#------------------------------------------------------------------------------
#$Date: 2026-03-05 13:21:57 +0100 (Thu 05 de Mar de 2026) $
#$Revision: 304873 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/62/1576206.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_1576206
loop_
_publ_author_name
'Escoudé, Emile'
'Pedrón, Manuel'
'Bourqui, Lilian'
'Gontard, Geoffrey'
'Vitale, Maxime R.'
'Ciofini, Ilaria'
'Lakhdar, Sami'
'Grimaud, Laurence'
_publ_section_title
;
 Photochemical activation of pincer-ligated phosphoranides: mechanistic
 insight for reduction of aryl halides.
;
_journal_issue                   1
_journal_name_full               'Chemical science'
_journal_page_first              579
_journal_page_last               584
_journal_paper_doi               10.1039/d5sc06960b
_journal_volume                  17
_journal_year                    2026
_chemical_formula_moiety         'C48 H69 K N O8 P, 2(C4 H10 O)'
_chemical_formula_sum            'C56 H89 K N O10 P'
_chemical_formula_weight         1006.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2025-10-01 deposited with the CCDC.	2025-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.870(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5374(4)
_cell_length_b                   21.5756(6)
_cell_length_c                   19.1473(5)
_cell_measurement_reflns_used    7328
_cell_measurement_temperature    200(1)
_cell_measurement_theta_max      67.35
_cell_measurement_theta_min      3.10
_cell_volume                     5962.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker APEX-II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker QUAZAR'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35832
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.596
_diffrn_reflns_theta_min         3.098
_diffrn_source                   micro-source
_diffrn_source_type              'Incoatec I\uS'
_exptl_absorpt_coefficient_mu    1.448
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS : Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.039
_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     811
_refine_ls_number_reflns         10486
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0474
_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)+(0.0703P)²+1.6059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                7824
_reflns_number_total             10486
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5sc06960b3.cif
_cod_data_source_block           ee600
_cod_depositor_comments
'Adding full bibliography for 1576202--1576209.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1576206
_shelx_shelxl_version_number     2019/3
_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
K1 K 0.67523(3) 0.35986(2) 0.57525(2) 0.04582(14) Uani 1 1 d . . . . .
P1 P 0.70565(3) 0.36839(2) 0.40522(2) 0.03600(13) Uani 1 1 d . . . . .
O1 O 0.59523(9) 0.34165(6) 0.43675(7) 0.0372(3) Uani 1 1 d . . . . .
O2 O 0.80066(9) 0.39541(7) 0.35902(7) 0.0418(3) Uani 1 1 d . . . . .
O3A O 0.8136(7) 0.4499(5) 0.5859(6) 0.081(3) Uani 0.5 1 d . . P A 1
O4A O 0.8555(13) 0.3243(7) 0.5743(11) 0.076(4) Uani 0.5 1 d . . P A 1
O5A O 0.7195(7) 0.2313(5) 0.5949(5) 0.0615(19) Uani 0.5 1 d . . P A 1
O6A O 0.6231(5) 0.2910(4) 0.6908(4) 0.0548(15) Uani 0.5 1 d . . P A 1
O7A O 0.5385(5) 0.4042(4) 0.6613(4) 0.089(2) Uani 0.5 1 d . . P A 1
O8A O 0.6219(7) 0.4820(4) 0.5656(4) 0.094(2) Uani 0.5 1 d . . P A 1
O3B O 0.8422(6) 0.4379(5) 0.5819(6) 0.0524(17) Uani 0.5 1 d . . P A 2
O4B O 0.8570(15) 0.3075(7) 0.5813(11) 0.067(3) Uani 0.5 1 d . . P A 2
O5B O 0.7054(13) 0.2371(7) 0.6141(7) 0.139(7) Uani 0.5 1 d . . P A 2
O6B O 0.6023(8) 0.3164(5) 0.6914(6) 0.098(3) Uani 0.5 1 d . . P A 2
O7B O 0.5253(4) 0.4203(3) 0.6289(3) 0.0680(14) Uani 0.5 1 d . . P A 2
O8B O 0.6661(4) 0.4919(3) 0.5763(4) 0.0588(15) Uani 0.5 1 d . . P A 2
O9 O 0.83609(16) 0.63373(10) 0.30092(12) 0.0825(6) Uani 1 1 d . . . . .
O10A O 1.0493(4) 0.2053(4) 0.4759(2) 0.176(2) Uani 0.5 1 d . . P B 1
O10B O 1.0493(4) 0.2053(4) 0.4759(2) 0.176(2) Uani 0.5 1 d . . P C 2
N1 N 0.63087(10) 0.39825(7) 0.33272(8) 0.0319(3) Uani 1 1 d . . . . .
C1 C 0.52627(13) 0.33633(9) 0.38311(10) 0.0335(4) Uani 1 1 d . . . . .
C2 C 0.44530(14) 0.30172(9) 0.38439(10) 0.0358(4) Uani 1 1 d . . . . .
C3 C 0.38013(13) 0.30497(9) 0.32436(10) 0.0372(4) Uani 1 1 d . . . . .
H3 H 0.323881 0.282540 0.324303 0.045 Uiso 1 1 calc R U . . .
C4 C 0.39329(13) 0.33917(9) 0.26497(10) 0.0354(4) Uani 1 1 d . . . . .
C5 C 0.47654(13) 0.37157(9) 0.26460(10) 0.0332(4) Uani 1 1 d . . . . .
H5 H 0.487803 0.394626 0.224214 0.040 Uiso 1 1 calc R U . . .
C6 C 0.54265(12) 0.37009(8) 0.32312(9) 0.0300(4) Uani 1 1 d . . . . .
C7 C 0.67700(12) 0.42325(8) 0.27857(10) 0.0306(4) Uani 1 1 d . . . . .
C8 C 0.63988(13) 0.45237(9) 0.21728(10) 0.0340(4) Uani 1 1 d . . . . .
H8 H 0.574861 0.458641 0.208312 0.041 Uiso 1 1 calc R U . . .
C9 C 0.69770(14) 0.47270(9) 0.16826(10) 0.0370(4) Uani 1 1 d . . . . .
C10 C 0.79208(14) 0.46381(10) 0.18383(11) 0.0384(4) Uani 1 1 d . . . . .
H10 H 0.831208 0.476309 0.150061 0.046 Uiso 1 1 calc R U . . .
C11 C 0.83305(13) 0.43736(9) 0.24671(11) 0.0371(4) Uani 1 1 d . . . . .
C12 C 0.77353(13) 0.41824(9) 0.29439(10) 0.0332(4) Uani 1 1 d . . . . .
C13 C 0.42953(16) 0.26279(10) 0.44871(11) 0.0460(5) Uani 1 1 d . . . . .
C14 C 0.4254(2) 0.30609(14) 0.51195(13) 0.0635(7) Uani 1 1 d . . . . .
H14A H 0.415262 0.281521 0.553406 0.095 Uiso 1 1 calc R U . . .
H14B H 0.483893 0.328822 0.521319 0.095 Uiso 1 1 calc R U . . .
H14C H 0.374252 0.335544 0.501470 0.095 Uiso 1 1 calc R U . . .
C15 C 0.50873(18) 0.21616(12) 0.46408(14) 0.0587(6) Uani 1 1 d . . . . .
H15A H 0.498601 0.191240 0.505266 0.088 Uiso 1 1 calc R U . . .
H15B H 0.510650 0.188928 0.423316 0.088 Uiso 1 1 calc R U . . .
H15C H 0.567635 0.238458 0.473498 0.088 Uiso 1 1 calc R U . . .
C16 C 0.33896(18) 0.22597(13) 0.43752(14) 0.0623(7) Uani 1 1 d . . . . .
H16A H 0.331886 0.201853 0.479920 0.093 Uiso 1 1 calc R U . . .
H16B H 0.286681 0.254638 0.427995 0.093 Uiso 1 1 calc R U . . .
H16C H 0.340335 0.197833 0.397474 0.093 Uiso 1 1 calc R U . . .
C17 C 0.31731(14) 0.34090(11) 0.20182(11) 0.0424(5) Uani 1 1 d . . . . .
C18 C 0.2998(2) 0.27546(14) 0.17186(15) 0.0697(7) Uani 1 1 d . . . . .
H18A H 0.283078 0.247831 0.208948 0.105 Uiso 1 1 calc R U . . .
H18B H 0.249146 0.276681 0.133240 0.105 Uiso 1 1 calc R U . . .
H18C H 0.356157 0.260045 0.154252 0.105 Uiso 1 1 calc R U . . .
C19 C 0.22767(18) 0.36501(15) 0.22593(16) 0.0697(8) Uani 1 1 d . . . . .
H19A H 0.210576 0.338942 0.264259 0.105 Uiso 1 1 calc R U . . .
H19B H 0.236721 0.407786 0.242565 0.105 Uiso 1 1 calc R U . . .
H19C H 0.178123 0.363806 0.186464 0.105 Uiso 1 1 calc R U . . .
C20 C 0.3429(2) 0.38167(17) 0.14251(15) 0.0786(9) Uani 1 1 d . . . . .
H20A H 0.400499 0.366509 0.126662 0.118 Uiso 1 1 calc R U . . .
H20B H 0.293108 0.380423 0.103239 0.118 Uiso 1 1 calc R U . . .
H20C H 0.351706 0.424403 0.159340 0.118 Uiso 1 1 calc R U . . .
C21 C 0.65386(16) 0.50152(11) 0.09927(11) 0.0473(5) Uani 1 1 d . . . . .
C22 C 0.5846(2) 0.55213(12) 0.11358(14) 0.0626(7) Uani 1 1 d . . . . .
H22A H 0.557147 0.570098 0.068881 0.094 Uiso 1 1 calc R U . . .
H22B H 0.535603 0.534064 0.138150 0.094 Uiso 1 1 calc R U . . .
H22C H 0.616705 0.584589 0.142872 0.094 Uiso 1 1 calc R U . . .
C23 C 0.7261(2) 0.53110(16) 0.05749(15) 0.0756(9) Uani 1 1 d . . . . .
H23A H 0.695064 0.548918 0.013832 0.113 Uiso 1 1 calc R U . . .
H23B H 0.759188 0.563850 0.085733 0.113 Uiso 1 1 calc R U . . .
H23C H 0.770380 0.499423 0.046203 0.113 Uiso 1 1 calc R U . . .
C24 C 0.6036(2) 0.45039(13) 0.05389(13) 0.0619(7) Uani 1 1 d . . . . .
H24A H 0.575106 0.468213 0.009413 0.093 Uiso 1 1 calc R U . . .
H24B H 0.648155 0.418341 0.044252 0.093 Uiso 1 1 calc R U . . .
H24C H 0.555444 0.431971 0.079028 0.093 Uiso 1 1 calc R U . . .
C25 C 0.93818(14) 0.42939(12) 0.26311(14) 0.0518(6) Uani 1 1 d . . . . .
C26 C 0.98941(17) 0.45269(17) 0.20293(18) 0.0783(9) Uani 1 1 d . . . . .
H26A H 0.968310 0.429537 0.159953 0.117 Uiso 1 1 calc R U . . .
H26B H 0.976543 0.496900 0.195131 0.117 Uiso 1 1 calc R U . . .
H26C H 1.056189 0.446560 0.215154 0.117 Uiso 1 1 calc R U . . .
C27 C 0.97300(18) 0.46659(15) 0.32897(17) 0.0733(8) Uani 1 1 d . . . . .
H27A H 0.941181 0.452538 0.368433 0.110 Uiso 1 1 calc R U . . .
H27B H 1.039885 0.460364 0.340355 0.110 Uiso 1 1 calc R U . . .
H27C H 0.960239 0.510705 0.320332 0.110 Uiso 1 1 calc R U . . .
C28 C 0.96056(17) 0.36044(14) 0.27424(18) 0.0699(8) Uani 1 1 d . . . . .
H28A H 0.937803 0.337327 0.231594 0.105 Uiso 1 1 calc R U . . .
H28B H 1.027768 0.355030 0.284360 0.105 Uiso 1 1 calc R U . . .
H28C H 0.930436 0.344875 0.313885 0.105 Uiso 1 1 calc R U . . .
C29 C 0.72581(14) 0.28978(10) 0.37809(11) 0.0413(5) Uani 1 1 d . . . . .
C30 C 0.74257(15) 0.23643(10) 0.36678(12) 0.0455(5) Uani 1 1 d . . . . .
C31 C 0.75991(16) 0.17242(11) 0.35308(13) 0.0500(5) Uani 1 1 d . . . . .
C32 C 0.7210(2) 0.12636(12) 0.39028(15) 0.0663(7) Uani 1 1 d . . . . .
H32 H 0.682841 0.137365 0.425258 0.080 Uiso 1 1 calc R U . . .
C33 C 0.7370(3) 0.06454(14) 0.3773(2) 0.0859(10) Uani 1 1 d . . . . .
H33 H 0.709863 0.033433 0.403377 0.103 Uiso 1 1 calc R U . . .
C34 C 0.7915(3) 0.04802(15) 0.3272(2) 0.0915(11) Uani 1 1 d . . . . .
H34 H 0.803565 0.005481 0.319211 0.110 Uiso 1 1 calc R U . . .
C35 C 0.8286(3) 0.09223(16) 0.2886(2) 0.0964(12) Uani 1 1 d . . . . .
H35 H 0.865071 0.080446 0.252837 0.116 Uiso 1 1 calc R U . . .
C36 C 0.8136(2) 0.15465(14) 0.30119(18) 0.0774(9) Uani 1 1 d . . . . .
H36 H 0.840178 0.185295 0.274147 0.093 Uiso 1 1 calc R U . . .
C37A C 0.8893(11) 0.4276(7) 0.5550(7) 0.098(4) Uani 0.5 1 d . . P A 1
H37A H 0.938605 0.459512 0.558624 0.118 Uiso 0.5 1 calc R U P A 1
H37B H 0.870116 0.419417 0.504495 0.118 Uiso 0.5 1 calc R U P A 1
C38A C 0.9255(14) 0.3708(8) 0.5893(12) 0.091(6) Uani 0.5 1 d . . P A 1
H38A H 0.983369 0.358115 0.570765 0.109 Uiso 0.5 1 calc R U P A 1
H38B H 0.938962 0.377192 0.640684 0.109 Uiso 0.5 1 calc R U P A 1
C39A C 0.8840(11) 0.2650(9) 0.6017(12) 0.089(7) Uani 0.5 1 d . . P A 1
H39A H 0.889239 0.265384 0.653725 0.107 Uiso 0.5 1 calc R U P A 1
H39B H 0.945034 0.253807 0.587313 0.107 Uiso 0.5 1 calc R U P A 1
C40A C 0.8118(14) 0.2194(7) 0.5725(9) 0.091(5) Uani 0.5 1 d . . P A 1
H40A H 0.806604 0.220582 0.520521 0.110 Uiso 0.5 1 calc R U P A 1
H40B H 0.832191 0.177166 0.587723 0.110 Uiso 0.5 1 calc R U P A 1
C41A C 0.7173(10) 0.2071(5) 0.6626(6) 0.068(3) Uani 0.5 1 d . . P A 1
H41A H 0.768588 0.224321 0.695521 0.082 Uiso 0.5 1 calc R U P A 1
H41B H 0.723361 0.161358 0.662062 0.082 Uiso 0.5 1 calc R U P A 1
C42A C 0.6257(9) 0.2254(6) 0.6845(7) 0.064(3) Uani 0.5 1 d . . P A 1
H42A H 0.574966 0.211196 0.648991 0.077 Uiso 0.5 1 calc R U P A 1
H42B H 0.617430 0.205875 0.730098 0.077 Uiso 0.5 1 calc R U P A 1
C43A C 0.5454(8) 0.3092(6) 0.7224(6) 0.078(3) Uani 0.5 1 d . . P A 1
H43A H 0.547132 0.290056 0.769466 0.093 Uiso 0.5 1 calc R U P A 1
H43B H 0.488076 0.295468 0.693311 0.093 Uiso 0.5 1 calc R U P A 1
C44A C 0.5459(8) 0.3757(7) 0.7286(6) 0.077(3) Uani 0.5 1 d . . P A 1
H44A H 0.493494 0.389012 0.753551 0.092 Uiso 0.5 1 calc R U P A 1
H44B H 0.604129 0.389092 0.756662 0.092 Uiso 0.5 1 calc R U P A 1
C45A C 0.5286(8) 0.4656(5) 0.6630(6) 0.120(4) Uani 0.5 1 d . . P A 1
H45A H 0.578919 0.483718 0.696224 0.144 Uiso 0.5 1 calc R U P A 1
H45B H 0.468785 0.475991 0.679968 0.144 Uiso 0.5 1 calc R U P A 1
C46A C 0.5316(13) 0.4929(8) 0.5911(9) 0.133(9) Uani 0.5 1 d . . P A 1
H46A H 0.481924 0.474208 0.557789 0.160 Uiso 0.5 1 calc R U P A 1
H46B H 0.519958 0.538084 0.592794 0.160 Uiso 0.5 1 calc R U P A 1
C47A C 0.6929(17) 0.5226(7) 0.5869(10) 0.170(11) Uani 0.5 1 d . . P A 1
H47A H 0.707400 0.521178 0.638727 0.204 Uiso 0.5 1 calc R U P A 1
H47B H 0.673935 0.565339 0.573155 0.204 Uiso 0.5 1 calc R U P A 1
C48A C 0.7767(10) 0.5048(6) 0.5531(8) 0.124(7) Uani 0.5 1 d . . P A 1
H48A H 0.759451 0.497527 0.502124 0.149 Uiso 0.5 1 calc R U P A 1
H48B H 0.823272 0.538387 0.558947 0.149 Uiso 0.5 1 calc R U P A 1
C37B C 0.9164(8) 0.4061(6) 0.5554(8) 0.060(2) Uani 0.5 1 d . . P A 2
H37C H 0.973094 0.431997 0.560823 0.072 Uiso 0.5 1 calc R U P A 2
H37D H 0.900241 0.396487 0.504877 0.072 Uiso 0.5 1 calc R U P A 2
C38B C 0.9324(15) 0.3468(7) 0.5977(12) 0.067(4) Uani 0.5 1 d . . P A 2
H38C H 0.989733 0.326348 0.586476 0.081 Uiso 0.5 1 calc R U P A 2
H38D H 0.939660 0.356499 0.648594 0.081 Uiso 0.5 1 calc R U P A 2
C39B C 0.8672(14) 0.2468(10) 0.6108(13) 0.100(7) Uani 0.5 1 d . . P A 2
H39C H 0.880493 0.249628 0.662593 0.121 Uiso 0.5 1 calc R U P A 2
H39D H 0.919794 0.225381 0.592729 0.121 Uiso 0.5 1 calc R U P A 2
C40B C 0.7815(18) 0.2111(8) 0.5919(10) 0.138(11) Uani 0.5 1 d . . P A 2
H40C H 0.771038 0.206650 0.540078 0.166 Uiso 0.5 1 calc R U P A 2
H40D H 0.789891 0.169054 0.612298 0.166 Uiso 0.5 1 calc R U P A 2
C41B C 0.6795(12) 0.2228(7) 0.6818(7) 0.095(7) Uani 0.5 1 d . . P A 2
H41C H 0.731689 0.233884 0.717588 0.114 Uiso 0.5 1 calc R U P A 2
H41D H 0.670429 0.177394 0.684470 0.114 Uiso 0.5 1 calc R U P A 2
C42B C 0.5961(9) 0.2532(8) 0.7003(7) 0.095(5) Uani 0.5 1 d . . P A 2
H42C H 0.541224 0.237108 0.670111 0.114 Uiso 0.5 1 calc R U P A 2
H42D H 0.588302 0.243912 0.749833 0.114 Uiso 0.5 1 calc R U P A 2
C43B C 0.5269(13) 0.3465(8) 0.7175(9) 0.100(6) Uani 0.5 1 d . . P A 2
H43C H 0.529262 0.339974 0.768864 0.120 Uiso 0.5 1 calc R U P A 2
H43D H 0.467382 0.330141 0.694257 0.120 Uiso 0.5 1 calc R U P A 2
C44B C 0.5359(8) 0.4113(6) 0.7020(7) 0.094(3) Uani 0.5 1 d . . P A 2
H44C H 0.488150 0.435258 0.723169 0.113 Uiso 0.5 1 calc R U P A 2
H44D H 0.597592 0.426388 0.722558 0.113 Uiso 0.5 1 calc R U P A 2
C45B C 0.5118(8) 0.4824(5) 0.6063(7) 0.065(4) Uani 0.5 1 d . . P A 2
H45C H 0.465986 0.502005 0.633634 0.079 Uiso 0.5 1 calc R U P A 2
H45D H 0.485063 0.482373 0.556198 0.079 Uiso 0.5 1 calc R U P A 2
C46B C 0.5990(6) 0.5213(3) 0.6139(6) 0.091(3) Uani 0.5 1 d . . P A 2
H46C H 0.585085 0.563344 0.594631 0.110 Uiso 0.5 1 calc R U P A 2
H46D H 0.623401 0.525366 0.664170 0.110 Uiso 0.5 1 calc R U P A 2
C47B C 0.7469(7) 0.5279(6) 0.5779(6) 0.063(2) Uani 0.5 1 d . . P A 2
H47C H 0.771319 0.537502 0.627237 0.075 Uiso 0.5 1 calc R U P A 2
H47D H 0.732624 0.567455 0.552752 0.075 Uiso 0.5 1 calc R U P A 2
C48B C 0.8180(5) 0.4922(4) 0.5432(5) 0.0523(18) Uani 0.5 1 d . . P A 2
H48C H 0.792541 0.481269 0.494545 0.063 Uiso 0.5 1 calc R U P A 2
H48D H 0.873794 0.518182 0.541132 0.063 Uiso 0.5 1 calc R U P A 2
C49 C 0.7584(3) 0.59865(18) 0.3127(2) 0.0973(11) Uani 1 1 d . . . . .
H49A H 0.759707 0.558565 0.287702 0.117 Uiso 1 1 calc R U . . .
H49B H 0.701464 0.620987 0.293604 0.117 Uiso 1 1 calc R U . . .
C50 C 0.7565(4) 0.5874(3) 0.3863(3) 0.153(2) Uani 1 1 d . . . . .
H50A H 0.701629 0.562851 0.393080 0.229 Uiso 1 1 calc R U . . .
H50B H 0.812443 0.564725 0.405131 0.229 Uiso 1 1 calc R U . . .
H50C H 0.754260 0.627081 0.411027 0.229 Uiso 1 1 calc R U . . .
C51 C 0.8391(3) 0.6448(2) 0.2294(2) 0.1049(12) Uani 1 1 d . . . . .
H51A H 0.779785 0.663403 0.208773 0.126 Uiso 1 1 calc R U . . .
H51B H 0.847211 0.605044 0.205086 0.126 Uiso 1 1 calc R U . . .
C52 C 0.9136(4) 0.6856(3) 0.2190(3) 0.153(2) Uani 1 1 d . . . . .
H52A H 0.914391 0.692680 0.168571 0.230 Uiso 1 1 calc R U . . .
H52B H 0.905039 0.725136 0.242544 0.230 Uiso 1 1 calc R U . . .
H52C H 0.972377 0.666853 0.238861 0.230 Uiso 1 1 calc R U . . .
C53A C 0.9937(12) 0.1553(10) 0.4671(8) 0.155(4) Uani 0.5 1 d . . P B 1
H53A H 0.976690 0.149336 0.415875 0.186 Uiso 0.5 1 calc R U P B 1
H53B H 0.935900 0.165124 0.487394 0.186 Uiso 0.5 1 calc R U P B 1
C54A C 1.0333(19) 0.0884(12) 0.5007(13) 0.192(9) Uani 0.5 1 d . . P B 1
H54A H 0.985939 0.056356 0.490341 0.287 Uiso 0.5 1 calc R U P B 1
H54B H 1.089256 0.076746 0.479908 0.287 Uiso 0.5 1 calc R U P B 1
H54C H 1.048275 0.092607 0.551763 0.287 Uiso 0.5 1 calc R U P B 1
C55A C 1.0059(7) 0.2601(6) 0.4431(4) 0.122(3) Uani 0.5 1 d . . P B 1
H55A H 0.985716 0.252956 0.392545 0.146 Uiso 0.5 1 calc R U P B 1
H55B H 0.951713 0.272842 0.466464 0.146 Uiso 0.5 1 calc R U P B 1
C56A C 1.0775(6) 0.3058(5) 0.4526(4) 0.199(3) Uani 0.5 1 d . . P B 1
H56A H 1.054169 0.345067 0.431764 0.299 Uiso 0.5 1 calc R U P B 1
H56B H 1.096815 0.311661 0.502981 0.299 Uiso 0.5 1 calc R U P B 1
H56C H 1.130569 0.291921 0.429604 0.299 Uiso 0.5 1 calc R U P B 1
C55B C 1.1087(15) 0.244(2) 0.5087(10) 0.48(4) Uani 0.5 1 d . . P C 2
H55C H 1.173731 0.230379 0.507537 0.575 Uiso 0.5 1 calc R U P C 2
H55D H 1.096859 0.251618 0.557702 0.575 Uiso 0.5 1 calc R U P C 2
C53B C 1.0559(19) 0.1317(13) 0.5135(12) 0.199(8) Uani 0.5 1 d . . P C 2
H53C H 1.118355 0.113539 0.512963 0.239 Uiso 0.5 1 calc R U P C 2
H53D H 1.040960 0.132891 0.562638 0.239 Uiso 0.5 1 calc R U P C 2
C54B C 0.998(2) 0.1027(17) 0.4763(15) 0.310(19) Uani 0.5 1 d . . P C 2
H54D H 0.996758 0.059955 0.493393 0.466 Uiso 0.5 1 calc R U P C 2
H54E H 0.937513 0.121926 0.477287 0.466 Uiso 0.5 1 calc R U P C 2
H54F H 1.014313 0.102722 0.427994 0.466 Uiso 0.5 1 calc R U P C 2
C56B C 1.0775(6) 0.3058(5) 0.4526(4) 0.199(3) Uani 0.5 1 d . . P C 2
H56D H 1.115360 0.341973 0.467923 0.299 Uiso 0.5 1 calc R U P C 2
H56E H 1.087636 0.294689 0.404494 0.299 Uiso 0.5 1 calc R U P C 2
H56F H 1.011898 0.315616 0.453921 0.299 Uiso 0.5 1 calc R U P C 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.3868 1.0657 '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
O4A K1 O8A 122.2(4) . . ?
O6B K1 O5B 61.3(4) . . ?
O4A K1 O3A 60.8(4) . . ?
O8A K1 O3A 62.1(3) . . ?
O4A K1 O1 104.2(5) . . ?
O6B K1 O1 124.4(2) . . ?
O8A K1 O1 89.38(16) . . ?
O5B K1 O1 98.9(3) . . ?
O3A K1 O1 112.5(2) . . ?
O6B K1 O7B 58.3(3) . . ?
O5B K1 O7B 116.5(4) . . ?
O1 K1 O7B 99.08(13) . . ?
O4A K1 O6A 101.8(4) . . ?
O8A K1 O6A 117.0(2) . . ?
O3A K1 O6A 124.4(3) . . ?
O1 K1 O6A 123.10(16) . . ?
O6B K1 O8B 108.2(3) . . ?
O5B K1 O8B 163.4(3) . . ?
O1 K1 O8B 97.64(15) . . ?
O7B K1 O8B 60.00(17) . . ?
O4A K1 O5A 61.8(4) . . ?
O8A K1 O5A 174.7(3) . . ?
O3A K1 O5A 121.1(3) . . ?
O1 K1 O5A 92.88(16) . . ?
O6A K1 O5A 57.8(3) . . ?
O6B K1 O4B 106.1(4) . . ?
O5B K1 O4B 59.8(5) . . ?
O1 K1 O4B 105.1(4) . . ?
O7B K1 O4B 155.8(5) . . ?
O8B K1 O4B 115.9(4) . . ?
O4A K1 O7A 145.3(5) . . ?
O8A K1 O7A 60.9(3) . . ?
O3A K1 O7A 105.5(3) . . ?
O1 K1 O7A 110.54(14) . . ?
O6A K1 O7A 57.6(2) . . ?
O5A K1 O7A 113.8(3) . . ?
N1 P1 C29 102.74(8) . . ?
N1 P1 O2 86.17(7) . . ?
C29 P1 O2 90.13(8) . . ?
N1 P1 O1 84.01(7) . . ?
C29 P1 O1 88.75(8) . . ?
O2 P1 O1 169.62(6) . . ?
N1 P1 K1 129.83(5) . . ?
C29 P1 K1 105.85(7) . . ?
O2 P1 K1 133.36(5) . . ?
O1 P1 K1 56.68(4) . . ?
C1 O1 P1 111.58(11) . . ?
C1 O1 K1 156.95(11) . . ?
P1 O1 K1 89.26(5) . . ?
C12 O2 P1 114.04(12) . . ?
C37A O3A C48A 112.1(11) . . ?
C37A O3A K1 109.1(8) . . ?
C48A O3A K1 108.5(7) . . ?
C39A O4A C38A 112.7(16) . . ?
C39A O4A K1 119.1(12) . . ?
C38A O4A K1 117.4(11) . . ?
C41A O5A C40A 109.0(10) . . ?
C41A O5A K1 117.0(7) . . ?
C40A O5A K1 109.1(8) . . ?
C43A O6A C42A 110.3(9) . . ?
C43A O6A K1 119.6(7) . . ?
C42A O6A K1 116.2(7) . . ?
C45A O7A C44A 113.8(10) . . ?
C45A O7A K1 115.2(7) . . ?
C44A O7A K1 113.0(5) . . ?
C47A O8A C46A 117.8(13) . . ?
C47A O8A K1 113.2(8) . . ?
C46A O8A K1 112.8(9) . . ?
C48B O3B C37B 111.5(9) . . ?
C48B O3B K1 107.5(6) . . ?
C37B O3B K1 111.4(8) . . ?
C38B O4B C39B 115.4(17) . . ?
C38B O4B K1 117.8(10) . . ?
C39B O4B K1 115.4(13) . . ?
C40B O5B C41B 120.7(16) . . ?
C40B O5B K1 114.8(12) . . ?
C41B O5B K1 113.6(10) . . ?
C42B O6B C43B 110.2(11) . . ?
C42B O6B K1 118.4(9) . . ?
C43B O6B K1 121.4(9) . . ?
C44B O7B C45B 115.5(8) . . ?
C44B O7B K1 107.5(6) . . ?
C45B O7B K1 114.1(5) . . ?
C47B O8B C46B 111.2(7) . . ?
C47B O8B K1 120.9(5) . . ?
C46B O8B K1 118.9(5) . . ?
C51 O9 C49 111.8(3) . . ?
C53A O10A C55A 112.1(9) . . ?
C55B O10B C53B 112.3(18) . . ?
C7 N1 C6 125.07(15) . . ?
C7 N1 P1 114.40(12) . . ?
C6 N1 P1 114.01(12) . . ?
O1 C1 C2 125.61(17) . . ?
O1 C1 C6 113.24(16) . . ?
C2 C1 C6 121.16(18) . . ?
C1 C2 C3 116.59(17) . . ?
C1 C2 C13 121.01(18) . . ?
C3 C2 C13 122.40(18) . . ?
C4 C3 C2 123.55(18) . . ?
C3 C4 C5 118.31(18) . . ?
C3 C4 C17 120.05(17) . . ?
C5 C4 C17 121.64(17) . . ?
C6 C5 C4 120.07(17) . . ?
C5 C6 C1 120.26(17) . . ?
C5 C6 N1 128.80(17) . . ?
C1 C6 N1 110.93(16) . . ?
C8 C7 C12 119.78(17) . . ?
C8 C7 N1 128.85(17) . . ?
C12 C7 N1 111.32(16) . . ?
C7 C8 C9 120.38(18) . . ?
C10 C9 C8 118.08(18) . . ?
C10 C9 C21 122.92(18) . . ?
C8 C9 C21 118.96(18) . . ?
C9 C10 C11 123.48(18) . . ?
C12 C11 C10 116.79(17) . . ?
C12 C11 C25 120.97(19) . . ?
C10 C11 C25 122.24(19) . . ?
O2 C12 C11 125.03(17) . . ?
O2 C12 C7 113.69(16) . . ?
C11 C12 C7 121.25(18) . . ?
C2 C13 C16 112.42(19) . . ?
C2 C13 C15 109.50(18) . . ?
C16 C13 C15 107.5(2) . . ?
C2 C13 C14 108.92(18) . . ?
C16 C13 C14 108.2(2) . . ?
C15 C13 C14 110.4(2) . . ?
C20 C17 C19 108.9(2) . . ?
C20 C17 C18 107.4(2) . . ?
C19 C17 C18 108.5(2) . . ?
C20 C17 C4 112.65(18) . . ?
C19 C17 C4 109.25(18) . . ?
C18 C17 C4 110.06(19) . . ?
C9 C21 C22 110.51(19) . . ?
C9 C21 C23 112.28(19) . . ?
C22 C21 C23 107.6(2) . . ?
C9 C21 C24 108.55(19) . . ?
C22 C21 C24 109.6(2) . . ?
C23 C21 C24 108.3(2) . . ?
C27 C25 C26 107.8(2) . . ?
C27 C25 C28 110.6(2) . . ?
C26 C25 C28 108.0(2) . . ?
C27 C25 C11 109.5(2) . . ?
C26 C25 C11 111.8(2) . . ?
C28 C25 C11 109.11(19) . . ?
C30 C29 P1 173.60(19) . . ?
C29 C30 C31 178.4(2) . . ?
C32 C31 C36 118.0(2) . . ?
C32 C31 C30 120.4(2) . . ?
C36 C31 C30 121.5(2) . . ?
C33 C32 C31 120.9(3) . . ?
C34 C33 C32 120.2(3) . . ?
C35 C34 C33 120.1(3) . . ?
C34 C35 C36 120.4(3) . . ?
C31 C36 C35 120.3(3) . . ?
O3A C37A C38A 111.0(13) . . ?
O3A C37A K1 48.8(6) . . ?
C38A C37A K1 82.9(10) . . ?
O4A C38A C37A 106.8(15) . . ?
O4A C39A C40A 107.0(16) . . ?
O5A C40A C39A 113.4(12) . . ?
O5A C41A C42A 106.3(12) . . ?
O6A C42A C41A 108.8(9) . . ?
O6A C43A C44A 108.6(10) . . ?
O7A C44A C43A 110.9(9) . . ?
O7A C45A C46A 110.6(11) . . ?
O8A C46A C45A 111.3(11) . . ?
O8A C47A C48A 109.2(13) . . ?
O8A C47A K1 45.7(5) . . ?
C48A C47A K1 76.9(7) . . ?
O3A C48A C47A 107.9(11) . . ?
O3A C48A K1 49.0(6) . . ?
C47A C48A K1 78.5(7) . . ?
O3B C37B C38B 106.9(13) . . ?
O4B C38B C37B 109.2(17) . . ?
O4B C39B C40B 109.7(17) . . ?
O5B C40B C39B 114.0(17) . . ?
O5B C41B C42B 116.1(12) . . ?
O6B C42B C41B 110.3(12) . . ?
O6B C43B C44B 106.2(11) . . ?
O7B C44B C43B 109.7(9) . . ?
O7B C44B K1 50.2(4) . . ?
C43B C44B K1 84.8(8) . . ?
O7B C45B C46B 114.3(10) . . ?
O8B C46B C45B 108.7(7) . . ?
O8B C47B C48B 108.9(10) . . ?
O3B C48B C47B 109.6(10) . . ?
O9 C49 C50 111.2(4) . . ?
O9 C51 C52 110.8(4) . . ?
O10A C53A C54A 118.2(17) . . ?
C56A C55A O10A 103.6(7) . . ?
O10B C55B C56B 94.8(12) . . ?
C54B C53B O10B 103(2) . . ?
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
K1 O4A 2.733(18) . ?
K1 O6B 2.740(12) . ?
K1 O8A 2.746(7) . ?
K1 O5B 2.772(15) . ?
K1 O3A 2.787(11) . ?
K1 O1 2.7931(13) . ?
K1 O7B 2.836(6) . ?
K1 O6A 2.842(9) . ?
K1 O8B 2.851(7) . ?
K1 O5A 2.863(13) . ?
K1 O4B 2.864(19) . ?
K1 O7A 2.891(8) . ?
P1 N1 1.7785(16) . ?
P1 C29 1.808(2) . ?
P1 O2 1.8227(14) . ?
P1 O1 1.8724(14) . ?
O1 C1 1.352(2) . ?
O2 C12 1.346(2) . ?
O3A C37A 1.394(16) . ?
O3A C48A 1.416(15) . ?
O4A C39A 1.426(17) . ?
O4A C38A 1.43(3) . ?
O5A C41A 1.400(17) . ?
O5A C40A 1.48(2) . ?
O6A C43A 1.399(14) . ?
O6A C42A 1.422(16) . ?
O7A C45A 1.335(13) . ?
O7A C44A 1.421(15) . ?
O8A C47A 1.378(18) . ?
O8A C46A 1.473(19) . ?
O3B C48B 1.407(13) . ?
O3B C37B 1.423(10) . ?
O4B C38B 1.39(3) . ?
O4B C39B 1.428(18) . ?
O5B C40B 1.35(3) . ?
O5B C41B 1.43(2) . ?
O6B C42B 1.379(15) . ?
O6B C43B 1.42(2) . ?
O7B C44B 1.404(13) . ?
O7B C45B 1.415(14) . ?
O8B C47B 1.405(14) . ?
O8B C46B 1.429(11) . ?
O9 C51 1.395(4) . ?
O9 C49 1.400(4) . ?
O10A C53A 1.346(19) . ?
O10A C55A 1.448(11) . ?
O10B C55B 1.30(4) . ?
O10B C53B 1.74(3) . ?
N1 C7 1.408(2) . ?
N1 C6 1.411(2) . ?
C1 C2 1.397(3) . ?
C1 C6 1.404(3) . ?
C2 C3 1.401(3) . ?
C2 C13 1.531(3) . ?
C3 C4 1.388(3) . ?
C4 C5 1.398(3) . ?
C4 C17 1.538(3) . ?
C5 C6 1.387(3) . ?
C7 C8 1.383(3) . ?
C7 C12 1.404(3) . ?
C8 C9 1.403(3) . ?
C9 C10 1.382(3) . ?
C9 C21 1.528(3) . ?
C10 C11 1.399(3) . ?
C11 C12 1.393(3) . ?
C11 C25 1.533(3) . ?
C13 C16 1.531(3) . ?
C13 C15 1.531(3) . ?
C13 C14 1.536(3) . ?
C17 C20 1.518(3) . ?
C17 C19 1.525(3) . ?
C17 C18 1.534(4) . ?
C21 C22 1.532(4) . ?
C21 C23 1.534(3) . ?
C21 C24 1.534(3) . ?
C25 C27 1.529(4) . ?
C25 C26 1.530(4) . ?
C25 C28 1.532(4) . ?
C29 C30 1.202(3) . ?
C30 C31 1.434(3) . ?
C31 C32 1.382(4) . ?
C31 C36 1.389(4) . ?
C32 C33 1.381(4) . ?
C33 C34 1.363(5) . ?
C34 C35 1.356(5) . ?
C35 C36 1.390(4) . ?
C37A C38A 1.459(19) . ?
C39A C40A 1.50(3) . ?
C41A C42A 1.496(18) . ?
C43A C44A 1.438(18) . ?
C45A C46A 1.503(18) . ?
C47A C48A 1.50(3) . ?
C37B C38B 1.517(17) . ?
C39B C40B 1.47(3) . ?
C41B C42B 1.459(19) . ?
C43B C44B 1.44(2) . ?
C45B C46B 1.513(13) . ?
C47B C48B 1.506(12) . ?
C49 C50 1.433(6) . ?
C51 C52 1.427(7) . ?
C53A C54A 1.66(3) . ?
C55A C56A 1.428(13) . ?
C55B C56B 1.74(4) . ?
C53B C54B 1.21(4) . ?
