#------------------------------------------------------------------------------
#$Date: 2022-03-05 00:15:00 +0200 (Sat, 05 Mar 2022) $
#$Revision: 273373 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/94/7709415.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7709415
loop_
_publ_author_name
'Schmer, Alexander'
'García Alcaraz, Antonio'
'Kyri, Andreas Wolfgang'
'Schnakenburg, Gregor'
'Espinosa Ferao, Arturo'
'Streubel, Rainer'
_publ_section_title
;
 Synthesis of azadiphosphiridine complexes. Theoretical studies on ring
 formation, the P-to-P' metal shift and the resulting nitrogen geometry.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3275
_journal_page_last               3279
_journal_paper_doi               10.1039/d1dt04252a
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C33 H36 N2 O5 P2 W'
_chemical_formula_sum            'C33 H36 N2 O5 P2 W'
_chemical_formula_weight         786.43
_chemical_name_systematic        AS-241
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2021-06-23 deposited with the CCDC.	2022-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                100.746(4)
_cell_angle_beta                 90.409(3)
_cell_angle_gamma                97.893(4)
_cell_formula_units_Z            4
_cell_length_a                   10.5675(6)
_cell_length_b                   16.9702(11)
_cell_length_c                   18.6599(10)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.27
_cell_volume                     3254.7(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8-KappaApexII'
_diffrn_measurement_method       'fine slicing ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0979
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            139084
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.999
_diffrn_reflns_theta_min         1.810
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6152
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1036 before and 0.0743 after correction. The Ratio of minimum to maximum transmission is 0.8246. The λ/2 correction factor is 0.00150.'
_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    1.605
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.312
_refine_diff_density_min         -1.521
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         15651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0352
_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)+(0.0207P)²+4.7752P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11791
_reflns_number_total             15651
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt04252a2.cif
_cod_data_source_block           5575f
_cod_depositor_comments
'Adding full bibliography for 7709415--7709416.cif.'
_cod_database_code               7709415
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.732
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C26(H26), C20'(H20'), C23'(H23'), C26'(H26')
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C3'(H3'), C4'(H4'),
  C5'(H5'), C6'(H6'), C7'(H7'), C9'(H9'), C10'(H10'), C11'(H11'), C12'(H12'),
 C13'(H13'), C15'(H15'), C16'(H16'), C17'(H17'), C18'(H18'), C19'(H19')
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C21'(H21D,H21E,H21F),
 C22'(H22D,H22E,H22F), C24'(H24D,H24E,H24F), C25'(H25D,H25E,H25F), C27'(H27D,
 H27E,H27F), C28'(H28D,H28E,H28F)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.67063(2) 0.67577(2) 0.97937(2) 0.01861(5) Uani 1 1 d . . . . .
P1 P 0.88248(10) 0.74255(7) 0.93202(6) 0.0180(2) Uani 1 1 d . . . . .
P2 P 1.07865(10) 0.78127(7) 0.98946(6) 0.0207(2) Uani 1 1 d . . . . .
O1 O 0.4299(3) 0.5956(2) 1.04955(17) 0.0347(8) Uani 1 1 d . . . . .
O2 O 0.5824(4) 0.5369(2) 0.84218(19) 0.0480(10) Uani 1 1 d . . . . .
O3 O 0.4753(3) 0.7746(2) 0.91671(18) 0.0334(8) Uani 1 1 d . . . . .
O4 O 0.7115(3) 0.8192(2) 1.11685(17) 0.0367(8) Uani 1 1 d . . . . .
O5 O 0.7917(3) 0.5414(2) 1.0435(2) 0.0498(10) Uani 1 1 d . . . . .
N1 N 1.0166(3) 0.6972(2) 0.92901(17) 0.0213(8) Uani 1 1 d . . . . .
N2 N 1.0997(3) 0.7535(2) 1.06953(18) 0.0226(8) Uani 1 1 d . . . . .
C1 C 0.8801(4) 0.8014(2) 0.8505(2) 0.0159(8) Uani 1 1 d . . . . .
C2 C 0.8451(4) 0.7397(2) 0.7792(2) 0.0171(8) Uani 1 1 d . . . . .
C3 C 0.9233(4) 0.7318(3) 0.7190(2) 0.0241(10) Uani 1 1 d . . . . .
H3 H 1.0030 0.7659 0.7212 0.029 Uiso 1 1 calc R . . . .
C4 C 0.8870(5) 0.6753(3) 0.6561(2) 0.0310(11) Uani 1 1 d . . . . .
H4 H 0.9426 0.6708 0.6162 0.037 Uiso 1 1 calc R . . . .
C5 C 0.7725(5) 0.6260(3) 0.6507(2) 0.0278(10) Uani 1 1 d . . . . .
H5 H 0.7488 0.5868 0.6076 0.033 Uiso 1 1 calc R . . . .
C6 C 0.6917(4) 0.6340(3) 0.7086(2) 0.0286(10) Uani 1 1 d . . . . .
H6 H 0.6112 0.6006 0.7053 0.034 Uiso 1 1 calc R . . . .
C7 C 0.7281(4) 0.6904(3) 0.7713(2) 0.0234(10) Uani 1 1 d . . . . .
H7 H 0.6708 0.6956 0.8104 0.028 Uiso 1 1 calc R . . . .
C8 C 1.0103(4) 0.8533(3) 0.8469(2) 0.0197(9) Uani 1 1 d . . . . .
C9 C 1.0208(4) 0.9367(3) 0.8538(2) 0.0251(10) Uani 1 1 d . . . . .
H9 H 0.9462 0.9622 0.8621 0.030 Uiso 1 1 calc R . . . .
C10 C 1.1372(4) 0.9839(3) 0.8490(2) 0.0315(11) Uani 1 1 d . . . . .
H10 H 1.1409 1.0409 0.8536 0.038 Uiso 1 1 calc R . . . .
C11 C 1.2478(4) 0.9491(3) 0.8375(2) 0.0296(11) Uani 1 1 d . . . . .
H11 H 1.3278 0.9816 0.8351 0.036 Uiso 1 1 calc R . . . .
C12 C 1.2399(4) 0.8662(3) 0.8296(2) 0.0304(11) Uani 1 1 d . . . . .
H12 H 1.3149 0.8411 0.8214 0.036 Uiso 1 1 calc R . . . .
C13 C 1.1232(4) 0.8193(3) 0.8337(2) 0.0222(9) Uani 1 1 d . . . . .
H13 H 1.1196 0.7621 0.8274 0.027 Uiso 1 1 calc R . . . .
C14 C 0.7764(4) 0.8561(2) 0.8698(2) 0.0168(8) Uani 1 1 d . . . . .
C15 C 0.6911(4) 0.8692(2) 0.8175(2) 0.0185(9) Uani 1 1 d . . . . .
H15 H 0.6940 0.8417 0.7684 0.022 Uiso 1 1 calc R . . . .
C16 C 0.6020(4) 0.9217(3) 0.8358(2) 0.0248(10) Uani 1 1 d . . . . .
H16 H 0.5444 0.9299 0.7994 0.030 Uiso 1 1 calc R . . . .
C17 C 0.5966(4) 0.9622(3) 0.9070(2) 0.0244(10) Uani 1 1 d . . . . .
H17 H 0.5339 0.9971 0.9197 0.029 Uiso 1 1 calc R . . . .
C18 C 0.6823(4) 0.9521(3) 0.9600(2) 0.0253(10) Uani 1 1 d . . . . .
H18 H 0.6801 0.9809 1.0087 0.030 Uiso 1 1 calc R . . . .
C19 C 0.7719(4) 0.8993(3) 0.9410(2) 0.0222(9) Uani 1 1 d . . . . .
H19 H 0.8309 0.8924 0.9773 0.027 Uiso 1 1 calc R . . . .
C20 C 1.0573(4) 0.6182(3) 0.8990(2) 0.0240(10) Uani 1 1 d . . . . .
H20 H 1.0307 0.5807 0.9333 0.029 Uiso 1 1 calc R . . . .
C21 C 1.2017(4) 0.6287(3) 0.8968(3) 0.0300(11) Uani 1 1 d . . . . .
H21A H 1.2305 0.6658 0.8640 0.045 Uiso 1 1 calc GR . . . .
H21B H 1.2297 0.5760 0.8790 0.045 Uiso 1 1 calc GR . . . .
H21C H 1.2383 0.6509 0.9460 0.045 Uiso 1 1 calc GR . . . .
C22 C 0.9920(4) 0.5820(3) 0.8259(2) 0.0294(11) Uani 1 1 d . . . . .
H22A H 0.8991 0.5779 0.8307 0.044 Uiso 1 1 calc GR . . . .
H22B H 1.0153 0.5278 0.8089 0.044 Uiso 1 1 calc GR . . . .
H22C H 1.0190 0.6166 0.7906 0.044 Uiso 1 1 calc GR . . . .
C23 C 1.1917(4) 0.8088(3) 1.1235(2) 0.0269(10) Uani 1 1 d . . . . .
H23 H 1.1982 0.7822 1.1666 0.032 Uiso 1 1 calc R . . . .
C24 C 1.3256(4) 0.8192(3) 1.0918(2) 0.0303(11) Uani 1 1 d . . . . .
H24A H 1.3530 0.7659 1.0763 0.045 Uiso 1 1 calc GR . . . .
H24B H 1.3862 0.8523 1.1292 0.045 Uiso 1 1 calc GR . . . .
H24C H 1.3231 0.8460 1.0497 0.045 Uiso 1 1 calc GR . . . .
C25 C 1.1451(5) 0.8899(3) 1.1506(3) 0.0374(12) Uani 1 1 d . . . . .
H25A H 1.1398 0.9183 1.1098 0.056 Uiso 1 1 calc GR . . . .
H25B H 1.2052 0.9228 1.1884 0.056 Uiso 1 1 calc GR . . . .
H25C H 1.0604 0.8806 1.1711 0.056 Uiso 1 1 calc GR . . . .
C26 C 1.0356(4) 0.6802(3) 1.0927(2) 0.0258(10) Uani 1 1 d . . . . .
H26 H 0.9734 0.6517 1.0525 0.031 Uiso 1 1 calc R . . . .
C27 C 1.1276(4) 0.6218(3) 1.1029(3) 0.0338(11) Uani 1 1 d . . . . .
H27A H 1.1741 0.6086 1.0579 0.051 Uiso 1 1 calc GR . . . .
H27B H 1.0798 0.5721 1.1140 0.051 Uiso 1 1 calc GR . . . .
H27C H 1.1885 0.6469 1.1432 0.051 Uiso 1 1 calc GR . . . .
C28 C 0.9584(4) 0.7004(3) 1.1609(2) 0.0362(12) Uani 1 1 d . . . . .
H28A H 1.0166 0.7265 1.2023 0.054 Uiso 1 1 calc GR . . . .
H28B H 0.9107 0.6505 1.1717 0.054 Uiso 1 1 calc GR . . . .
H28C H 0.8985 0.7373 1.1525 0.054 Uiso 1 1 calc GR . . . .
C29 C 0.5181(4) 0.6257(3) 1.0240(2) 0.0239(10) Uani 1 1 d . . . . .
C30 C 0.6206(4) 0.5872(3) 0.8898(3) 0.0288(11) Uani 1 1 d . . . . .
C31 C 0.5531(4) 0.7431(3) 0.9377(2) 0.0216(9) Uani 1 1 d . . . . .
C32 C 0.7015(4) 0.7671(3) 1.0684(2) 0.0239(10) Uani 1 1 d . . . . .
C33 C 0.7564(4) 0.5933(3) 1.0205(3) 0.0325(11) Uani 1 1 d . . . . .
W' W 0.83595(2) 0.32339(2) 0.60785(2) 0.01746(5) Uani 1 1 d . . . . .
P1' P 0.62071(10) 0.26063(7) 0.53675(5) 0.0161(2) Uani 1 1 d . . . . .
P2' P 0.42308(10) 0.21803(7) 0.57590(5) 0.0169(2) Uani 1 1 d . . . . .
O1' O 1.0888(3) 0.40191(19) 0.69657(16) 0.0292(7) Uani 1 1 d . . . . .
O2' O 0.8812(3) 0.48198(19) 0.53813(17) 0.0324(8) Uani 1 1 d . . . . .
O3' O 1.0241(3) 0.2362(2) 0.49718(16) 0.0307(8) Uani 1 1 d . . . . .
O4' O 0.8124(3) 0.16757(19) 0.68214(17) 0.0306(7) Uani 1 1 d . . . . .
O5' O 0.7263(3) 0.4393(2) 0.73919(17) 0.0319(8) Uani 1 1 d . . . . .
N1' N 0.4874(3) 0.3056(2) 0.55174(17) 0.0171(7) Uani 1 1 d . . . . .
N2' N 0.4002(3) 0.2380(2) 0.66533(17) 0.0180(7) Uani 1 1 d . . . . .
C1' C 0.6216(4) 0.2099(2) 0.4328(2) 0.0154(8) Uani 1 1 d . . . . .
C2' C 0.6515(4) 0.2742(2) 0.3846(2) 0.0172(8) Uani 1 1 d . . . . .
C3' C 0.5909(4) 0.2704(3) 0.3185(2) 0.0378(13) Uani 1 1 d . . . . .
H3' H 0.5245 0.2270 0.3015 0.045 Uiso 1 1 calc R . . . .
C4' C 0.6241(5) 0.3285(4) 0.2758(3) 0.0468(15) Uani 1 1 d . . . . .
H4' H 0.5802 0.3237 0.2303 0.056 Uiso 1 1 calc R . . . .
C5' C 0.7173(5) 0.3914(3) 0.2975(3) 0.0334(12) Uani 1 1 d . . . . .
H5' H 0.7363 0.4323 0.2691 0.040 Uiso 1 1 calc R . . . .
C6' C 0.7841(6) 0.3947(3) 0.3618(3) 0.0511(16) Uani 1 1 d . . . . .
H6' H 0.8532 0.4367 0.3771 0.061 Uiso 1 1 calc R . . . .
C7' C 0.7510(5) 0.3370(3) 0.4041(3) 0.0446(15) Uani 1 1 d . . . . .
H7' H 0.7982 0.3405 0.4483 0.054 Uiso 1 1 calc R . . . .
C8' C 0.4904(4) 0.1587(2) 0.4101(2) 0.0160(8) Uani 1 1 d . . . . .
C9' C 0.4759(4) 0.0749(3) 0.3915(2) 0.0230(9) Uani 1 1 d . . . . .
H9' H 0.5483 0.0479 0.3943 0.028 Uiso 1 1 calc R . . . .
C10' C 0.3591(4) 0.0296(3) 0.3691(2) 0.0290(10) Uani 1 1 d . . . . .
H10' H 0.3521 -0.0277 0.3564 0.035 Uiso 1 1 calc R . . . .
C11' C 0.2514(4) 0.0676(3) 0.3650(2) 0.0257(10) Uani 1 1 d . . . . .
H11' H 0.1709 0.0367 0.3493 0.031 Uiso 1 1 calc R . . . .
C12' C 0.2636(4) 0.1506(3) 0.3842(2) 0.0232(10) Uani 1 1 d . . . . .
H12' H 0.1902 0.1770 0.3829 0.028 Uiso 1 1 calc R . . . .
C13' C 0.3805(4) 0.1959(3) 0.4054(2) 0.0205(9) Uani 1 1 d . . . . .
H13' H 0.3870 0.2533 0.4171 0.025 Uiso 1 1 calc R . . . .
C14' C 0.7254(4) 0.1555(2) 0.4296(2) 0.0175(9) Uani 1 1 d . . . . .
C15' C 0.8089(4) 0.1475(3) 0.3714(2) 0.0197(9) Uani 1 1 d . . . . .
H15' H 0.8045 0.1788 0.3345 0.024 Uiso 1 1 calc R . . . .
C16' C 0.8978(4) 0.0941(3) 0.3676(2) 0.0239(10) Uani 1 1 d . . . . .
H16' H 0.9532 0.0890 0.3276 0.029 Uiso 1 1 calc R . . . .
C17' C 0.9076(4) 0.0482(3) 0.4204(2) 0.0244(10) Uani 1 1 d . . . . .
H17' H 0.9703 0.0127 0.4175 0.029 Uiso 1 1 calc R . . . .
C18' C 0.8252(4) 0.0544(3) 0.4779(2) 0.0226(9) Uani 1 1 d . . . . .
H18' H 0.8300 0.0226 0.5143 0.027 Uiso 1 1 calc R . . . .
C19' C 0.7353(4) 0.1075(3) 0.4819(2) 0.0201(9) Uani 1 1 d . . . . .
H19' H 0.6789 0.1112 0.5214 0.024 Uiso 1 1 calc R . . . .
C20' C 0.4390(4) 0.3776(2) 0.5346(2) 0.0187(9) Uani 1 1 d . . . . .
H20' H 0.4570 0.3807 0.4826 0.022 Uiso 1 1 calc R . . . .
C21' C 0.2960(4) 0.3694(3) 0.5436(2) 0.0245(10) Uani 1 1 d . . . . .
H21D H 0.2549 0.3200 0.5114 0.037 Uiso 1 1 calc GR . . . .
H21E H 0.2635 0.4166 0.5308 0.037 Uiso 1 1 calc GR . . . .
H21F H 0.2768 0.3663 0.5944 0.037 Uiso 1 1 calc GR . . . .
C22' C 0.5062(4) 0.4543(3) 0.5833(2) 0.0273(10) Uani 1 1 d . . . . .
H22D H 0.4884 0.4524 0.6344 0.041 Uiso 1 1 calc GR . . . .
H22E H 0.4750 0.5017 0.5702 0.041 Uiso 1 1 calc GR . . . .
H22F H 0.5986 0.4581 0.5765 0.041 Uiso 1 1 calc GR . . . .
C23' C 0.3084(4) 0.1780(3) 0.6944(2) 0.0221(9) Uani 1 1 d . . . . .
H23' H 0.3052 0.1979 0.7482 0.027 Uiso 1 1 calc R . . . .
C24' C 0.1737(4) 0.1725(3) 0.6626(2) 0.0288(10) Uani 1 1 d . . . . .
H24D H 0.1495 0.2269 0.6682 0.043 Uiso 1 1 calc GR . . . .
H24E H 0.1139 0.1391 0.6885 0.043 Uiso 1 1 calc GR . . . .
H24F H 0.1712 0.1478 0.6107 0.043 Uiso 1 1 calc GR . . . .
C25' C 0.3535(4) 0.0946(3) 0.6837(3) 0.0304(11) Uani 1 1 d . . . . .
H25D H 0.3573 0.0729 0.6314 0.046 Uiso 1 1 calc GR . . . .
H25E H 0.2934 0.0578 0.7060 0.046 Uiso 1 1 calc GR . . . .
H25F H 0.4386 0.0999 0.7068 0.046 Uiso 1 1 calc GR . . . .
C26' C 0.4672(4) 0.3057(3) 0.7196(2) 0.0206(9) Uani 1 1 d . . . . .
H26' H 0.5263 0.3399 0.6924 0.025 Uiso 1 1 calc R . . . .
C27' C 0.3753(4) 0.3594(3) 0.7592(2) 0.0266(10) Uani 1 1 d . . . . .
H27D H 0.3212 0.3758 0.7233 0.040 Uiso 1 1 calc GR . . . .
H27E H 0.4242 0.4077 0.7892 0.040 Uiso 1 1 calc GR . . . .
H27F H 0.3216 0.3294 0.7905 0.040 Uiso 1 1 calc GR . . . .
C28' C 0.5488(4) 0.2756(3) 0.7735(2) 0.0295(11) Uani 1 1 d . . . . .
H28D H 0.4934 0.2437 0.8027 0.044 Uiso 1 1 calc GR . . . .
H28E H 0.5979 0.3221 0.8058 0.044 Uiso 1 1 calc GR . . . .
H28F H 0.6076 0.2418 0.7468 0.044 Uiso 1 1 calc GR . . . .
C29' C 0.9964(4) 0.3712(3) 0.6639(2) 0.0219(9) Uani 1 1 d . . . . .
C30' C 0.8609(4) 0.4237(3) 0.5611(2) 0.0248(10) Uani 1 1 d . . . . .
C31' C 0.9491(4) 0.2646(3) 0.5332(2) 0.0237(10) Uani 1 1 d . . . . .
C32' C 0.8177(4) 0.2234(3) 0.6557(2) 0.0233(10) Uani 1 1 d . . . . .
C33' C 0.7561(4) 0.3940(3) 0.6913(2) 0.0223(9) Uani 1 1 d . . . . .
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'
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
C29 W P1 174.73(12) . . ?
C29 W C30 85.79(18) . . ?
C29 W C31 87.35(17) . . ?
C29 W C32 90.56(17) . . ?
C29 W C33 82.74(18) . . ?
C30 W P1 97.98(13) . . ?
C31 W P1 96.47(12) . . ?
C31 W C30 87.47(18) . . ?
C31 W C32 87.59(17) . . ?
C32 W P1 85.99(12) . . ?
C32 W C30 173.98(18) . . ?
C33 W P1 93.75(13) . . ?
C33 W C30 86.94(19) . . ?
C33 W C31 168.95(17) . . ?
C33 W C32 97.35(19) . . ?
P2 P1 W 129.64(5) . . ?
N1 P1 W 120.71(13) . . ?
N1 P1 P2 47.65(12) . . ?
N1 P1 C1 109.33(17) . . ?
C1 P1 W 120.77(12) . . ?
C1 P1 P2 106.79(13) . . ?
N1 P2 P1 47.85(12) . . ?
N2 P2 P1 117.38(13) . . ?
N2 P2 N1 107.46(18) . . ?
P2 N1 P1 84.50(17) . . ?
C20 N1 P1 138.9(3) . . ?
C20 N1 P2 135.9(3) . . ?
C23 N2 P2 116.9(3) . . ?
C26 N2 P2 126.7(3) . . ?
C26 N2 C23 116.5(3) . . ?
C2 C1 P1 108.9(3) . . ?
C8 C1 P1 110.0(3) . . ?
C8 C1 C2 111.9(3) . . ?
C14 C1 P1 104.2(2) . . ?
C14 C1 C2 111.5(3) . . ?
C14 C1 C8 110.0(3) . . ?
C3 C2 C1 123.7(4) . . ?
C7 C2 C1 119.8(3) . . ?
C7 C2 C3 116.4(4) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 C2 121.3(4) . . ?
C4 C3 H3 119.3 . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 120.9(4) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 H5 120.5 . . ?
C4 C5 C6 119.1(4) . . ?
C6 C5 H5 120.5 . . ?
C5 C6 H6 120.0 . . ?
C5 C6 C7 120.0(4) . . ?
C7 C6 H6 120.0 . . ?
C2 C7 H7 118.9 . . ?
C6 C7 C2 122.3(4) . . ?
C6 C7 H7 118.9 . . ?
C9 C8 C1 121.2(4) . . ?
C9 C8 C13 116.4(4) . . ?
C13 C8 C1 122.3(4) . . ?
C8 C9 H9 119.1 . . ?
C8 C9 C10 121.7(4) . . ?
C10 C9 H9 119.1 . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(4) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 120.7 . . ?
C12 C11 C10 118.7(4) . . ?
C12 C11 H11 120.7 . . ?
C11 C12 H12 119.9 . . ?
C11 C12 C13 120.3(4) . . ?
C13 C12 H12 119.9 . . ?
C8 C13 H13 118.9 . . ?
C12 C13 C8 122.1(4) . . ?
C12 C13 H13 118.9 . . ?
C15 C14 C1 122.2(3) . . ?
C15 C14 C19 118.0(4) . . ?
C19 C14 C1 119.6(3) . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.1(4) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 119.9 . . ?
C17 C16 C15 120.1(4) . . ?
C17 C16 H16 119.9 . . ?
C16 C17 H17 119.9 . . ?
C16 C17 C18 120.2(4) . . ?
C18 C17 H17 119.9 . . ?
C17 C18 H18 120.4 . . ?
C17 C18 C19 119.3(4) . . ?
C19 C18 H18 120.4 . . ?
C14 C19 H19 119.4 . . ?
C18 C19 C14 121.3(4) . . ?
C18 C19 H19 119.4 . . ?
N1 C20 H20 107.7 . . ?
N1 C20 C21 109.0(4) . . ?
N1 C20 C22 111.0(3) . . ?
C21 C20 H20 107.7 . . ?
C22 C20 H20 107.7 . . ?
C22 C20 C21 113.4(4) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C23 H23 107.3 . . ?
N2 C23 C24 110.6(4) . . ?
N2 C23 C25 112.1(4) . . ?
C24 C23 H23 107.3 . . ?
C25 C23 H23 107.3 . . ?
C25 C23 C24 112.1(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N2 C26 H26 106.9 . . ?
N2 C26 C27 112.4(4) . . ?
N2 C26 C28 112.1(4) . . ?
C27 C26 H26 106.9 . . ?
C27 C26 C28 111.1(4) . . ?
C28 C26 H26 106.9 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 W 179.1(4) . . ?
O2 C30 W 174.1(4) . . ?
O3 C31 W 171.7(4) . . ?
O4 C32 W 175.7(4) . . ?
O5 C33 W 172.3(4) . . ?
C29' W' P1' 178.58(12) . . ?
C29' W' C30' 85.74(17) . . ?
C29' W' C31' 86.13(16) . . ?
C29' W' C32' 92.36(17) . . ?
C29' W' C33' 82.84(16) . . ?
C30' W' P1' 94.82(12) . . ?
C30' W' C31' 91.68(17) . . ?
C30' W' C32' 177.96(16) . . ?
C30' W' C33' 85.83(17) . . ?
C31' W' P1' 95.15(11) . . ?
C32' W' P1' 87.09(11) . . ?
C32' W' C31' 87.42(17) . . ?
C33' W' P1' 95.90(11) . . ?
C33' W' C31' 168.84(16) . . ?
C33' W' C32' 94.70(17) . . ?
P2' P1' W' 131.76(5) . . ?
N1' P1' W' 121.12(12) . . ?
N1' P1' P2' 47.41(12) . . ?
N1' P1' C1' 108.86(16) . . ?
C1' P1' W' 119.95(12) . . ?
C1' P1' P2' 105.90(12) . . ?
N1' P2' P1' 47.59(11) . . ?
N2' P2' P1' 117.49(13) . . ?
N2' P2' N1' 107.31(17) . . ?
P2' N1' P1' 84.99(16) . . ?
C20' N1' P1' 137.3(3) . . ?
C20' N1' P2' 136.1(3) . . ?
C23' N2' P2' 116.3(3) . . ?
C26' N2' P2' 127.2(3) . . ?
C26' N2' C23' 116.3(3) . . ?
C2' C1' P1' 111.2(3) . . ?
C2' C1' C8' 110.4(3) . . ?
C8' C1' P1' 109.1(2) . . ?
C14' C1' P1' 104.0(2) . . ?
C14' C1' C2' 111.7(3) . . ?
C14' C1' C8' 110.4(3) . . ?
C3' C2' C1' 123.7(4) . . ?
C3' C2' C7' 115.9(4) . . ?
C7' C2' C1' 120.2(4) . . ?
C2' C3' H3' 119.2 . . ?
C2' C3' C4' 121.6(5) . . ?
C4' C3' H3' 119.2 . . ?
C3' C4' H4' 119.2 . . ?
C5' C4' C3' 121.5(5) . . ?
C5' C4' H4' 119.2 . . ?
C4' C5' H5' 120.9 . . ?
C4' C5' C6' 118.2(5) . . ?
C6' C5' H5' 120.9 . . ?
C5' C6' H6' 119.9 . . ?
C5' C6' C7' 120.1(5) . . ?
C7' C6' H6' 119.9 . . ?
C2' C7' H7' 118.7 . . ?
C6' C7' C2' 122.5(5) . . ?
C6' C7' H7' 118.7 . . ?
C9' C8' C1' 122.0(4) . . ?
C9' C8' C13' 117.1(4) . . ?
C13' C8' C1' 120.9(4) . . ?
C8' C9' H9' 119.1 . . ?
C10' C9' C8' 121.7(4) . . ?
C10' C9' H9' 119.2 . . ?
C9' C10' H10' 119.9 . . ?
C9' C10' C11' 120.3(4) . . ?
C11' C10' H10' 119.9 . . ?
C10' C11' H11' 120.6 . . ?
C12' C11' C10' 118.9(4) . . ?
C12' C11' H11' 120.6 . . ?
C11' C12' H12' 119.5 . . ?
C11' C12' C13' 120.9(4) . . ?
C13' C12' H12' 119.5 . . ?
C8' C13' H13' 119.4 . . ?
C12' C13' C8' 121.1(4) . . ?
C12' C13' H13' 119.4 . . ?
C15' C14' C1' 121.4(4) . . ?
C19' C14' C1' 121.0(3) . . ?
C19' C14' C15' 117.4(4) . . ?
C14' C15' H15' 119.9 . . ?
C16' C15' C14' 120.3(4) . . ?
C16' C15' H15' 119.9 . . ?
C15' C16' H16' 119.3 . . ?
C17' C16' C15' 121.5(4) . . ?
C17' C16' H16' 119.3 . . ?
C16' C17' H17' 120.4 . . ?
C16' C17' C18' 119.3(4) . . ?
C18' C17' H17' 120.4 . . ?
C17' C18' H18' 120.2 . . ?
C17' C18' C19' 119.6(4) . . ?
C19' C18' H18' 120.2 . . ?
C14' C19' H19' 119.1 . . ?
C18' C19' C14' 121.9(4) . . ?
C18' C19' H19' 119.1 . . ?
N1' C20' H20' 108.6 . . ?
N1' C20' C21' 109.5(3) . . ?
N1' C20' C22' 110.4(3) . . ?
C21' C20' H20' 108.6 . . ?
C21' C20' C22' 111.1(3) . . ?
C22' C20' H20' 108.6 . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21E 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C20' C22' H22D 109.5 . . ?
C20' C22' H22E 109.5 . . ?
C20' C22' H22F 109.5 . . ?
H22D C22' H22E 109.5 . . ?
H22D C22' H22F 109.5 . . ?
H22E C22' H22F 109.5 . . ?
N2' C23' H23' 107.1 . . ?
N2' C23' C24' 111.8(3) . . ?
N2' C23' C25' 111.9(3) . . ?
C24' C23' H23' 107.1 . . ?
C24' C23' C25' 111.5(4) . . ?
C25' C23' H23' 107.1 . . ?
C23' C24' H24D 109.5 . . ?
C23' C24' H24E 109.5 . . ?
C23' C24' H24F 109.5 . . ?
H24D C24' H24E 109.5 . . ?
H24D C24' H24F 109.5 . . ?
H24E C24' H24F 109.5 . . ?
C23' C25' H25D 109.5 . . ?
C23' C25' H25E 109.5 . . ?
C23' C25' H25F 109.5 . . ?
H25D C25' H25E 109.5 . . ?
H25D C25' H25F 109.5 . . ?
H25E C25' H25F 109.5 . . ?
N2' C26' H26' 107.2 . . ?
N2' C26' C27' 112.1(3) . . ?
N2' C26' C28' 111.7(4) . . ?
C27' C26' H26' 107.2 . . ?
C28' C26' H26' 107.2 . . ?
C28' C26' C27' 111.1(3) . . ?
C26' C27' H27D 109.5 . . ?
C26' C27' H27E 109.5 . . ?
C26' C27' H27F 109.5 . . ?
H27D C27' H27E 109.5 . . ?
H27D C27' H27F 109.5 . . ?
H27E C27' H27F 109.5 . . ?
C26' C28' H28D 109.5 . . ?
C26' C28' H28E 109.5 . . ?
C26' C28' H28F 109.5 . . ?
H28D C28' H28E 109.5 . . ?
H28D C28' H28F 109.5 . . ?
H28E C28' H28F 109.5 . . ?
O1' C29' W' 177.5(4) . . ?
O2' C30' W' 175.6(4) . . ?
O3' C31' W' 171.8(4) . . ?
O4' C32' W' 177.4(4) . . ?
O5' C33' W' 171.3(4) . . ?
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 P1 2.6042(11) . ?
W C29 1.980(5) . ?
W C30 2.041(5) . ?
W C31 2.040(4) . ?
W C32 2.040(5) . ?
W C33 2.026(5) . ?
P1 P2 2.2824(15) . ?
P1 N1 1.700(4) . ?
P1 C1 1.972(4) . ?
P2 N1 1.694(4) . ?
P2 N2 1.671(3) . ?
O1 C29 1.151(5) . ?
O2 C30 1.139(5) . ?
O3 C31 1.144(5) . ?
O4 C32 1.134(5) . ?
O5 C33 1.153(6) . ?
N1 C20 1.475(5) . ?
N2 C23 1.491(5) . ?
N2 C26 1.472(5) . ?
C1 C2 1.539(5) . ?
C1 C8 1.537(5) . ?
C1 C14 1.534(5) . ?
C2 C3 1.397(5) . ?
C2 C7 1.385(6) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.365(6) . ?
C5 H5 0.9500 . ?
C5 C6 1.380(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.383(6) . ?
C7 H7 0.9500 . ?
C8 C9 1.386(6) . ?
C8 C13 1.400(6) . ?
C9 H9 0.9500 . ?
C9 C10 1.386(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.381(6) . ?
C11 H11 0.9500 . ?
C11 C12 1.378(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.384(6) . ?
C13 H13 0.9500 . ?
C14 C15 1.393(5) . ?
C14 C19 1.397(5) . ?
C15 H15 0.9500 . ?
C15 C16 1.385(6) . ?
C16 H16 0.9500 . ?
C16 C17 1.383(6) . ?
C17 H17 0.9500 . ?
C17 C18 1.386(6) . ?
C18 H18 0.9500 . ?
C18 C19 1.395(6) . ?
C19 H19 0.9500 . ?
C20 H20 1.0000 . ?
C20 C21 1.513(6) . ?
C20 C22 1.507(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23 1.0000 . ?
C23 C24 1.538(6) . ?
C23 C25 1.524(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.515(6) . ?
C26 C28 1.526(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
W' P1' 2.6139(10) . ?
W' C29' 1.977(4) . ?
W' C30' 2.041(5) . ?
W' C31' 2.050(5) . ?
W' C32' 2.048(5) . ?
W' C33' 2.043(5) . ?
P1' P2' 2.2852(14) . ?
P1' N1' 1.694(3) . ?
P1' C1' 1.971(4) . ?
P2' N1' 1.689(3) . ?
P2' N2' 1.666(3) . ?
O1' C29' 1.153(5) . ?
O2' C30' 1.143(5) . ?
O3' C31' 1.142(5) . ?
O4' C32' 1.141(5) . ?
O5' C33' 1.142(5) . ?
N1' C20' 1.473(5) . ?
N2' C23' 1.488(5) . ?
N2' C26' 1.475(5) . ?
C1' C2' 1.542(5) . ?
C1' C8' 1.543(5) . ?
C1' C14' 1.523(5) . ?
C2' C3' 1.372(6) . ?
C2' C7' 1.384(6) . ?
C3' H3' 0.9500 . ?
C3' C4' 1.389(7) . ?
C4' H4' 0.9500 . ?
C4' C5' 1.348(7) . ?
C5' H5' 0.9500 . ?
C5' C6' 1.376(7) . ?
C6' H6' 0.9500 . ?
C6' C7' 1.378(7) . ?
C7' H7' 0.9500 . ?
C8' C9' 1.387(6) . ?
C8' C13' 1.405(5) . ?
C9' H9' 0.9500 . ?
C9' C10' 1.378(6) . ?
C10' H10' 0.9500 . ?
C10' C11' 1.391(6) . ?
C11' H11' 0.9500 . ?
C11' C12' 1.374(6) . ?
C12' H12' 0.9500 . ?
C12' C13' 1.375(6) . ?
C13' H13' 0.9500 . ?
C14' C15' 1.402(5) . ?
C14' C19' 1.396(6) . ?
C15' H15' 0.9500 . ?
C15' C16' 1.385(6) . ?
C16' H16' 0.9500 . ?
C16' C17' 1.377(6) . ?
C17' H17' 0.9500 . ?
C17' C18' 1.384(6) . ?
C18' H18' 0.9500 . ?
C18' C19' 1.389(6) . ?
C19' H19' 0.9500 . ?
C20' H20' 1.0000 . ?
C20' C21' 1.511(6) . ?
C20' C22' 1.523(6) . ?
C21' H21D 0.9800 . ?
C21' H21E 0.9800 . ?
C21' H21F 0.9800 . ?
C22' H22D 0.9800 . ?
C22' H22E 0.9800 . ?
C22' H22F 0.9800 . ?
C23' H23' 1.0000 . ?
C23' C24' 1.522(6) . ?
C23' C25' 1.533(6) . ?
C24' H24D 0.9800 . ?
C24' H24E 0.9800 . ?
C24' H24F 0.9800 . ?
C25' H25D 0.9800 . ?
C25' H25E 0.9800 . ?
C25' H25F 0.9800 . ?
C26' H26' 1.0000 . ?
C26' C27' 1.524(6) . ?
C26' C28' 1.521(6) . ?
C27' H27D 0.9800 . ?
C27' H27E 0.9800 . ?
C27' H27F 0.9800 . ?
C28' H28D 0.9800 . ?
C28' H28E 0.9800 . ?
C28' H28F 0.9800 . ?
