# Electronic Supplementary Material (ESI) for Chemical Communications.
# 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_js173_3_a
_database_code_depnum_ccdc_archive 'CCDC 2163856'
loop_
_audit_author_name
_audit_author_address
'Manuela Weber'
;Freie Universitaet Berlin, Anorganische Chemie
Germany
;
_audit_update_record             
;
2022-05-30 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;
_audit_creation_date             2016-04-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H5 F6 N2 P'
_chemical_formula_sum            'C10 H5 F6 N2 P'
_chemical_formula_weight         298.13
_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'
F F 0.0171 0.0103 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_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'
'-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                   7.5247(5)
_cell_length_b                   12.9354(9)
_cell_length_c                   22.6658(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2206.2(3)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.11
_cell_measurement_theta_min      3.15
_shelx_estimated_absorpt_T_max   0.981
_shelx_estimated_absorpt_T_min   0.939
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6452
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0831 before and 0.0485 after correction.
The Ratio of minimum to maximum transmission is 0.8655.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plateltte
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.06
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            18484
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.168
_diffrn_reflns_theta_min         3.250
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2187
_reflns_number_total             2444
_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       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/6 (Sheldrick, 2014)'
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         2444
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0440
_refine_ls_restrained_S_all      1.171
_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)+(0.0411P)²+2.8966P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1017
_refine_ls_wR_factor_ref         0.1047
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00F(H00F), C00H(H00H), C00I(H00I)
;
_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
P001 P 0.62632(7) 0.60792(4) 0.45554(2) 0.01327(15) Uani 1 1 d . . . . .
F002 F 0.7007(2) 0.46534(10) 0.35998(6) 0.0244(3) Uani 1 1 d . . . . .
F003 F 0.69280(19) 0.57674(10) 0.28900(6) 0.0223(3) Uani 1 1 d . . . . .
F004 F 0.39511(19) 0.71241(11) 0.27913(6) 0.0230(3) Uani 1 1 d . . . . .
F005 F 0.62285(18) 0.81160(11) 0.28712(6) 0.0230(3) Uani 1 1 d . . . . .
F006 F 0.37049(19) 0.86067(11) 0.32187(6) 0.0240(3) Uani 1 1 d . . . . .
F007 F 0.45193(19) 0.50370(11) 0.31844(6) 0.0266(3) Uani 1 1 d . . . . .
N008 N 0.5599(2) 0.73104(13) 0.46803(7) 0.0113(4) Uani 1 1 d . . . . .
N009 N 0.5102(2) 0.78789(13) 0.42094(7) 0.0121(4) Uani 1 1 d . . . . .
C00A C 0.5613(3) 0.78109(16) 0.52458(9) 0.0119(4) Uani 1 1 d . . . . .
C00B C 0.5220(3) 0.72896(15) 0.37337(9) 0.0126(4) Uani 1 1 d . . . . .
C00C C 0.6076(3) 0.88484(16) 0.52834(9) 0.0143(4) Uani 1 1 d . . . . .
H00C H 0.6368 0.9228 0.4938 0.017 Uiso 1 1 calc R . . . .
C00D C 0.6105(3) 0.93248(18) 0.58334(10) 0.0179(5) Uani 1 1 d . . . . .
H00D H 0.6413 1.0035 0.5864 0.021 Uiso 1 1 calc R . . . .
C00E C 0.5818(3) 0.62717(16) 0.38230(9) 0.0136(4) Uani 1 1 d . . . . .
C00F C 0.5173(3) 0.72499(17) 0.57474(9) 0.0160(4) Uani 1 1 d . . . . .
H00F H 0.4840 0.6544 0.5715 0.019 Uiso 1 1 calc R . . . .
C00G C 0.6061(3) 0.54438(17) 0.33698(10) 0.0172(5) Uani 1 1 d . . . . .
C00H C 0.5685(3) 0.87645(18) 0.63390(10) 0.0188(5) Uani 1 1 d . . . . .
H00H H 0.5713 0.9091 0.6714 0.023 Uiso 1 1 calc R . . . .
C00I C 0.5223(3) 0.77254(18) 0.62945(9) 0.0185(5) Uani 1 1 d . . . . .
H00I H 0.4942 0.7342 0.6640 0.022 Uiso 1 1 calc R . . . .
C00J C 0.4770(3) 0.77920(16) 0.31523(9) 0.0157(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
P001 N008 1.6930(17) . ?
P001 C00E 1.712(2) . ?
F002 C00G 1.350(3) . ?
F003 C00G 1.336(3) . ?
F004 C00J 1.340(2) . ?
F005 C00J 1.337(3) . ?
F006 C00J 1.332(3) . ?
F007 C00G 1.341(3) . ?
N008 N009 1.349(2) . ?
N008 C00A 1.436(2) . ?
N009 C00B 1.323(3) . ?
C00A C00C 1.389(3) . ?
C00A C00F 1.389(3) . ?
C00B C00E 1.406(3) . ?
C00B C00J 1.508(3) . ?
C00C H00C 0.9500 . ?
C00C C00D 1.391(3) . ?
C00D H00D 0.9500 . ?
C00D C00H 1.392(3) . ?
C00E C00G 1.495(3) . ?
C00F H00F 0.9500 . ?
C00F C00I 1.385(3) . ?
C00H H00H 0.9500 . ?
C00H C00I 1.392(3) . ?
C00I H00I 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
N008 P001 C00E 88.14(9) . . ?
N009 N008 P001 117.54(13) . . ?
N009 N008 C00A 117.55(16) . . ?
C00A N008 P001 124.82(13) . . ?
C00B N009 N008 108.17(16) . . ?
C00C C00A N008 119.49(18) . . ?
C00F C00A N008 119.56(18) . . ?
C00F C00A C00C 120.95(19) . . ?
N009 C00B C00E 116.34(19) . . ?
N009 C00B C00J 116.66(18) . . ?
C00E C00B C00J 126.95(19) . . ?
C00A C00C H00C 120.4 . . ?
C00A C00C C00D 119.2(2) . . ?
C00D C00C H00C 120.4 . . ?
C00C C00D H00D 119.9 . . ?
C00C C00D C00H 120.2(2) . . ?
C00H C00D H00D 119.9 . . ?
C00B C00E P001 109.78(15) . . ?
C00B C00E C00G 127.66(19) . . ?
C00G C00E P001 122.56(16) . . ?
C00A C00F H00F 120.2 . . ?
C00I C00F C00A 119.6(2) . . ?
C00I C00F H00F 120.2 . . ?
F002 C00G C00E 109.96(18) . . ?
F003 C00G F002 107.10(17) . . ?
F003 C00G F007 106.89(18) . . ?
F003 C00G C00E 113.24(17) . . ?
F007 C00G F002 106.25(17) . . ?
F007 C00G C00E 113.00(18) . . ?
C00D C00H H00H 120.0 . . ?
C00I C00H C00D 120.0(2) . . ?
C00I C00H H00H 120.0 . . ?
C00F C00I C00H 120.0(2) . . ?
C00F C00I H00I 120.0 . . ?
C00H C00I H00I 120.0 . . ?
F004 C00J C00B 111.05(17) . . ?
F005 C00J F004 106.78(17) . . ?
F005 C00J C00B 111.55(18) . . ?
F006 C00J F004 107.60(17) . . ?
F006 C00J F005 107.44(17) . . ?
F006 C00J C00B 112.16(17) . . ?

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
P001 N008 N009 C00B 1.6(2) . . . . ?
P001 N008 C00A C00C 142.14(17) . . . . ?
P001 N008 C00A C00F -37.6(3) . . . . ?
P001 C00E C00G F002 -13.1(2) . . . . ?
P001 C00E C00G F003 -132.91(17) . . . . ?
P001 C00E C00G F007 105.4(2) . . . . ?
N008 P001 C00E C00B 1.18(15) . . . . ?
N008 P001 C00E C00G -178.84(18) . . . . ?
N008 N009 C00B C00E -0.6(2) . . . . ?
N008 N009 C00B C00J -178.27(17) . . . . ?
N008 C00A C00C C00D -179.31(19) . . . . ?
N008 C00A C00F C00I 178.64(19) . . . . ?
N009 N008 C00A C00C -34.4(3) . . . . ?
N009 N008 C00A C00F 145.84(19) . . . . ?
N009 C00B C00E P001 -0.6(2) . . . . ?
N009 C00B C00E C00G 179.4(2) . . . . ?
N009 C00B C00J F004 -144.23(19) . . . . ?
N009 C00B C00J F005 96.8(2) . . . . ?
N009 C00B C00J F006 -23.8(3) . . . . ?
C00A N008 N009 C00B 178.45(17) . . . . ?
C00A C00C C00D C00H 0.3(3) . . . . ?
C00A C00F C00I C00H 1.0(3) . . . . ?
C00B C00E C00G F002 166.8(2) . . . . ?
C00B C00E C00G F003 47.1(3) . . . . ?
C00B C00E C00G F007 -74.6(3) . . . . ?
C00C C00A C00F C00I -1.1(3) . . . . ?
C00C C00D C00H C00I -0.4(3) . . . . ?
C00D C00H C00I C00F -0.3(3) . . . . ?
C00E P001 N008 N009 -1.67(16) . . . . ?
C00E P001 N008 C00A -178.26(17) . . . . ?
C00E C00B C00J F004 38.4(3) . . . . ?
C00E C00B C00J F005 -80.6(3) . . . . ?
C00E C00B C00J F006 158.8(2) . . . . ?
C00F C00A C00C C00D 0.4(3) . . . . ?
C00J C00B C00E P001 176.82(17) . . . . ?
C00J C00B C00E C00G -3.2(3) . . . . ?

_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_pap228_5
_database_code_depnum_ccdc_archive 'CCDC 2163857'
loop_
_audit_author_name
_audit_author_address
'Manuela Weber'
;Freie Universitaet Berlin, Anorganische Chemie
Germany
;
_audit_update_record             
;
2022-05-30 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;
_audit_creation_date             2019-02-18
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C15 H5 F6 N2 O5 P W'
_chemical_formula_sum            'C15 H5 F6 N2 O5 P W'
_chemical_formula_weight         622.03
_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'
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      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                   6.6629(3)
_cell_length_b                   18.3901(8)
_cell_length_c                   15.6561(7)
_cell_angle_alpha                90
_cell_angle_beta                 100.123(2)
_cell_angle_gamma                90
_cell_volume                     1888.50(15)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      2.58
_shelx_estimated_absorpt_T_max   0.885
_shelx_estimated_absorpt_T_min   0.314
_exptl_absorpt_coefficient_mu    6.290
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.4846
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.6495.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.188
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.4846
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30420
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.557
_diffrn_reflns_theta_min         2.579
_diffrn_ambient_temperature      99.97
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5238
_reflns_number_total             5650
_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 V8.38A (?, 2016)'
_computing_data_collection       APEX2
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.569
_refine_diff_density_min         -1.704
_refine_diff_density_rms         0.130
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0192
_refine_ls_restrained_S_all      1.178
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0127P)²+2.2436P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0413
_refine_ls_wR_factor_ref         0.0422
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C5(H5), C4(H4), C3(H3), C2(H2)
;
_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
W1 W 0.75158(2) 0.33702(2) 0.52660(2) 0.00971(3) Uani 1 1 d . . . . .
P1 P 0.59535(8) 0.23125(3) 0.45521(4) 0.01069(10) Uani 1 1 d . . . . .
F4 F 0.2163(2) 0.25207(8) 0.24012(9) 0.0257(3) Uani 1 1 d . . . . .
F5 F 0.0639(2) 0.24597(9) 0.35027(10) 0.0276(3) Uani 1 1 d . . . . .
F3 F 0.1059(2) 0.10642(9) 0.27129(10) 0.0242(3) Uani 1 1 d . . . . .
F1 F 0.3560(3) 0.10688(9) 0.20176(10) 0.0290(4) Uani 1 1 d . . . . .
F6 F 0.2914(3) 0.32789(8) 0.34619(12) 0.0323(4) Uani 1 1 d . . . . .
F2 F 0.3263(3) 0.02011(8) 0.29077(11) 0.0295(4) Uani 1 1 d . . . . .
O5 O 1.1933(2) 0.26420(9) 0.55395(11) 0.0184(3) Uani 1 1 d . . . . .
O2 O 0.3361(3) 0.42578(10) 0.51069(12) 0.0235(4) Uani 1 1 d . . . . .
O3 O 0.9698(3) 0.48110(9) 0.60623(13) 0.0261(4) Uani 1 1 d . . . . .
O4 O 0.6956(3) 0.27823(11) 0.71317(12) 0.0263(4) Uani 1 1 d . . . . .
O1 O 0.7767(3) 0.38791(10) 0.33352(12) 0.0272(4) Uani 1 1 d . . . . .
N1 N 0.5821(3) 0.09849(10) 0.39917(12) 0.0136(3) Uani 1 1 d . . . . .
N2 N 0.6825(3) 0.14554(10) 0.45900(12) 0.0120(3) Uani 1 1 d . . . . .
C13 C 0.8920(4) 0.42913(12) 0.57798(15) 0.0171(4) Uani 1 1 d . . . . .
C15 C 1.0339(3) 0.28876(12) 0.54323(14) 0.0131(4) Uani 1 1 d . . . . .
C12 C 0.4814(3) 0.39227(12) 0.51590(15) 0.0152(4) Uani 1 1 d . . . . .
C11 C 0.7737(3) 0.37110(12) 0.40340(15) 0.0157(4) Uani 1 1 d . . . . .
C8 C 0.4073(3) 0.20829(12) 0.37077(14) 0.0127(4) Uani 1 1 d . . . . .
C14 C 0.7163(3) 0.29968(12) 0.64725(15) 0.0161(4) Uani 1 1 d . . . . .
C7 C 0.4308(3) 0.13411(12) 0.35119(14) 0.0135(4) Uani 1 1 d . . . . .
C10 C 0.2451(4) 0.25803(13) 0.32697(15) 0.0178(4) Uani 1 1 d . . . . .
C9 C 0.3048(4) 0.09147(12) 0.27863(15) 0.0164(4) Uani 1 1 d . . . . .
C1 C 0.8585(3) 0.11871(11) 0.51734(14) 0.0121(4) Uani 1 1 d . . . . .
C6 C 0.8565(4) 0.11585(12) 0.60572(15) 0.0158(4) Uani 1 1 d . . . . .
H6 H 0.739088 0.130458 0.628051 0.019 Uiso 1 1 calc R . . . .
C5 C 1.0294(4) 0.09124(13) 0.66098(16) 0.0197(5) Uani 1 1 d . . . . .
H5 H 1.030692 0.089177 0.721704 0.024 Uiso 1 1 calc R . . . .
C4 C 1.1997(4) 0.06972(13) 0.62813(17) 0.0200(5) Uani 1 1 d . . . . .
H4 H 1.317713 0.053323 0.666395 0.024 Uiso 1 1 calc R . . . .
C3 C 1.1987(4) 0.07201(13) 0.53930(17) 0.0190(5) Uani 1 1 d . . . . .
H3 H 1.315417 0.056592 0.516991 0.023 Uiso 1 1 calc R . . . .
C2 C 1.0274(3) 0.09681(12) 0.48301(15) 0.0158(4) Uani 1 1 d . . . . .
H2 H 1.025952 0.098743 0.422266 0.019 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 P1 2.3891(6) . ?
W1 C13 2.032(2) . ?
W1 C15 2.055(2) . ?
W1 C12 2.048(2) . ?
W1 C11 2.058(2) . ?
W1 C14 2.062(2) . ?
P1 N2 1.6770(19) . ?
P1 C8 1.707(2) . ?
F4 C10 1.344(3) . ?
F5 C10 1.340(3) . ?
F3 C9 1.338(3) . ?
F1 C9 1.338(3) . ?
F6 C10 1.343(3) . ?
F2 C9 1.330(3) . ?
O5 C15 1.139(3) . ?
O2 C12 1.138(3) . ?
O3 C13 1.139(3) . ?
O4 C14 1.135(3) . ?
O1 C11 1.141(3) . ?
N1 N2 1.361(3) . ?
N1 C7 1.321(3) . ?
N2 C1 1.441(3) . ?
C8 C7 1.413(3) . ?
C8 C10 1.488(3) . ?
C7 C9 1.508(3) . ?
C1 C6 1.387(3) . ?
C1 C2 1.390(3) . ?
C6 C5 1.389(3) . ?
C5 C4 1.383(3) . ?
C4 C3 1.390(4) . ?
C3 C2 1.391(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
C13 W1 P1 175.27(7) . . ?
C13 W1 C15 87.84(9) . . ?
C13 W1 C12 87.47(9) . . ?
C13 W1 C11 90.76(9) . . ?
C13 W1 C14 91.93(9) . . ?
C15 W1 P1 91.23(6) . . ?
C15 W1 C11 92.04(9) . . ?
C15 W1 C14 89.39(9) . . ?
C12 W1 P1 93.51(6) . . ?
C12 W1 C15 175.24(9) . . ?
C12 W1 C11 88.79(9) . . ?
C12 W1 C14 90.01(9) . . ?
C11 W1 P1 84.64(6) . . ?
C11 W1 C14 177.00(9) . . ?
C14 W1 P1 92.69(7) . . ?
N2 P1 W1 128.98(7) . . ?
N2 P1 C8 89.85(10) . . ?
C8 P1 W1 139.81(8) . . ?
C7 N1 N2 108.03(18) . . ?
N1 N2 P1 116.62(15) . . ?
N1 N2 C1 117.70(17) . . ?
C1 N2 P1 125.62(15) . . ?
O3 C13 W1 179.4(2) . . ?
O5 C15 W1 177.54(19) . . ?
O2 C12 W1 176.9(2) . . ?
O1 C11 W1 176.3(2) . . ?
C7 C8 P1 108.21(16) . . ?
C7 C8 C10 126.4(2) . . ?
C10 C8 P1 125.43(16) . . ?
O4 C14 W1 179.0(2) . . ?
N1 C7 C8 117.3(2) . . ?
N1 C7 C9 116.03(19) . . ?
C8 C7 C9 126.7(2) . . ?
F4 C10 C8 112.28(19) . . ?
F5 C10 F4 106.66(19) . . ?
F5 C10 F6 106.3(2) . . ?
F5 C10 C8 112.9(2) . . ?
F6 C10 F4 106.9(2) . . ?
F6 C10 C8 111.42(19) . . ?
F3 C9 C7 111.68(18) . . ?
F1 C9 F3 106.53(19) . . ?
F1 C9 C7 111.80(18) . . ?
F2 C9 F3 107.16(19) . . ?
F2 C9 F1 107.42(19) . . ?
F2 C9 C7 111.9(2) . . ?
C6 C1 N2 119.73(19) . . ?
C6 C1 C2 121.7(2) . . ?
C2 C1 N2 118.6(2) . . ?
C1 C6 C5 118.8(2) . . ?
C4 C5 C6 120.4(2) . . ?
C5 C4 C3 120.2(2) . . ?
C4 C3 C2 120.2(2) . . ?
C1 C2 C3 118.7(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_LD1209
_database_code_depnum_ccdc_archive 'CCDC 2163858'
loop_
_audit_author_name
_audit_author_address
'Manuela Weber'
;Freie Universitaet Berlin, Anorganische Chemie
Germany
;
_audit_update_record             
;
2022-05-30 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C22 H26 N3 O5 P W'
_chemical_formula_weight         627.28

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.1075(2)
_cell_length_b                   14.6470(2)
_cell_length_c                   16.9008(3)
_cell_angle_alpha                112.5214(6)
_cell_angle_beta                 102.9855(5)
_cell_angle_gamma                91.3575(5)
_cell_volume                     2456.50(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9661
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      30.55
_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_F_000             1232
_exptl_transmission_factor_min   0.2195
_exptl_transmission_factor_max   0.4010
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    4.804
_shelx_estimated_absorpt_T_min   0.250
_shelx_estimated_absorpt_T_max   0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2195
_exptl_absorpt_correction_T_max  0.4010
_exptl_absorpt_process_details   
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1252 before and 0.0583 after correction.
The Ratio of minimum to maximum transmission is 0.5474.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker Photon CMOS Detector, D8 Venture'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68480
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.896
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12174
_reflns_number_gt                11237
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX3'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0125P)²+1.6662P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12174
_refine_ls_number_parameters     591
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0220
_refine_ls_R_factor_gt           0.0192
_refine_ls_wR_factor_ref         0.0452
_refine_ls_wR_factor_gt          0.0440
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.040
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.47619(2) 0.69029(2) 0.14882(2) 0.01778(3) Uani 1 1 d . . . . .
P1 P 0.38485(5) 0.71329(4) 0.27340(3) 0.01369(10) Uani 1 1 d . . . . .
O1 O 0.69454(19) 0.85319(16) 0.29445(14) 0.0439(5) Uani 1 1 d . . . . .
O2 O 0.3278(2) 0.84870(15) 0.09229(13) 0.0413(5) Uani 1 1 d . . . . .
O3 O 0.6058(2) 0.67284(16) -0.00300(15) 0.0494(6) Uani 1 1 d . . . . .
O4 O 0.26357(18) 0.51938(15) 0.00889(13) 0.0378(4) Uani 1 1 d . . . . .
O5 O 0.6228(2) 0.51304(16) 0.16697(14) 0.0448(5) Uani 1 1 d . . . . .
N1 N 0.27698(15) 0.78786(12) 0.30406(11) 0.0133(3) Uani 1 1 d . . . . .
N2 N 0.25121(17) 0.79379(14) 0.38060(12) 0.0186(4) Uani 1 1 d . . . . .
N3 N 0.31866(17) 0.73912(14) 0.41370(12) 0.0190(4) Uani 1 1 d . . . . .
C1 C 0.39858(19) 0.69022(15) 0.36675(13) 0.0147(4) Uani 1 1 d . . . . .
C2 C 0.21711(19) 0.85122(15) 0.26332(13) 0.0138(4) Uani 1 1 d . . . . .
C3 C 0.27489(19) 0.94834(15) 0.29141(14) 0.0163(4) Uani 1 1 d . . . . .
C4 C 0.2159(2) 1.00821(16) 0.25112(15) 0.0195(4) Uani 1 1 d . . . . .
H4 H 0.252319 1.074509 0.268508 0.023 Uiso 1 1 calc R U . . .
C5 C 0.1053(2) 0.97251(16) 0.18632(15) 0.0207(4) Uani 1 1 d . . . . .
H5 H 0.067112 1.014074 0.159040 0.025 Uiso 1 1 calc R U . . .
C6 C 0.0496(2) 0.87644(16) 0.16082(14) 0.0196(4) Uani 1 1 d . . . . .
H6 H -0.026945 0.853110 0.116655 0.024 Uiso 1 1 calc R U . . .
C7 C 0.10430(19) 0.81390(15) 0.19902(14) 0.0161(4) Uani 1 1 d . . . . .
C8 C 0.3946(2) 0.98988(16) 0.36439(16) 0.0226(5) Uani 1 1 d . . . . .
H8 H 0.434477 0.932473 0.372457 0.027 Uiso 1 1 calc R U . . .
C9 C 0.4874(3) 1.0488(2) 0.3419(2) 0.0387(7) Uani 1 1 d . . . . .
H9A H 0.501496 1.007801 0.284220 0.058 Uiso 1 1 calc R U . . .
H9B H 0.566381 1.067004 0.387438 0.058 Uiso 1 1 calc R U . . .
H9C H 0.453925 1.109303 0.339725 0.058 Uiso 1 1 calc R U . . .
C10 C 0.3636(3) 1.05398(19) 0.45120(17) 0.0339(6) Uani 1 1 d . . . . .
H10A H 0.318397 1.107884 0.443515 0.051 Uiso 1 1 calc R U . . .
H10B H 0.440844 1.082400 0.497979 0.051 Uiso 1 1 calc R U . . .
H10C H 0.311722 1.012737 0.467738 0.051 Uiso 1 1 calc R U . . .
C11 C 0.0400(2) 0.70986(16) 0.17158(15) 0.0201(4) Uani 1 1 d . . . . .
H11 H 0.099121 0.672973 0.198415 0.024 Uiso 1 1 calc R U . . .
C12 C 0.0063(3) 0.65284(19) 0.07185(17) 0.0329(6) Uani 1 1 d . . . . .
H12A H -0.058371 0.683659 0.044400 0.049 Uiso 1 1 calc R U . . .
H12B H -0.024890 0.583616 0.057041 0.049 Uiso 1 1 calc R U . . .
H12C H 0.080252 0.654412 0.049692 0.049 Uiso 1 1 calc R U . . .
C13 C -0.0756(3) 0.7148(2) 0.2074(2) 0.0377(6) Uani 1 1 d . . . . .
H13A H -0.134629 0.751453 0.182567 0.057 Uiso 1 1 calc R U . . .
H13B H -0.051363 0.748883 0.272060 0.057 Uiso 1 1 calc R U . . .
H13C H -0.114814 0.647084 0.190413 0.057 Uiso 1 1 calc R U . . .
C14 C 0.4846(2) 0.62601(15) 0.39980(14) 0.0174(4) Uani 1 1 d . . . . .
C15 C 0.4426(2) 0.51583(16) 0.33918(16) 0.0258(5) Uani 1 1 d . . . . .
H15A H 0.442141 0.505128 0.278211 0.039 Uiso 1 1 calc R U . . .
H15B H 0.358554 0.497274 0.341639 0.039 Uiso 1 1 calc R U . . .
H15C H 0.500171 0.474713 0.358974 0.039 Uiso 1 1 calc R U . . .
C16 C 0.4820(2) 0.64336(18) 0.49458(15) 0.0262(5) Uani 1 1 d . . . . .
H16A H 0.397300 0.624999 0.495849 0.039 Uiso 1 1 calc R U . . .
H16B H 0.508536 0.713795 0.533189 0.039 Uiso 1 1 calc R U . . .
H16C H 0.538701 0.602385 0.515425 0.039 Uiso 1 1 calc R U . . .
C17 C 0.6180(2) 0.65398(18) 0.39942(16) 0.0240(5) Uani 1 1 d . . . . .
H17A H 0.621661 0.641738 0.338837 0.036 Uiso 1 1 calc R U . . .
H17B H 0.673673 0.613479 0.421761 0.036 Uiso 1 1 calc R U . . .
H17C H 0.644224 0.724619 0.437422 0.036 Uiso 1 1 calc R U . . .
C18 C 0.6172(2) 0.79591(19) 0.24122(18) 0.0292(5) Uani 1 1 d . . . . .
C19 C 0.3797(2) 0.79452(19) 0.11691(16) 0.0274(5) Uani 1 1 d . . . . .
C20 C 0.5592(3) 0.67940(19) 0.05238(18) 0.0306(6) Uani 1 1 d . . . . .
C21 C 0.3377(2) 0.58188(18) 0.05968(15) 0.0237(5) Uani 1 1 d . . . . .
C22 C 0.5705(2) 0.57796(19) 0.16362(16) 0.0273(5) Uani 1 1 d . . . . .
W1B W 0.76535(2) 0.17700(2) 0.16632(2) 0.01653(3) Uani 1 1 d . . . . .
P1B P 0.95569(5) 0.21210(4) 0.28371(3) 0.01324(10) Uani 1 1 d . . . . .
O1B O 0.91194(17) 0.07696(14) 0.02002(12) 0.0311(4) Uani 1 1 d . . . . .
O2B O 0.81014(19) 0.36284(14) 0.11789(13) 0.0382(5) Uani 1 1 d . . . . .
O3B O 0.50855(17) 0.12375(17) 0.02345(13) 0.0411(5) Uani 1 1 d . . . . .
O4B O 0.64391(18) 0.30339(17) 0.32258(13) 0.0444(5) Uani 1 1 d . . . . .
O5B O 0.6995(2) -0.03454(16) 0.16798(14) 0.0504(6) Uani 1 1 d . . . . .
N1B N 1.08982(15) 0.27948(13) 0.29938(11) 0.0139(3) Uani 1 1 d . . . . .
N2B N 1.17996(17) 0.28601(14) 0.37155(12) 0.0190(4) Uani 1 1 d . . . . .
N3B N 1.14016(17) 0.23631(14) 0.41211(12) 0.0190(4) Uani 1 1 d . . . . .
C01A C 1.16761(18) 0.31031(15) 0.18566(14) 0.0149(4) Uani 1 1 d . . . . .
C1B C 1.02104(19) 0.19123(15) 0.37624(13) 0.0146(4) Uani 1 1 d . . . . .
C2B C 1.11033(18) 0.34421(15) 0.25581(14) 0.0149(4) Uani 1 1 d . . . . .
C4B C 1.1825(2) 0.37464(16) 0.14461(14) 0.0178(4) Uani 1 1 d . . . . .
H4B H 1.220780 0.354243 0.096629 0.021 Uiso 1 1 calc R U . . .
C5B C 1.1424(2) 0.46796(17) 0.17283(15) 0.0215(4) Uani 1 1 d . . . . .
H5B H 1.151500 0.510220 0.143161 0.026 Uiso 1 1 calc R U . . .
C6B C 1.0891(2) 0.50003(16) 0.24388(16) 0.0218(5) Uani 1 1 d . . . . .
H6B H 1.063805 0.564823 0.263301 0.026 Uiso 1 1 calc R U . . .
C7B C 1.0719(2) 0.43886(16) 0.28744(15) 0.0194(4) Uani 1 1 d . . . . .
C8B C 1.2219(2) 0.21214(16) 0.16031(15) 0.0189(4) Uani 1 1 d . . . . .
H8B H 1.173228 0.166110 0.175956 0.023 Uiso 1 1 calc R U . . .
C9B C 1.3569(2) 0.22929(19) 0.21487(17) 0.0278(5) Uani 1 1 d . . . . .
H9BA H 1.390800 0.165408 0.201289 0.042 Uiso 1 1 calc R U . . .
H9BB H 1.359719 0.259681 0.278071 0.042 Uiso 1 1 calc R U . . .
H9BC H 1.406726 0.273740 0.200148 0.042 Uiso 1 1 calc R U . . .
C10B C 1.2161(2) 0.16186(18) 0.06203(16) 0.0270(5) Uani 1 1 d . . . . .
H10D H 1.129648 0.152112 0.027497 0.041 Uiso 1 1 calc R U . . .
H10E H 1.247549 0.097158 0.049463 0.041 Uiso 1 1 calc R U . . .
H10F H 1.267279 0.203954 0.045871 0.041 Uiso 1 1 calc R U . . .
C11B C 1.0211(2) 0.47815(16) 0.36889(16) 0.0235(5) Uani 1 1 d . . . . .
H11B H 1.000806 0.420277 0.383170 0.028 Uiso 1 1 calc R U . . .
C12B C 0.9018(3) 0.5261(2) 0.3545(2) 0.0372(6) Uani 1 1 d . . . . .
H12D H 0.918089 0.581743 0.338258 0.056 Uiso 1 1 calc R U . . .
H12E H 0.873882 0.550676 0.409268 0.056 Uiso 1 1 calc R U . . .
H12F H 0.836975 0.476542 0.306908 0.056 Uiso 1 1 calc R U . . .
C13B C 1.1217(3) 0.5504(2) 0.44746(17) 0.0344(6) Uani 1 1 d . . . . .
H13D H 1.193183 0.515453 0.459503 0.052 Uiso 1 1 calc R U . . .
H13E H 1.088253 0.576545 0.499743 0.052 Uiso 1 1 calc R U . . .
H13F H 1.148207 0.605596 0.433571 0.052 Uiso 1 1 calc R U . . .
C14B C 0.9648(2) 0.13405(15) 0.42031(14) 0.0166(4) Uani 1 1 d . . . . .
C15B C 0.8276(2) 0.14881(18) 0.41403(16) 0.0229(5) Uani 1 1 d . . . . .
H15D H 0.780989 0.121219 0.351691 0.034 Uiso 1 1 calc R U . . .
H15E H 0.820201 0.220081 0.440861 0.034 Uiso 1 1 calc R U . . .
H15F H 0.793837 0.114597 0.445516 0.034 Uiso 1 1 calc R U . . .
C16B C 1.0341(2) 0.1725(2) 0.51829(16) 0.0297(5) Uani 1 1 d . . . . .
H16D H 1.120912 0.159031 0.523512 0.045 Uiso 1 1 calc R U . . .
H16E H 0.994280 0.138702 0.547526 0.045 Uiso 1 1 calc R U . . .
H16F H 1.031516 0.244412 0.546546 0.045 Uiso 1 1 calc R U . . .
C17B C 0.9747(2) 0.02300(17) 0.37410(17) 0.0274(5) Uani 1 1 d . . . . .
H17D H 0.928408 -0.001325 0.311804 0.041 Uiso 1 1 calc R U . . .
H17E H 0.939611 -0.013733 0.403141 0.041 Uiso 1 1 calc R U . . .
H17F H 1.062344 0.012949 0.377764 0.041 Uiso 1 1 calc R U . . .
C18B C 0.8583(2) 0.11012(16) 0.07211(15) 0.0201(4) Uani 1 1 d . . . . .
C19B C 0.7972(2) 0.30043(18) 0.14076(16) 0.0254(5) Uani 1 1 d . . . . .
C20B C 0.6016(2) 0.1435(2) 0.07465(16) 0.0283(5) Uani 1 1 d . . . . .
C21B C 0.6837(2) 0.2562(2) 0.26549(16) 0.0283(5) Uani 1 1 d . . . . .
C22B C 0.7246(2) 0.0428(2) 0.17084(16) 0.0291(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
W1 C20 2.004(2) . ?
W1 C22 2.036(2) . ?
W1 C21 2.041(3) . ?
W1 C19 2.054(2) . ?
W1 C18 2.055(3) . ?
W1 P1 2.4512(5) . ?
P1 N1 1.6747(17) . ?
P1 C1 1.712(2) . ?
O1 C18 1.136(3) . ?
O2 C19 1.141(3) . ?
O3 C20 1.142(3) . ?
O4 C21 1.139(3) . ?
O5 C22 1.139(3) . ?
N1 N2 1.358(2) . ?
N1 C2 1.446(2) . ?
N2 N3 1.303(2) . ?
N3 C1 1.357(3) . ?
C1 C14 1.521(3) . ?
C2 C7 1.397(3) . ?
C2 C3 1.401(3) . ?
C3 C4 1.395(3) . ?
C3 C8 1.520(3) . ?
C4 C5 1.381(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(3) . ?
C6 H6 0.9500 . ?
C7 C11 1.519(3) . ?
C8 C9 1.528(4) . ?
C8 C10 1.530(3) . ?
C8 H8 1.0000 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C12 1.517(3) . ?
C11 C13 1.529(3) . ?
C11 H11 1.0000 . ?
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 C16 1.530(3) . ?
C14 C17 1.531(3) . ?
C14 C15 1.534(3) . ?
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 . ?
W1B C20B 2.015(2) . ?
W1B C18B 2.038(2) . ?
W1B C22B 2.040(3) . ?
W1B C19B 2.054(2) . ?
W1B C21B 2.055(3) . ?
W1B P1B 2.4398(5) . ?
P1B N1B 1.6783(17) . ?
P1B C1B 1.713(2) . ?
O1B C18B 1.135(3) . ?
O2B C19B 1.138(3) . ?
O3B C20B 1.137(3) . ?
O4B C21B 1.139(3) . ?
O5B C22B 1.140(3) . ?
N1B N2B 1.363(2) . ?
N1B C2B 1.447(2) . ?
N2B N3B 1.303(2) . ?
N3B C1B 1.359(3) . ?
C01A C4B 1.393(3) . ?
C01A C2B 1.400(3) . ?
C01A C8B 1.517(3) . ?
C1B C14B 1.519(3) . ?
C2B C7B 1.398(3) . ?
C4B C5B 1.386(3) . ?
C4B H4B 0.9500 . ?
C5B C6B 1.383(3) . ?
C5B H5B 0.9500 . ?
C6B C7B 1.393(3) . ?
C6B H6B 0.9500 . ?
C7B C11B 1.517(3) . ?
C8B C10B 1.522(3) . ?
C8B C9B 1.532(3) . ?
C8B H8B 1.0000 . ?
C9B H9BA 0.9800 . ?
C9B H9BB 0.9800 . ?
C9B H9BC 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11B C13B 1.527(4) . ?
C11B C12B 1.529(4) . ?
C11B H11B 1.0000 . ?
C12B H12D 0.9800 . ?
C12B H12E 0.9800 . ?
C12B H12F 0.9800 . ?
C13B H13D 0.9800 . ?
C13B H13E 0.9800 . ?
C13B H13F 0.9800 . ?
C14B C15B 1.530(3) . ?
C14B C17B 1.530(3) . ?
C14B C16B 1.531(3) . ?
C15B H15D 0.9800 . ?
C15B H15E 0.9800 . ?
C15B H15F 0.9800 . ?
C16B H16D 0.9800 . ?
C16B H16E 0.9800 . ?
C16B H16F 0.9800 . ?
C17B H17D 0.9800 . ?
C17B H17E 0.9800 . ?
C17B H17F 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
C20 W1 C22 87.47(10) . . ?
C20 W1 C21 90.20(10) . . ?
C22 W1 C21 86.58(10) . . ?
C20 W1 C19 86.51(10) . . ?
C22 W1 C19 172.66(9) . . ?
C21 W1 C19 89.25(10) . . ?
C20 W1 C18 90.89(11) . . ?
C22 W1 C18 91.52(10) . . ?
C21 W1 C18 177.76(9) . . ?
C19 W1 C18 92.77(10) . . ?
C20 W1 P1 176.17(8) . . ?
C22 W1 P1 93.24(7) . . ?
C21 W1 P1 93.60(6) . . ?
C19 W1 P1 93.04(6) . . ?
C18 W1 P1 85.33(7) . . ?
N1 P1 C1 88.67(9) . . ?
N1 P1 W1 126.61(6) . . ?
C1 P1 W1 144.14(7) . . ?
N2 N1 C2 117.28(16) . . ?
N2 N1 P1 114.45(13) . . ?
C2 N1 P1 128.07(14) . . ?
N3 N2 N1 110.82(16) . . ?
N2 N3 C1 115.31(17) . . ?
N3 C1 C14 120.26(18) . . ?
N3 C1 P1 110.73(15) . . ?
C14 C1 P1 129.01(16) . . ?
C7 C2 C3 122.98(18) . . ?
C7 C2 N1 119.01(18) . . ?
C3 C2 N1 118.00(18) . . ?
C4 C3 C2 117.15(19) . . ?
C4 C3 C8 120.20(19) . . ?
C2 C3 C8 122.63(18) . . ?
C5 C4 C3 121.0(2) . . ?
C5 C4 H4 119.5 . . ?
C3 C4 H4 119.5 . . ?
C4 C5 C6 120.5(2) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C5 C6 C7 120.8(2) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C6 C7 C2 117.57(19) . . ?
C6 C7 C11 119.86(19) . . ?
C2 C7 C11 122.56(18) . . ?
C3 C8 C9 112.6(2) . . ?
C3 C8 C10 109.34(19) . . ?
C9 C8 C10 110.9(2) . . ?
C3 C8 H8 107.9 . . ?
C9 C8 H8 107.9 . . ?
C10 C8 H8 107.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C7 111.71(19) . . ?
C12 C11 C13 110.7(2) . . ?
C7 C11 C13 110.46(19) . . ?
C12 C11 H11 108.0 . . ?
C7 C11 H11 108.0 . . ?
C13 C11 H11 108.0 . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1 C14 C16 110.24(18) . . ?
C1 C14 C17 109.47(17) . . ?
C16 C14 C17 108.44(19) . . ?
C1 C14 C15 109.54(18) . . ?
C16 C14 C15 109.53(19) . . ?
C17 C14 C15 109.59(19) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O1 C18 W1 177.6(2) . . ?
O2 C19 W1 174.3(2) . . ?
O3 C20 W1 179.5(3) . . ?
O4 C21 W1 177.6(2) . . ?
O5 C22 W1 176.2(2) . . ?
C20B W1B C18B 91.86(9) . . ?
C20B W1B C22B 85.82(10) . . ?
C18B W1B C22B 89.66(10) . . ?
C20B W1B C19B 87.78(10) . . ?
C18B W1B C19B 84.33(9) . . ?
C22B W1B C19B 171.08(10) . . ?
C20B W1B C21B 91.43(10) . . ?
C18B W1B C21B 174.55(9) . . ?
C22B W1B C21B 94.91(11) . . ?
C19B W1B C21B 91.46(10) . . ?
C20B W1B P1B 175.53(7) . . ?
C18B W1B P1B 91.02(6) . . ?
C22B W1B P1B 90.78(7) . . ?
C19B W1B P1B 95.91(7) . . ?
C21B W1B P1B 85.96(6) . . ?
N1B P1B C1B 88.79(9) . . ?
N1B P1B W1B 128.04(6) . . ?
C1B P1B W1B 143.17(7) . . ?
N2B N1B C2B 117.66(16) . . ?
N2B N1B P1B 114.37(13) . . ?
C2B N1B P1B 126.86(14) . . ?
N3B N2B N1B 110.57(17) . . ?
N2B N3B C1B 115.71(17) . . ?
C4B C01A C2B 117.06(19) . . ?
C4B C01A C8B 120.83(19) . . ?
C2B C01A C8B 121.89(18) . . ?
N3B C1B C14B 119.68(18) . . ?
N3B C1B P1B 110.55(15) . . ?
C14B C1B P1B 129.76(15) . . ?
C7B C2B C01A 123.46(18) . . ?
C7B C2B N1B 117.21(18) . . ?
C01A C2B N1B 119.33(18) . . ?
C5B C4B C01A 120.9(2) . . ?
C5B C4B H4B 119.6 . . ?
C01A C4B H4B 119.6 . . ?
C6B C5B C4B 120.5(2) . . ?
C6B C5B H5B 119.8 . . ?
C4B C5B H5B 119.8 . . ?
C5B C6B C7B 121.1(2) . . ?
C5B C6B H6B 119.5 . . ?
C7B C6B H6B 119.5 . . ?
C6B C7B C2B 117.0(2) . . ?
C6B C7B C11B 120.05(19) . . ?
C2B C7B C11B 122.85(19) . . ?
C01A C8B C10B 113.57(18) . . ?
C01A C8B C9B 109.20(18) . . ?
C10B C8B C9B 109.89(19) . . ?
C01A C8B H8B 108.0 . . ?
C10B C8B H8B 108.0 . . ?
C9B C8B H8B 108.0 . . ?
C8B C9B H9BA 109.5 . . ?
C8B C9B H9BB 109.5 . . ?
H9BA C9B H9BB 109.5 . . ?
C8B C9B H9BC 109.5 . . ?
H9BA C9B H9BC 109.5 . . ?
H9BB C9B H9BC 109.5 . . ?
C8B C10B H10D 109.5 . . ?
C8B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C8B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C7B C11B C13B 109.63(19) . . ?
C7B C11B C12B 113.0(2) . . ?
C13B C11B C12B 111.3(2) . . ?
C7B C11B H11B 107.6 . . ?
C13B C11B H11B 107.6 . . ?
C12B C11B H11B 107.6 . . ?
C11B C12B H12D 109.5 . . ?
C11B C12B H12E 109.5 . . ?
H12D C12B H12E 109.5 . . ?
C11B C12B H12F 109.5 . . ?
H12D C12B H12F 109.5 . . ?
H12E C12B H12F 109.5 . . ?
C11B C13B H13D 109.5 . . ?
C11B C13B H13E 109.5 . . ?
H13D C13B H13E 109.5 . . ?
C11B C13B H13F 109.5 . . ?
H13D C13B H13F 109.5 . . ?
H13E C13B H13F 109.5 . . ?
C1B C14B C15B 110.37(17) . . ?
C1B C14B C17B 109.49(17) . . ?
C15B C14B C17B 108.99(18) . . ?
C1B C14B C16B 109.55(18) . . ?
C15B C14B C16B 108.41(19) . . ?
C17B C14B C16B 110.03(19) . . ?
C14B C15B H15D 109.5 . . ?
C14B C15B H15E 109.5 . . ?
H15D C15B H15E 109.5 . . ?
C14B C15B H15F 109.5 . . ?
H15D C15B H15F 109.5 . . ?
H15E C15B H15F 109.5 . . ?
C14B C16B H16D 109.5 . . ?
C14B C16B H16E 109.5 . . ?
H16D C16B H16E 109.5 . . ?
C14B C16B H16F 109.5 . . ?
H16D C16B H16F 109.5 . . ?
H16E C16B H16F 109.5 . . ?
C14B C17B H17D 109.5 . . ?
C14B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
C14B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?
O1B C18B W1B 177.0(2) . . ?
O2B C19B W1B 173.1(2) . . ?
O3B C20B W1B 179.0(2) . . ?
O4B C21B W1B 176.5(2) . . ?
O5B C22B W1B 175.9(2) . . ?

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
C1 P1 N1 N2 -0.93(15) . . . . ?
W1 P1 N1 N2 -174.00(11) . . . . ?
C1 P1 N1 C2 173.70(18) . . . . ?
W1 P1 N1 C2 0.6(2) . . . . ?
C2 N1 N2 N3 -174.85(18) . . . . ?
P1 N1 N2 N3 0.4(2) . . . . ?
N1 N2 N3 C1 0.6(3) . . . . ?
N2 N3 C1 C14 178.52(18) . . . . ?
N2 N3 C1 P1 -1.3(2) . . . . ?
N1 P1 C1 N3 1.20(16) . . . . ?
W1 P1 C1 N3 171.69(10) . . . . ?
N1 P1 C1 C14 -178.6(2) . . . . ?
W1 P1 C1 C14 -8.1(3) . . . . ?
N2 N1 C2 C7 -92.8(2) . . . . ?
P1 N1 C2 C7 92.7(2) . . . . ?
N2 N1 C2 C3 86.3(2) . . . . ?
P1 N1 C2 C3 -88.1(2) . . . . ?
C7 C2 C3 C4 -1.0(3) . . . . ?
N1 C2 C3 C4 179.80(18) . . . . ?
C7 C2 C3 C8 177.1(2) . . . . ?
N1 C2 C3 C8 -2.0(3) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C8 C3 C4 C5 -178.3(2) . . . . ?
C3 C4 C5 C6 0.9(3) . . . . ?
C4 C5 C6 C7 -0.7(3) . . . . ?
C5 C6 C7 C2 -0.3(3) . . . . ?
C5 C6 C7 C11 178.5(2) . . . . ?
C3 C2 C7 C6 1.2(3) . . . . ?
N1 C2 C7 C6 -179.63(18) . . . . ?
C3 C2 C7 C11 -177.6(2) . . . . ?
N1 C2 C7 C11 1.6(3) . . . . ?
C4 C3 C8 C9 -45.2(3) . . . . ?
C2 C3 C8 C9 136.7(2) . . . . ?
C4 C3 C8 C10 78.6(3) . . . . ?
C2 C3 C8 C10 -99.5(2) . . . . ?
C6 C7 C11 C12 52.4(3) . . . . ?
C2 C7 C11 C12 -128.8(2) . . . . ?
C6 C7 C11 C13 -71.2(3) . . . . ?
C2 C7 C11 C13 107.6(2) . . . . ?
N3 C1 C14 C16 -10.6(3) . . . . ?
P1 C1 C14 C16 169.14(17) . . . . ?
N3 C1 C14 C17 -129.8(2) . . . . ?
P1 C1 C14 C17 49.9(3) . . . . ?
N3 C1 C14 C15 110.0(2) . . . . ?
P1 C1 C14 C15 -70.3(2) . . . . ?
C1B P1B N1B N2B -0.11(16) . . . . ?
W1B P1B N1B N2B 179.79(11) . . . . ?
C1B P1B N1B C2B -167.69(18) . . . . ?
W1B P1B N1B C2B 12.2(2) . . . . ?
C2B N1B N2B N3B 169.39(18) . . . . ?
P1B N1B N2B N3B 0.6(2) . . . . ?
N1B N2B N3B C1B -0.9(3) . . . . ?
N2B N3B C1B C14B -178.19(18) . . . . ?
N2B N3B C1B P1B 0.8(2) . . . . ?
N1B P1B C1B N3B -0.38(16) . . . . ?
W1B P1B C1B N3B 179.74(10) . . . . ?
N1B P1B C1B C14B 178.5(2) . . . . ?
W1B P1B C1B C14B -1.4(3) . . . . ?
C4B C01A C2B C7B -2.0(3) . . . . ?
C8B C01A C2B C7B 172.6(2) . . . . ?
C4B C01A C2B N1B 178.53(18) . . . . ?
C8B C01A C2B N1B -6.9(3) . . . . ?
N2B N1B C2B C7B -87.7(2) . . . . ?
P1B N1B C2B C7B 79.5(2) . . . . ?
N2B N1B C2B C01A 91.7(2) . . . . ?
P1B N1B C2B C01A -101.0(2) . . . . ?
C2B C01A C4B C5B 0.2(3) . . . . ?
C8B C01A C4B C5B -174.4(2) . . . . ?
C01A C4B C5B C6B 1.5(3) . . . . ?
C4B C5B C6B C7B -1.5(4) . . . . ?
C5B C6B C7B C2B -0.3(3) . . . . ?
C5B C6B C7B C11B 176.0(2) . . . . ?
C01A C2B C7B C6B 2.0(3) . . . . ?
N1B C2B C7B C6B -178.49(19) . . . . ?
C01A C2B C7B C11B -174.1(2) . . . . ?
N1B C2B C7B C11B 5.4(3) . . . . ?
C4B C01A C8B C10B -36.5(3) . . . . ?
C2B C01A C8B C10B 149.1(2) . . . . ?
C4B C01A C8B C9B 86.5(2) . . . . ?
C2B C01A C8B C9B -87.8(2) . . . . ?
C6B C7B C11B C13B -73.8(3) . . . . ?
C2B C7B C11B C13B 102.2(3) . . . . ?
C6B C7B C11B C12B 51.0(3) . . . . ?
C2B C7B C11B C12B -133.0(2) . . . . ?
N3B C1B C14B C15B 142.7(2) . . . . ?
P1B C1B C14B C15B -36.1(3) . . . . ?
N3B C1B C14B C17B -97.3(2) . . . . ?
P1B C1B C14B C17B 83.9(2) . . . . ?
N3B C1B C14B C16B 23.4(3) . . . . ?
P1B C1B C14B C16B -155.40(18) . . . . ?

_refine_diff_density_max         1.151
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.087

