6 C12 H12B 109.5 . . ?
C6 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14A 109.5 . . ?
C10 C14 H14B 109.5 . . ?
C10 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O3 C15 W 177.3(3) . . ?
O4 C16 W 177.44(19) . . ?
O5 C17 W 177.4(2) . . ?
O6 C18 W 175.73(19) . . ?
O7 C19 W 178.7(2) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_6a
_database_code_depnum_ccdc_archive 'CCDC 2132111'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_audit_creation_date             2020-12-10
_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        PB-208
_chemical_formula_moiety         'C10 H12 N O6 P W'
_chemical_formula_sum            'C10 H12 N O6 P W'
_chemical_formula_weight         457.03
_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                   6.5169(11)
_cell_length_b                   18.469(4)
_cell_length_c                   12.033(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.349(13)
_cell_angle_gamma                90
_cell_volume                     1414.8(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    665
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.20
_shelx_estimated_absorpt_T_max   0.557
_shelx_estimated_absorpt_T_min   0.369
_exptl_absorpt_coefficient_mu    8.297
_exptl_absorpt_correction_T_max  0.0396
_exptl_absorpt_correction_T_min  0.0104
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.146
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7225
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.997
_diffrn_reflns_theta_min         2.805
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS-2T'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2588
_reflns_number_total             3401
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_refine_diff_density_max         1.321
_refine_diff_density_min         -1.632
_refine_diff_density_rms         0.150
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.876
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         3401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0268
_refine_ls_restrained_S_all      0.876
_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)+(0.0285P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0542
_refine_ls_wR_factor_ref         0.0566
_refine_special_details          ?
_olex2_refinement_description    
;
1. 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 C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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 0.40319(3) 0.04468(2) 0.70721(2) 0.02251(6) Uani 1 1 d . . . . .
P P 0.3285(2) 0.16895(6) 0.75641(10) 0.0267(3) Uani 1 1 d . . . . .
H H 0.187(10) 0.205(3) 0.697(5) 0.032 Uiso 1 1 d R . . . .
O1 O 0.4947(8) 0.22935(19) 0.7352(3) 0.0373(10) Uani 1 1 d . . . . .
O2 O 0.5157(7) -0.1131(2) 0.6358(3) 0.0379(9) Uani 1 1 d . . . . .
O3 O 0.1030(7) 0.0710(2) 0.4638(3) 0.0335(9) Uani 1 1 d . . . . .
O4 O 0.7914(7) 0.1103(2) 0.6193(4) 0.0407(10) Uani 1 1 d . . . . .
O5 O 0.6963(7) 0.0299(2) 0.9556(3) 0.0401(10) Uani 1 1 d . . . . .
O6 O 0.0178(7) -0.0226(2) 0.7964(3) 0.0348(9) Uani 1 1 d . . . . .
N N 0.3382(8) 0.1932(2) 0.8908(4) 0.0309(10) Uani 1 1 d . . . . .
C1 C 0.4176(10) 0.2676(3) 0.9125(5) 0.0355(12) Uani 1 1 d . . . . .
H1A H 0.542750 0.268327 0.975818 0.043 Uiso 1 1 calc R . . . .
H1B H 0.308400 0.299214 0.932579 0.043 Uiso 1 1 calc R . . . .
C2 C 0.4743(12) 0.2929(3) 0.8028(5) 0.0409(14) Uani 1 1 d . . . . .
H2A H 0.363116 0.325176 0.760603 0.049 Uiso 1 1 calc R . . . .
H2B H 0.608196 0.320135 0.819831 0.049 Uiso 1 1 calc R . . . .
C3 C 0.2105(11) 0.1598(3) 0.9628(4) 0.0358(13) Uani 1 1 d . . . . .
H3 H 0.188926 0.108005 0.939039 0.043 Uiso 1 1 calc R . . . .
C4 C -0.0065(11) 0.1940(3) 0.9498(5) 0.0423(14) Uani 1 1 d . . . . .
H4A H 0.008496 0.244309 0.976351 0.063 Uiso 1 1 calc GR . . . .
H4B H -0.088541 0.166784 0.995002 0.063 Uiso 1 1 calc GR . . . .
H4C H -0.078783 0.193030 0.869491 0.063 Uiso 1 1 calc GR . . . .
C5 C 0.3297(12) 0.1603(3) 1.0867(5) 0.0425(15) Uani 1 1 d . . . . .
H5A H 0.466369 0.136800 1.092691 0.064 Uiso 1 1 calc GR . . . .
H5B H 0.248366 0.134066 1.133530 0.064 Uiso 1 1 calc GR . . . .
H5C H 0.350735 0.210435 1.113526 0.064 Uiso 1 1 calc GR . . . .
C6 C 0.4730(9) -0.0562(2) 0.6615(4) 0.0287(11) Uani 1 1 d . . . . .
C7 C 0.2115(9) 0.0614(2) 0.5514(4) 0.0264(11) Uani 1 1 d . . . . .
C8 C 0.6531(9) 0.0865(3) 0.6494(4) 0.0276(10) Uani 1 1 d . . . . .
C9 C 0.5934(9) 0.0341(3) 0.8674(4) 0.0295(11) Uani 1 1 d . . . . .
C10 C 0.1516(9) 0.0026(3) 0.7645(4) 0.0255(10) 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 2.4451(13) . ?
W C6 2.022(5) . ?
W C7 2.042(5) . ?
W C8 2.053(5) . ?
W C9 2.066(5) . ?
W C10 2.061(5) . ?
P O1 1.613(4) . ?
P N 1.666(4) . ?
O1 C2 1.450(6) . ?
O2 C6 1.146(6) . ?
O3 C7 1.150(6) . ?
O4 C8 1.131(7) . ?
O5 C9 1.130(7) . ?
O6 C10 1.126(6) . ?
N C1 1.471(6) . ?
N C3 1.461(7) . ?
C1 C2 1.519(8) . ?
C3 C4 1.526(9) . ?
C3 C5 1.527(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
C6 W P 177.32(15) . . ?
C6 W C7 91.07(19) . . ?
C6 W C8 90.8(2) . . ?
C6 W C9 92.4(2) . . ?
C6 W C10 89.2(2) . . ?
C7 W P 88.06(13) . . ?
C7 W C8 90.3(2) . . ?
C7 W C9 176.6(2) . . ?
C7 W C10 89.4(2) . . ?
C8 W P 86.72(14) . . ?
C8 W C9 89.5(2) . . ?
C8 W C10 179.7(2) . . ?
C9 W P 88.52(14) . . ?
C10 W P 93.38(14) . . ?
C10 W C9 90.8(2) . . ?
O1 P W 115.83(15) . . ?
O1 P N 94.6(2) . . ?
N P W 121.27(16) . . ?
C2 O1 P 109.0(4) . . ?
C1 N P 111.2(3) . . ?
C3 N P 123.7(4) . . ?
C3 N C1 120.8(4) . . ?
N C1 C2 106.0(4) . . ?
O1 C2 C1 107.8(4) . . ?
N C3 C4 113.4(5) . . ?
N C3 C5 110.0(5) . . ?
C4 C3 C5 111.4(5) . . ?
O2 C6 W 179.0(5) . . ?
O3 C7 W 179.7(5) . . ?
O4 C8 W 178.7(5) . . ?
O5 C9 W 178.3(5) . . ?
O6 C10 W 177.6(4) . . ?

_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_7b
_database_code_depnum_ccdc_archive 'CCDC 2132114'
loop_
_audit_author_name
_audit_author_address
'Gregor Schnakenburg'
;University of Bonn
Germany
;
_audit_update_record             
;
2022-01-03 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_audit_creation_date             2021-08-09
_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        PB-242.EI
_chemical_formula_moiety         'C20 H30 N O8 P W'
_chemical_formula_sum            'C20 H30 N O8 P W'
_chemical_formula_weight         627.27
_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                   11.1040(2)
_cell_length_b                   14.0762(2)
_cell_length_c                   15.5766(3)
_cell_angle_alpha                90
_cell_angle_beta                 93.904(2)
_cell_angle_gamma                90
_cell_volume                     2429.01(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    35705
_cell_measurement_temperature    123
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.62
_shelx_estimated_absorpt_T_max   0.475
_shelx_estimated_absorpt_T_min   0.376
_exptl_absorpt_coefficient_mu    4.864
_exptl_absorpt_correction_T_max  0.8542
_exptl_absorpt_correction_T_min  0.4419
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XRed32 V1.53'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0550
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38270
_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         27.999
_diffrn_reflns_theta_min         2.620
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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                5337
_reflns_number_total             5876
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_refine_diff_density_max         3.046
_refine_diff_density_min         -1.743
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         5876
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0280
_refine_ls_R_factor_gt           0.0243
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0430P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0598
_refine_ls_wR_factor_ref         0.0611
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,
 H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_atom_sites_solution_hydrogens   geom
_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 0.53205(2) 0.39660(2) 0.81005(2) 0.01402(5) Uani 1 1 d . . . . .
P P 0.47986(5) 0.30019(4) 0.68023(4) 0.01215(12) Uani 1 1 d . . . . .
O1 O 0.34909(16) 0.30303(12) 0.62736(11) 0.0153(3) Uani 1 1 d . . . . .
O2 O 0.50157(16) 0.18804(12) 0.69362(11) 0.0148(3) Uani 1 1 d . . . . .
O3 O 0.56472(16) 0.31126(12) 0.60080(12) 0.0163(3) Uani 1 1 d . . . . .
O4 O 0.62995(19) 0.50989(16) 0.97528(14) 0.0306(5) Uani 1 1 d . . . . .
O5 O 0.42649(19) 0.23246(15) 0.92336(14) 0.0263(4) Uani 1 1 d . . . . .
O6 O 0.7920(2) 0.30300(19) 0.83474(16) 0.0387(6) Uani 1 1 d . . . . .
O7 O 0.6242(3) 0.55868(19) 0.68803(17) 0.0456(7) Uani 1 1 d . . . . .
O8 O 0.27931(19) 0.50142(15) 0.82315(14) 0.0282(4) Uani 1 1 d . . . . .
N N 0.25333(18) 0.36363(14) 0.65711(13) 0.0132(4) Uani 1 1 d . . . . .
C1 C 0.2260(3) 0.43393(17) 0.58597(17) 0.0189(5) Uani 1 1 d . . . . .
C2 C 0.1179(3) 0.49250(19) 0.6132(2) 0.0263(6) Uani 1 1 d . . . . .
H2A H 0.144361 0.531521 0.663933 0.032 Uiso 1 1 calc R . . . .
H2B H 0.091845 0.536386 0.565893 0.032 Uiso 1 1 calc R . . . .
C3 C 0.0110(3) 0.4326(2) 0.6353(2) 0.0288(6) Uani 1 1 d . . . . .
H3A H -0.021468 0.397752 0.583579 0.035 Uiso 1 1 calc R . . . .
H3B H -0.053651 0.474031 0.655054 0.035 Uiso 1 1 calc R . . . .
C4 C 0.0509(3) 0.3626(2) 0.70586(18) 0.0238(6) Uani 1 1 d . . . . .
H4A H -0.018806 0.322628 0.719177 0.029 Uiso 1 1 calc R . . . .
H4B H 0.077327 0.398240 0.758592 0.029 Uiso 1 1 calc R . . . .
C5 C 0.1548(2) 0.29774(17) 0.68065(16) 0.0164(5) Uani 1 1 d . . . . .
C6 C 0.2008(3) 0.39140(19) 0.49577(19) 0.0238(6) Uani 1 1 d . . . . .
H6A H 0.258950 0.340581 0.486856 0.036 Uiso 1 1 calc GR . . . .
H6B H 0.208537 0.441068 0.452411 0.036 Uiso 1 1 calc GR . . . .
H6C H 0.118739 0.365393 0.490480 0.036 Uiso 1 1 calc GR . . . .
C7 C 0.3358(3) 0.4993(2) 0.5838(2) 0.0288(6) Uani 1 1 d . . . . .
H7A H 0.353906 0.526994 0.640897 0.043 Uiso 1 1 calc GR . . . .
H7B H 0.318353 0.550216 0.541829 0.043 Uiso 1 1 calc GR . . . .
H7C H 0.405469 0.462567 0.567106 0.043 Uiso 1 1 calc GR . . . .
C8 C 0.1107(2) 0.22518(19) 0.61195(18) 0.0209(5) Uani 1 1 d . . . . .
H8A H 0.059219 0.257156 0.567202 0.031 Uiso 1 1 calc GR . . . .
H8B H 0.064299 0.175277 0.638634 0.031 Uiso 1 1 calc GR . . . .
H8C H 0.180252 0.196804 0.586158 0.031 Uiso 1 1 calc GR . . . .
C9 C 0.2024(2) 0.24335(19) 0.76082(18) 0.0209(5) Uani 1 1 d . . . . .
H9A H 0.266565 0.199893 0.745743 0.031 Uiso 1 1 calc GR . . . .
H9B H 0.136436 0.206892 0.783586 0.031 Uiso 1 1 calc GR . . . .
H9C H 0.234559 0.288383 0.804545 0.031 Uiso 1 1 calc GR . . . .
C10 C 0.5443(2) 0.14326(16) 0.61567(16) 0.0149(5) Uani 1 1 d . . . . .
C11 C 0.6243(2) 0.22209(17) 0.57842(17) 0.0166(5) Uani 1 1 d . . . . .
C12 C 0.4358(2) 0.11655(18) 0.55569(19) 0.0193(5) Uani 1 1 d . . . . .
H12A H 0.463264 0.083625 0.505146 0.029 Uiso 1 1 calc GR . . . .
H12B H 0.391777 0.174208 0.537311 0.029 Uiso 1 1 calc GR . . . .
H12C H 0.382401 0.074620 0.585967 0.029 Uiso 1 1 calc GR . . . .
C13 C 0.6138(3) 0.05518(18) 0.6459(2) 0.0231(6) Uani 1 1 d . . . . .
H13A H 0.669004 0.071281 0.695559 0.035 Uiso 1 1 calc GR . . . .
H13B H 0.660218 0.031146 0.599211 0.035 Uiso 1 1 calc GR . . . .
H13C H 0.557040 0.006268 0.662505 0.035 Uiso 1 1 calc GR . . . .
C14 C 0.6267(3) 0.2199(2) 0.48111(18) 0.0264(6) Uani 1 1 d . . . . .
H14A H 0.544687 0.228816 0.454981 0.040 Uiso 1 1 calc GR . . . .
H14B H 0.658046 0.158408 0.463192 0.040 Uiso 1 1 calc GR . . . .
H14C H 0.678882 0.270891 0.462351 0.040 Uiso 1 1 calc GR . . . .
C15 C 0.7520(3) 0.2257(2) 0.6204(2) 0.0270(6) Uani 1 1 d . . . . .
H15A H 0.790328 0.285669 0.605463 0.040 Uiso 1 1 calc GR . . . .
H15B H 0.798902 0.172377 0.599815 0.040 Uiso 1 1 calc GR . . . .
H15C H 0.749168 0.221477 0.683049 0.040 Uiso 1 1 calc GR . . . .
C16 C 0.5911(2) 0.46979(19) 0.91596(17) 0.0208(5) Uani 1 1 d . . . . .
C17 C 0.4662(2) 0.29075(18) 0.88254(17) 0.0174(5) Uani 1 1 d . . . . .
C18 C 0.6976(3) 0.3346(2) 0.82207(18) 0.0237(6) Uani 1 1 d . . . . .
C19 C 0.5917(3) 0.5007(2) 0.73144(19) 0.0266(6) Uani 1 1 d . . . . .
C20 C 0.3679(3) 0.46275(17) 0.81398(17) 0.0186(5) 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 2.4713(6) . ?
W C16 2.016(3) . ?
W C17 2.035(3) . ?
W C18 2.032(3) . ?
W C19 2.049(3) . ?
W C20 2.051(3) . ?
P O1 1.6203(18) . ?
P O2 1.6084(18) . ?
P O3 1.6130(18) . ?
O1 N 1.463(2) . ?
O2 C10 1.475(3) . ?
O3 C11 1.472(3) . ?
O4 C16 1.142(3) . ?
O5 C17 1.144(3) . ?
O6 C18 1.143(4) . ?
O7 C19 1.134(4) . ?
O8 C20 1.142(3) . ?
N C1 1.501(3) . ?
N C5 1.498(3) . ?
C1 C2 1.540(4) . ?
C1 C6 1.535(4) . ?
C1 C7 1.530(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.514(5) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.520(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C4 C5 1.543(4) . ?
C5 C8 1.535(4) . ?
C5 C9 1.528(3) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.558(3) . ?
C10 C12 1.521(4) . ?
C10 C13 1.518(3) . ?
C11 C14 1.518(4) . ?
C11 C15 1.522(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 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
C16 W P 174.37(8) . . ?
C16 W C17 91.67(10) . . ?
C16 W C18 84.39(11) . . ?
C16 W C19 91.33(11) . . ?
C16 W C20 89.06(11) . . ?
C17 W P 88.79(7) . . ?
C17 W C19 176.76(10) . . ?
C17 W C20 87.83(10) . . ?
C18 W P 90.00(8) . . ?
C18 W C17 89.53(11) . . ?
C18 W C19 91.99(13) . . ?
C18 W C20 172.86(11) . . ?
C19 W P 88.35(8) . . ?
C19 W C20 91.00(12) . . ?
C20 W P 96.57(7) . . ?
O1 P W 123.67(7) . . ?
O2 P W 114.09(7) . . ?
O2 P O1 102.20(10) . . ?
O2 P O3 95.97(9) . . ?
O3 P W 117.25(7) . . ?
O3 P O1 99.08(10) . . ?
N O1 P 119.93(14) . . ?
C10 O2 P 111.50(14) . . ?
C11 O3 P 113.26(15) . . ?
O1 N C1 105.38(18) . . ?
O1 N C5 105.96(17) . . ?
C5 N C1 118.3(2) . . ?
N C1 C2 105.8(2) . . ?
N C1 C6 115.7(2) . . ?
N C1 C7 107.0(2) . . ?
C6 C1 C2 111.3(2) . . ?
C7 C1 C2 108.8(2) . . ?
C7 C1 C6 108.1(2) . . ?
C1 C2 H2A 108.8 . . ?
C1 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
C3 C2 C1 113.7(2) . . ?
C3 C2 H2A 108.8 . . ?
C3 C2 H2B 108.8 . . ?
C2 C3 H3A 109.8 . . ?
C2 C3 H3B 109.8 . . ?
C2 C3 C4 109.3(2) . . ?
H3A C3 H3B 108.3 . . ?
C4 C3 H3A 109.8 . . ?
C4 C3 H3B 109.8 . . ?
C3 C4 H4A 109.1 . . ?
C3 C4 H4B 109.1 . . ?
C3 C4 C5 112.7(2) . . ?
H4A C4 H4B 107.8 . . ?
C5 C4 H4A 109.1 . . ?
C5 C4 H4B 109.1 . . ?
N C5 C4 105.5(2) . . ?
N C5 C8 116.4(2) . . ?
N C5 C9 107.0(2) . . ?
C8 C5 C4 111.2(2) . . ?
C9 C5 C4 108.1(2) . . ?
C9 C5 C8 108.2(2) . . ?
C1 C6 H6A 109.5 . . ?
C1 C6 H6B 109.5 . . ?
C1 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 C7 H7A 109.5 . . ?
C1 C7 H7B 109.5 . . ?
C1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C5 C9 H9A 109.5 . . ?
C5 C9 H9B 109.5 . . ?
C5 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C10 C11 103.06(18) . . ?
O2 C10 C12 109.0(2) . . ?
O2 C10 C13 106.2(2) . . ?
C12 C10 C11 113.3(2) . . ?
C13 C10 C11 114.0(2) . . ?
C13 C10 C12 110.7(2) . . ?
O3 C11 C10 104.01(18) . . ?
O3 C11 C14 107.0(2) . . ?
O3 C11 C15 106.9(2) . . ?
C14 C11 C10 114.0(2) . . ?
C14 C11 C15 110.6(2) . . ?
C15 C11 C10 113.7(2) . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 C15 H15A 109.5 . . ?
C11 C15 H15B 109.5 . . ?
C11 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O4 C16 W 176.7(2) . . ?
O5 C17 W 178.3(2) . . ?
O6 C18 W 174.9(3) . . ?
O7 C19 W 179.6(3) . . ?
O8 C20 W 174.3(2) . . ?

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