#------------------------------------------------------------------------------
#$Date: 2020-04-08 02:28:59 +0300 (Wed, 08 Apr 2020) $
#$Revision: 250460 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/82/4038215.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_4038215
loop_
_publ_author_name
'Helberg, Julian'
'Ampßler, Torsten'
'Zipse, Hendrik'
_publ_section_title
;
 Pyridinyl Amide Ion Pairs as Lewis Base Organocatalysts.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c00114
_journal_year                    2020
_chemical_formula_moiety         'C17 H14 N2 O P, C16 H36 P'
_chemical_formula_sum            'C33 H50 N2 O P2'
_chemical_formula_weight         552.69
_chemical_name_common            389b
_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
_audit_block_code                C17H14N2OP_C16H36P_wo026_zipse
_audit_creation_date             2018-06-05
_audit_creation_method           SHELXL-2014
_audit_update_record             05-Jun-18
_cell_angle_alpha                97.836(3)
_cell_angle_beta                 99.154(4)
_cell_angle_gamma                94.177(3)
_cell_formula_units_Z            6
_cell_length_a                   10.0606(4)
_cell_length_b                   17.2822(5)
_cell_length_c                   28.0572(12)
_cell_measurement_reflns_used    2585
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      25.9750
_cell_measurement_theta_min      4.3140
_cell_volume                     4748.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement
;
Sheldrick, G. M. (2008).
Acta Cryst. A64, 112--122.
;
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -89.00   4.00   0.75   20.00    --  -18.25 -57.00 -60.00  124
  2  ω    -20.00  26.50   0.75   20.00    --  -18.25 -99.00-150.00   62
  3  ω    -42.00  51.00   0.75   20.00    --  -18.25  57.00  90.00  124
  4  ω    -10.00  89.00   0.75   20.00    --   19.43  38.00-120.00  132
;
_diffrn_measurement_device       'CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0556377000
_diffrn_orient_matrix_UB_12      0.0059055000
_diffrn_orient_matrix_UB_13      -0.0122015000
_diffrn_orient_matrix_UB_21      -0.0452725000
_diffrn_orient_matrix_UB_22      0.0023496000
_diffrn_orient_matrix_UB_23      -0.0217694000
_diffrn_orient_matrix_UB_31      0.0016148000
_diffrn_orient_matrix_UB_32      0.0411357000
_diffrn_orient_matrix_UB_33      0.0069323000
_diffrn_radiation_collimation    '0.5 mm collimator'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_unetI/netI     0.1289
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            25735
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         4.214
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40_mA
_diffrn_source_power             2.00_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50_kV
_exptl_absorpt_coefficient_mu    0.165
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         16587
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1607
_refine_ls_R_factor_gt           0.0733
_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)+(0.0593P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8233
_reflns_number_total             16587
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo0c00114_si_002.cif
_cod_data_source_block           wo026
_cod_original_cell_volume        4748.9(3)
_cod_database_code               4038215
_shelx_estimated_absorpt_t_min   0.932
_shelx_estimated_absorpt_t_max   0.978
_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.
;
_shelxl_version_number           2014-3
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
C1 C 0.2671(5) 0.5620(3) 0.09439(18) 0.0425(13) Uani 1 1 d . . . . .
H1 H 0.3086 0.5288 0.0724 0.051 Uiso 1 1 calc R U . . .
C2 C 0.2682(5) 0.6397(2) 0.08891(16) 0.0337(12) Uani 1 1 d . . . . .
H2 H 0.3083 0.6579 0.0635 0.040 Uiso 1 1 calc R U . . .
C3 C 0.2108(4) 0.6928(2) 0.12040(15) 0.0262(10) Uani 1 1 d . . . . .
C4 C 0.1546(4) 0.6585(2) 0.15657(15) 0.0302(11) Uani 1 1 d . . . . .
H4 H 0.1149 0.6902 0.1798 0.036 Uiso 1 1 calc R U . . .
C5 C 0.1572(5) 0.5800(3) 0.15839(18) 0.0440(13) Uani 1 1 d . . . . .
H5 H 0.1166 0.5597 0.1831 0.053 Uiso 1 1 calc R U . . .
C6 C 0.1508(4) 0.9172(2) 0.11214(14) 0.0226(10) Uani 1 1 d . . . . .
C7 C 0.1740(4) 0.9088(2) 0.06409(15) 0.0289(11) Uani 1 1 d . . . . .
H7 H 0.2026 0.8611 0.0499 0.035 Uiso 1 1 calc R U . . .
C8 C 0.1556(5) 0.9694(3) 0.03700(16) 0.0345(11) Uani 1 1 d . . . . .
H8 H 0.1732 0.9638 0.0045 0.041 Uiso 1 1 calc R U . . .
C9 C 0.1114(5) 1.0385(3) 0.05742(17) 0.0379(12) Uani 1 1 d . . . . .
H9 H 0.0961 1.0797 0.0385 0.045 Uiso 1 1 calc R U . . .
C10 C 0.0896(5) 1.0476(2) 0.10505(17) 0.0345(11) Uani 1 1 d . . . . .
H10 H 0.0609 1.0953 0.1192 0.041 Uiso 1 1 calc R U . . .
C11 C 0.1094(4) 0.9876(2) 0.13206(16) 0.0310(11) Uani 1 1 d . . . . .
H11 H 0.0945 0.9943 0.1649 0.037 Uiso 1 1 calc R U . . .
C12 C 0.2926(4) 0.8764(2) 0.19947(14) 0.0224(10) Uani 1 1 d . . . . .
C13 C 0.4117(4) 0.9179(2) 0.19305(15) 0.0257(10) Uani 1 1 d . . . . .
H13 H 0.4218 0.9284 0.1614 0.031 Uiso 1 1 calc R U . . .
C14 C 0.5148(5) 0.9438(2) 0.23209(16) 0.0326(11) Uani 1 1 d . . . . .
H14 H 0.5939 0.9731 0.2273 0.039 Uiso 1 1 calc R U . . .
C15 C 0.5028(5) 0.9269(2) 0.27798(17) 0.0352(12) Uani 1 1 d . . . . .
H15 H 0.5742 0.9440 0.3047 0.042 Uiso 1 1 calc R U . . .
C16 C 0.3873(5) 0.8854(3) 0.28493(16) 0.0369(12) Uani 1 1 d . . . . .
H16 H 0.3795 0.8735 0.3165 0.044 Uiso 1 1 calc R U . . .
C17 C 0.2819(5) 0.8609(2) 0.24619(15) 0.0307(11) Uani 1 1 d . . . . .
H17 H 0.2018 0.8332 0.2516 0.037 Uiso 1 1 calc R U . . .
C18 C 0.5326(4) 0.7159(2) 0.20400(15) 0.0279(10) Uani 1 1 d . . . . .
H18A H 0.5473 0.7613 0.2306 0.034 Uiso 1 1 calc R U . . .
H18B H 0.4546 0.7248 0.1797 0.034 Uiso 1 1 calc R U . . .
C19 C 0.4967(5) 0.6422(2) 0.22512(16) 0.0382(12) Uani 1 1 d . . . . .
H19A H 0.5812 0.6212 0.2388 0.046 Uiso 1 1 calc R U . . .
H19B H 0.4470 0.6019 0.1985 0.046 Uiso 1 1 calc R U . . .
C20 C 0.4106(5) 0.6565(3) 0.26492(15) 0.0388(12) Uani 1 1 d . . . . .
H20A H 0.3373 0.6885 0.2538 0.047 Uiso 1 1 calc R U . . .
H20B H 0.3678 0.6055 0.2699 0.047 Uiso 1 1 calc R U . . .
C21 C 0.4898(5) 0.6976(3) 0.31296(17) 0.0568(15) Uani 1 1 d . . . . .
H21A H 0.4284 0.7074 0.3365 0.085 Uiso 1 1 calc R U . . .
H21B H 0.5343 0.7476 0.3082 0.085 Uiso 1 1 calc R U . . .
H21C H 0.5583 0.6645 0.3255 0.085 Uiso 1 1 calc R U . . .
C22 C 0.8235(4) 0.7012(2) 0.21910(14) 0.0281(10) Uani 1 1 d . . . . .
H22A H 0.8099 0.6492 0.2295 0.034 Uiso 1 1 calc R U . . .
H22B H 0.9038 0.7012 0.2028 0.034 Uiso 1 1 calc R U . . .
C23 C 0.8541(5) 0.7635(2) 0.26481(16) 0.0428(13) Uani 1 1 d . . . . .
H23A H 0.9080 0.8093 0.2576 0.051 Uiso 1 1 calc R U . . .
H23B H 0.7678 0.7812 0.2728 0.051 Uiso 1 1 calc R U . . .
C24 C 0.9305(6) 0.7346(4) 0.3090(2) 0.086(2) Uani 1 1 d . . . . .
H24A H 0.9501 0.7794 0.3360 0.104 Uiso 1 1 calc R U . . .
H24B H 0.8690 0.6950 0.3191 0.104 Uiso 1 1 calc R U . . .
C25 C 1.0543(6) 0.7011(3) 0.3046(2) 0.0764(19) Uani 1 1 d . . . . .
H25A H 1.0935 0.6864 0.3360 0.115 Uiso 1 1 calc R U . . .
H25B H 1.1178 0.7396 0.2951 0.115 Uiso 1 1 calc R U . . .
H25C H 1.0367 0.6544 0.2796 0.115 Uiso 1 1 calc R U . . .
C26 C 0.6566(4) 0.6310(2) 0.12711(15) 0.0312(11) Uani 1 1 d . . . . .
H26A H 0.6341 0.5825 0.1405 0.037 Uiso 1 1 calc R U . . .
H26B H 0.5791 0.6378 0.1020 0.037 Uiso 1 1 calc R U . . .
C27 C 0.7813(4) 0.6213(2) 0.10308(15) 0.0314(11) Uani 1 1 d . . . . .
H27A H 0.8095 0.6716 0.0927 0.038 Uiso 1 1 calc R U . . .
H27B H 0.8563 0.6088 0.1274 0.038 Uiso 1 1 calc R U . . .
C28 C 0.7566(5) 0.5575(3) 0.05934(16) 0.0453(13) Uani 1 1 d . . . . .
H28A H 0.6952 0.5751 0.0326 0.054 Uiso 1 1 calc R U . . .
H28B H 0.7105 0.5102 0.0681 0.054 Uiso 1 1 calc R U . . .
C29 C 0.8857(5) 0.5357(3) 0.04101(17) 0.0507(15) Uani 1 1 d . . . . .
H29A H 0.8623 0.4985 0.0106 0.076 Uiso 1 1 calc R U . . .
H29B H 0.9417 0.5115 0.0657 0.076 Uiso 1 1 calc R U . . .
H29C H 0.9360 0.5831 0.0349 0.076 Uiso 1 1 calc R U . . .
C30 C 0.7041(4) 0.8028(2) 0.15112(14) 0.0266(10) Uani 1 1 d . . . . .
H30A H 0.7017 0.8473 0.1771 0.032 Uiso 1 1 calc R U . . .
H30B H 0.7954 0.8065 0.1422 0.032 Uiso 1 1 calc R U . . .
C31 C 0.6013(4) 0.8115(2) 0.10682(15) 0.0306(11) Uani 1 1 d . . . . .
H31A H 0.5090 0.8024 0.1142 0.037 Uiso 1 1 calc R U . . .
H31B H 0.6109 0.7713 0.0792 0.037 Uiso 1 1 calc R U . . .
C32 C 0.6198(5) 0.8931(2) 0.09201(16) 0.0372(12) Uani 1 1 d . . . . .
H32A H 0.5418 0.8992 0.0669 0.045 Uiso 1 1 calc R U . . .
H32B H 0.6190 0.9330 0.1208 0.045 Uiso 1 1 calc R U . . .
C33 C 0.7488(5) 0.9094(3) 0.07212(18) 0.0520(14) Uani 1 1 d . . . . .
H33A H 0.7569 0.9640 0.0661 0.078 Uiso 1 1 calc R U . . .
H33B H 0.7463 0.8741 0.0415 0.078 Uiso 1 1 calc R U . . .
H33C H 0.8267 0.9008 0.0959 0.078 Uiso 1 1 calc R U . . .
C34 C 0.7971(5) 0.4477(3) 0.18188(19) 0.0498(14) Uani 1 1 d . . . . .
H34 H 0.8412 0.4699 0.1587 0.060 Uiso 1 1 calc R U . . .
C35 C 0.7998(5) 0.3690(2) 0.18221(17) 0.0393(12) Uani 1 1 d . . . . .
H35 H 0.8411 0.3387 0.1588 0.047 Uiso 1 1 calc R U . . .
C36 C 0.7417(4) 0.3321(2) 0.21690(15) 0.0304(11) Uani 1 1 d . . . . .
C37 C 0.6804(5) 0.3838(2) 0.24828(16) 0.0377(12) Uani 1 1 d . . . . .
H37 H 0.6379 0.3644 0.2728 0.045 Uiso 1 1 calc R U . . .
C38 C 0.6817(5) 0.4619(3) 0.24361(19) 0.0482(14) Uani 1 1 d . . . . .
H38 H 0.6384 0.4939 0.2656 0.058 Uiso 1 1 calc R U . . .
C39 C 0.6831(4) 0.1479(2) 0.13601(15) 0.0240(10) Uani 1 1 d . . . . .
C40 C 0.5625(4) 0.1079(2) 0.14037(15) 0.0274(10) Uani 1 1 d . . . . .
H40 H 0.5441 0.1019 0.1719 0.033 Uiso 1 1 calc R U . . .
C41 C 0.4683(5) 0.0764(2) 0.09964(17) 0.0369(12) Uani 1 1 d . . . . .
H41 H 0.3865 0.0485 0.1032 0.044 Uiso 1 1 calc R U . . .
C42 C 0.4935(5) 0.0857(3) 0.05386(17) 0.0405(13) Uani 1 1 d . . . . .
H42 H 0.4281 0.0650 0.0259 0.049 Uiso 1 1 calc R U . . .
C43 C 0.6133(5) 0.1251(3) 0.04842(17) 0.0443(13) Uani 1 1 d . . . . .
H43 H 0.6313 0.1307 0.0168 0.053 Uiso 1 1 calc R U . . .
C44 C 0.7063(5) 0.1560(2) 0.08910(16) 0.0368(12) Uani 1 1 d . . . . .
H44 H 0.7882 0.1835 0.0852 0.044 Uiso 1 1 calc R U . . .
C45 C 0.8217(4) 0.1104(2) 0.22478(15) 0.0240(10) Uani 1 1 d . . . . .
C46 C 0.8028(4) 0.1168(2) 0.27258(15) 0.0287(11) Uani 1 1 d . . . . .
H46 H 0.7723 0.1634 0.2875 0.034 Uiso 1 1 calc R U . . .
C47 C 0.8277(5) 0.0560(2) 0.29922(16) 0.0351(12) Uani 1 1 d . . . . .
H47 H 0.8137 0.0611 0.3322 0.042 Uiso 1 1 calc R U . . .
C48 C 0.8729(4) -0.0124(2) 0.27808(15) 0.0304(11) Uani 1 1 d . . . . .
H48 H 0.8923 -0.0536 0.2966 0.037 Uiso 1 1 calc R U . . .
C49 C 0.8894(4) -0.0196(2) 0.22952(15) 0.0264(10) Uani 1 1 d . . . . .
H49 H 0.9182 -0.0665 0.2143 0.032 Uiso 1 1 calc R U . . .
C50 C 0.8642(4) 0.0409(2) 0.20357(15) 0.0261(10) Uani 1 1 d . . . . .
H50 H 0.8759 0.0354 0.1704 0.031 Uiso 1 1 calc R U . . .
C51 C 0.3358(5) 0.2345(2) 0.18543(15) 0.0353(12) Uani 1 1 d . . . . .
H51A H 0.3460 0.1917 0.1593 0.042 Uiso 1 1 calc R U . . .
H51B H 0.4279 0.2553 0.2026 0.042 Uiso 1 1 calc R U . . .
C52 C 0.2612(5) 0.1993(2) 0.22147(16) 0.0374(12) Uani 1 1 d . . . . .
H52A H 0.1657 0.1842 0.2060 0.045 Uiso 1 1 calc R U . . .
H52B H 0.2622 0.2397 0.2502 0.045 Uiso 1 1 calc R U . . .
C53 C 0.3220(5) 0.1279(2) 0.23860(16) 0.0344(12) Uani 1 1 d D . . . .
H53A H 0.3211 0.0873 0.2100 0.041 Uiso 1 1 calc R U . . .
H53B H 0.4173 0.1428 0.2543 0.041 Uiso 1 1 calc R U . . .
C54 C 0.2460(5) 0.0944(3) 0.27398(16) 0.0441(13) Uani 1 1 d D . . . .
H54A H 0.2849 0.0468 0.2827 0.066 Uiso 1 1 calc R U . . .
H54B H 0.1508 0.0814 0.2590 0.066 Uiso 1 1 calc R U . . .
H54C H 0.2526 0.1331 0.3035 0.066 Uiso 1 1 calc R U . . .
C55 C 0.3876(5) 0.3681(2) 0.13556(16) 0.0359(12) Uani 1 1 d . . . . .
H55A H 0.3483 0.4149 0.1246 0.043 Uiso 1 1 calc R U . . .
H55B H 0.4627 0.3868 0.1630 0.043 Uiso 1 1 calc R U . . .
C56 C 0.4445(5) 0.3248(3) 0.09419(17) 0.0423(13) Uani 1 1 d . . . . .
H56A H 0.3691 0.2973 0.0692 0.051 Uiso 1 1 calc R U . . .
H56B H 0.5005 0.2848 0.1067 0.051 Uiso 1 1 calc R U . . .
C57 C 0.5295(5) 0.3792(3) 0.07077(17) 0.0518(15) Uani 1 1 d D . . . .
H57A H 0.4730 0.4196 0.0590 0.062 Uiso 1 1 calc R U . . .
H57B H 0.6042 0.4065 0.0961 0.062 Uiso 1 1 calc R U . . .
C58 C 0.5880(6) 0.3413(3) 0.0297(2) 0.079(2) Uani 1 1 d D . . . .
H58A H 0.6426 0.3808 0.0173 0.118 Uiso 1 1 calc R U . . .
H58B H 0.5150 0.3162 0.0035 0.118 Uiso 1 1 calc R U . . .
H58C H 0.6452 0.3015 0.0408 0.118 Uiso 1 1 calc R U . . .
C59 C 0.1330(5) 0.2699(2) 0.10675(16) 0.0369(12) Uani 1 1 d . . . . .
H59A H 0.1741 0.2330 0.0844 0.044 Uiso 1 1 calc R U . . .
H59B H 0.0627 0.2388 0.1190 0.044 Uiso 1 1 calc R U . . .
C60 C 0.0641(5) 0.3282(3) 0.07724(17) 0.0458(14) Uani 1 1 d . . . . .
H60A H 0.1336 0.3682 0.0720 0.055 Uiso 1 1 calc R U . . .
H60B H 0.0017 0.3553 0.0963 0.055 Uiso 1 1 calc R U . . .
C61 C -0.0155(5) 0.2892(3) 0.02762(17) 0.0526(14) Uani 1 1 d D . . . .
H61A H -0.0804 0.2465 0.0328 0.063 Uiso 1 1 calc R U . . .
H61B H -0.0683 0.3284 0.0125 0.063 Uiso 1 1 calc R U . . .
C62 C 0.0712(6) 0.2559(3) -0.00692(18) 0.0628(17) Uani 1 1 d D . . . .
H62A H 0.0161 0.2395 -0.0393 0.094 Uiso 1 1 calc R U . . .
H62B H 0.1111 0.2105 0.0048 0.094 Uiso 1 1 calc R U . . .
H62C H 0.1434 0.2959 -0.0090 0.094 Uiso 1 1 calc R U . . .
C63 C 0.1847(5) 0.3730(2) 0.20041(17) 0.0438(13) Uani 1 1 d . . . . .
H63A H 0.1358 0.4117 0.1833 0.053 Uiso 1 1 calc R U . . .
H63B H 0.1180 0.3404 0.2134 0.053 Uiso 1 1 calc R U . . .
C64 C 0.2873(6) 0.4154(3) 0.24188(17) 0.0639(18) Uani 1 1 d . . . . .
H64A H 0.3274 0.4625 0.2309 0.077 Uiso 1 1 calc R U . . .
H64B H 0.3606 0.3811 0.2483 0.077 Uiso 1 1 calc R U . . .
C65 C 0.2409(7) 0.4419(4) 0.2903(2) 0.102(2) Uiso 1 1 d D . . . .
H65A H 0.2176 0.3952 0.3053 0.122 Uiso 1 1 calc R U . . .
H65B H 0.3162 0.4745 0.3129 0.122 Uiso 1 1 calc R U . . .
C66 C 0.1271(7) 0.4856(4) 0.2841(3) 0.109(2) Uiso 1 1 d D . . . .
H66A H 0.1449 0.5273 0.2649 0.163 Uiso 1 1 calc R U . . .
H66B H 0.1102 0.5090 0.3162 0.163 Uiso 1 1 calc R U . . .
H66C H 0.0476 0.4508 0.2671 0.163 Uiso 1 1 calc R U . . .
C67 C 0.8228(5) 0.4352(3) 0.50713(19) 0.0488(14) Uani 1 1 d . . . . .
H67 H 0.8630 0.4554 0.4824 0.059 Uiso 1 1 calc R U . . .
C68 C 0.8273(5) 0.3564(2) 0.50942(16) 0.0340(11) Uani 1 1 d . . . . .
H68 H 0.8693 0.3251 0.4867 0.041 Uiso 1 1 calc R U . . .
C69 C 0.7704(4) 0.3219(2) 0.54499(15) 0.0281(10) Uani 1 1 d . . . . .
C70 C 0.7108(5) 0.3756(2) 0.57591(17) 0.0401(13) Uani 1 1 d . . . . .
H70 H 0.6694 0.3578 0.6011 0.048 Uiso 1 1 calc R U . . .
C71 C 0.7120(6) 0.4532(3) 0.5699(2) 0.0559(16) Uani 1 1 d . . . . .
H71 H 0.6697 0.4864 0.5915 0.067 Uiso 1 1 calc R U . . .
C72 C 0.6890(4) 0.1332(2) 0.46917(14) 0.0235(10) Uani 1 1 d . . . . .
C73 C 0.5717(4) 0.0949(2) 0.47854(15) 0.0257(10) Uani 1 1 d . . . . .
H73 H 0.5627 0.0906 0.5113 0.031 Uiso 1 1 calc R U . . .
C74 C 0.4681(4) 0.0629(2) 0.44115(16) 0.0300(11) Uani 1 1 d . . . . .
H74 H 0.3893 0.0363 0.4483 0.036 Uiso 1 1 calc R U . . .
C75 C 0.4786(5) 0.0696(2) 0.39325(17) 0.0372(12) Uani 1 1 d . . . . .
H75 H 0.4067 0.0483 0.3675 0.045 Uiso 1 1 calc R U . . .
C76 C 0.5928(5) 0.1070(3) 0.38322(17) 0.0396(13) Uani 1 1 d . . . . .
H76 H 0.6003 0.1115 0.3504 0.047 Uiso 1 1 calc R U . . .
C77 C 0.6980(5) 0.1384(2) 0.42061(16) 0.0335(11) Uani 1 1 d . . . . .
H77 H 0.7772 0.1639 0.4130 0.040 Uiso 1 1 calc R U . . .
C78 C 0.8419(4) 0.1007(2) 0.55586(15) 0.0241(10) Uani 1 1 d . . . . .
C79 C 0.8261(4) 0.1107(2) 0.60475(15) 0.0306(11) Uani 1 1 d . . . . .
H79 H 0.7974 0.1585 0.6189 0.037 Uiso 1 1 calc R U . . .
C80 C 0.8516(4) 0.0520(2) 0.63282(16) 0.0340(11) Uani 1 1 d . . . . .
H80 H 0.8404 0.0597 0.6661 0.041 Uiso 1 1 calc R U . . .
C81 C 0.8935(4) -0.0179(2) 0.61290(16) 0.0320(11) Uani 1 1 d . . . . .
H81 H 0.9118 -0.0580 0.6324 0.038 Uiso 1 1 calc R U . . .
C82 C 0.9085(4) -0.0290(2) 0.56424(15) 0.0280(11) Uani 1 1 d . . . . .
H82 H 0.9366 -0.0770 0.5502 0.034 Uiso 1 1 calc R U . . .
C83 C 0.8828(4) 0.0292(2) 0.53628(15) 0.0241(10) Uani 1 1 d . . . . .
H83 H 0.8930 0.0208 0.5029 0.029 Uiso 1 1 calc R U . . .
C84 C 0.4475(4) 0.2875(2) 0.45973(16) 0.0352(11) Uani 1 1 d . . . . .
H84A H 0.5271 0.2821 0.4844 0.042 Uiso 1 1 calc R U . . .
H84B H 0.4331 0.2395 0.4352 0.042 Uiso 1 1 calc R U . . .
C85 C 0.4801(5) 0.3573(3) 0.43452(18) 0.0474(14) Uani 1 1 d . . . . .
H85A H 0.3945 0.3753 0.4193 0.057 Uiso 1 1 calc R U . . .
H85B H 0.5280 0.4008 0.4593 0.057 Uiso 1 1 calc R U . . .
C86 C 0.5665(5) 0.3388(3) 0.39579(19) 0.0551(15) Uani 1 1 d . . . . .
H86A H 0.6032 0.3887 0.3871 0.066 Uiso 1 1 calc R U . . .
H86B H 0.6442 0.3121 0.4098 0.066 Uiso 1 1 calc R U . . .
C87 C 0.4940(6) 0.2880(3) 0.34991(18) 0.0655(17) Uani 1 1 d . . . . .
H87A H 0.5576 0.2773 0.3273 0.098 Uiso 1 1 calc R U . . .
H87B H 0.4204 0.3153 0.3345 0.098 Uiso 1 1 calc R U . . .
H87C H 0.4566 0.2384 0.3580 0.098 Uiso 1 1 calc R U . . .
C88 C 0.2785(5) 0.2039(2) 0.51530(15) 0.0321(11) Uani 1 1 d . . . . .
H88A H 0.1867 0.1994 0.5237 0.039 Uiso 1 1 calc R U . . .
H88B H 0.2839 0.1587 0.4901 0.039 Uiso 1 1 calc R U . . .
C89 C 0.3805(5) 0.1988(2) 0.56033(15) 0.0329(11) Uani 1 1 d . . . . .
H89A H 0.3710 0.2415 0.5866 0.039 Uiso 1 1 calc R U . . .
H89B H 0.4729 0.2065 0.5527 0.039 Uiso 1 1 calc R U . . .
C90 C 0.3622(5) 0.1199(2) 0.57860(16) 0.0360(12) Uani 1 1 d . . . . .
H90A H 0.3572 0.0773 0.5507 0.043 Uiso 1 1 calc R U . . .
H90B H 0.4431 0.1147 0.6027 0.043 Uiso 1 1 calc R U . . .
C91 C 0.2384(5) 0.1088(3) 0.60178(17) 0.0496(14) Uani 1 1 d . . . . .
H91A H 0.2312 0.0561 0.6108 0.074 Uiso 1 1 calc R U . . .
H91B H 0.1578 0.1152 0.5785 0.074 Uiso 1 1 calc R U . . .
H91C H 0.2458 0.1480 0.6311 0.074 Uiso 1 1 calc R U . . .
C92 C 0.3260(5) 0.3757(2) 0.53657(15) 0.0371(12) Uani 1 1 d . . . . .
H92A H 0.4071 0.3708 0.5607 0.045 Uiso 1 1 calc R U . . .
H92B H 0.3433 0.4238 0.5220 0.045 Uiso 1 1 calc R U . . .
C93 C 0.2058(5) 0.3844(2) 0.56280(17) 0.0416(13) Uani 1 1 d . . . . .
H93A H 0.1832 0.3346 0.5748 0.050 Uiso 1 1 calc R U . . .
H93B H 0.1266 0.3943 0.5394 0.050 Uiso 1 1 calc R U . . .
C94 C 0.2336(6) 0.4510(3) 0.60563(18) 0.0541(15) Uani 1 1 d . . . . .
H94A H 0.3027 0.4370 0.6315 0.065 Uiso 1 1 calc R U . . .
H94B H 0.2705 0.4989 0.5947 0.065 Uiso 1 1 calc R U . . .
C95 C 0.1087(6) 0.4680(3) 0.6265(2) 0.079(2) Uani 1 1 d . . . . .
H95A H 0.1319 0.5099 0.6546 0.119 Uiso 1 1 calc R U . . .
H95B H 0.0710 0.4205 0.6371 0.119 Uiso 1 1 calc R U . . .
H95C H 0.0417 0.4847 0.6016 0.119 Uiso 1 1 calc R U . . .
C96 C 0.1557(4) 0.3019(2) 0.44599(15) 0.0334(11) Uani 1 1 d . . . . .
H96A H 0.0747 0.2948 0.4614 0.040 Uiso 1 1 calc R U . A 1
H96B H 0.1615 0.3560 0.4381 0.040 Uiso 1 1 calc R U . A 1
C97B C 0.1350(6) 0.2457(3) 0.39881(19) 0.0571(16) Uani 0.27(2) 1 d . . P B 1
H97A H 0.2054 0.2615 0.3801 0.068 Uiso 0.27(2) 1 calc R U P B 1
H97B H 0.1529 0.1931 0.4072 0.068 Uiso 0.27(2) 1 calc R U P B 1
C98B C 0.008(2) 0.2370(12) 0.3666(9) 0.031(6) Uiso 0.27(2) 1 d . . P B 1
H98A H -0.0671 0.2262 0.3845 0.037 Uiso 0.27(2) 1 calc R U P B 1
H98B H 0.0049 0.1931 0.3397 0.037 Uiso 0.27(2) 1 calc R U P B 1
C99B C -0.006(4) 0.3209(16) 0.3448(11) 0.068(9) Uiso 0.27(2) 1 d . . P B 1
H99A H -0.0950 0.3386 0.3476 0.102 Uiso 0.27(2) 1 calc R U P B 1
H99B H 0.0047 0.3133 0.3104 0.102 Uiso 0.27(2) 1 calc R U P B 1
H99C H 0.0647 0.3605 0.3635 0.102 Uiso 0.27(2) 1 calc R U P B 1
C97 C 0.1350(6) 0.2457(3) 0.39881(19) 0.0571(16) Uani 0.73(2) 1 d . . P B 2
H97C H 0.2238 0.2407 0.3883 0.068 Uiso 0.73(2) 1 calc R U P B 2
H97D H 0.1015 0.1934 0.4051 0.068 Uiso 0.73(2) 1 calc R U P B 2
C98 C 0.0397(14) 0.2680(9) 0.3581(4) 0.094(4) Uani 0.73(2) 1 d . . P B 2
H98C H 0.0962 0.2993 0.3404 0.113 Uiso 0.73(2) 1 calc R U P B 2
H98D H 0.0076 0.2184 0.3358 0.113 Uiso 0.73(2) 1 calc R U P B 2
C99 C -0.0748(11) 0.3076(6) 0.3610(4) 0.069(4) Uani 0.73(2) 1 d . . P B 2
H99D H -0.1179 0.3141 0.3281 0.103 Uiso 0.73(2) 1 calc R U P B 2
H99E H -0.1385 0.2774 0.3761 0.103 Uiso 0.73(2) 1 calc R U P B 2
H99F H -0.0488 0.3593 0.3808 0.103 Uiso 0.73(2) 1 calc R U P B 2
N1 N 0.2154(3) 0.76962(18) 0.11448(12) 0.0264(8) Uani 1 1 d . . . . .
N2 N 0.2119(4) 0.5288(2) 0.12835(16) 0.0479(11) Uani 1 1 d . . . . .
N3 N 0.7406(4) 0.25481(18) 0.22231(12) 0.0288(9) Uani 1 1 d . . . . .
N4 N 0.7374(5) 0.4969(2) 0.21165(17) 0.0526(12) Uani 1 1 d . . . . .
N5 N 0.7675(4) 0.24569(18) 0.55147(12) 0.0287(9) Uani 1 1 d . . . . .
N6 N 0.7670(5) 0.4860(2) 0.53650(17) 0.0539(13) Uani 1 1 d . . . . .
O1 O 0.0310(3) 0.82374(14) 0.16737(10) 0.0295(7) Uani 1 1 d . . . . .
O2 O 0.9378(3) 0.21008(15) 0.17282(11) 0.0358(8) Uani 1 1 d . . . . .
O3 O 0.9495(3) 0.19163(15) 0.49720(10) 0.0320(7) Uani 1 1 d . . . . .
P1 P 0.15965(11) 0.83776(6) 0.14823(4) 0.0238(3) Uani 1 1 d . . . . .
P2 P 0.67957(11) 0.71321(6) 0.17541(4) 0.0246(3) Uani 1 1 d . . . . .
P3 P 0.80670(12) 0.19044(6) 0.18939(4) 0.0257(3) Uani 1 1 d . . . . .
P4 P 0.26063(13) 0.31098(6) 0.15732(4) 0.0299(3) Uani 1 1 d . . . . .
P5 P 0.82445(12) 0.17734(6) 0.51836(4) 0.0259(3) Uani 1 1 d . . . . .
P6 P 0.30125(12) 0.29278(6) 0.48962(4) 0.0276(3) 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'
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
N2 C1 C2 125.4(4) . . ?
C1 C2 C3 120.8(4) . . ?
N1 C3 C2 119.4(4) . . ?
N1 C3 C4 126.6(4) . . ?
C2 C3 C4 114.0(4) . . ?
C5 C4 C3 120.5(4) . . ?
N2 C5 C4 125.8(4) . . ?
C11 C6 C7 118.7(4) . . ?
C11 C6 P1 118.3(3) . . ?
C7 C6 P1 122.8(3) . . ?
C8 C7 C6 120.3(4) . . ?
C7 C8 C9 119.8(4) . . ?
C10 C9 C8 120.1(4) . . ?
C11 C10 C9 119.9(4) . . ?
C10 C11 C6 121.1(4) . . ?
C17 C12 C13 118.0(4) . . ?
C17 C12 P1 120.2(3) . . ?
C13 C12 P1 121.6(3) . . ?
C14 C13 C12 121.0(4) . . ?
C15 C14 C13 120.0(4) . . ?
C16 C15 C14 119.9(5) . . ?
C15 C16 C17 120.5(4) . . ?
C16 C17 C12 120.5(4) . . ?
C19 C18 P2 114.6(3) . . ?
C18 C19 C20 113.0(3) . . ?
C21 C20 C19 113.4(4) . . ?
C23 C22 P2 115.7(3) . . ?
C24 C23 C22 113.6(4) . . ?
C25 C24 C23 118.3(5) . . ?
C27 C26 P2 113.0(3) . . ?
C28 C27 C26 112.6(4) . . ?
C27 C28 C29 113.4(4) . . ?
C31 C30 P2 115.1(3) . . ?
C30 C31 C32 111.6(4) . . ?
C33 C32 C31 114.4(4) . . ?
N4 C34 C35 125.7(5) . . ?
C34 C35 C36 120.7(4) . . ?
N3 C36 C35 126.9(4) . . ?
N3 C36 C37 119.7(4) . . ?
C35 C36 C37 113.5(4) . . ?
C38 C37 C36 120.4(4) . . ?
N4 C38 C37 126.4(5) . . ?
C40 C39 C44 117.8(4) . . ?
C40 C39 P3 121.5(3) . . ?
C44 C39 P3 120.7(3) . . ?
C41 C40 C39 121.2(4) . . ?
C42 C41 C40 119.8(4) . . ?
C41 C42 C43 120.3(5) . . ?
C44 C43 C42 119.5(5) . . ?
C43 C44 C39 121.5(4) . . ?
C46 C45 C50 118.5(4) . . ?
C46 C45 P3 123.2(3) . . ?
C50 C45 P3 118.1(3) . . ?
C45 C46 C47 120.7(4) . . ?
C46 C47 C48 120.4(4) . . ?
C49 C48 C47 118.9(4) . . ?
C50 C49 C48 120.0(4) . . ?
C49 C50 C45 121.5(4) . . ?
C52 C51 P4 116.7(3) . . ?
C51 C52 C53 113.2(4) . . ?
C54 C53 C52 111.9(4) . . ?
C56 C55 P4 114.4(3) . . ?
C55 C56 C57 112.1(4) . . ?
C58 C57 C56 115.4(4) . . ?
C60 C59 P4 116.1(3) . . ?
C59 C60 C61 112.9(4) . . ?
C62 C61 C60 113.8(4) . . ?
C64 C63 P4 112.2(4) . . ?
C63 C64 C65 118.3(5) . . ?
C66 C65 C64 112.0(6) . . ?
N6 C67 C68 126.1(5) . . ?
C67 C68 C69 120.6(4) . . ?
N5 C69 C68 126.9(4) . . ?
N5 C69 C70 119.7(4) . . ?
C68 C69 C70 113.4(4) . . ?
C71 C70 C69 120.7(5) . . ?
N6 C71 C70 126.0(5) . . ?
C73 C72 C77 117.6(4) . . ?
C73 C72 P5 121.5(3) . . ?
C77 C72 P5 120.9(3) . . ?
C74 C73 C72 121.2(4) . . ?
C73 C74 C75 120.2(4) . . ?
C76 C75 C74 119.6(5) . . ?
C75 C76 C77 120.5(4) . . ?
C76 C77 C72 120.9(4) . . ?
C79 C78 C83 117.8(4) . . ?
C79 C78 P5 123.3(3) . . ?
C83 C78 P5 118.7(3) . . ?
C80 C79 C78 120.7(4) . . ?
C79 C80 C81 120.5(4) . . ?
C80 C81 C82 119.5(4) . . ?
C83 C82 C81 120.0(4) . . ?
C82 C83 C78 121.4(4) . . ?
C85 C84 P6 115.4(3) . . ?
C86 C85 C84 113.1(4) . . ?
C87 C86 C85 114.7(4) . . ?
C89 C88 P6 114.5(3) . . ?
C88 C89 C90 112.2(4) . . ?
C91 C90 C89 114.4(4) . . ?
C93 C92 P6 113.1(3) . . ?
C92 C93 C94 112.3(4) . . ?
C95 C94 C93 112.3(5) . . ?
C97B C96 P6 116.2(3) . . ?
C98B C97B C96 119.7(10) . . ?
C97B C98B C99B 106.3(19) . . ?
C3 N1 P1 125.6(3) . . ?
C5 N2 C1 113.5(4) . . ?
C36 N3 P3 124.6(3) . . ?
C38 N4 C34 113.3(4) . . ?
C69 N5 P5 125.8(3) . . ?
C71 N6 C67 113.3(4) . . ?
O1 P1 N1 121.19(17) . . ?
O1 P1 C6 110.95(17) . . ?
N1 P1 C6 103.57(18) . . ?
O1 P1 C12 108.33(17) . . ?
N1 P1 C12 108.45(18) . . ?
C6 P1 C12 102.80(18) . . ?
C22 P2 C30 110.6(2) . . ?
C22 P2 C18 109.7(2) . . ?
C30 P2 C18 108.72(18) . . ?
C22 P2 C26 108.11(19) . . ?
C30 P2 C26 109.97(19) . . ?
C18 P2 C26 109.75(19) . . ?
O2 P3 N3 121.05(18) . . ?
O2 P3 C45 110.13(18) . . ?
N3 P3 C45 103.88(18) . . ?
O2 P3 C39 108.12(18) . . ?
N3 P3 C39 109.38(19) . . ?
C45 P3 C39 102.74(18) . . ?
C59 P4 C51 109.9(2) . . ?
C59 P4 C55 108.7(2) . . ?
C51 P4 C55 109.3(2) . . ?
C59 P4 C63 108.8(2) . . ?
C51 P4 C63 110.4(2) . . ?
C55 P4 C63 109.8(2) . . ?
O3 P5 N5 121.72(18) . . ?
O3 P5 C78 110.65(17) . . ?
N5 P5 C78 103.86(18) . . ?
O3 P5 C72 108.40(18) . . ?
N5 P5 C72 108.51(18) . . ?
C78 P5 C72 101.88(19) . . ?
C92 P6 C96 109.0(2) . . ?
C92 P6 C88 110.1(2) . . ?
C96 P6 C88 110.0(2) . . ?
C92 P6 C84 110.2(2) . . ?
C96 P6 C84 109.5(2) . . ?
C88 P6 C84 108.0(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
C1 N2 1.348(6) . ?
C1 C2 1.373(6) . ?
C2 C3 1.405(5) . ?
C3 N1 1.358(5) . ?
C3 C4 1.414(5) . ?
C4 C5 1.366(5) . ?
C5 N2 1.347(5) . ?
C6 C11 1.388(5) . ?
C6 C7 1.395(5) . ?
C6 P1 1.813(4) . ?
C7 C8 1.383(5) . ?
C8 C9 1.387(6) . ?
C9 C10 1.378(5) . ?
C10 C11 1.374(6) . ?
C12 C17 1.392(5) . ?
C12 C13 1.401(5) . ?
C12 P1 1.816(4) . ?
C13 C14 1.383(6) . ?
C14 C15 1.380(6) . ?
C15 C16 1.376(6) . ?
C16 C17 1.389(6) . ?
C18 C19 1.521(5) . ?
C18 P2 1.792(4) . ?
C19 C20 1.524(5) . ?
C20 C21 1.507(6) . ?
C22 C23 1.532(5) . ?
C22 P2 1.786(4) . ?
C23 C24 1.516(7) . ?
C24 C25 1.428(7) . ?
C26 C27 1.525(5) . ?
C26 P2 1.799(4) . ?
C27 C28 1.509(5) . ?
C28 C29 1.525(6) . ?
C30 C31 1.517(6) . ?
C30 P2 1.791(4) . ?
C31 C32 1.531(5) . ?
C32 C33 1.515(6) . ?
C34 N4 1.350(5) . ?
C34 C35 1.365(6) . ?
C35 C36 1.411(6) . ?
C36 N3 1.364(5) . ?
C36 C37 1.411(5) . ?
C37 C38 1.374(6) . ?
C38 N4 1.319(6) . ?
C39 C40 1.383(5) . ?
C39 C44 1.396(5) . ?
C39 P3 1.818(4) . ?
C40 C41 1.382(6) . ?
C41 C42 1.376(6) . ?
C42 C43 1.381(6) . ?
C43 C44 1.373(6) . ?
C45 C46 1.375(5) . ?
C45 C50 1.393(5) . ?
C45 P3 1.811(4) . ?
C46 C47 1.385(6) . ?
C47 C48 1.390(5) . ?
C48 C49 1.389(5) . ?
C49 C50 1.370(5) . ?
C51 C52 1.516(5) . ?
C51 P4 1.784(4) . ?
C52 C53 1.519(6) . ?
C53 C54 1.496(5) . ?
C55 C56 1.507(5) . ?
C55 P4 1.791(4) . ?
C56 C57 1.508(6) . ?
C57 C58 1.473(5) . ?
C59 C60 1.526(6) . ?
C59 P4 1.783(5) . ?
C60 C61 1.531(6) . ?
C61 C62 1.490(5) . ?
C63 C64 1.494(7) . ?
C63 P4 1.803(4) . ?
C64 C65 1.528(7) . ?
C65 C66 1.417(6) . ?
C67 N6 1.337(5) . ?
C67 C68 1.376(5) . ?
C68 C69 1.405(5) . ?
C69 N5 1.353(5) . ?
C69 C70 1.414(5) . ?
C70 C71 1.373(6) . ?
C71 N6 1.330(6) . ?
C72 C73 1.390(5) . ?
C72 C77 1.394(5) . ?
C72 P5 1.819(4) . ?
C73 C74 1.379(6) . ?
C74 C75 1.385(6) . ?
C75 C76 1.364(6) . ?
C76 C77 1.387(6) . ?
C78 C79 1.395(5) . ?
C78 C83 1.400(5) . ?
C78 P5 1.802(4) . ?
C79 C80 1.381(6) . ?
C80 C81 1.384(5) . ?
C81 C82 1.386(5) . ?
C82 C83 1.372(5) . ?
C84 C85 1.519(6) . ?
C84 P6 1.808(4) . ?
C85 C86 1.512(6) . ?
C86 C87 1.503(6) . ?
C88 C89 1.512(6) . ?
C88 P6 1.798(4) . ?
C89 C90 1.530(5) . ?
C90 C91 1.506(5) . ?
C92 C93 1.518(6) . ?
C92 P6 1.784(4) . ?
C93 C94 1.522(6) . ?
C94 C95 1.500(7) . ?
C96 C97B 1.508(6) . ?
C96 P6 1.784(4) . ?
C97B C98B 1.43(3) . ?
C98B C99B 1.66(4) . ?
C98 C99 1.390(14) . ?
N1 P1 1.600(3) . ?
N3 P3 1.599(3) . ?
N5 P5 1.599(3) . ?
O1 P1 1.494(3) . ?
O2 P3 1.498(3) . ?
O3 P5 1.493(3) . ?
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
N2 C1 C2 C3 1.0(8) . . . . ?
C1 C2 C3 N1 179.0(4) . . . . ?
C1 C2 C3 C4 0.0(6) . . . . ?
N1 C3 C4 C5 -179.9(4) . . . . ?
C2 C3 C4 C5 -1.0(6) . . . . ?
C3 C4 C5 N2 1.1(8) . . . . ?
C11 C6 C7 C8 -0.1(6) . . . . ?
P1 C6 C7 C8 174.9(3) . . . . ?
C6 C7 C8 C9 -1.2(6) . . . . ?
C7 C8 C9 C10 1.9(7) . . . . ?
C8 C9 C10 C11 -1.1(7) . . . . ?
C9 C10 C11 C6 -0.2(7) . . . . ?
C7 C6 C11 C10 0.9(6) . . . . ?
P1 C6 C11 C10 -174.4(3) . . . . ?
C17 C12 C13 C14 -1.0(6) . . . . ?
P1 C12 C13 C14 -176.9(3) . . . . ?
C12 C13 C14 C15 1.8(6) . . . . ?
C13 C14 C15 C16 -1.0(6) . . . . ?
C14 C15 C16 C17 -0.6(6) . . . . ?
C15 C16 C17 C12 1.4(6) . . . . ?
C13 C12 C17 C16 -0.6(6) . . . . ?
P1 C12 C17 C16 175.4(3) . . . . ?
P2 C18 C19 C20 157.6(3) . . . . ?
C18 C19 C20 C21 -75.7(5) . . . . ?
P2 C22 C23 C24 154.2(4) . . . . ?
C22 C23 C24 C25 54.3(8) . . . . ?
P2 C26 C27 C28 -174.1(3) . . . . ?
C26 C27 C28 C29 -168.5(4) . . . . ?
P2 C30 C31 C32 173.5(3) . . . . ?
C30 C31 C32 C33 68.1(5) . . . . ?
N4 C34 C35 C36 -2.7(8) . . . . ?
C34 C35 C36 N3 -178.0(4) . . . . ?
C34 C35 C36 C37 1.8(7) . . . . ?
N3 C36 C37 C38 179.4(4) . . . . ?
C35 C36 C37 C38 -0.4(6) . . . . ?
C36 C37 C38 N4 -0.4(8) . . . . ?
C44 C39 C40 C41 0.5(6) . . . . ?
P3 C39 C40 C41 179.3(3) . . . . ?
C39 C40 C41 C42 -0.9(6) . . . . ?
C40 C41 C42 C43 1.2(7) . . . . ?
C41 C42 C43 C44 -1.1(7) . . . . ?
C42 C43 C44 C39 0.7(7) . . . . ?
C40 C39 C44 C43 -0.4(6) . . . . ?
P3 C39 C44 C43 -179.2(3) . . . . ?
C50 C45 C46 C47 1.1(6) . . . . ?
P3 C45 C46 C47 -174.0(3) . . . . ?
C45 C46 C47 C48 0.3(7) . . . . ?
C46 C47 C48 C49 -1.6(6) . . . . ?
C47 C48 C49 C50 1.5(6) . . . . ?
C48 C49 C50 C45 -0.1(6) . . . . ?
C46 C45 C50 C49 -1.2(6) . . . . ?
P3 C45 C50 C49 174.2(3) . . . . ?
P4 C51 C52 C53 172.5(3) . . . . ?
C51 C52 C53 C54 -179.8(4) . . . . ?
P4 C55 C56 C57 168.7(4) . . . . ?
C55 C56 C57 C58 -179.6(5) . . . . ?
P4 C59 C60 C61 164.9(3) . . . . ?
C59 C60 C61 C62 -66.8(5) . . . . ?
P4 C63 C64 C65 -155.1(4) . . . . ?
C63 C64 C65 C66 -52.1(8) . . . . ?
N6 C67 C68 C69 -0.1(8) . . . . ?
C67 C68 C69 N5 180.0(4) . . . . ?
C67 C68 C69 C70 0.4(6) . . . . ?
N5 C69 C70 C71 -179.7(5) . . . . ?
C68 C69 C70 C71 -0.1(7) . . . . ?
C69 C70 C71 N6 -0.5(9) . . . . ?
C77 C72 C73 C74 0.3(6) . . . . ?
P5 C72 C73 C74 178.6(3) . . . . ?
C72 C73 C74 C75 -1.0(6) . . . . ?
C73 C74 C75 C76 0.9(6) . . . . ?
C74 C75 C76 C77 -0.1(7) . . . . ?
C75 C76 C77 C72 -0.5(7) . . . . ?
C73 C72 C77 C76 0.5(6) . . . . ?
P5 C72 C77 C76 -177.9(3) . . . . ?
C83 C78 C79 C80 0.7(6) . . . . ?
P5 C78 C79 C80 -174.6(3) . . . . ?
C78 C79 C80 C81 0.0(7) . . . . ?
C79 C80 C81 C82 -0.6(7) . . . . ?
C80 C81 C82 C83 0.4(6) . . . . ?
C81 C82 C83 C78 0.3(6) . . . . ?
C79 C78 C83 C82 -0.9(6) . . . . ?
P5 C78 C83 C82 174.6(3) . . . . ?
P6 C84 C85 C86 -159.0(4) . . . . ?
C84 C85 C86 C87 72.8(6) . . . . ?
P6 C88 C89 C90 -176.2(3) . . . . ?
C88 C89 C90 C91 -71.7(5) . . . . ?
P6 C92 C93 C94 174.8(3) . . . . ?
C92 C93 C94 C95 170.9(4) . . . . ?
P6 C96 C97B C98B 166.3(11) . . . . ?
C96 C97B C98B C99B 68(2) . . . . ?
C2 C3 N1 P1 -177.7(3) . . . . ?
C4 C3 N1 P1 1.1(6) . . . . ?
C4 C5 N2 C1 -0.1(7) . . . . ?
C2 C1 N2 C5 -0.9(7) . . . . ?
C35 C36 N3 P3 0.0(7) . . . . ?
C37 C36 N3 P3 -179.8(3) . . . . ?
C37 C38 N4 C34 -0.1(8) . . . . ?
C35 C34 N4 C38 1.7(8) . . . . ?
C68 C69 N5 P5 -2.3(7) . . . . ?
C70 C69 N5 P5 177.2(3) . . . . ?
C70 C71 N6 C67 0.8(8) . . . . ?
C68 C67 N6 C71 -0.5(8) . . . . ?
C3 N1 P1 O1 -39.1(4) . . . . ?
C3 N1 P1 C6 -164.2(3) . . . . ?
C3 N1 P1 C12 87.1(4) . . . . ?
C11 C6 P1 O1 50.5(4) . . . . ?
C7 C6 P1 O1 -124.6(3) . . . . ?
C11 C6 P1 N1 -178.0(3) . . . . ?
C7 C6 P1 N1 7.0(4) . . . . ?
C11 C6 P1 C12 -65.1(4) . . . . ?
C7 C6 P1 C12 119.8(4) . . . . ?
C17 C12 P1 O1 24.5(4) . . . . ?
C13 C12 P1 O1 -159.6(3) . . . . ?
C17 C12 P1 N1 -108.8(3) . . . . ?
C13 C12 P1 N1 67.1(4) . . . . ?
C17 C12 P1 C6 142.0(3) . . . . ?
C13 C12 P1 C6 -42.1(3) . . . . ?
C23 C22 P2 C30 63.2(4) . . . . ?
C23 C22 P2 C18 -56.8(4) . . . . ?
C23 C22 P2 C26 -176.4(3) . . . . ?
C31 C30 P2 C22 168.6(3) . . . . ?
C31 C30 P2 C18 -71.0(3) . . . . ?
C31 C30 P2 C26 49.2(3) . . . . ?
C19 C18 P2 C22 -60.7(4) . . . . ?
C19 C18 P2 C30 178.3(3) . . . . ?
C19 C18 P2 C26 58.0(4) . . . . ?
C27 C26 P2 C22 -56.6(4) . . . . ?
C27 C26 P2 C30 64.3(4) . . . . ?
C27 C26 P2 C18 -176.2(3) . . . . ?
C36 N3 P3 O2 38.1(4) . . . . ?
C36 N3 P3 C45 162.4(4) . . . . ?
C36 N3 P3 C39 -88.5(4) . . . . ?
C46 C45 P3 O2 119.8(4) . . . . ?
C50 C45 P3 O2 -55.3(4) . . . . ?
C46 C45 P3 N3 -11.2(4) . . . . ?
C50 C45 P3 N3 173.7(3) . . . . ?
C46 C45 P3 C39 -125.2(4) . . . . ?
C50 C45 P3 C39 59.7(4) . . . . ?
C40 C39 P3 O2 165.2(3) . . . . ?
C44 C39 P3 O2 -16.0(4) . . . . ?
C40 C39 P3 N3 -61.1(4) . . . . ?
C44 C39 P3 N3 117.6(3) . . . . ?
C40 C39 P3 C45 48.8(4) . . . . ?
C44 C39 P3 C45 -132.5(3) . . . . ?
C60 C59 P4 C51 -177.0(3) . . . . ?
C60 C59 P4 C55 -57.5(4) . . . . ?
C60 C59 P4 C63 62.0(4) . . . . ?
C52 C51 P4 C59 -82.5(4) . . . . ?
C52 C51 P4 C55 158.3(3) . . . . ?
C52 C51 P4 C63 37.5(4) . . . . ?
C56 C55 P4 C59 -53.1(4) . . . . ?
C56 C55 P4 C51 66.9(4) . . . . ?
C56 C55 P4 C63 -172.0(3) . . . . ?
C64 C63 P4 C59 -174.9(3) . . . . ?
C64 C63 P4 C51 64.4(4) . . . . ?
C64 C63 P4 C55 -56.1(4) . . . . ?
C69 N5 P5 O3 36.4(5) . . . . ?
C69 N5 P5 C78 161.9(4) . . . . ?
C69 N5 P5 C72 -90.3(4) . . . . ?
C79 C78 P5 O3 123.7(3) . . . . ?
C83 C78 P5 O3 -51.6(4) . . . . ?
C79 C78 P5 N5 -8.5(4) . . . . ?
C83 C78 P5 N5 176.2(3) . . . . ?
C79 C78 P5 C72 -121.2(4) . . . . ?
C83 C78 P5 C72 63.5(3) . . . . ?
C73 C72 P5 O3 163.1(3) . . . . ?
C77 C72 P5 O3 -18.6(4) . . . . ?
C73 C72 P5 N5 -62.8(4) . . . . ?
C77 C72 P5 N5 115.5(3) . . . . ?
C73 C72 P5 C78 46.4(4) . . . . ?
C77 C72 P5 C78 -135.4(3) . . . . ?
C93 C92 P6 C96 59.0(4) . . . . ?
C93 C92 P6 C88 -61.7(4) . . . . ?
C93 C92 P6 C84 179.2(3) . . . . ?
C97B C96 P6 C92 168.4(4) . . . . ?
C97B C96 P6 C88 -70.8(4) . . . . ?
C97B C96 P6 C84 47.7(4) . . . . ?
C89 C88 P6 C92 -46.9(4) . . . . ?
C89 C88 P6 C96 -167.0(3) . . . . ?
C89 C88 P6 C84 73.5(3) . . . . ?
C85 C84 P6 C92 -61.3(4) . . . . ?
C85 C84 P6 C96 58.6(4) . . . . ?
C85 C84 P6 C88 178.4(3) . . . . ?
