#------------------------------------------------------------------------------
#$Date: 2025-11-29 18:40:28 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303529 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/49/7134935.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_7134935
loop_
_publ_author_name
'Groth, Lucie J.'
'Bockfeld, Dirk'
'Tamm, Matthias'
_publ_section_title
;
 Heavy alkali metal complexes of N-heterocyclic carbenes.
;
_journal_issue                   81
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              15806
_journal_page_last               15809
_journal_paper_doi               10.1039/d5cc04534g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety
'C53 H51 B F15 K N2 O2, 0.354(C4 H8 O), 0.146(C5 H12)'
_chemical_formula_sum            'C55.15 H55.58 B F15 K N2 O2.36'
_chemical_formula_weight         1118.93
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-08-06 deposited with the CCDC.	2025-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.8760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.40850(10)
_cell_length_b                   21.4020(3)
_cell_length_c                   23.6416(4)
_cell_measurement_reflns_used    55210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      79.2740
_cell_measurement_theta_min      2.7700
_cell_volume                     5238.80(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.64a (Rigaku OD, 2022)'
_computing_publication_material
'OLEX2 v1.3 (O. V. Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)'
_computing_structure_refinement
'SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3-8)'
_computing_structure_solution
'SHELXT 2018/2 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3-8)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       'ω scans'
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            116504
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.270
_diffrn_reflns_theta_min         2.792
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.754
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.64a (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            colourless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       'fragment of needle'
_exptl_crystal_F_000             2313
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.627
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         11349
_refine_ls_number_restraints     141
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0451
_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)+(0.0591P)²+3.1933P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1213
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10234
_reflns_number_total             11349
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5cc04534g2.cif
_cod_data_source_block           lgr02db
_cod_depositor_comments
'Adding full bibliography for 7134934--7134942.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7134935
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.721
_shelx_estimated_absorpt_t_max   0.917
_oxdiff_exptl_absorpt_empirical_full_min 0.692
_oxdiff_exptl_absorpt_empirical_full_max 1.822
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.56357(4) 0.23128(2) 0.41215(2) 0.04028(11) Uani 1 1 d . . . . .
F1 F 0.46318(9) 0.03399(5) 0.22610(5) 0.0366(2) Uani 1 1 d . . . . .
F2 F 0.29106(10) -0.04414(6) 0.17565(6) 0.0482(3) Uani 1 1 d . . . . .
F3 F 0.35853(10) -0.16337(5) 0.15001(5) 0.0435(3) Uani 1 1 d . . . . .
F4 F 0.60190(11) -0.20368(5) 0.18132(5) 0.0395(3) Uani 1 1 d . . . . .
F5 F 0.77928(9) -0.12615(4) 0.23122(5) 0.0323(2) Uani 1 1 d . . . . .
F6 F 0.74989(12) -0.03352(7) 0.13607(5) 0.0497(3) Uani 1 1 d . . . . .
F7 F 0.92909(14) -0.00542(8) 0.07047(5) 0.0607(4) Uani 1 1 d . . . . .
F8 F 1.14399(11) 0.05957(6) 0.11053(5) 0.0452(3) Uani 1 1 d . . . . .
F9 F 1.17361(9) 0.09494(5) 0.22189(5) 0.0385(2) Uani 1 1 d . . . . .
F10 F 0.99437(9) 0.06805(5) 0.28994(4) 0.0307(2) Uani 1 1 d . . . . .
F11 F 0.59069(8) -0.03781(4) 0.34865(4) 0.0272(2) Uani 1 1 d . . . . .
F12 F 0.65094(10) -0.11039(5) 0.43846(4) 0.0348(2) Uani 1 1 d . . . . .
F13 F 0.89360(12) -0.15858(5) 0.45964(4) 0.0402(3) Uani 1 1 d . . . . .
F14 F 1.07690(10) -0.12700(5) 0.39078(5) 0.0408(3) Uani 1 1 d . . . . .
F15 F 1.02091(9) -0.05539(5) 0.30113(4) 0.0327(2) Uani 1 1 d . . . . .
O1 O 0.36161(18) 0.28449(8) 0.45376(9) 0.0642(5) Uani 1 1 d . . . . .
O2 O 0.72111(19) 0.28221(9) 0.49314(7) 0.0633(5) Uani 1 1 d . . . . .
N1 N 0.65428(12) 0.10652(6) 0.32195(5) 0.0208(2) Uani 1 1 d . . . . .
N2 N 0.65919(12) 0.17542(6) 0.25734(6) 0.0226(3) Uani 1 1 d . . . . .
C1 C 0.62755(14) 0.16852(7) 0.31098(7) 0.0231(3) Uani 1 1 d . . . . .
C2 C 0.70457(13) 0.07468(7) 0.27618(7) 0.0214(3) Uani 1 1 d . . . . .
C3 C 0.70638(14) 0.12043(7) 0.23634(7) 0.0237(3) Uani 1 1 d . . . . .
H3 H 0.735448 0.115488 0.199797 0.028 Uiso 1 1 calc R U . . .
C4 C 0.63460(14) 0.08795(7) 0.37915(6) 0.0221(3) Uani 1 1 d . . . . .
C5 C 0.74097(15) 0.08678(7) 0.42078(7) 0.0260(3) Uani 1 1 d . . . . .
C6 C 0.71712(18) 0.07805(8) 0.47726(7) 0.0333(4) Uani 1 1 d . . . . .
H6 H 0.787711 0.076269 0.506060 0.040 Uiso 1 1 calc R U . . .
C7 C 0.59272(19) 0.07194(9) 0.49205(8) 0.0371(4) Uani 1 1 d . . . . .
H7 H 0.578290 0.066739 0.530798 0.044 Uiso 1 1 calc R U . . .
C8 C 0.48918(18) 0.07338(8) 0.45043(8) 0.0332(4) Uani 1 1 d . . . . .
H8 H 0.404049 0.069020 0.461057 0.040 Uiso 1 1 calc R U . . .
C9 C 0.50717(15) 0.08112(7) 0.39315(7) 0.0253(3) Uani 1 1 d . . . . .
C10 C 0.87686(15) 0.09984(8) 0.40602(7) 0.0301(3) Uani 1 1 d . . . . .
H10 H 0.878910 0.091776 0.364461 0.036 Uiso 1 1 calc R U . . .
C11 C 0.97789(17) 0.05776(9) 0.43847(9) 0.0374(4) Uani 1 1 d . . . . .
H11A H 0.986194 0.068884 0.478884 0.056 Uiso 1 1 calc R U . . .
H11B H 1.061300 0.063408 0.423315 0.056 Uiso 1 1 calc R U . . .
H11C H 0.950886 0.014017 0.433981 0.056 Uiso 1 1 calc R U . . .
C12 C 0.91013(18) 0.16885(9) 0.41721(9) 0.0393(4) Uani 1 1 d . . . . .
H12A H 0.848172 0.195174 0.394069 0.059 Uiso 1 1 calc R U . . .
H12B H 0.997519 0.177235 0.407159 0.059 Uiso 1 1 calc R U . . .
H12C H 0.905943 0.178226 0.457555 0.059 Uiso 1 1 calc R U . . .
C13 C 0.38977(15) 0.08243(8) 0.34892(8) 0.0286(3) Uani 1 1 d . . . . .
H13 H 0.421639 0.085067 0.310503 0.034 Uiso 1 1 calc R U . . .
C14 C 0.30987(17) 0.02272(8) 0.35087(10) 0.0422(5) Uani 1 1 d . . . . .
H14A H 0.363533 -0.013439 0.343552 0.063 Uiso 1 1 calc R U . . .
H14B H 0.235764 0.024758 0.321811 0.063 Uiso 1 1 calc R U . . .
H14C H 0.279083 0.018531 0.388497 0.063 Uiso 1 1 calc R U . . .
C15 C 0.30401(19) 0.13947(9) 0.35609(9) 0.0405(4) Uani 1 1 d . . . . .
H15A H 0.278007 0.140072 0.394774 0.061 Uiso 1 1 calc R U . . .
H15C H 0.226956 0.137176 0.328634 0.061 Uiso 1 1 calc R U . . .
H15B H 0.352200 0.177663 0.349453 0.061 Uiso 1 1 calc R U . . .
C16 C 0.65121(15) 0.23411(7) 0.22752(7) 0.0256(3) Uani 1 1 d . . . . .
C17 C 0.53783(16) 0.24796(8) 0.19249(7) 0.0284(3) Uani 1 1 d . . . . .
C18 C 0.53409(18) 0.30404(8) 0.16264(9) 0.0380(4) Uani 1 1 d . . . . .
H18 H 0.459260 0.314466 0.138016 0.046 Uiso 1 1 calc R U . . .
C19 C 0.6374(2) 0.34479(9) 0.16825(10) 0.0435(5) Uani 1 1 d . . . . .
H19 H 0.633354 0.382654 0.147172 0.052 Uiso 1 1 calc R U . . .
C20 C 0.7468(2) 0.33090(8) 0.20435(9) 0.0402(4) Uani 1 1 d . . . . .
H20 H 0.816069 0.359967 0.208541 0.048 Uiso 1 1 calc R U . . .
C21 C 0.75700(17) 0.27485(8) 0.23475(8) 0.0315(4) Uani 1 1 d . . . . .
C22 C 0.42437(16) 0.20287(8) 0.18586(8) 0.0327(4) Uani 1 1 d . . . . .
H22 H 0.426062 0.178039 0.221763 0.039 Uiso 1 1 calc R U . . .
C23 C 0.4368(2) 0.15709(10) 0.13711(10) 0.0453(5) Uani 1 1 d . . . . .
H23A H 0.519453 0.134992 0.143534 0.068 Uiso 1 1 calc R U . . .
H23B H 0.433019 0.180099 0.101143 0.068 Uiso 1 1 calc R U . . .
H23C H 0.365838 0.126824 0.135405 0.068 Uiso 1 1 calc R U . . .
C24 C 0.29410(18) 0.23608(10) 0.17688(10) 0.0430(4) Uani 1 1 d . . . . .
H24A H 0.287546 0.266382 0.207524 0.064 Uiso 1 1 calc R U . . .
H24B H 0.224450 0.205294 0.177106 0.064 Uiso 1 1 calc R U . . .
H24C H 0.286661 0.257873 0.140234 0.064 Uiso 1 1 calc R U . . .
C25 C 0.87993(17) 0.25806(9) 0.27204(9) 0.0386(4) Uani 1 1 d . . . . .
H25 H 0.858502 0.223707 0.298162 0.046 Uiso 1 1 calc R U . . .
C26 C 0.9822(2) 0.23360(11) 0.23621(11) 0.0515(5) Uani 1 1 d . . . . .
H26A H 0.947720 0.197760 0.213736 0.077 Uiso 1 1 calc R U . . .
H26B H 1.058527 0.220601 0.261153 0.077 Uiso 1 1 calc R U . . .
H26C H 1.006302 0.266665 0.210631 0.077 Uiso 1 1 calc R U . . .
C27 C 0.9350(2) 0.31233(13) 0.30865(12) 0.0598(7) Uani 1 1 d . . . . .
H27A H 0.967682 0.344441 0.284279 0.090 Uiso 1 1 calc R U . . .
H27B H 1.005674 0.297217 0.335767 0.090 Uiso 1 1 calc R U . . .
H27C H 0.866966 0.330207 0.329443 0.090 Uiso 1 1 calc R U . . .
C28 C 0.63198(14) -0.04178(7) 0.23296(7) 0.0232(3) Uani 1 1 d . . . . .
C29 C 0.50485(15) -0.02459(7) 0.21707(7) 0.0273(3) Uani 1 1 d . . . . .
C30 C 0.41208(16) -0.06434(8) 0.19052(8) 0.0332(4) Uani 1 1 d . . . . .
C31 C 0.44482(16) -0.12475(8) 0.17840(8) 0.0319(4) Uani 1 1 d . . . . .
C32 C 0.56868(16) -0.14477(7) 0.19405(7) 0.0292(3) Uani 1 1 d . . . . .
C33 C 0.65772(15) -0.10377(7) 0.22029(7) 0.0254(3) Uani 1 1 d . . . . .
C34 C 0.86207(14) 0.01330(7) 0.21885(7) 0.0244(3) Uani 1 1 d . . . . .
C35 C 0.85397(17) -0.00278(9) 0.16167(8) 0.0325(4) Uani 1 1 d . . . . .
C36 C 0.94635(19) 0.01155(10) 0.12540(8) 0.0383(4) Uani 1 1 d . . . . .
C37 C 1.05463(17) 0.04451(9) 0.14528(8) 0.0340(4) Uani 1 1 d . . . . .
C38 C 1.06859(15) 0.06250(8) 0.20136(8) 0.0295(3) Uani 1 1 d . . . . .
C39 C 0.97391(15) 0.04741(7) 0.23585(7) 0.0258(3) Uani 1 1 d . . . . .
C40 C 0.80327(14) -0.03821(7) 0.32106(7) 0.0228(3) Uani 1 1 d . . . . .
C41 C 0.71497(14) -0.05633(7) 0.35843(7) 0.0237(3) Uani 1 1 d . . . . .
C42 C 0.74221(16) -0.09515(7) 0.40474(7) 0.0275(3) Uani 1 1 d . . . . .
C43 C 0.86496(17) -0.11960(7) 0.41552(7) 0.0296(3) Uani 1 1 d . . . . .
C44 C 0.95645(16) -0.10411(8) 0.38025(7) 0.0296(3) Uani 1 1 d . . . . .
C45 C 0.92493(15) -0.06469(7) 0.33417(7) 0.0256(3) Uani 1 1 d . . . . .
C50 C 0.8097(5) 0.3301(2) 0.49291(17) 0.1053(14) Uani 1 1 d . . . . .
H50A H 0.770646 0.367036 0.472582 0.126 Uiso 0.722(12) 1 calc R U P A 3
H50B H 0.886045 0.316745 0.474270 0.126 Uiso 0.722(12) 1 calc R U P A 3
H50C H 0.770036 0.371956 0.495381 0.126 Uiso 0.278(12) 1 calc R U P A 4
H50D H 0.861459 0.328177 0.460093 0.126 Uiso 0.278(12) 1 calc R U P A 4
B1 B 0.75013(16) 0.00270(8) 0.26364(8) 0.0219(3) Uani 1 1 d . . . . .
C46 C 0.2920(5) 0.34027(19) 0.43563(19) 0.0688(13) Uani 0.693(4) 1 d . . P A 1
H46A H 0.237805 0.333151 0.399286 0.083 Uiso 0.693(4) 1 calc R U P A 1
H46B H 0.352215 0.375163 0.430615 0.083 Uiso 0.693(4) 1 calc R U P A 1
C47 C 0.2099(7) 0.3542(3) 0.4825(3) 0.083(2) Uani 0.693(4) 1 d . . P A 1
H47A H 0.257933 0.379835 0.512418 0.099 Uiso 0.693(4) 1 calc R U P A 1
H47B H 0.130566 0.376832 0.467693 0.099 Uiso 0.693(4) 1 calc R U P A 1
C48 C 0.1784(4) 0.29417(19) 0.50457(18) 0.0631(10) Uani 0.693(4) 1 d . . P A 1
H48A H 0.095257 0.278724 0.485617 0.076 Uiso 0.693(4) 1 calc R U P A 1
H48B H 0.172409 0.296462 0.546036 0.076 Uiso 0.693(4) 1 calc R U P A 1
C49 C 0.2886(4) 0.25208(15) 0.49164(14) 0.0552(10) Uani 0.693(4) 1 d . . P A 1
H49A H 0.343532 0.241779 0.527108 0.066 Uiso 0.693(4) 1 calc R U P A 1
H49B H 0.254519 0.212671 0.474060 0.066 Uiso 0.693(4) 1 calc R U P A 1
C46A C 0.2176(15) 0.2844(8) 0.4301(7) 0.112(5) Uani 0.307(4) 1 d . U P A 2
H46C H 0.210342 0.281759 0.388112 0.134 Uiso 0.307(4) 1 calc R U P A 2
H46D H 0.174429 0.247277 0.444584 0.134 Uiso 0.307(4) 1 calc R U P A 2
C47A C 0.1619(12) 0.3337(7) 0.4450(5) 0.096(4) Uani 0.307(4) 1 d . U P A 2
H47C H 0.089154 0.322639 0.467005 0.115 Uiso 0.307(4) 1 calc R U P A 2
H47D H 0.127043 0.357506 0.410941 0.115 Uiso 0.307(4) 1 calc R U P A 2
C48A C 0.2614(14) 0.3742(8) 0.4820(6) 0.082(4) Uani 0.307(4) 1 d . U P A 2
H48C H 0.252366 0.418919 0.471715 0.098 Uiso 0.307(4) 1 calc R U P A 2
H48D H 0.251130 0.369288 0.522973 0.098 Uiso 0.307(4) 1 calc R U P A 2
C49A C 0.3892(11) 0.3488(5) 0.4683(5) 0.075(3) Uani 0.307(4) 1 d . U P A 2
H49C H 0.420527 0.371515 0.435869 0.090 Uiso 0.307(4) 1 calc R U P A 2
H49D H 0.454964 0.351924 0.501508 0.090 Uiso 0.307(4) 1 calc R U P A 2
C51 C 0.8472(8) 0.3451(4) 0.5552(3) 0.120(3) Uani 0.722(12) 1 d . U P A 3
H51A H 0.937786 0.359568 0.561882 0.144 Uiso 0.722(12) 1 calc R U P A 3
H51B H 0.789466 0.377073 0.569256 0.144 Uiso 0.722(12) 1 calc R U P A 3
C52 C 0.8293(9) 0.2820(4) 0.5826(3) 0.106(3) Uani 0.722(12) 1 d . U P A 3
H52A H 0.908345 0.256316 0.582421 0.127 Uiso 0.722(12) 1 calc R U P A 3
H52B H 0.809323 0.287163 0.622426 0.127 Uiso 0.722(12) 1 calc R U P A 3
C53 C 0.7229(6) 0.2534(3) 0.5487(2) 0.0717(15) Uani 0.722(12) 1 d . U P A 3
H53A H 0.640759 0.261290 0.565190 0.086 Uiso 0.722(12) 1 calc R U P A 3
H53B H 0.735845 0.207685 0.546055 0.086 Uiso 0.722(12) 1 calc R U P A 3
C51A C 0.8987(12) 0.3060(7) 0.5585(6) 0.069(4) Uani 0.278(12) 1 d . U P A 4
H51C H 0.933671 0.263000 0.557795 0.083 Uiso 0.278(12) 1 calc R U P A 4
H51D H 0.965844 0.336045 0.573774 0.083 Uiso 0.278(12) 1 calc R U P A 4
C52A C 0.7695(14) 0.3112(9) 0.5860(5) 0.076(4) Uani 0.278(12) 1 d . U P A 4
H52C H 0.774121 0.290519 0.623585 0.091 Uiso 0.278(12) 1 calc R U P A 4
H52D H 0.741460 0.355144 0.589436 0.091 Uiso 0.278(12) 1 calc R U P A 4
C53A C 0.687(3) 0.2767(14) 0.5421(10) 0.125(8) Uani 0.278(12) 1 d . U P A 4
H53D H 0.687628 0.231837 0.552427 0.150 Uiso 0.278(12) 1 calc R U P A 4
H53C H 0.596864 0.291848 0.541887 0.150 Uiso 0.278(12) 1 calc R U P A 4
O3 O 0.5477(11) 0.4478(5) 0.4619(4) 0.111(3) Uani 0.354(6) 1 d . U P B -1
C57 C 0.519(2) 0.5082(10) 0.4445(8) 0.073(4) Uani 0.354(6) 1 d . U P B -1
H57A H 0.472264 0.508166 0.405796 0.088 Uiso 0.354(6) 1 calc R U P B -1
H57B H 0.598678 0.532989 0.443924 0.088 Uiso 0.354(6) 1 calc R U P B -1
C56 C 0.438(3) 0.5345(12) 0.4843(12) 0.094(6) Uani 0.354(6) 1 d . U P B -1
H56A H 0.346277 0.533006 0.469036 0.112 Uiso 0.354(6) 1 calc R U P B -1
H56B H 0.462661 0.578461 0.492921 0.112 Uiso 0.354(6) 1 calc R U P B -1
C55 C 0.464(2) 0.4919(14) 0.5402(9) 0.085(6) Uani 0.354(6) 1 d . U P B -1
H55A H 0.504263 0.516444 0.572805 0.102 Uiso 0.354(6) 1 calc R U P B -1
H55B H 0.382286 0.473335 0.550659 0.102 Uiso 0.354(6) 1 calc R U P B -1
C54 C 0.552(2) 0.4436(9) 0.5231(7) 0.077(4) Uani 0.354(6) 1 d . U P B -1
H54A H 0.640568 0.451005 0.541043 0.092 Uiso 0.354(6) 1 calc R U P B -1
H54B H 0.523317 0.401706 0.534485 0.092 Uiso 0.354(6) 1 calc R U P B -1
C58 C 0.734(4) 0.4320(18) 0.4476(16) 0.128(10) Uani 0.146(6) 1 d . U P B -2
H58A H 0.788877 0.434938 0.483598 0.192 Uiso 0.146(6) 1 calc R U P B -2
H58B H 0.785218 0.439997 0.415915 0.192 Uiso 0.146(6) 1 calc R U P B -2
H58C H 0.696076 0.390014 0.443688 0.192 Uiso 0.146(6) 1 calc R U P B -2
C59 C 0.625(4) 0.4807(17) 0.4468(16) 0.103(8) Uani 0.146(6) 1 d . U P B -2
H59A H 0.657281 0.521215 0.434007 0.123 Uiso 0.146(6) 1 calc R U P B -2
H59B H 0.552769 0.467574 0.418557 0.123 Uiso 0.146(6) 1 calc R U P B -2
C60 C 0.574(5) 0.490(2) 0.502(2) 0.107(9) Uani 0.146(6) 1 d . U P B -2
H60A H 0.642574 0.500955 0.532039 0.129 Uiso 0.146(6) 1 calc R U P B -2
H60B H 0.525396 0.452995 0.513130 0.129 Uiso 0.146(6) 1 calc R U P B -2
C61 C 0.488(5) 0.544(4) 0.484(3) 0.112(10) Uani 0.146(6) 1 d . U P B -2
H61A H 0.526123 0.584587 0.495931 0.134 Uiso 0.146(6) 1 calc R U P B -2
H61B H 0.457954 0.543799 0.442992 0.134 Uiso 0.146(6) 1 calc R U P B -2
C62 C 0.395(5) 0.524(3) 0.518(2) 0.112(10) Uani 0.146(6) 1 d . U P B -2
H62A H 0.341654 0.559185 0.526626 0.168 Uiso 0.146(6) 1 calc R U P B -2
H62B H 0.437414 0.505745 0.552916 0.168 Uiso 0.146(6) 1 calc R U P B -2
H62C H 0.341136 0.491869 0.497133 0.168 Uiso 0.146(6) 1 calc R U P B -2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
K K 0.3868 1.0657 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 0 1 0.0255
0 0 -1 0.0382
-7 2 0 0.0453
7 -2 0 0.1434
0 -14 -1 0.0462
6 6 -7 0.1255
-5 -6 7 0.0517
-5 6 8 0.0475
0 -1 1 0.0350
0 1 -1 0.0175
0 11 9 0.0102
0 -11 -9 0.0434
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
O2 K1 O1 90.62(7) . . ?
O2 K1 F3 81.86(5) . 2_655 ?
O1 K1 F3 97.40(5) . 2_655 ?
O2 K1 C1 128.22(5) . . ?
O1 K1 C1 139.79(6) . . ?
F3 K1 C1 80.72(4) 2_655 . ?
O2 K1 F4 127.78(5) . 2_655 ?
O1 K1 F4 70.05(5) . 2_655 ?
F3 K1 F4 54.99(3) 2_655 2_655 ?
C1 K1 F4 76.63(4) . 2_655 ?
O2 K1 C4 115.08(5) . . ?
O1 K1 C4 134.04(5) . . ?
F3 K1 C4 122.37(4) 2_655 . ?
C1 K1 C4 44.51(4) . . ?
F4 K1 C4 112.72(4) 2_655 . ?
O2 K1 C9 126.47(6) . . ?
O1 K1 C9 109.35(5) . . ?
F3 K1 C9 139.26(4) 2_655 . ?
C1 K1 C9 58.95(4) . . ?
F4 K1 C9 105.76(4) 2_655 . ?
C4 K1 C9 24.78(4) . . ?
O2 K1 C53A 19.8(4) . . ?
O1 K1 C53A 77.3(5) . . ?
F3 K1 C53A 98.1(4) 2_655 . ?
C1 K1 C53A 142.9(5) . . ?
F4 K1 C53A 132.7(5) 2_655 . ?
C4 K1 C53A 114.6(5) . . ?
C9 K1 C53A 117.1(5) . . ?
O2 K1 C49A 74.4(2) . . ?
O1 K1 C49A 23.05(19) . . ?
F3 K1 C49A 79.05(19) 2_655 . ?
C1 K1 C49A 146.7(2) . . ?
F4 K1 C49A 70.11(19) 2_655 . ?
C4 K1 C49A 156.62(19) . . ?
C9 K1 C49A 132.23(19) . . ?
O2 K1 C15 155.72(6) . . ?
O1 K1 C15 76.80(6) . . ?
F3 K1 C15 119.92(4) 2_655 . ?
C1 K1 C15 70.00(5) . . ?
F4 K1 C15 67.54(4) 2_655 . ?
C4 K1 C15 64.29(4) . . ?
C9 K1 C15 43.76(4) . . ?
C53A K1 C15 136.1(4) . . ?
C49A K1 C15 98.02(19) . . ?
O2 K1 C53 21.87(11) . . ?
O1 K1 C53 85.37(12) . . ?
F3 K1 C53 103.58(11) 2_655 . ?
C1 K1 C53 134.40(11) . . ?
F4 K1 C53 142.83(11) 2_655 . ?
C4 K1 C53 104.43(11) . . ?
C9 K1 C53 108.57(11) . . ?
C15 K1 C53 134.44(11) . . ?
C31 F3 K1 122.07(10) . 2_645 ?
C32 F4 K1 117.17(9) . 2_645 ?
C49 O1 C46 108.0(3) . . ?
C49A O1 C46A 104.5(8) . . ?
C49 O1 K1 121.27(17) . . ?
C46 O1 K1 129.5(2) . . ?
C49A O1 K1 110.5(5) . . ?
C46A O1 K1 129.7(6) . . ?
C53A O2 C50 109.1(12) . . ?
C50 O2 C53 111.9(3) . . ?
C53A O2 K1 114.8(12) . . ?
C50 O2 K1 132.3(2) . . ?
C53 O2 K1 115.6(3) . . ?
C1 N1 C2 113.69(13) . . ?
C1 N1 C4 113.38(12) . . ?
C2 N1 C4 132.74(12) . . ?
C1 N2 C3 111.90(12) . . ?
C1 N2 C16 123.24(13) . . ?
C3 N2 C16 124.77(13) . . ?
N2 C1 N1 102.61(13) . . ?
N2 C1 K1 145.92(10) . . ?
N1 C1 K1 110.67(10) . . ?
C3 C2 N1 102.36(12) . . ?
C3 C2 B1 121.59(14) . . ?
N1 C2 B1 136.02(13) . . ?
C2 C3 N2 109.42(14) . . ?
C5 C4 C9 121.86(15) . . ?
C5 C4 N1 118.95(14) . . ?
C9 C4 N1 118.45(13) . . ?
C5 C4 K1 91.76(9) . . ?
C9 C4 K1 78.44(9) . . ?
N1 C4 K1 91.29(8) . . ?
C6 C5 C4 117.92(15) . . ?
C6 C5 C10 120.40(15) . . ?
C4 C5 C10 121.49(15) . . ?
C7 C6 C5 121.19(16) . . ?
C6 C7 C8 120.01(17) . . ?
C7 C8 C9 121.37(17) . . ?
C8 C9 C4 117.64(15) . . ?
C8 C9 C13 119.32(15) . . ?
C4 C9 C13 123.04(15) . . ?
C8 C9 K1 91.33(10) . . ?
C4 C9 K1 76.78(8) . . ?
C13 C9 K1 101.24(9) . . ?
C5 C10 C11 112.68(15) . . ?
C5 C10 C12 109.69(14) . . ?
C11 C10 C12 110.43(14) . . ?
C9 C13 C14 111.37(14) . . ?
C9 C13 C15 111.96(14) . . ?
C14 C13 C15 109.76(14) . . ?
C21 C16 C17 122.95(15) . . ?
C21 C16 N2 118.57(14) . . ?
C17 C16 N2 118.48(14) . . ?
C18 C17 C16 117.40(16) . . ?
C18 C17 C22 120.95(15) . . ?
C16 C17 C22 121.63(14) . . ?
C19 C18 C17 121.03(17) . . ?
C18 C19 C20 120.48(17) . . ?
C19 C20 C21 121.10(17) . . ?
C20 C21 C16 117.00(16) . . ?
C20 C21 C25 121.09(16) . . ?
C16 C21 C25 121.86(15) . . ?
C17 C22 C24 112.85(15) . . ?
C17 C22 C23 111.08(16) . . ?
C24 C22 C23 109.64(16) . . ?
C26 C25 C21 110.74(17) . . ?
C26 C25 C27 109.57(17) . . ?
C21 C25 C27 113.22(18) . . ?
C29 C28 C33 113.18(14) . . ?
C29 C28 B1 127.50(13) . . ?
C33 C28 B1 119.32(13) . . ?
F1 C29 C28 121.07(14) . . ?
F1 C29 C30 114.87(14) . . ?
C28 C29 C30 124.05(15) . . ?
F2 C30 C31 119.58(15) . . ?
F2 C30 C29 120.75(15) . . ?
C31 C30 C29 119.66(15) . . ?
F3 C31 C32 120.15(15) . . ?
F3 C31 C30 120.91(15) . . ?
C32 C31 C30 118.91(15) . . ?
F4 C32 C31 119.11(14) . . ?
F4 C32 C33 121.32(15) . . ?
C31 C32 C33 119.52(15) . . ?
F5 C33 C32 115.70(14) . . ?
F5 C33 C28 119.55(13) . . ?
C32 C33 C28 124.67(14) . . ?
C35 C34 C39 112.03(15) . . ?
C35 C34 B1 127.39(14) . . ?
C39 C34 B1 120.25(14) . . ?
F6 C35 C36 113.84(16) . . ?
F6 C35 C34 121.39(15) . . ?
C36 C35 C34 124.76(16) . . ?
F7 C36 C37 119.64(17) . . ?
F7 C36 C35 120.37(17) . . ?
C37 C36 C35 119.97(17) . . ?
F8 C37 C36 120.71(17) . . ?
F8 C37 C38 120.81(16) . . ?
C36 C37 C38 118.48(16) . . ?
F9 C38 C37 119.69(15) . . ?
F9 C38 C39 120.75(16) . . ?
C37 C38 C39 119.56(15) . . ?
F10 C39 C38 115.50(14) . . ?
F10 C39 C34 119.32(14) . . ?
C38 C39 C34 125.19(16) . . ?
C45 C40 C41 112.91(14) . . ?
C45 C40 B1 127.96(14) . . ?
C41 C40 B1 118.59(13) . . ?
F11 C41 C42 115.34(14) . . ?
F11 C41 C40 119.48(13) . . ?
C42 C41 C40 125.10(14) . . ?
F12 C42 C43 119.79(15) . . ?
F12 C42 C41 121.14(15) . . ?
C43 C42 C41 119.06(15) . . ?
F13 C43 C44 120.65(15) . . ?
F13 C43 C42 120.38(16) . . ?
C44 C43 C42 118.97(15) . . ?
F14 C44 C43 119.48(15) . . ?
F14 C44 C45 120.44(16) . . ?
C43 C44 C45 120.07(15) . . ?
F15 C45 C44 114.54(14) . . ?
F15 C45 C40 121.54(14) . . ?
C44 C45 C40 123.88(15) . . ?
O2 C50 C51 105.0(4) . . ?
O2 C50 C51A 93.9(5) . . ?
C2 B1 C28 113.60(12) . . ?
C2 B1 C40 115.05(13) . . ?
C28 B1 C40 102.96(12) . . ?
C2 B1 C34 102.69(12) . . ?
C28 B1 C34 109.55(12) . . ?
C40 B1 C34 113.23(12) . . ?
O1 C46 C47 104.6(4) . . ?
C48 C47 C46 105.1(4) . . ?
C47 C48 C49 104.7(4) . . ?
O1 C49 C48 107.6(3) . . ?
C47A C46A O1 110.6(12) . . ?
C46A C47A C48A 108.9(12) . . ?
C49A C48A C47A 103.3(10) . . ?
O1 C49A C48A 103.7(9) . . ?
C52 C51 C50 101.3(5) . . ?
C53 C52 C51 105.2(5) . . ?
C52 C53 O2 105.2(5) . . ?
C52A C51A C50 87.0(9) . . ?
C53A C52A C51A 97.9(13) . . ?
O2 C53A C52A 113.6(19) . . ?
C57 O3 C54 109.8(13) . . ?
O3 C57 C56 107.2(18) . . ?
C57 C56 C55 105(2) . . ?
C54 C55 C56 103.1(18) . . ?
O3 C54 C55 106.2(14) . . ?
C60 C59 C58 114(4) . . ?
C59 C60 C61 97(5) . . ?
C62 C61 C60 92(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O2 2.6268(17) . ?
K1 O1 2.6658(18) . ?
K1 F3 2.8540(12) 2_655 ?
K1 C1 2.8799(16) . ?
K1 F4 3.0014(11) 2_655 ?
K1 C4 3.2686(15) . ?
K1 C9 3.2895(15) . ?
K1 C53A 3.35(3) . ?
K1 C49A 3.445(11) . ?
K1 C15 3.4904(19) . ?
K1 C53 3.506(5) . ?
F1 C29 1.3508(18) . ?
F2 C30 1.3440(19) . ?
F3 C31 1.3479(18) . ?
F4 C32 1.3495(18) . ?
F5 C33 1.3529(17) . ?
F6 C35 1.3560(19) . ?
F7 C36 1.343(2) . ?
F8 C37 1.342(2) . ?
F9 C38 1.3431(19) . ?
F10 C39 1.3491(19) . ?
F11 C41 1.3500(17) . ?
F12 C42 1.341(2) . ?
F13 C43 1.3451(19) . ?
F14 C44 1.3453(19) . ?
F15 C45 1.3445(19) . ?
O1 C49 1.414(4) . ?
O1 C46 1.439(4) . ?
O1 C49A 1.440(10) . ?
O1 C46A 1.545(16) . ?
O2 C53A 1.25(2) . ?
O2 C50 1.379(4) . ?
O2 C53 1.449(6) . ?
N1 C1 1.3751(18) . ?
N1 C2 1.423(2) . ?
N1 C4 1.444(2) . ?
N2 C1 1.351(2) . ?
N2 C3 1.3866(19) . ?
N2 C16 1.4388(19) . ?
C2 C3 1.360(2) . ?
C2 B1 1.648(2) . ?
C4 C5 1.404(2) . ?
C4 C9 1.407(2) . ?
C5 C6 1.395(2) . ?
C5 C10 1.517(2) . ?
C6 C7 1.382(3) . ?
C7 C8 1.383(3) . ?
C8 C9 1.396(2) . ?
C9 C13 1.525(2) . ?
C10 C11 1.530(2) . ?
C10 C12 1.534(3) . ?
C13 C14 1.528(2) . ?
C13 C15 1.532(2) . ?
C16 C21 1.401(2) . ?
C16 C17 1.402(2) . ?
C17 C18 1.391(2) . ?
C17 C22 1.521(2) . ?
C18 C19 1.380(3) . ?
C19 C20 1.383(3) . ?
C20 C21 1.397(2) . ?
C21 C25 1.521(3) . ?
C22 C24 1.526(2) . ?
C22 C23 1.528(3) . ?
C25 C26 1.520(3) . ?
C25 C27 1.525(3) . ?
C28 C29 1.388(2) . ?
C28 C33 1.392(2) . ?
C28 B1 1.662(2) . ?
C29 C30 1.388(2) . ?
C30 C31 1.375(2) . ?
C31 C32 1.373(2) . ?
C32 C33 1.377(2) . ?
C34 C35 1.389(2) . ?
C34 C39 1.398(2) . ?
C34 B1 1.668(2) . ?
C35 C36 1.387(3) . ?
C36 C37 1.371(3) . ?
C37 C38 1.374(3) . ?
C38 C39 1.380(2) . ?
C40 C45 1.393(2) . ?
C40 C41 1.394(2) . ?
C40 B1 1.662(2) . ?
C41 C42 1.381(2) . ?
C42 C43 1.380(2) . ?
C43 C44 1.369(3) . ?
C44 C45 1.390(2) . ?
C50 C51 1.519(7) . ?
C50 C51A 1.800(13) . ?
C46 C47 1.497(7) . ?
C47 C48 1.436(7) . ?
C48 C49 1.514(5) . ?
C46A C47A 1.272(18) . ?
C47A C48A 1.550(18) . ?
C48A C49A 1.504(17) . ?
C51 C52 1.518(12) . ?
C52 C53 1.437(9) . ?
C51A C52A 1.56(2) . ?
C52A C53A 1.48(3) . ?
O3 C57 1.38(2) . ?
O3 C54 1.44(2) . ?
C57 C56 1.44(3) . ?
C56 C55 1.60(4) . ?
C55 C54 1.47(4) . ?
C58 C59 1.54(5) . ?
C59 C60 1.46(7) . ?
C60 C61 1.49(8) . ?
C61 C62 1.38(8) . ?
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
C3 N2 C1 N1 -1.34(16) . . . . ?
C16 N2 C1 N1 -177.99(13) . . . . ?
C3 N2 C1 K1 166.15(14) . . . . ?
C16 N2 C1 K1 -10.5(3) . . . . ?
C2 N1 C1 N2 1.09(16) . . . . ?
C4 N1 C1 N2 176.78(12) . . . . ?
C2 N1 C1 K1 -171.46(9) . . . . ?
C4 N1 C1 K1 4.24(14) . . . . ?
C1 N1 C2 C3 -0.42(16) . . . . ?
C4 N1 C2 C3 -175.05(14) . . . . ?
C1 N1 C2 B1 -178.39(15) . . . . ?
C4 N1 C2 B1 7.0(3) . . . . ?
N1 C2 C3 N2 -0.43(16) . . . . ?
B1 C2 C3 N2 177.92(12) . . . . ?
C1 N2 C3 C2 1.18(17) . . . . ?
C16 N2 C3 C2 177.77(13) . . . . ?
C1 N1 C4 C5 -96.22(16) . . . . ?
C2 N1 C4 C5 78.4(2) . . . . ?
C1 N1 C4 C9 74.05(17) . . . . ?
C2 N1 C4 C9 -111.32(18) . . . . ?
C1 N1 C4 K1 -3.49(11) . . . . ?
C2 N1 C4 K1 171.14(14) . . . . ?
C9 C4 C5 C6 0.5(2) . . . . ?
N1 C4 C5 C6 170.43(14) . . . . ?
K1 C4 C5 C6 77.99(14) . . . . ?
C9 C4 C5 C10 -174.55(14) . . . . ?
N1 C4 C5 C10 -4.6(2) . . . . ?
K1 C4 C5 C10 -97.08(14) . . . . ?
C4 C5 C6 C7 -1.2(3) . . . . ?
C10 C5 C6 C7 173.89(17) . . . . ?
C5 C6 C7 C8 1.1(3) . . . . ?
C6 C7 C8 C9 -0.2(3) . . . . ?
C7 C8 C9 C4 -0.5(2) . . . . ?
C7 C8 C9 C13 -179.96(16) . . . . ?
C7 C8 C9 K1 -76.28(17) . . . . ?
C5 C4 C9 C8 0.3(2) . . . . ?
N1 C4 C9 C8 -169.62(14) . . . . ?
K1 C4 C9 C8 -84.48(14) . . . . ?
C5 C4 C9 C13 179.76(14) . . . . ?
N1 C4 C9 C13 9.8(2) . . . . ?
K1 C4 C9 C13 94.94(14) . . . . ?
C5 C4 C9 K1 84.83(14) . . . . ?
N1 C4 C9 K1 -85.14(12) . . . . ?
C6 C5 C10 C11 43.9(2) . . . . ?
C4 C5 C10 C11 -141.14(15) . . . . ?
C6 C5 C10 C12 -79.54(19) . . . . ?
C4 C5 C10 C12 95.40(18) . . . . ?
C8 C9 C13 C14 -57.7(2) . . . . ?
C4 C9 C13 C14 122.92(17) . . . . ?
K1 C9 C13 C14 -155.64(13) . . . . ?
C8 C9 C13 C15 65.6(2) . . . . ?
C4 C9 C13 C15 -113.76(18) . . . . ?
K1 C9 C13 C15 -32.32(15) . . . . ?
C1 N2 C16 C21 86.51(19) . . . . ?
C3 N2 C16 C21 -89.7(2) . . . . ?
C1 N2 C16 C17 -93.50(19) . . . . ?
C3 N2 C16 C17 90.28(19) . . . . ?
C21 C16 C17 C18 2.1(3) . . . . ?
N2 C16 C17 C18 -177.92(16) . . . . ?
C21 C16 C17 C22 -179.59(16) . . . . ?
N2 C16 C17 C22 0.4(2) . . . . ?
C16 C17 C18 C19 -1.1(3) . . . . ?
C22 C17 C18 C19 -179.47(18) . . . . ?
C17 C18 C19 C20 -0.7(3) . . . . ?
C18 C19 C20 C21 1.7(3) . . . . ?
C19 C20 C21 C16 -0.8(3) . . . . ?
C19 C20 C21 C25 176.78(19) . . . . ?
C17 C16 C21 C20 -1.1(3) . . . . ?
N2 C16 C21 C20 178.88(16) . . . . ?
C17 C16 C21 C25 -178.69(17) . . . . ?
N2 C16 C21 C25 1.3(3) . . . . ?
C18 C17 C22 C24 -34.6(2) . . . . ?
C16 C17 C22 C24 147.11(17) . . . . ?
C18 C17 C22 C23 89.0(2) . . . . ?
C16 C17 C22 C23 -89.3(2) . . . . ?
C20 C21 C25 C26 -79.0(2) . . . . ?
C16 C21 C25 C26 98.5(2) . . . . ?
C20 C21 C25 C27 44.5(3) . . . . ?
C16 C21 C25 C27 -138.0(2) . . . . ?
C33 C28 C29 F1 -179.85(15) . . . . ?
B1 C28 C29 F1 -0.3(3) . . . . ?
C33 C28 C29 C30 -0.8(3) . . . . ?
B1 C28 C29 C30 178.69(17) . . . . ?
F1 C29 C30 F2 0.0(3) . . . . ?
C28 C29 C30 F2 -179.10(17) . . . . ?
F1 C29 C30 C31 178.88(17) . . . . ?
C28 C29 C30 C31 -0.2(3) . . . . ?
K1 F3 C31 C32 -21.2(2) 2_645 . . . ?
K1 F3 C31 C30 156.58(14) 2_645 . . . ?
F2 C30 C31 F3 2.4(3) . . . . ?
C29 C30 C31 F3 -176.51(17) . . . . ?
F2 C30 C31 C32 -179.75(17) . . . . ?
C29 C30 C31 C32 1.3(3) . . . . ?
K1 F4 C32 C31 20.5(2) 2_645 . . . ?
K1 F4 C32 C33 -156.87(13) 2_645 . . . ?
F3 C31 C32 F4 -0.9(3) . . . . ?
C30 C31 C32 F4 -178.80(17) . . . . ?
F3 C31 C32 C33 176.48(16) . . . . ?
C30 C31 C32 C33 -1.4(3) . . . . ?
F4 C32 C33 F5 1.1(2) . . . . ?
C31 C32 C33 F5 -176.22(16) . . . . ?
F4 C32 C33 C28 177.66(16) . . . . ?
C31 C32 C33 C28 0.3(3) . . . . ?
C29 C28 C33 F5 177.17(14) . . . . ?
B1 C28 C33 F5 -2.4(2) . . . . ?
C29 C28 C33 C32 0.8(2) . . . . ?
B1 C28 C33 C32 -178.78(16) . . . . ?
C39 C34 C35 F6 -176.95(16) . . . . ?
B1 C34 C35 F6 -3.7(3) . . . . ?
C39 C34 C35 C36 1.5(3) . . . . ?
B1 C34 C35 C36 174.75(17) . . . . ?
F6 C35 C36 F7 -0.7(3) . . . . ?
C34 C35 C36 F7 -179.21(18) . . . . ?
F6 C35 C36 C37 177.78(18) . . . . ?
C34 C35 C36 C37 -0.7(3) . . . . ?
F7 C36 C37 F8 -0.5(3) . . . . ?
C35 C36 C37 F8 -178.99(18) . . . . ?
F7 C36 C37 C38 178.58(18) . . . . ?
C35 C36 C37 C38 0.1(3) . . . . ?
F8 C37 C38 F9 -0.8(3) . . . . ?
C36 C37 C38 F9 -179.87(16) . . . . ?
F8 C37 C38 C39 178.74(15) . . . . ?
C36 C37 C38 C39 -0.3(3) . . . . ?
F9 C38 C39 F10 0.8(2) . . . . ?
C37 C38 C39 F10 -178.68(15) . . . . ?
F9 C38 C39 C34 -179.21(15) . . . . ?
C37 C38 C39 C34 1.3(3) . . . . ?
C35 C34 C39 F10 178.22(14) . . . . ?
B1 C34 C39 F10 4.4(2) . . . . ?
C35 C34 C39 C38 -1.7(2) . . . . ?
B1 C34 C39 C38 -175.57(14) . . . . ?
C45 C40 C41 F11 -175.39(13) . . . . ?
B1 C40 C41 F11 -3.2(2) . . . . ?
C45 C40 C41 C42 1.4(2) . . . . ?
B1 C40 C41 C42 173.62(14) . . . . ?
F11 C41 C42 F12 -2.9(2) . . . . ?
C40 C41 C42 F12 -179.76(14) . . . . ?
F11 C41 C42 C43 175.72(13) . . . . ?
C40 C41 C42 C43 -1.2(2) . . . . ?
F12 C42 C43 F13 0.0(2) . . . . ?
C41 C42 C43 F13 -178.63(14) . . . . ?
F12 C42 C43 C44 179.23(14) . . . . ?
C41 C42 C43 C44 0.6(2) . . . . ?
F13 C43 C44 F14 -1.6(2) . . . . ?
C42 C43 C44 F14 179.12(14) . . . . ?
F13 C43 C44 C45 178.80(14) . . . . ?
C42 C43 C44 C45 -0.5(2) . . . . ?
F14 C44 C45 F15 3.5(2) . . . . ?
C43 C44 C45 F15 -176.90(14) . . . . ?
F14 C44 C45 C40 -178.78(14) . . . . ?
C43 C44 C45 C40 0.8(3) . . . . ?
C41 C40 C45 F15 176.35(13) . . . . ?
B1 C40 C45 F15 5.0(2) . . . . ?
C41 C40 C45 C44 -1.2(2) . . . . ?
B1 C40 C45 C44 -172.51(15) . . . . ?
C53 O2 C50 C51 -15.5(6) . . . . ?
K1 O2 C50 C51 168.4(4) . . . . ?
C53A O2 C50 C51A 44.1(18) . . . . ?
K1 O2 C50 C51A -159.5(5) . . . . ?
C3 C2 B1 C28 -87.25(17) . . . . ?
N1 C2 B1 C28 90.4(2) . . . . ?
C3 C2 B1 C40 154.44(14) . . . . ?
N1 C2 B1 C40 -27.9(2) . . . . ?
C3 C2 B1 C34 30.96(17) . . . . ?
N1 C2 B1 C34 -151.37(15) . . . . ?
C29 C28 B1 C2 0.8(2) . . . . ?
C33 C28 B1 C2 -179.75(14) . . . . ?
C29 C28 B1 C40 125.85(17) . . . . ?
C33 C28 B1 C40 -54.67(18) . . . . ?
C29 C28 B1 C34 -113.41(17) . . . . ?
C33 C28 B1 C34 66.08(18) . . . . ?
C45 C40 B1 C2 -119.50(16) . . . . ?
C41 C40 B1 C2 69.60(17) . . . . ?
C45 C40 B1 C28 116.38(16) . . . . ?
C41 C40 B1 C28 -54.52(17) . . . . ?
C45 C40 B1 C34 -1.8(2) . . . . ?
C41 C40 B1 C34 -172.72(13) . . . . ?
C35 C34 B1 C2 -111.46(17) . . . . ?
C39 C34 B1 C2 61.35(17) . . . . ?
C35 C34 B1 C28 9.6(2) . . . . ?
C39 C34 B1 C28 -177.63(13) . . . . ?
C35 C34 B1 C40 123.86(17) . . . . ?
C39 C34 B1 C40 -63.33(18) . . . . ?
C49 O1 C46 C47 25.0(5) . . . . ?
K1 O1 C46 C47 -167.6(3) . . . . ?
O1 C46 C47 C48 -32.4(6) . . . . ?
C46 C47 C48 C49 26.6(6) . . . . ?
C46 O1 C49 C48 -8.7(4) . . . . ?
K1 O1 C49 C48 -177.3(2) . . . . ?
C47 C48 C49 O1 -11.8(5) . . . . ?
C49A O1 C46A C47A -18.0(15) . . . . ?
K1 O1 C46A C47A -151.2(10) . . . . ?
O1 C46A C47A C48A -0.8(18) . . . . ?
C46A C47A C48A C49A 18.5(18) . . . . ?
C46A O1 C49A C48A 28.3(11) . . . . ?
K1 O1 C49A C48A 171.5(7) . . . . ?
C47A C48A C49A O1 -28.8(13) . . . . ?
O2 C50 C51 C52 29.4(8) . . . . ?
C50 C51 C52 C53 -33.4(10) . . . . ?
C51 C52 C53 O2 25.0(9) . . . . ?
C50 O2 C53 C52 -6.1(6) . . . . ?
K1 O2 C53 C52 170.8(4) . . . . ?
O2 C50 C51A C52A -56.4(10) . . . . ?
C50 C51A C52A C53A 47.6(14) . . . . ?
C50 O2 C53A C52A -13(3) . . . . ?
K1 O2 C53A C52A -174.0(14) . . . . ?
C51A C52A C53A O2 -31(2) . . . . ?
C54 O3 C57 C56 -31(2) . . . . ?
O3 C57 C56 C55 20(3) . . . . ?
C57 C56 C55 C54 -3(3) . . . . ?
C57 O3 C54 C55 28(2) . . . . ?
C56 C55 C54 O3 -14(3) . . . . ?
C58 C59 C60 C61 173(4) . . . . ?
C59 C60 C61 C62 144(4) . . . . ?
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
-0.0000 0.0000 1.0000 -0.0132 -0.0560 0.0313
0.0000 -0.0000 -1.0000 0.0132 0.0560 -0.0313
-6.6539 2.1057 0.2172 0.1284 0.5375 0.8334
6.6633 -2.1078 -0.4899 -0.1249 -0.5230 -0.8431
-0.0984 -13.8471 -1.1553 -0.9607 0.2300 -0.1551
5.5433 5.5997 -7.4783 0.5075 -0.1222 -0.8529
-5.3758 -6.4744 7.1544 -0.5644 0.1358 0.8142
-5.3277 5.7260 8.2281 0.2812 -0.0666 0.9573
-0.0000 -1.0000 1.0000 -0.0837 -0.0447 0.0218
0.0000 1.0000 -1.0000 0.0837 0.0447 -0.0218
0.0635 11.2093 8.9985 0.6713 -0.6366 0.3796
0.0919 -11.1421 -9.1342 -0.6644 0.6300 -0.4021
