#------------------------------------------------------------------------------
#$Date: 2024-10-04 21:22:16 +0300 (Fri, 04 Oct 2024) $
#$Revision: 295056 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/71/7717155.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_7717155
loop_
_publ_author_name
'Calder, Ethan D. E.'
'Male, Louise'
'Jupp, Andrew R.'
_publ_section_title
;
 Accessing five- and seven-membered phosphorus-based heterocycles
 via cycloaddition reactions of azophosphines.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15032
_journal_page_last               15039
_journal_paper_doi               10.1039/d4dt02248c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C23 H35 N2 O4 P'
_chemical_formula_sum            'C23 H35 N2 O4 P'
_chemical_formula_weight         434.50
_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
_audit_creation_date             2024-05-01
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-05-17 deposited with the CCDC.	2024-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.910(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.0832(4)
_cell_length_b                   9.8167(2)
_cell_length_c                   28.9289(6)
_cell_measurement_reflns_used    14342
_cell_measurement_temperature    99.96(14)
_cell_measurement_theta_max      72.7750
_cell_measurement_theta_min      3.6930
_cell_volume                     4816.16(18)
_computing_cell_refinement       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.73a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.96(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3537
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -64.00  31.00   1.00    5.13    --  -41.81  38.00-120.00   95
  2  ω   -120.00  -5.00   1.00    5.13    --  -41.81 -19.00  60.00  115
  3  ω     27.00  95.00   1.00    5.13    --   41.81-125.00   0.00   68
  4  ω     33.00 130.00   1.00   20.50    --  102.88 -61.00  30.00   97
  5  ω     79.00 174.00   1.00   20.50    --  102.88  45.00 120.00   95
  6  ω    104.00 175.00   1.00   20.50    --  102.88 111.00  30.00   71
  7  ω     61.00 146.00   1.00   20.50    --  102.88 178.00 -30.00   85
  8  ω    103.00 177.00   1.00   20.50    --  102.88  77.00-180.00   74
  9  ω    104.00 175.00   1.00   20.50    --  102.88 111.00  60.00   71
 10  ω    103.00 177.00   1.00   20.50    --  102.88  77.00 150.00   74
 11  ω     31.00 108.00   1.00   20.50    --  102.88-111.00   0.00   77
 12  ω     15.00 112.00   1.00    5.13    --   41.81  57.00 -90.00   97
 13  ω     15.00 112.00   1.00    5.13    --   41.81  57.00-180.00   97
 14  ω     15.00 112.00   1.00    5.13    --   41.81  57.00   0.00   97
 15  ω     57.00 122.00   1.00   20.50    --  102.88  15.00 -30.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0825975000
_diffrn_orient_matrix_UB_12      0.0273313000
_diffrn_orient_matrix_UB_13      -0.0143695000
_diffrn_orient_matrix_UB_21      0.0267399000
_diffrn_orient_matrix_UB_22      0.0593012000
_diffrn_orient_matrix_UB_23      0.0486807000
_diffrn_orient_matrix_UB_31      0.0267737000
_diffrn_orient_matrix_UB_32      -0.1425782000
_diffrn_orient_matrix_UB_33      0.0174306000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            36542
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.009
_diffrn_reflns_theta_min         3.787
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.251
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.73a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_description       plate
_exptl_crystal_F_000             1872
_exptl_crystal_preparation       'Slow evaporation of hexane'
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9464
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0393
_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)+(0.0569P)²+0.6224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0990
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7213
_reflns_number_total             9464
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02248c2.cif
_cod_data_source_block           edec_098_f_gaussian
_cod_database_code               7717155
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C23 H35 O4 N2 P1'
_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   0.941
_shelx_estimated_absorpt_t_min   0.761
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C21(H21), C18(H18), C121(H121), C118(H118)
1.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C114(H11D,H11E), C116(H11I,H11J)
1.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C103(H103), C105(H105)
1.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C),
 C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C15(H15A,H15B,
 H15C), C17(H17A,H17B,H17C), C107(H10A,H10B,H10C), C108(H10D,H10E,H10F),
 C109(H10G,H10H,H10I), C122(H12A,H12B,H12C), C123(H12D,H12E,H12F), C120(H12G,
 H12H,H12I), C119(H11A,H11B,H11C), C115(H11F,H11G,H11H), C117(H11K,H11L,H11M)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.536
_oxdiff_exptl_absorpt_empirical_full_min 0.823
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
C1 C 0.51982(9) 0.03316(17) 0.36396(5) 0.0189(3) Uani 1 1 d . . . . .
C2 C 0.56149(10) -0.08953(17) 0.36786(5) 0.0211(3) Uani 1 1 d . . . . .
C3 C 0.51969(11) -0.20792(18) 0.37494(6) 0.0238(3) Uani 1 1 d . . . . .
H3 H 0.546832 -0.292549 0.377585 0.029 Uiso 1 1 calc R U . . .
C4 C 0.43880(11) -0.20527(18) 0.37826(6) 0.0251(4) Uani 1 1 d . . . . .
C5 C 0.39981(10) -0.08097(18) 0.37444(5) 0.0240(4) Uani 1 1 d . . . . .
H5 H 0.344885 -0.078445 0.376945 0.029 Uiso 1 1 calc R U . . .
C6 C 0.43883(10) 0.03996(18) 0.36703(5) 0.0217(3) Uani 1 1 d . . . . .
C7 C 0.64872(10) -0.09320(18) 0.36483(6) 0.0265(4) Uani 1 1 d . . . . .
H7A H 0.659000 -0.062233 0.333927 0.040 Uiso 1 1 calc R U . . .
H7B H 0.668124 -0.186587 0.369944 0.040 Uiso 1 1 calc R U . . .
H7C H 0.675875 -0.033182 0.388653 0.040 Uiso 1 1 calc R U . . .
C8 C 0.39476(10) 0.17224(18) 0.36165(6) 0.0257(4) Uani 1 1 d . . . . .
H8A H 0.411915 0.231476 0.388216 0.039 Uiso 1 1 calc R U . . .
H8B H 0.338075 0.154721 0.360429 0.039 Uiso 1 1 calc R U . . .
H8C H 0.405499 0.216966 0.332788 0.039 Uiso 1 1 calc R U . . .
C9 C 0.39415(12) -0.3349(2) 0.38512(7) 0.0332(4) Uani 1 1 d . . . . .
H9A H 0.368312 -0.366871 0.354989 0.050 Uiso 1 1 calc R U . . .
H9B H 0.354229 -0.317408 0.406050 0.050 Uiso 1 1 calc R U . . .
H9C H 0.430901 -0.404752 0.398790 0.050 Uiso 1 1 calc R U . . .
C21 C 0.56334(10) 0.45452(18) 0.27085(6) 0.0231(3) Uani 1 1 d . . . . .
H21 H 0.556482 0.413802 0.238928 0.028 Uiso 1 1 calc R U . . .
C23 C 0.48138(10) 0.4746(2) 0.28566(6) 0.0289(4) Uani 1 1 d . . . . .
H23A H 0.454588 0.386326 0.285917 0.043 Uiso 1 1 calc R U . . .
H23B H 0.450721 0.535772 0.263658 0.043 Uiso 1 1 calc R U . . .
H23C H 0.486164 0.514434 0.316931 0.043 Uiso 1 1 calc R U . . .
C22 C 0.60638(11) 0.59064(19) 0.26794(7) 0.0311(4) Uani 1 1 d . . . . .
H22A H 0.618667 0.628799 0.299275 0.047 Uiso 1 1 calc R U . . .
H22B H 0.572607 0.654191 0.248496 0.047 Uiso 1 1 calc R U . . .
H22C H 0.655401 0.575978 0.254186 0.047 Uiso 1 1 calc R U . . .
C18 C 0.71647(10) 0.32056(18) 0.29055(6) 0.0221(3) Uani 1 1 d . . . . .
H18 H 0.743514 0.410468 0.296023 0.027 Uiso 1 1 calc R U . . .
C19 C 0.76406(10) 0.21306(19) 0.31976(7) 0.0300(4) Uani 1 1 d . . . . .
H19A H 0.766776 0.237115 0.352795 0.045 Uiso 1 1 calc R U . . .
H19B H 0.817493 0.208852 0.310745 0.045 Uiso 1 1 calc R U . . .
H19C H 0.738497 0.124091 0.314531 0.045 Uiso 1 1 calc R U . . .
C20 C 0.71107(12) 0.2869(2) 0.23856(7) 0.0380(5) Uani 1 1 d . . . . .
H20A H 0.682023 0.201498 0.232367 0.057 Uiso 1 1 calc R U . . .
H20B H 0.764302 0.277154 0.229581 0.057 Uiso 1 1 calc R U . . .
H20C H 0.683449 0.360624 0.220477 0.057 Uiso 1 1 calc R U . . .
C10 C 0.58717(9) 0.24836(17) 0.38786(5) 0.0185(3) Uani 1 1 d . . . . .
C11 C 0.62265(9) 0.36260(16) 0.36997(5) 0.0186(3) Uani 1 1 d . . . . .
C12 C 0.57773(10) 0.21854(16) 0.43785(5) 0.0201(3) Uani 1 1 d . . . . .
C13 C 0.66723(9) 0.46760(16) 0.39575(5) 0.0189(3) Uani 1 1 d . . . . .
C14 C 0.50232(11) 0.2678(2) 0.49928(6) 0.0301(4) Uani 1 1 d . . . . .
H14A H 0.487315 0.352929 0.514299 0.036 Uiso 1 1 calc R U . . .
H14B H 0.548731 0.228623 0.518532 0.036 Uiso 1 1 calc R U . . .
C15 C 0.43476(12) 0.1681(2) 0.49603(7) 0.0357(4) Uani 1 1 d . . . . .
H15A H 0.388679 0.208061 0.477455 0.054 Uiso 1 1 calc R U . . .
H15B H 0.421765 0.147516 0.527365 0.054 Uiso 1 1 calc R U . . .
H15C H 0.449917 0.084045 0.481158 0.054 Uiso 1 1 calc R U . . .
C16 C 0.71244(12) 0.5539(2) 0.47101(6) 0.0311(4) Uani 1 1 d . . . . .
H16A H 0.691246 0.645782 0.462777 0.037 Uiso 1 1 calc R U . . .
H16B H 0.768901 0.552046 0.466345 0.037 Uiso 1 1 calc R U . . .
C17 C 0.70277(12) 0.5209(2) 0.52083(6) 0.0356(4) Uani 1 1 d . . . . .
H17A H 0.646731 0.524069 0.525041 0.053 Uiso 1 1 calc R U . . .
H17B H 0.731796 0.587659 0.541469 0.053 Uiso 1 1 calc R U . . .
H17C H 0.723502 0.429472 0.528422 0.053 Uiso 1 1 calc R U . . .
N1 N 0.56179(8) 0.15664(14) 0.35589(4) 0.0182(3) Uani 1 1 d . . . . .
N2 N 0.57150(8) 0.18605(14) 0.30923(4) 0.0200(3) Uani 1 1 d . . . . .
O1 O 0.61440(8) 0.13190(13) 0.46028(4) 0.0297(3) Uani 1 1 d . . . . .
O2 O 0.52212(7) 0.29741(12) 0.45253(4) 0.0240(3) Uani 1 1 d . . . . .
O3 O 0.70101(7) 0.56107(12) 0.37852(4) 0.0248(3) Uani 1 1 d . . . . .
O4 O 0.66931(7) 0.45191(12) 0.44241(4) 0.0264(3) Uani 1 1 d . . . . .
P1 P 0.61830(2) 0.33250(4) 0.30974(2) 0.01747(10) Uani 1 1 d . . . . .
C101 C 0.02196(9) 0.58792(17) 0.36584(5) 0.0188(3) Uani 1 1 d . . . . .
C102 C -0.05797(10) 0.58153(17) 0.37175(5) 0.0215(3) Uani 1 1 d . . . . .
C103 C -0.09679(10) 0.70409(18) 0.37804(5) 0.0238(4) Uani 1 1 d . . . . .
H103 H -0.150905 0.701974 0.382656 0.029 Uiso 1 1 calc R U . . .
C104 C -0.05874(11) 0.82880(18) 0.37773(5) 0.0244(4) Uani 1 1 d . . . . .
C105 C 0.02121(11) 0.83046(18) 0.37181(6) 0.0246(4) Uani 1 1 d . . . . .
H105 H 0.047895 0.915357 0.371780 0.029 Uiso 1 1 calc R U . . .
C106 C 0.06273(10) 0.71131(17) 0.36595(5) 0.0216(3) Uani 1 1 d . . . . .
C107 C -0.10217(10) 0.44864(19) 0.37084(7) 0.0285(4) Uani 1 1 d . . . . .
H10A H -0.083048 0.387684 0.347827 0.043 Uiso 1 1 calc R U . . .
H10B H -0.158618 0.465615 0.362415 0.043 Uiso 1 1 calc R U . . .
H10C H -0.093622 0.406136 0.401689 0.043 Uiso 1 1 calc R U . . .
C108 C 0.14917(11) 0.71451(19) 0.36019(7) 0.0296(4) Uani 1 1 d . . . . .
H10D H 0.178054 0.653526 0.383040 0.044 Uiso 1 1 calc R U . . .
H10E H 0.169200 0.807591 0.365089 0.044 Uiso 1 1 calc R U . . .
H10F H 0.156505 0.684503 0.328687 0.044 Uiso 1 1 calc R U . . .
C109 C -0.10234(12) 0.95980(19) 0.38350(6) 0.0323(4) Uani 1 1 d . . . . .
H10G H -0.067887 1.023195 0.402587 0.048 Uiso 1 1 calc R U . . .
H10H H -0.149345 0.941113 0.398810 0.048 Uiso 1 1 calc R U . . .
H10I H -0.118159 1.000381 0.352844 0.048 Uiso 1 1 calc R U . . .
C121 C 0.21647(9) 0.31104(18) 0.28687(6) 0.0216(3) Uani 1 1 d . . . . .
H121 H 0.243344 0.220543 0.290674 0.026 Uiso 1 1 calc R U . . .
C122 C 0.20968(12) 0.3516(2) 0.23546(7) 0.0360(4) Uani 1 1 d . . . . .
H12A H 0.182441 0.279477 0.216415 0.054 Uiso 1 1 calc R U . . .
H12B H 0.262539 0.364786 0.226273 0.054 Uiso 1 1 calc R U . . .
H12C H 0.179723 0.436681 0.230782 0.054 Uiso 1 1 calc R U . . .
C123 C 0.26516(10) 0.41471(18) 0.31714(7) 0.0279(4) Uani 1 1 d . . . . .
H12D H 0.239925 0.504328 0.313360 0.042 Uiso 1 1 calc R U . . .
H12E H 0.318280 0.419737 0.307688 0.042 Uiso 1 1 calc R U . . .
H12F H 0.268600 0.386772 0.349841 0.042 Uiso 1 1 calc R U . . .
C118 C 0.06188(10) 0.18175(17) 0.26589(5) 0.0217(3) Uani 1 1 d . . . . .
H118 H 0.053340 0.228734 0.235019 0.026 Uiso 1 1 calc R U . . .
C120 C 0.10408(11) 0.04683(19) 0.25898(6) 0.0296(4) Uani 1 1 d . . . . .
H12G H 0.152865 0.064763 0.245341 0.044 Uiso 1 1 calc R U . . .
H12H H 0.069659 -0.012029 0.238056 0.044 Uiso 1 1 calc R U . . .
H12I H 0.116705 0.001461 0.289134 0.044 Uiso 1 1 calc R U . . .
C119 C -0.01900(10) 0.15862(19) 0.28212(6) 0.0287(4) Uani 1 1 d . . . . .
H11A H -0.012534 0.111376 0.312178 0.043 Uiso 1 1 calc R U . . .
H11B H -0.051508 0.103034 0.259108 0.043 Uiso 1 1 calc R U . . .
H11C H -0.044797 0.246633 0.285475 0.043 Uiso 1 1 calc R U . . .
C110 C 0.08871(9) 0.36714(16) 0.38662(5) 0.0182(3) Uani 1 1 d . . . . .
C111 C 0.12432(9) 0.25706(16) 0.36633(5) 0.0184(3) Uani 1 1 d . . . . .
C112 C 0.07678(9) 0.38338(16) 0.43691(5) 0.0197(3) Uani 1 1 d . . . . .
C113 C 0.16949(9) 0.14674(16) 0.38832(5) 0.0189(3) Uani 1 1 d . . . . .
C114 C 0.01355(12) 0.2869(2) 0.49791(6) 0.0307(4) Uani 1 1 d . . . . .
H11D H 0.002970 0.380692 0.508138 0.037 Uiso 1 1 calc R U . . .
H11E H 0.059830 0.250828 0.518067 0.037 Uiso 1 1 calc R U . . .
C115 C -0.05615(17) 0.1990(3) 0.50092(8) 0.0700(9) Uani 1 1 d . . . . .
H11F H -0.101294 0.235129 0.480485 0.105 Uiso 1 1 calc R U . . .
H11G H -0.068634 0.197455 0.533106 0.105 Uiso 1 1 calc R U . . .
H11H H -0.044609 0.106284 0.491170 0.105 Uiso 1 1 calc R U . . .
C116 C 0.22006(11) 0.03793(18) 0.45884(6) 0.0262(4) Uani 1 1 d . . . . .
H11I H 0.275308 0.037584 0.451707 0.031 Uiso 1 1 calc R U . . .
H11J H 0.195232 -0.049733 0.448459 0.031 Uiso 1 1 calc R U . . .
C117 C 0.21762(11) 0.0571(2) 0.51016(6) 0.0306(4) Uani 1 1 d . . . . .
H11K H 0.162670 0.057158 0.516740 0.046 Uiso 1 1 calc R U . . .
H11L H 0.242359 0.144175 0.519967 0.046 Uiso 1 1 calc R U . . .
H11M H 0.246225 -0.017398 0.527243 0.046 Uiso 1 1 calc R U . . .
N101 N 0.06355(7) 0.46453(14) 0.35659(4) 0.0179(3) Uani 1 1 d . . . . .
N102 N 0.07349(8) 0.44335(14) 0.30959(4) 0.0193(3) Uani 1 1 d . . . . .
O101 O 0.10613(8) 0.47227(13) 0.46170(4) 0.0283(3) Uani 1 1 d . . . . .
O102 O 0.02857(7) 0.28702(12) 0.44931(4) 0.0238(3) Uani 1 1 d . . . . .
O103 O 0.20032(7) 0.05736(12) 0.36712(4) 0.0229(2) Uani 1 1 d . . . . .
O104 O 0.17712(7) 0.15054(12) 0.43543(4) 0.0234(3) Uani 1 1 d . . . . .
P101 P 0.11910(2) 0.29645(4) 0.30675(2) 0.01666(10) 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 0.0181 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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-4 6 -6 0.0691
-8 -4 -3 0.0570
9 -1 7 0.0482
-2 2 18 0.0361
-1 0 19 0.0259
1 0 -19 0.0203
1 0 18 0.0295
11 0 -1 0.0759
-11 2 4 0.0975
-3 1 18 0.0313
4 -6 0 0.1058
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
C2 C1 C6 122.31(15) . . ?
C2 C1 N1 118.66(14) . . ?
C6 C1 N1 119.02(15) . . ?
C1 C2 C7 121.00(15) . . ?
C3 C2 C1 117.80(15) . . ?
C3 C2 C7 121.20(15) . . ?
C2 C3 H3 119.2 . . ?
C2 C3 C4 121.59(16) . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C9 120.87(17) . . ?
C5 C4 C3 118.69(16) . . ?
C5 C4 C9 120.43(16) . . ?
C4 C5 H5 119.1 . . ?
C4 C5 C6 121.89(16) . . ?
C6 C5 H5 119.1 . . ?
C1 C6 C8 121.52(15) . . ?
C5 C6 C1 117.73(16) . . ?
C5 C6 C8 120.74(15) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C23 C21 H21 107.5 . . ?
C23 C21 C22 111.45(15) . . ?
C23 C21 P1 109.45(11) . . ?
C22 C21 H21 107.5 . . ?
C22 C21 P1 113.05(12) . . ?
P1 C21 H21 107.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C18 H18 108.5 . . ?
C19 C18 C20 111.12(16) . . ?
C19 C18 P1 108.83(11) . . ?
C20 C18 H18 108.5 . . ?
C20 C18 P1 111.23(12) . . ?
P1 C18 H18 108.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C11 C10 C12 127.71(14) . . ?
N1 C10 C11 113.90(14) . . ?
N1 C10 C12 118.35(14) . . ?
C10 C11 C13 127.43(14) . . ?
C10 C11 P1 105.21(11) . . ?
C13 C11 P1 126.25(12) . . ?
O1 C12 C10 123.29(15) . . ?
O1 C12 O2 125.79(15) . . ?
O2 C12 C10 110.88(13) . . ?
O3 C13 C11 125.04(14) . . ?
O3 C13 O4 122.34(15) . . ?
O4 C13 C11 112.62(14) . . ?
H14A C14 H14B 108.2 . . ?
C15 C14 H14A 109.8 . . ?
C15 C14 H14B 109.8 . . ?
O2 C14 H14A 109.8 . . ?
O2 C14 H14B 109.8 . . ?
O2 C14 C15 109.39(14) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
H16A C16 H16B 108.6 . . ?
C17 C16 H16A 110.3 . . ?
C17 C16 H16B 110.3 . . ?
O4 C16 H16A 110.3 . . ?
O4 C16 H16B 110.3 . . ?
O4 C16 C17 106.98(15) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C10 N1 C1 125.84(13) . . ?
C10 N1 N2 117.55(13) . . ?
N2 N1 C1 116.45(12) . . ?
N1 N2 P1 106.47(10) . . ?
C12 O2 C14 115.59(13) . . ?
C13 O4 C16 116.27(13) . . ?
C21 P1 C18 106.08(8) . . ?
C11 P1 C21 117.23(8) . . ?
C11 P1 C18 112.31(8) . . ?
N2 P1 C21 110.79(7) . . ?
N2 P1 C18 113.77(8) . . ?
N2 P1 C11 96.80(7) . . ?
C102 C101 N101 119.62(14) . . ?
C106 C101 C102 122.19(15) . . ?
C106 C101 N101 118.09(14) . . ?
C101 C102 C107 122.13(15) . . ?
C103 C102 C101 117.62(16) . . ?
C103 C102 C107 120.24(15) . . ?
C102 C103 H103 119.0 . . ?
C104 C103 C102 121.97(16) . . ?
C104 C103 H103 119.0 . . ?
C103 C104 C105 118.49(16) . . ?
C103 C104 C109 121.00(16) . . ?
C105 C104 C109 120.51(17) . . ?
C104 C105 H105 119.1 . . ?
C106 C105 C104 121.76(16) . . ?
C106 C105 H105 119.1 . . ?
C101 C106 C108 120.87(15) . . ?
C105 C106 C101 117.94(15) . . ?
C105 C106 C108 121.19(16) . . ?
C102 C107 H10A 109.5 . . ?
C102 C107 H10B 109.5 . . ?
C102 C107 H10C 109.5 . . ?
H10A C107 H10B 109.5 . . ?
H10A C107 H10C 109.5 . . ?
H10B C107 H10C 109.5 . . ?
C106 C108 H10D 109.5 . . ?
C106 C108 H10E 109.5 . . ?
C106 C108 H10F 109.5 . . ?
H10D C108 H10E 109.5 . . ?
H10D C108 H10F 109.5 . . ?
H10E C108 H10F 109.5 . . ?
C104 C109 H10G 109.5 . . ?
C104 C109 H10H 109.5 . . ?
C104 C109 H10I 109.5 . . ?
H10G C109 H10H 109.5 . . ?
H10G C109 H10I 109.5 . . ?
H10H C109 H10I 109.5 . . ?
C122 C121 H121 108.6 . . ?
C122 C121 P101 111.13(12) . . ?
C123 C121 H121 108.6 . . ?
C123 C121 C122 110.91(15) . . ?
C123 C121 P101 109.01(11) . . ?
P101 C121 H121 108.6 . . ?
C121 C122 H12A 109.5 . . ?
C121 C122 H12B 109.5 . . ?
C121 C122 H12C 109.5 . . ?
H12A C122 H12B 109.5 . . ?
H12A C122 H12C 109.5 . . ?
H12B C122 H12C 109.5 . . ?
C121 C123 H12D 109.5 . . ?
C121 C123 H12E 109.5 . . ?
C121 C123 H12F 109.5 . . ?
H12D C123 H12E 109.5 . . ?
H12D C123 H12F 109.5 . . ?
H12E C123 H12F 109.5 . . ?
C120 C118 H118 107.6 . . ?
C120 C118 P101 113.16(12) . . ?
C119 C118 H118 107.6 . . ?
C119 C118 C120 111.61(15) . . ?
C119 C118 P101 108.99(11) . . ?
P101 C118 H118 107.6 . . ?
C118 C120 H12G 109.5 . . ?
C118 C120 H12H 109.5 . . ?
C118 C120 H12I 109.5 . . ?
H12G C120 H12H 109.5 . . ?
H12G C120 H12I 109.5 . . ?
H12H C120 H12I 109.5 . . ?
C118 C119 H11A 109.5 . . ?
C118 C119 H11B 109.5 . . ?
C118 C119 H11C 109.5 . . ?
H11A C119 H11B 109.5 . . ?
H11A C119 H11C 109.5 . . ?
H11B C119 H11C 109.5 . . ?
C111 C110 C112 127.11(14) . . ?
N101 C110 C111 113.78(13) . . ?
N101 C110 C112 119.11(14) . . ?
C110 C111 C113 129.31(14) . . ?
C110 C111 P101 105.51(11) . . ?
C113 C111 P101 124.22(12) . . ?
O101 C112 C110 124.09(15) . . ?
O101 C112 O102 125.65(15) . . ?
O102 C112 C110 110.25(13) . . ?
O103 C113 C111 124.04(14) . . ?
O103 C113 O104 121.91(14) . . ?
O104 C113 C111 114.04(14) . . ?
H11D C114 H11E 108.6 . . ?
C115 C114 H11D 110.3 . . ?
C115 C114 H11E 110.3 . . ?
O102 C114 H11D 110.3 . . ?
O102 C114 H11E 110.3 . . ?
O102 C114 C115 107.03(15) . . ?
C114 C115 H11F 109.5 . . ?
C114 C115 H11G 109.5 . . ?
C114 C115 H11H 109.5 . . ?
H11F C115 H11G 109.5 . . ?
H11F C115 H11H 109.5 . . ?
H11G C115 H11H 109.5 . . ?
H11I C116 H11J 108.6 . . ?
C117 C116 H11I 110.3 . . ?
C117 C116 H11J 110.3 . . ?
O104 C116 H11I 110.3 . . ?
O104 C116 H11J 110.3 . . ?
O104 C116 C117 107.07(14) . . ?
C116 C117 H11K 109.5 . . ?
C116 C117 H11L 109.5 . . ?
C116 C117 H11M 109.5 . . ?
H11K C117 H11L 109.5 . . ?
H11K C117 H11M 109.5 . . ?
H11L C117 H11M 109.5 . . ?
C110 N101 C101 127.56(13) . . ?
C110 N101 N102 117.33(13) . . ?
N102 N101 C101 114.98(12) . . ?
N101 N102 P101 106.90(10) . . ?
C112 O102 C114 116.51(13) . . ?
C113 O104 C116 115.56(13) . . ?
C118 P101 C121 106.28(8) . . ?
C111 P101 C121 112.62(8) . . ?
C111 P101 C118 117.29(8) . . ?
N102 P101 C121 113.63(8) . . ?
N102 P101 C118 110.63(7) . . ?
N102 P101 C111 96.45(7) . . ?
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 C2 1.397(2) . ?
C1 C6 1.399(2) . ?
C1 N1 1.442(2) . ?
C2 C3 1.392(2) . ?
C2 C7 1.504(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.397(2) . ?
C4 C5 1.388(3) . ?
C4 C9 1.509(2) . ?
C5 H5 0.9500 . ?
C5 C6 1.391(2) . ?
C6 C8 1.500(2) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C21 H21 1.0000 . ?
C21 C23 1.526(2) . ?
C21 C22 1.532(2) . ?
C21 P1 1.8244(17) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.524(2) . ?
C18 C20 1.532(2) . ?
C18 P1 1.8326(16) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C10 C11 1.403(2) . ?
C10 C12 1.503(2) . ?
C10 N1 1.326(2) . ?
C11 C13 1.436(2) . ?
C11 P1 1.7599(15) . ?
C12 O1 1.200(2) . ?
C12 O2 1.334(2) . ?
C13 O3 1.222(2) . ?
C13 O4 1.3546(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C15 1.507(3) . ?
C14 O2 1.4624(19) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C17 1.506(2) . ?
C16 O4 1.444(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
N1 N2 1.4096(17) . ?
N2 P1 1.6442(14) . ?
C101 C102 1.398(2) . ?
C101 C106 1.397(2) . ?
C101 N101 1.446(2) . ?
C102 C103 1.396(2) . ?
C102 C107 1.506(2) . ?
C103 H103 0.9500 . ?
C103 C104 1.387(3) . ?
C104 C105 1.397(3) . ?
C104 C109 1.505(2) . ?
C105 H105 0.9500 . ?
C105 C106 1.389(2) . ?
C106 C108 1.506(2) . ?
C107 H10A 0.9800 . ?
C107 H10B 0.9800 . ?
C107 H10C 0.9800 . ?
C108 H10D 0.9800 . ?
C108 H10E 0.9800 . ?
C108 H10F 0.9800 . ?
C109 H10G 0.9800 . ?
C109 H10H 0.9800 . ?
C109 H10I 0.9800 . ?
C121 H121 1.0000 . ?
C121 C122 1.530(2) . ?
C121 C123 1.523(2) . ?
C121 P101 1.8299(16) . ?
C122 H12A 0.9800 . ?
C122 H12B 0.9800 . ?
C122 H12C 0.9800 . ?
C123 H12D 0.9800 . ?
C123 H12E 0.9800 . ?
C123 H12F 0.9800 . ?
C118 H118 1.0000 . ?
C118 C120 1.533(2) . ?
C118 C119 1.529(2) . ?
C118 P101 1.8283(16) . ?
C120 H12G 0.9800 . ?
C120 H12H 0.9800 . ?
C120 H12I 0.9800 . ?
C119 H11A 0.9800 . ?
C119 H11B 0.9800 . ?
C119 H11C 0.9800 . ?
C110 C111 1.403(2) . ?
C110 C112 1.501(2) . ?
C110 N101 1.328(2) . ?
C111 C113 1.433(2) . ?
C111 P101 1.7581(15) . ?
C112 O101 1.200(2) . ?
C112 O102 1.332(2) . ?
C113 O103 1.225(2) . ?
C113 O104 1.3539(19) . ?
C114 H11D 0.9900 . ?
C114 H11E 0.9900 . ?
C114 C115 1.482(3) . ?
C114 O102 1.4590(19) . ?
C115 H11F 0.9800 . ?
C115 H11G 0.9800 . ?
C115 H11H 0.9800 . ?
C116 H11I 0.9900 . ?
C116 H11J 0.9900 . ?
C116 C117 1.502(2) . ?
C116 O104 1.449(2) . ?
C117 H11K 0.9800 . ?
C117 H11L 0.9800 . ?
C117 H11M 0.9800 . ?
N101 N102 1.4058(17) . ?
N102 P101 1.6458(14) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -0.2(2) . . . . ?
C1 N1 N2 P1 178.39(11) . . . . ?
C2 C1 C6 C5 0.3(2) . . . . ?
C2 C1 C6 C8 -178.55(15) . . . . ?
C2 C1 N1 C10 -100.35(19) . . . . ?
C2 C1 N1 N2 84.35(17) . . . . ?
C2 C3 C4 C5 -0.1(2) . . . . ?
C2 C3 C4 C9 178.94(15) . . . . ?
C3 C4 C5 C6 0.6(2) . . . . ?
C4 C5 C6 C1 -0.6(2) . . . . ?
C4 C5 C6 C8 178.21(15) . . . . ?
C6 C1 C2 C3 0.1(2) . . . . ?
C6 C1 C2 C7 -179.43(15) . . . . ?
C6 C1 N1 C10 80.4(2) . . . . ?
C6 C1 N1 N2 -94.86(17) . . . . ?
C7 C2 C3 C4 179.35(15) . . . . ?
C9 C4 C5 C6 -178.51(15) . . . . ?
C23 C21 P1 C18 -177.89(12) . . . . ?
C23 C21 P1 C11 -51.55(15) . . . . ?
C23 C21 P1 N2 58.19(14) . . . . ?
C22 C21 P1 C18 -53.01(14) . . . . ?
C22 C21 P1 C11 73.33(14) . . . . ?
C22 C21 P1 N2 -176.93(12) . . . . ?
C19 C18 P1 C21 -176.45(12) . . . . ?
C19 C18 P1 C11 54.28(14) . . . . ?
C19 C18 P1 N2 -54.41(14) . . . . ?
C20 C18 P1 C21 -53.71(15) . . . . ?
C20 C18 P1 C11 177.02(13) . . . . ?
C20 C18 P1 N2 68.33(15) . . . . ?
C10 C11 C13 O3 175.43(16) . . . . ?
C10 C11 C13 O4 -3.7(2) . . . . ?
C10 C11 P1 C21 119.25(12) . . . . ?
C10 C11 P1 C18 -117.53(12) . . . . ?
C10 C11 P1 N2 1.65(12) . . . . ?
C10 C12 O2 C14 174.11(13) . . . . ?
C10 N1 N2 P1 2.68(17) . . . . ?
C11 C10 C12 O1 -108.5(2) . . . . ?
C11 C10 C12 O2 73.6(2) . . . . ?
C11 C10 N1 C1 -176.78(14) . . . . ?
C11 C10 N1 N2 -1.5(2) . . . . ?
C11 C13 O4 C16 -179.49(14) . . . . ?
C12 C10 C11 C13 9.2(3) . . . . ?
C12 C10 C11 P1 177.61(14) . . . . ?
C12 C10 N1 C1 5.1(2) . . . . ?
C12 C10 N1 N2 -179.69(13) . . . . ?
C13 C11 P1 C21 -72.13(16) . . . . ?
C13 C11 P1 C18 51.09(16) . . . . ?
C13 C11 P1 N2 170.27(14) . . . . ?
C15 C14 O2 C12 -91.98(18) . . . . ?
C17 C16 O4 C13 176.70(15) . . . . ?
N1 C1 C2 C3 -179.05(14) . . . . ?
N1 C1 C2 C7 1.4(2) . . . . ?
N1 C1 C6 C5 179.46(13) . . . . ?
N1 C1 C6 C8 0.6(2) . . . . ?
N1 C10 C11 C13 -168.78(15) . . . . ?
N1 C10 C11 P1 -0.34(17) . . . . ?
N1 C10 C12 O1 69.4(2) . . . . ?
N1 C10 C12 O2 -108.53(16) . . . . ?
N1 N2 P1 C21 -124.93(10) . . . . ?
N1 N2 P1 C18 115.68(11) . . . . ?
N1 N2 P1 C11 -2.37(11) . . . . ?
O1 C12 O2 C14 -3.7(2) . . . . ?
O3 C13 O4 C16 1.3(2) . . . . ?
P1 C11 C13 O3 9.3(2) . . . . ?
P1 C11 C13 O4 -169.85(12) . . . . ?
C101 C102 C103 C104 1.1(2) . . . . ?
C101 N101 N102 P101 -178.18(10) . . . . ?
C102 C101 C106 C105 -0.5(2) . . . . ?
C102 C101 C106 C108 179.09(15) . . . . ?
C102 C101 N101 C110 -75.7(2) . . . . ?
C102 C101 N101 N102 99.97(16) . . . . ?
C102 C103 C104 C105 -1.2(2) . . . . ?
C102 C103 C104 C109 178.60(15) . . . . ?
C103 C104 C105 C106 0.5(2) . . . . ?
C104 C105 C106 C101 0.4(2) . . . . ?
C104 C105 C106 C108 -179.23(16) . . . . ?
C106 C101 C102 C103 -0.2(2) . . . . ?
C106 C101 C102 C107 178.98(15) . . . . ?
C106 C101 N101 C110 107.78(18) . . . . ?
C106 C101 N101 N102 -76.51(17) . . . . ?
C107 C102 C103 C104 -178.10(15) . . . . ?
C109 C104 C105 C106 -179.35(15) . . . . ?
C122 C121 P101 C118 52.83(15) . . . . ?
C122 C121 P101 C111 -177.44(13) . . . . ?
C122 C121 P101 N102 -69.07(15) . . . . ?
C123 C121 P101 C118 175.37(12) . . . . ?
C123 C121 P101 C111 -54.90(14) . . . . ?
C123 C121 P101 N102 53.46(14) . . . . ?
C120 C118 P101 C121 52.01(14) . . . . ?
C120 C118 P101 C111 -74.97(14) . . . . ?
C120 C118 P101 N102 175.80(12) . . . . ?
C119 C118 P101 C121 176.82(12) . . . . ?
C119 C118 P101 C111 49.84(15) . . . . ?
C119 C118 P101 N102 -59.39(14) . . . . ?
C110 C111 C113 O103 -177.58(16) . . . . ?
C110 C111 C113 O104 1.0(2) . . . . ?
C110 C111 P101 C121 118.52(12) . . . . ?
C110 C111 P101 C118 -117.64(12) . . . . ?
C110 C111 P101 N102 -0.43(12) . . . . ?
C110 C112 O102 C114 177.95(14) . . . . ?
C110 N101 N102 P101 -2.01(16) . . . . ?
C111 C110 C112 O101 117.1(2) . . . . ?
C111 C110 C112 O102 -63.8(2) . . . . ?
C111 C110 N101 C101 177.42(14) . . . . ?
C111 C110 N101 N102 1.8(2) . . . . ?
C111 C113 O104 C116 177.90(14) . . . . ?
C112 C110 C111 C113 -12.0(3) . . . . ?
C112 C110 C111 P101 179.04(13) . . . . ?
C112 C110 N101 C101 -2.3(2) . . . . ?
C112 C110 N101 N102 -177.94(13) . . . . ?
C113 C111 P101 C121 -51.15(16) . . . . ?
C113 C111 P101 C118 72.68(16) . . . . ?
C113 C111 P101 N102 -170.10(14) . . . . ?
C115 C114 O102 C112 165.01(19) . . . . ?
C117 C116 O104 C113 -176.72(14) . . . . ?
N101 C101 C102 C103 -176.51(13) . . . . ?
N101 C101 C102 C107 2.6(2) . . . . ?
N101 C101 C106 C105 175.85(14) . . . . ?
N101 C101 C106 C108 -4.5(2) . . . . ?
N101 C110 C111 C113 168.29(16) . . . . ?
N101 C110 C111 P101 -0.67(17) . . . . ?
N101 C110 C112 O101 -63.2(2) . . . . ?
N101 C110 C112 O102 115.85(16) . . . . ?
N101 N102 P101 C121 -116.86(10) . . . . ?
N101 N102 P101 C118 123.69(10) . . . . ?
N101 N102 P101 C111 1.30(11) . . . . ?
O101 C112 O102 C114 -3.0(2) . . . . ?
O103 C113 O104 C116 -3.5(2) . . . . ?
P101 C111 C113 O103 -10.5(2) . . . . ?
P101 C111 C113 O104 168.14(11) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-3.6707 5.5770 -5.9025 -0.0659 -0.0548 -0.9963
-7.9911 -4.0689 -3.3634 -0.7229 -0.6187 0.3076
9.2506 -1.4521 7.4998 0.6166 0.5263 0.5854
-2.0074 1.5849 18.1325 -0.3830 0.9230 0.0363
-1.1306 -0.0759 18.7635 -0.3651 0.8787 0.3076
1.3858 -0.3904 -18.7310 0.3730 -0.8979 -0.2337
1.0943 0.0515 18.3207 -0.1715 0.9242 0.3413
11.0396 0.2576 -0.7178 0.9292 0.2755 0.2463
-10.5928 1.7594 4.1536 -0.8865 0.0233 -0.4621
-2.8496 0.9154 18.3814 -0.4745 0.8729 0.1136
3.6178 -6.0179 0.4561 0.1278 -0.2379 0.9628
