#------------------------------------------------------------------------------
#$Date: 2024-10-04 20:22:16 +0200 (Fri 04 de Oct de 2024) $
#$Revision: 295056 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/71/7717160.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_7717160
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         'C49 H45 B F15 N2 O8 P'
_chemical_formula_sum            'C49 H45 B F15 N2 O8 P'
_chemical_formula_weight         1116.65
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-03
_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                112.034(3)
_cell_angle_beta                 97.787(3)
_cell_angle_gamma                107.389(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6836(4)
_cell_length_b                   14.3392(5)
_cell_length_c                   15.9046(5)
_cell_measurement_reflns_used    14828
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      72.6470
_cell_measurement_theta_min      3.7570
_cell_volume                     2456.51(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.81a (Rigaku OD, 2023)'
_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      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3537
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -71.00  32.00   1.00    1.00    --  -41.27  67.00  63.00  103
  2  ω   -114.00 -11.00   1.00    1.00    --  -41.27 -67.00 -70.00  103
  3  ω     11.00 114.00   1.00    1.00    --   41.27  67.00  63.00  103
  4  ω    -32.00  71.00   1.00    1.00    --   41.27 -67.00 -70.00  103
  5  ω     30.00 133.00   1.00    2.49    --  102.80 -67.00 -70.00  103
  6  ω     73.00 176.00   1.00    2.49    --  102.80  67.00  63.00  103
  7  ω     17.00 116.00   1.00    1.00    --   41.27  38.00-180.00   99
  8  ω      7.00  33.00   1.00    1.00    --   41.27  84.00 142.70   26
  9  ω    -31.00  69.00   1.00    1.00    --   41.27 -57.00 150.00  100
 10  ω     61.00 146.00   1.00    2.49    --  102.80 178.00-150.00   85
 11  ω     20.00 107.00   1.00    2.49    --  102.80 -94.00  30.00   87
 12  ω     29.00 108.00   1.00    2.49    --  102.80-111.00   0.00   79
 13  ω     29.00 108.00   1.00    2.49    --  102.80-111.00 -90.00   79
 14  ω     76.00 175.00   1.00    2.49    --  102.80  52.00 -64.75   99
 15  ω    104.00 176.00   1.00    2.49    --  102.80 111.00 -30.00   72
 16  ω    104.00 176.00   1.00    2.49    --  102.80 111.00-180.00   72
 17  ω    104.00 176.00   1.00    2.49    --  102.80 111.00-150.00   72
 18  ω     27.00 109.00   1.00    2.49    --  102.80-108.00 177.76   82
 19  ω     29.00 108.00   1.00    2.49    --  102.80-111.00 -60.00   79
 20  ω     77.00 176.00   1.00    2.49    --  102.80  45.00 150.00   99
 21  ω    103.00 178.00   1.00    2.49    --  102.80  77.00   0.00   75
 22  ω    104.00 176.00   1.00    2.49    --  102.80 111.00 -60.00   72
 23  ω      6.00  32.00   1.00    1.00    --   41.27  85.00-122.68   26
 24  ω     13.00 114.00   1.00    1.00    --   41.27  57.00-120.00  101
 25  ω     13.00  70.00   1.00    1.00    --   41.27  57.00  30.00   57
 26  ω      5.00  31.00   1.00    1.00    --   41.27  87.00 -85.86   26
;
_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      0.0459387000
_diffrn_orient_matrix_UB_12      -0.0514560000
_diffrn_orient_matrix_UB_13      -0.0833409000
_diffrn_orient_matrix_UB_21      0.0615063000
_diffrn_orient_matrix_UB_22      0.1131677000
_diffrn_orient_matrix_UB_23      0.0052253000
_diffrn_orient_matrix_UB_31      0.1080901000
_diffrn_orient_matrix_UB_32      0.0160106000
_diffrn_orient_matrix_UB_33      0.0698162000
_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  0.0418
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32120
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.823
_diffrn_reflns_theta_min         3.579
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.515
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.81a (Rigaku Oxford Diffraction, 2023)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_preparation       'Slow evaporation of hexane'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.049
_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     696
_refine_ls_number_reflns         9592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0356
_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)+(0.0455P)²+0.9279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7976
_reflns_number_total             9592
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02248c2.cif
_cod_data_source_block           edec_107_c_120_gaussian
_cod_original_cell_volume        2456.51(15)
_cod_database_code               7717160
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'C49 H45 F15 O8 N2 P1 B1'
_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   0.808
_shelx_estimated_absorpt_t_min   0.701
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C29(H29), C26(H26)
1.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B)
1.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5)
1.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C31(H31A,H31B,H31C),
 C30(H30A,H30B,H30C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C19(H19A,H19B,
 H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C)
;
_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 1.457
_oxdiff_exptl_absorpt_empirical_full_min 0.881
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
B1 B 0.31481(15) 0.53461(15) 0.14655(12) 0.0178(3) Uani 1 1 d . . . . .
C1 C 0.44794(13) 0.79365(13) 0.65521(11) 0.0194(3) Uani 1 1 d . . . . .
C2 C 0.44938(15) 0.78777(14) 0.74113(12) 0.0236(3) Uani 1 1 d . . . . .
C3 C 0.55641(16) 0.83391(16) 0.80750(13) 0.0298(4) Uani 1 1 d . . . . .
H3 H 0.560120 0.832284 0.866970 0.036 Uiso 1 1 calc R U . . .
C4 C 0.65799(16) 0.88227(16) 0.78947(14) 0.0329(4) Uani 1 1 d . . . . .
C5 C 0.65193(15) 0.88407(15) 0.70243(14) 0.0302(4) Uani 1 1 d . . . . .
H5 H 0.720943 0.916566 0.689493 0.036 Uiso 1 1 calc R U . . .
C6 C 0.54715(14) 0.83943(13) 0.63310(12) 0.0226(3) Uani 1 1 d . . . . .
C7 C 0.34249(16) 0.73434(17) 0.76244(13) 0.0305(4) Uani 1 1 d . . . . .
H7A H 0.286405 0.766542 0.753117 0.046 Uiso 1 1 calc R U . . .
H7B H 0.361404 0.745229 0.828120 0.046 Uiso 1 1 calc R U . . .
H7C H 0.309660 0.656261 0.720052 0.046 Uiso 1 1 calc R U . . .
C8 C 0.54428(15) 0.84241(15) 0.53932(13) 0.0289(4) Uani 1 1 d . . . . .
H8A H 0.486955 0.773914 0.488913 0.043 Uiso 1 1 calc R U . . .
H8B H 0.620258 0.852114 0.528502 0.043 Uiso 1 1 calc R U . . .
H8C H 0.523755 0.903133 0.539435 0.043 Uiso 1 1 calc R U . . .
C9 C 0.77248(19) 0.9311(2) 0.86316(18) 0.0539(6) Uani 1 1 d . . . . .
H9A H 0.776948 0.997034 0.915839 0.081 Uiso 1 1 calc R U . . .
H9B H 0.835015 0.949502 0.834946 0.081 Uiso 1 1 calc R U . . .
H9C H 0.779657 0.878286 0.886434 0.081 Uiso 1 1 calc R U . . .
C29 C 0.19473(14) 0.76039(13) 0.30707(11) 0.0212(3) Uani 1 1 d . . . . .
H29 H 0.226383 0.716091 0.260115 0.025 Uiso 1 1 calc R U . . .
C31 C 0.29279(15) 0.87148(15) 0.36573(13) 0.0275(4) Uani 1 1 d . . . . .
H31A H 0.264187 0.920973 0.408756 0.041 Uiso 1 1 calc R U . . .
H31B H 0.322035 0.901414 0.323543 0.041 Uiso 1 1 calc R U . . .
H31C H 0.354966 0.863204 0.402467 0.041 Uiso 1 1 calc R U . . .
C30 C 0.09373(16) 0.76866(15) 0.24888(12) 0.0278(4) Uani 1 1 d . . . . .
H30A H 0.034806 0.695679 0.209388 0.042 Uiso 1 1 calc R U . . .
H30B H 0.121428 0.802316 0.208525 0.042 Uiso 1 1 calc R U . . .
H30C H 0.060572 0.813271 0.291640 0.042 Uiso 1 1 calc R U . . .
C26 C 0.00313(13) 0.60145(14) 0.33724(11) 0.0204(3) Uani 1 1 d . . . . .
H26 H -0.040384 0.645124 0.325320 0.024 Uiso 1 1 calc R U . . .
C27 C -0.02408(14) 0.50251(14) 0.24333(12) 0.0227(3) Uani 1 1 d . . . . .
H27A H 0.002220 0.526929 0.197242 0.034 Uiso 1 1 calc R U . . .
H27B H -0.107312 0.460664 0.219716 0.034 Uiso 1 1 calc R U . . .
H27C H 0.015425 0.456545 0.252891 0.034 Uiso 1 1 calc R U . . .
C28 C -0.03824(15) 0.56768(15) 0.41094(13) 0.0276(4) Uani 1 1 d . . . . .
H28A H 0.001769 0.523414 0.423488 0.041 Uiso 1 1 calc R U . . .
H28B H -0.121330 0.525144 0.387208 0.041 Uiso 1 1 calc R U . . .
H28C H -0.021750 0.632771 0.469481 0.041 Uiso 1 1 calc R U . . .
C10 C 0.28400(13) 0.81204(13) 0.57239(11) 0.0180(3) Uani 1 1 d . . . . .
C11 C 0.18956(13) 0.78501(13) 0.50044(11) 0.0181(3) Uani 1 1 d . . . . .
C12 C 0.24890(12) 0.57689(12) 0.45731(11) 0.0155(3) Uani 1 1 d . . . . .
C13 C 0.24124(12) 0.61014(12) 0.38087(11) 0.0154(3) Uani 1 1 d . . . . .
C14 C 0.34193(14) 0.92897(13) 0.65011(12) 0.0214(3) Uani 1 1 d . . . . .
C15 C 0.12167(13) 0.85381(13) 0.51127(11) 0.0195(3) Uani 1 1 d . . . . .
C16 C 0.21126(13) 0.45566(13) 0.43307(11) 0.0175(3) Uani 1 1 d . . . . .
C17 C 0.27755(12) 0.55783(12) 0.30488(11) 0.0148(3) Uani 1 1 d . . . . .
C18 C 0.37254(18) 1.04517(17) 0.80972(14) 0.0392(5) Uani 1 1 d . . . . .
H18A H 0.350605 1.097083 0.791454 0.047 Uiso 1 1 calc R U . . .
H18B H 0.457507 1.070341 0.827940 0.047 Uiso 1 1 calc R U . . .
C19 C 0.3270(2) 1.0374(2) 0.89011(15) 0.0553(7) Uani 1 1 d . . . . .
H19A H 0.242726 1.007059 0.869476 0.083 Uiso 1 1 calc R U . . .
H19B H 0.354465 1.110077 0.942960 0.083 Uiso 1 1 calc R U . . .
H19C H 0.354211 0.989980 0.910444 0.083 Uiso 1 1 calc R U . . .
C20 C 0.07696(15) 0.99781(14) 0.61384(12) 0.0235(3) Uani 1 1 d . . . . .
H20A H 0.077984 1.021562 0.562891 0.028 Uiso 1 1 calc R U . . .
H20B H 0.118068 1.063079 0.674902 0.028 Uiso 1 1 calc R U . . .
C21 C -0.04569(15) 0.94577(15) 0.61261(14) 0.0287(4) Uani 1 1 d . . . . .
H21A H -0.086110 0.880181 0.552810 0.043 Uiso 1 1 calc R U . . .
H21B H -0.083989 0.997141 0.618907 0.043 Uiso 1 1 calc R U . . .
H21C H -0.046838 0.926091 0.665297 0.043 Uiso 1 1 calc R U . . .
C22 C 0.07605(16) 0.27967(14) 0.33029(13) 0.0284(4) Uani 1 1 d . . . . .
H22A H 0.076823 0.262695 0.385178 0.034 Uiso 1 1 calc R U . . .
H22B H 0.127682 0.251094 0.296234 0.034 Uiso 1 1 calc R U . . .
C23 C -0.04340(18) 0.22858(18) 0.26614(17) 0.0448(6) Uani 1 1 d . . . . .
H23A H -0.043478 0.246860 0.212625 0.067 Uiso 1 1 calc R U . . .
H23B H -0.094214 0.255954 0.300926 0.067 Uiso 1 1 calc R U . . .
H23C H -0.070907 0.149401 0.242767 0.067 Uiso 1 1 calc R U . . .
C24 C 0.44050(13) 0.52840(13) 0.37987(11) 0.0186(3) Uani 1 1 d . . . . .
H24A H 0.429696 0.556638 0.443853 0.022 Uiso 1 1 calc R U . . .
H24B H 0.502103 0.586739 0.375672 0.022 Uiso 1 1 calc R U . . .
C25 C 0.47089(15) 0.42999(15) 0.35992(13) 0.0263(4) Uani 1 1 d . . . . .
H25A H 0.469937 0.396750 0.293432 0.039 Uiso 1 1 calc R U . . .
H25B H 0.414647 0.377232 0.373012 0.039 Uiso 1 1 calc R U . . .
H25C H 0.547880 0.451864 0.400310 0.039 Uiso 1 1 calc R U . . .
C32 C 0.29204(14) 0.60644(13) 0.09031(11) 0.0186(3) Uani 1 1 d . . . . .
C33 C 0.37274(14) 0.66826(14) 0.06152(11) 0.0216(3) Uani 1 1 d . . . . .
C34 C 0.34914(15) 0.72818(15) 0.01588(12) 0.0256(4) Uani 1 1 d . . . . .
C35 C 0.24048(16) 0.72895(15) -0.00311(12) 0.0266(4) Uani 1 1 d . . . . .
C36 C 0.15657(15) 0.66805(15) 0.02221(12) 0.0242(4) Uani 1 1 d . . . . .
C37 C 0.18297(14) 0.60786(14) 0.06619(11) 0.0205(3) Uani 1 1 d . . . . .
C38 C 0.24912(14) 0.40560(13) 0.07240(11) 0.0195(3) Uani 1 1 d . . . . .
C39 C 0.27057(15) 0.36774(14) -0.01525(12) 0.0239(3) Uani 1 1 d . . . . .
C40 C 0.21384(17) 0.26285(16) -0.08549(12) 0.0293(4) Uani 1 1 d . . . . .
C41 C 0.13063(16) 0.18886(15) -0.07007(13) 0.0295(4) Uani 1 1 d . . . . .
C42 C 0.10689(14) 0.22074(14) 0.01546(13) 0.0245(4) Uani 1 1 d . . . . .
C43 C 0.16536(14) 0.32698(14) 0.08395(11) 0.0199(3) Uani 1 1 d . . . . .
C44 C 0.45249(13) 0.57519(14) 0.19556(11) 0.0190(3) Uani 1 1 d . . . . .
C45 C 0.51254(14) 0.68327(14) 0.26127(12) 0.0205(3) Uani 1 1 d . . . . .
C46 C 0.62830(14) 0.72684(15) 0.30887(13) 0.0248(4) Uani 1 1 d . . . . .
C47 C 0.68994(14) 0.66044(16) 0.29056(14) 0.0289(4) Uani 1 1 d . . . . .
C48 C 0.63541(15) 0.55364(16) 0.22589(14) 0.0288(4) Uani 1 1 d . . . . .
C49 C 0.51917(15) 0.51252(14) 0.18023(12) 0.0230(3) Uani 1 1 d . . . . .
F1 F 0.48240(8) 0.67400(9) 0.07699(7) 0.0292(2) Uani 1 1 d . . . . .
F2 F 0.43234(9) 0.78673(10) -0.00908(8) 0.0357(3) Uani 1 1 d . . . . .
F3 F 0.21728(10) 0.78810(10) -0.04596(8) 0.0381(3) Uani 1 1 d . . . . .
F4 F 0.05031(9) 0.66876(10) 0.00489(8) 0.0340(3) Uani 1 1 d . . . . .
F5 F 0.09512(8) 0.54751(9) 0.08592(7) 0.0261(2) Uani 1 1 d . . . . .
F6 F 0.35173(9) 0.43579(9) -0.03461(7) 0.0308(2) Uani 1 1 d . . . . .
F7 F 0.23882(11) 0.23151(10) -0.16886(8) 0.0427(3) Uani 1 1 d . . . . .
F8 F 0.07312(11) 0.08657(9) -0.13862(8) 0.0425(3) Uani 1 1 d . . . . .
F9 F 0.02485(9) 0.14992(9) 0.03133(8) 0.0341(2) Uani 1 1 d . . . . .
F10 F 0.13297(8) 0.35065(8) 0.16436(7) 0.0252(2) Uani 1 1 d . . . . .
F11 F 0.45658(8) 0.75202(8) 0.28156(7) 0.0253(2) Uani 1 1 d . . . . .
F12 F 0.68139(8) 0.83193(9) 0.37174(8) 0.0328(2) Uani 1 1 d . . . . .
F13 F 0.80252(9) 0.70215(11) 0.33563(10) 0.0447(3) Uani 1 1 d . . . . .
F14 F 0.69611(10) 0.48930(11) 0.20650(10) 0.0429(3) Uani 1 1 d . . . . .
F15 F 0.47290(9) 0.40576(9) 0.11992(7) 0.0302(2) Uani 1 1 d . . . . .
N1 N 0.33837(11) 0.74859(11) 0.58383(9) 0.0177(3) Uani 1 1 d . . . . .
N2 N 0.29057(11) 0.63448(11) 0.54685(9) 0.0175(3) Uani 1 1 d . . . . .
O1 O 0.39965(11) 1.00110(10) 0.63567(9) 0.0302(3) Uani 1 1 d . . . . .
O2 O 0.32134(10) 0.93594(10) 0.73149(8) 0.0253(3) Uani 1 1 d . . . . .
O3 O 0.05447(10) 0.84571(10) 0.44406(8) 0.0245(3) Uani 1 1 d . . . . .
O4 O 0.13682(10) 0.92253(10) 0.60073(8) 0.0235(3) Uani 1 1 d . . . . .
O5 O 0.26255(10) 0.42021(9) 0.47430(8) 0.0235(2) Uani 1 1 d . . . . .
O6 O 0.11507(9) 0.39683(9) 0.36204(8) 0.0209(2) Uani 1 1 d . . . . .
O7 O 0.25579(9) 0.56392(9) 0.22564(7) 0.0165(2) Uani 1 1 d . . . . .
O8 O 0.33239(9) 0.49126(9) 0.30720(8) 0.0174(2) Uani 1 1 d . . . . .
P1 P 0.15647(3) 0.68900(3) 0.38044(3) 0.01566(9) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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
-1 0 -9 0.0633
0 -9 3 0.0808
-5 -3 -2 0.0914
1 8 -3 0.0628
5 3 2 0.0869
6 -5 6 0.0915
-1 0 9 0.0838
-6 3 7 0.0876
-7 4 6 0.0986
-1 1 -9 0.0607
2 -1 -9 0.0625
8 -4 -2 0.1156
7 -4 5 0.0918
0 -6 -4 0.0778
-2 -4 -5 0.0743
7 0 -6 0.0835
8 -2 1 0.0855
0 4 -10 0.0605
8 0 -1 0.0773
-1 -8 7 0.0751
1 -3 -8 0.0680
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
C38 B1 C32 107.71(12) . . ?
C44 B1 C32 110.59(13) . . ?
C44 B1 C38 115.99(13) . . ?
O7 B1 C32 103.52(12) . . ?
O7 B1 C38 110.08(13) . . ?
O7 B1 C44 108.23(12) . . ?
C2 C1 N1 119.34(15) . . ?
C6 C1 C2 123.16(15) . . ?
C6 C1 N1 117.50(14) . . ?
C1 C2 C7 122.59(15) . . ?
C3 C2 C1 116.89(17) . . ?
C3 C2 C7 120.52(16) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 C2 122.17(17) . . ?
C4 C3 H3 118.9 . . ?
C3 C4 C9 120.6(2) . . ?
C5 C4 C3 118.58(16) . . ?
C5 C4 C9 120.8(2) . . ?
C4 C5 H5 119.0 . . ?
C4 C5 C6 121.91(18) . . ?
C6 C5 H5 119.0 . . ?
C1 C6 C5 117.25(16) . . ?
C1 C6 C8 122.46(15) . . ?
C5 C6 C8 120.29(16) . . ?
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 . . ?
C31 C29 H29 106.0 . . ?
C31 C29 C30 111.77(14) . . ?
C31 C29 P1 110.95(11) . . ?
C30 C29 H29 106.0 . . ?
C30 C29 P1 115.50(13) . . ?
P1 C29 H29 106.0 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C27 C26 H26 107.3 . . ?
C27 C26 P1 111.53(11) . . ?
C28 C26 H26 107.3 . . ?
C28 C26 C27 111.47(14) . . ?
C28 C26 P1 111.67(11) . . ?
P1 C26 H26 107.3 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C11 C10 C14 119.60(14) . . ?
N1 C10 C11 128.48(15) . . ?
N1 C10 C14 111.89(13) . . ?
C10 C11 C15 121.01(14) . . ?
C10 C11 P1 125.60(12) . . ?
C15 C11 P1 111.78(11) . . ?
C13 C12 C16 119.45(13) . . ?
N2 C12 C13 130.24(14) . . ?
N2 C12 C16 110.14(13) . . ?
C12 C13 P1 116.87(11) . . ?
C17 C13 C12 116.81(13) . . ?
C17 C13 P1 124.59(11) . . ?
O1 C14 C10 121.62(16) . . ?
O1 C14 O2 127.04(16) . . ?
O2 C14 C10 111.32(14) . . ?
O3 C15 C11 122.20(14) . . ?
O3 C15 O4 123.16(14) . . ?
O4 C15 C11 114.59(13) . . ?
O5 C16 C12 123.49(14) . . ?
O5 C16 O6 125.42(15) . . ?
O6 C16 C12 111.09(13) . . ?
O7 C17 C13 123.01(13) . . ?
O7 C17 O8 115.54(13) . . ?
O8 C17 C13 121.33(13) . . ?
H18A C18 H18B 108.6 . . ?
C19 C18 H18A 110.4 . . ?
C19 C18 H18B 110.4 . . ?
O2 C18 H18A 110.4 . . ?
O2 C18 H18B 110.4 . . ?
O2 C18 C19 106.41(18) . . ?
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 . . ?
H20A C20 H20B 108.0 . . ?
C21 C20 H20A 109.3 . . ?
C21 C20 H20B 109.3 . . ?
O4 C20 H20A 109.3 . . ?
O4 C20 H20B 109.3 . . ?
O4 C20 C21 111.61(14) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
H22A C22 H22B 108.4 . . ?
C23 C22 H22A 110.1 . . ?
C23 C22 H22B 110.1 . . ?
O6 C22 H22A 110.1 . . ?
O6 C22 H22B 110.1 . . ?
O6 C22 C23 108.02(15) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
H24A C24 H24B 108.7 . . ?
C25 C24 H24A 110.6 . . ?
C25 C24 H24B 110.6 . . ?
O8 C24 H24A 110.6 . . ?
O8 C24 H24B 110.6 . . ?
O8 C24 C25 105.73(13) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C33 C32 B1 126.48(14) . . ?
C33 C32 C37 113.22(14) . . ?
C37 C32 B1 120.29(14) . . ?
C34 C33 C32 123.96(15) . . ?
F1 C33 C32 121.27(14) . . ?
F1 C33 C34 114.78(15) . . ?
C35 C34 C33 119.89(17) . . ?
F2 C34 C33 120.37(16) . . ?
F2 C34 C35 119.73(16) . . ?
C36 C35 C34 118.87(15) . . ?
F3 C35 C34 120.32(17) . . ?
F3 C35 C36 120.82(16) . . ?
C35 C36 C37 119.52(15) . . ?
F4 C36 C35 119.54(15) . . ?
F4 C36 C37 120.93(16) . . ?
C36 C37 C32 124.47(16) . . ?
F5 C37 C32 119.62(14) . . ?
F5 C37 C36 115.91(14) . . ?
C39 C38 B1 119.31(15) . . ?
C43 C38 B1 126.93(14) . . ?
C43 C38 C39 113.61(15) . . ?
C40 C39 C38 124.07(17) . . ?
F6 C39 C38 119.40(15) . . ?
F6 C39 C40 116.53(15) . . ?
C41 C40 C39 119.54(16) . . ?
F7 C40 C39 121.03(17) . . ?
F7 C40 C41 119.43(16) . . ?
C42 C41 C40 119.16(16) . . ?
F8 C41 C40 120.21(17) . . ?
F8 C41 C42 120.62(18) . . ?
C41 C42 C43 119.50(17) . . ?
F9 C42 C41 119.96(16) . . ?
F9 C42 C43 120.51(16) . . ?
C42 C43 C38 124.10(15) . . ?
F10 C43 C38 121.21(15) . . ?
F10 C43 C42 114.67(15) . . ?
C45 C44 B1 118.75(14) . . ?
C49 C44 B1 127.08(15) . . ?
C49 C44 C45 114.16(14) . . ?
C46 C45 C44 124.25(15) . . ?
F11 C45 C44 119.39(14) . . ?
F11 C45 C46 116.36(15) . . ?
C47 C46 C45 118.86(17) . . ?
F12 C46 C45 121.44(15) . . ?
F12 C46 C47 119.69(15) . . ?
C48 C47 C46 119.33(15) . . ?
F13 C47 C46 119.33(17) . . ?
F13 C47 C48 121.33(16) . . ?
C47 C48 C49 120.25(16) . . ?
F14 C48 C47 119.37(16) . . ?
F14 C48 C49 120.38(17) . . ?
C48 C49 C44 123.14(17) . . ?
F15 C49 C44 121.21(15) . . ?
F15 C49 C48 115.65(15) . . ?
C10 N1 C1 121.59(13) . . ?
C10 N1 N2 126.26(13) . . ?
N2 N1 C1 110.79(12) . . ?
C12 N2 N1 119.42(13) . . ?
C14 O2 C18 115.11(15) . . ?
C15 O4 C20 116.10(12) . . ?
C16 O6 C22 115.12(12) . . ?
C17 O7 B1 127.47(12) . . ?
C17 O8 C24 122.27(12) . . ?
C26 P1 C29 110.76(8) . . ?
C11 P1 C29 110.14(8) . . ?
C11 P1 C26 109.71(8) . . ?
C13 P1 C29 110.28(7) . . ?
C13 P1 C26 110.02(7) . . ?
C13 P1 C11 105.82(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
B1 C32 1.656(2) . ?
B1 C38 1.638(2) . ?
B1 C44 1.637(2) . ?
B1 O7 1.538(2) . ?
C1 C2 1.398(2) . ?
C1 C6 1.392(2) . ?
C1 N1 1.4571(19) . ?
C2 C3 1.395(2) . ?
C2 C7 1.496(3) . ?
C3 H3 0.9500 . ?
C3 C4 1.392(3) . ?
C4 C5 1.386(3) . ?
C4 C9 1.513(3) . ?
C5 H5 0.9500 . ?
C5 C6 1.399(2) . ?
C6 C8 1.504(3) . ?
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 . ?
C29 H29 1.0000 . ?
C29 C31 1.530(2) . ?
C29 C30 1.537(2) . ?
C29 P1 1.8434(17) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.530(2) . ?
C26 C28 1.525(2) . ?
C26 P1 1.8336(16) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C10 C11 1.383(2) . ?
C10 C14 1.530(2) . ?
C10 N1 1.342(2) . ?
C11 C15 1.471(2) . ?
C11 P1 1.7833(16) . ?
C12 C13 1.465(2) . ?
C12 C16 1.533(2) . ?
C12 N2 1.281(2) . ?
C13 C17 1.383(2) . ?
C13 P1 1.7791(15) . ?
C14 O1 1.196(2) . ?
C14 O2 1.328(2) . ?
C15 O3 1.218(2) . ?
C15 O4 1.3391(19) . ?
C16 O5 1.201(2) . ?
C16 O6 1.3314(19) . ?
C17 O7 1.2942(19) . ?
C17 O8 1.3463(18) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.499(3) . ?
C18 O2 1.461(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C20 C21 1.505(2) . ?
C20 O4 1.4659(18) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C23 1.493(3) . ?
C22 O6 1.456(2) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.504(2) . ?
C24 O8 1.4738(18) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C32 C33 1.390(2) . ?
C32 C37 1.393(2) . ?
C33 C34 1.385(2) . ?
C33 F1 1.3511(19) . ?
C34 C35 1.375(3) . ?
C34 F2 1.345(2) . ?
C35 C36 1.372(3) . ?
C35 F3 1.3412(19) . ?
C36 C37 1.381(2) . ?
C36 F4 1.3424(19) . ?
C37 F5 1.3458(19) . ?
C38 C39 1.391(2) . ?
C38 C43 1.388(2) . ?
C39 C40 1.379(3) . ?
C39 F6 1.348(2) . ?
C40 C41 1.377(3) . ?
C40 F7 1.346(2) . ?
C41 C42 1.370(3) . ?
C41 F8 1.348(2) . ?
C42 C43 1.385(2) . ?
C42 F9 1.345(2) . ?
C43 F10 1.3490(19) . ?
C44 C45 1.392(2) . ?
C44 C49 1.388(2) . ?
C45 C46 1.384(2) . ?
C45 F11 1.3495(18) . ?
C46 C47 1.379(3) . ?
C46 F12 1.343(2) . ?
C47 C48 1.369(3) . ?
C47 F13 1.342(2) . ?
C48 C49 1.385(2) . ?
C48 F14 1.347(2) . ?
C49 F15 1.348(2) . ?
N1 N2 1.4068(18) . ?
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
B1 C32 C33 C34 -178.96(16) . . . . ?
B1 C32 C33 F1 0.9(3) . . . . ?
B1 C32 C37 C36 177.73(15) . . . . ?
B1 C32 C37 F5 -2.3(2) . . . . ?
B1 C38 C39 C40 -175.01(16) . . . . ?
B1 C38 C39 F6 5.3(2) . . . . ?
B1 C38 C43 C42 175.00(15) . . . . ?
B1 C38 C43 F10 -3.5(2) . . . . ?
B1 C44 C45 C46 178.66(16) . . . . ?
B1 C44 C45 F11 -1.2(2) . . . . ?
B1 C44 C49 C48 -179.22(17) . . . . ?
B1 C44 C49 F15 -0.3(3) . . . . ?
C1 C2 C3 C4 -1.0(3) . . . . ?
C1 N1 N2 C12 -134.62(14) . . . . ?
C2 C1 C6 C5 -2.0(2) . . . . ?
C2 C1 C6 C8 178.33(16) . . . . ?
C2 C1 N1 C10 99.19(19) . . . . ?
C2 C1 N1 N2 -68.29(18) . . . . ?
C2 C3 C4 C5 -0.2(3) . . . . ?
C2 C3 C4 C9 -179.8(2) . . . . ?
C3 C4 C5 C6 0.4(3) . . . . ?
C4 C5 C6 C1 0.7(3) . . . . ?
C4 C5 C6 C8 -179.62(17) . . . . ?
C6 C1 C2 C3 2.1(2) . . . . ?
C6 C1 C2 C7 -177.48(16) . . . . ?
C6 C1 N1 C10 -81.8(2) . . . . ?
C6 C1 N1 N2 110.72(16) . . . . ?
C7 C2 C3 C4 178.61(18) . . . . ?
C9 C4 C5 C6 180.0(2) . . . . ?
C31 C29 P1 C26 149.00(11) . . . . ?
C31 C29 P1 C11 27.46(14) . . . . ?
C31 C29 P1 C13 -88.97(13) . . . . ?
C30 C29 P1 C26 20.49(15) . . . . ?
C30 C29 P1 C11 -101.05(13) . . . . ?
C30 C29 P1 C13 142.52(12) . . . . ?
C27 C26 P1 C29 71.03(13) . . . . ?
C27 C26 P1 C11 -167.18(11) . . . . ?
C27 C26 P1 C13 -51.15(14) . . . . ?
C28 C26 P1 C29 -163.51(12) . . . . ?
C28 C26 P1 C11 -41.72(14) . . . . ?
C28 C26 P1 C13 74.31(13) . . . . ?
C10 C11 C15 O3 164.20(16) . . . . ?
C10 C11 C15 O4 -18.1(2) . . . . ?
C10 C11 P1 C29 -102.60(15) . . . . ?
C10 C11 P1 C26 135.23(15) . . . . ?
C10 C11 P1 C13 16.58(17) . . . . ?
C10 C14 O2 C18 -179.42(14) . . . . ?
C10 N1 N2 C12 58.6(2) . . . . ?
C11 C10 C14 O1 -73.1(2) . . . . ?
C11 C10 C14 O2 108.45(17) . . . . ?
C11 C10 N1 C1 169.88(16) . . . . ?
C11 C10 N1 N2 -24.7(3) . . . . ?
C11 C15 O4 C20 175.77(14) . . . . ?
C12 C13 C17 O7 166.57(13) . . . . ?
C12 C13 C17 O8 -9.3(2) . . . . ?
C12 C13 P1 C29 161.10(11) . . . . ?
C12 C13 P1 C26 -76.43(13) . . . . ?
C12 C13 P1 C11 42.01(13) . . . . ?
C12 C16 O6 C22 176.65(13) . . . . ?
C13 C12 C16 O5 139.10(16) . . . . ?
C13 C12 C16 O6 -41.55(18) . . . . ?
C13 C12 N2 N1 0.0(2) . . . . ?
C13 C17 O7 B1 163.51(15) . . . . ?
C13 C17 O8 C24 -58.1(2) . . . . ?
C14 C10 C11 C15 -19.3(2) . . . . ?
C14 C10 C11 P1 144.96(14) . . . . ?
C14 C10 N1 C1 -7.8(2) . . . . ?
C14 C10 N1 N2 157.61(14) . . . . ?
C15 C11 P1 C29 62.93(13) . . . . ?
C15 C11 P1 C26 -59.24(14) . . . . ?
C15 C11 P1 C13 -177.88(11) . . . . ?
C16 C12 C13 C17 -43.17(19) . . . . ?
C16 C12 C13 P1 122.51(13) . . . . ?
C16 C12 N2 N1 175.25(12) . . . . ?
C17 C13 P1 C29 -34.44(16) . . . . ?
C17 C13 P1 C26 88.03(15) . . . . ?
C17 C13 P1 C11 -153.53(13) . . . . ?
C19 C18 O2 C14 173.01(16) . . . . ?
C21 C20 O4 C15 83.80(18) . . . . ?
C23 C22 O6 C16 168.07(16) . . . . ?
C25 C24 O8 C17 178.05(14) . . . . ?
C32 B1 C38 C39 52.83(18) . . . . ?
C32 B1 C38 C43 -122.48(16) . . . . ?
C32 B1 C44 C45 58.80(19) . . . . ?
C32 B1 C44 C49 -122.25(17) . . . . ?
C32 B1 O7 C17 -156.59(14) . . . . ?
C32 C33 C34 C35 0.2(3) . . . . ?
C32 C33 C34 F2 179.46(15) . . . . ?
C33 C32 C37 C36 -3.0(2) . . . . ?
C33 C32 C37 F5 177.01(14) . . . . ?
C33 C34 C35 C36 -1.3(3) . . . . ?
C33 C34 C35 F3 178.95(16) . . . . ?
C34 C35 C36 C37 0.2(3) . . . . ?
C34 C35 C36 F4 179.40(16) . . . . ?
C35 C36 C37 C32 2.1(3) . . . . ?
C35 C36 C37 F5 -177.87(15) . . . . ?
C37 C32 C33 C34 1.8(2) . . . . ?
C37 C32 C33 F1 -178.37(14) . . . . ?
C38 B1 C32 C33 -109.01(18) . . . . ?
C38 B1 C32 C37 70.18(18) . . . . ?
C38 B1 C44 C45 -178.20(14) . . . . ?
C38 B1 C44 C49 0.8(2) . . . . ?
C38 B1 O7 C17 88.50(17) . . . . ?
C38 C39 C40 C41 -0.3(3) . . . . ?
C38 C39 C40 F7 179.97(16) . . . . ?
C39 C38 C43 C42 -0.5(2) . . . . ?
C39 C38 C43 F10 -178.99(14) . . . . ?
C39 C40 C41 C42 -0.8(3) . . . . ?
C39 C40 C41 F8 178.89(16) . . . . ?
C40 C41 C42 C43 1.2(3) . . . . ?
C40 C41 C42 F9 179.16(16) . . . . ?
C41 C42 C43 C38 -0.5(3) . . . . ?
C41 C42 C43 F10 178.07(15) . . . . ?
C43 C38 C39 C40 0.9(2) . . . . ?
C43 C38 C39 F6 -178.78(14) . . . . ?
C44 B1 C32 C33 18.7(2) . . . . ?
C44 B1 C32 C37 -162.13(14) . . . . ?
C44 B1 C38 C39 -71.67(19) . . . . ?
C44 B1 C38 C43 113.02(18) . . . . ?
C44 B1 O7 C17 -39.2(2) . . . . ?
C44 C45 C46 C47 0.5(3) . . . . ?
C44 C45 C46 F12 -179.85(15) . . . . ?
C45 C44 C49 C48 -0.2(2) . . . . ?
C45 C44 C49 F15 178.73(15) . . . . ?
C45 C46 C47 C48 0.2(3) . . . . ?
C45 C46 C47 F13 179.33(16) . . . . ?
C46 C47 C48 C49 -0.8(3) . . . . ?
C46 C47 C48 F14 178.60(17) . . . . ?
C47 C48 C49 C44 0.8(3) . . . . ?
C47 C48 C49 F15 -178.17(16) . . . . ?
C49 C44 C45 C46 -0.4(2) . . . . ?
C49 C44 C45 F11 179.71(14) . . . . ?
F1 C33 C34 C35 -179.62(15) . . . . ?
F1 C33 C34 F2 -0.4(2) . . . . ?
F2 C34 C35 C36 179.49(16) . . . . ?
F2 C34 C35 F3 -0.3(3) . . . . ?
F3 C35 C36 C37 179.95(16) . . . . ?
F3 C35 C36 F4 -0.8(3) . . . . ?
F4 C36 C37 C32 -177.11(15) . . . . ?
F4 C36 C37 F5 2.9(2) . . . . ?
F6 C39 C40 C41 179.43(16) . . . . ?
F6 C39 C40 F7 -0.3(3) . . . . ?
F7 C40 C41 C42 178.96(16) . . . . ?
F7 C40 C41 F8 -1.3(3) . . . . ?
F8 C41 C42 C43 -178.55(15) . . . . ?
F8 C41 C42 F9 -0.6(3) . . . . ?
F9 C42 C43 C38 -178.46(15) . . . . ?
F9 C42 C43 F10 0.1(2) . . . . ?
F11 C45 C46 C47 -179.67(15) . . . . ?
F11 C45 C46 F12 0.0(2) . . . . ?
F12 C46 C47 C48 -179.53(17) . . . . ?
F12 C46 C47 F13 -0.4(3) . . . . ?
F13 C47 C48 C49 -179.93(17) . . . . ?
F13 C47 C48 F14 -0.5(3) . . . . ?
F14 C48 C49 C44 -178.54(16) . . . . ?
F14 C48 C49 F15 2.5(3) . . . . ?
N1 C1 C2 C3 -178.90(15) . . . . ?
N1 C1 C2 C7 1.5(2) . . . . ?
N1 C1 C6 C5 179.04(15) . . . . ?
N1 C1 C6 C8 -0.7(2) . . . . ?
N1 C10 C11 C15 163.09(16) . . . . ?
N1 C10 C11 P1 -32.6(3) . . . . ?
N1 C10 C14 O1 104.80(18) . . . . ?
N1 C10 C14 O2 -73.60(17) . . . . ?
N2 C12 C13 C17 131.70(17) . . . . ?
N2 C12 C13 P1 -62.6(2) . . . . ?
N2 C12 C16 O5 -36.7(2) . . . . ?
N2 C12 C16 O6 142.62(13) . . . . ?
O1 C14 O2 C18 2.3(2) . . . . ?
O3 C15 O4 C20 -6.6(2) . . . . ?
O5 C16 O6 C22 -4.0(2) . . . . ?
O7 B1 C32 C33 134.41(16) . . . . ?
O7 B1 C32 C37 -46.40(18) . . . . ?
O7 B1 C38 C39 165.05(13) . . . . ?
O7 B1 C38 C43 -10.3(2) . . . . ?
O7 B1 C44 C45 -53.95(19) . . . . ?
O7 B1 C44 C49 125.00(17) . . . . ?
O7 C17 O8 C24 125.75(14) . . . . ?
O8 C17 O7 B1 -20.4(2) . . . . ?
P1 C11 C15 O3 -2.1(2) . . . . ?
P1 C11 C15 O4 175.58(12) . . . . ?
P1 C13 C17 O7 2.1(2) . . . . ?
P1 C13 C17 O8 -173.72(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
-1.3833 0.3982 -8.7864 0.6482 -0.0859 -0.7566
-0.2583 -8.6783 3.0248 0.1826 -0.9822 0.0443
-4.8594 -3.1786 -2.2244 0.1257 -0.6702 -0.7314
0.7545 8.3903 -2.5713 -0.1828 0.9825 0.0364
4.9550 2.9553 2.3738 -0.1223 0.6516 0.7486
5.9884 -4.8991 5.9975 0.0273 -0.1548 0.9876
-0.7692 0.1663 9.3247 -0.8210 0.0202 0.5705
-5.6539 2.9754 7.0083 -0.9969 0.0256 -0.0742
-6.5366 3.5033 5.8781 -0.9704 0.0251 -0.2401
-1.3025 0.9910 -9.1113 0.6485 -0.0156 -0.7610
1.7675 -0.7304 -9.2050 0.8859 -0.0220 -0.4633
7.9278 -4.3887 -2.2178 0.7749 -0.0206 0.6318
6.6659 -3.8805 4.8141 0.1047 -0.0040 0.9945
-0.3479 -5.8046 -3.7792 0.5977 -0.6980 -0.3944
-1.6300 -4.4261 -4.5928 0.5356 -0.6251 -0.5677
7.3386 0.1494 -5.7320 0.8072 0.4383 0.3954
7.9871 -2.3028 0.6339 0.4326 0.2340 0.8707
-0.1430 3.6954 -10.1976 0.6532 0.3561 -0.6683
7.7319 0.1454 -1.3577 0.4609 0.4849 0.7433
-1.1683 -8.0393 7.0382 -0.2266 -0.9449 0.2364
1.1551 -2.9016 -7.6427 0.8393 -0.2973 -0.4552
