#------------------------------------------------------------------------------
#$Date: 2025-11-29 18:40:28 +0100 (Sat 29 de Nov de 2025) $
#$Revision: 303529 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/49/7134939.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_7134939
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 N2 O2 Rb, 0.5(C5 H12)'
_chemical_formula_sum            'C55.5 H57 B F15 N2 O2 Rb'
_chemical_formula_weight         1165.31
_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                 95.879(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4449(3)
_cell_length_b                   21.3951(6)
_cell_length_c                   23.6633(10)
_cell_measurement_reflns_used    16090
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      71.5520
_cell_measurement_theta_min      2.7750
_cell_volume                     5260.2(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 43.104a 64-bit (release 22-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.112a (Rigaku OD, 2024)'
_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 1.000
_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  0.1556
_diffrn_reflns_av_unetI/netI     0.0689
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            90293
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.602
_diffrn_reflns_theta_max         66.602
_diffrn_reflns_theta_min         2.791
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.151
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.112a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       'fragment of needle'
_exptl_crystal_F_000             2388
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.835
_refine_diff_density_min         -1.597
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     908
_refine_ls_number_reflns         9302
_refine_ls_number_restraints     641
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0831
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1333P)²+10.5172P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2228
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6290
_reflns_number_total             9302
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5cc04534g2.cif
_cod_data_source_block           lgr11db
_cod_depositor_comments
'Adding full bibliography for 7134934--7134942.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C55.50 H57 B F15 N2 O2 Rb'
_cod_database_code               7134939
_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   0.830
_shelx_estimated_absorpt_t_max   0.958
_oxdiff_exptl_absorpt_empirical_full_min 0.581
_oxdiff_exptl_absorpt_empirical_full_max 2.178
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
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
F1 F 0.4101(2) 0.46116(12) 0.65168(13) 0.0392(6) Uani 1 1 d . . . . .
F2 F 0.3520(3) 0.38905(15) 0.56145(13) 0.0501(8) Uani 1 1 d . . . . .
F3 F 0.1119(4) 0.34079(15) 0.53892(15) 0.0595(9) Uani 1 1 d . . . . .
F4 F -0.0730(3) 0.37148(16) 0.60700(15) 0.0579(9) Uani 1 1 d . . . . .
F5 F -0.0195(3) 0.44266(14) 0.69753(14) 0.0474(7) Uani 1 1 d . . . . .
F6 F 0.2199(3) 0.37223(13) 0.76903(14) 0.0469(7) Uani 1 1 d . . . . .
F7 F 0.3972(3) 0.29417(15) 0.81742(18) 0.0652(10) Uani 1 1 d . . . . .
F8 F 0.6412(3) 0.33353(17) 0.84671(19) 0.0745(11) Uani 1 1 d . . . . .
F9 F 0.7091(3) 0.45211(17) 0.8199(2) 0.0722(11) Uani 1 1 d . . . . .
F10 F 0.5364(3) 0.53157(13) 0.77217(15) 0.0515(8) Uani 1 1 d . . . . .
F11 F 0.2484(4) 0.4641(2) 0.86277(16) 0.0780(13) Uani 1 1 d . . . . .
F12 F 0.0660(5) 0.4897(3) 0.92734(18) 0.1010(18) Uani 1 1 d . . . . .
F13 F -0.1482(3) 0.5541(2) 0.88729(17) 0.0726(11) Uani 1 1 d . . . . .
F14 F -0.1753(3) 0.59117(16) 0.77656(16) 0.0582(9) Uani 1 1 d . . . . .
F15 F 0.0057(2) 0.56634(14) 0.70935(14) 0.0456(7) Uani 1 1 d . . . . .
N1 N 0.3437(3) 0.60519(17) 0.67805(17) 0.0309(8) Uani 1 1 d . . . . .
N2 N 0.3413(4) 0.67356(18) 0.74320(19) 0.0372(9) Uani 1 1 d . . . . .
C1 C 0.3707(4) 0.6670(2) 0.6892(2) 0.0388(12) Uani 1 1 d . . . . .
C2 C 0.2950(4) 0.5731(2) 0.7241(2) 0.0329(10) Uani 1 1 d . . . . .
C3 C 0.2941(4) 0.6185(2) 0.7636(2) 0.0375(11) Uani 1 1 d . . . . .
H3 H 0.265249 0.613351 0.800091 0.045 Uiso 1 1 calc R U . . .
C4 C 0.3622(4) 0.5866(2) 0.6207(2) 0.0342(10) Uani 1 1 d . . . . .
C5 C 0.4895(4) 0.5798(2) 0.6060(2) 0.0396(12) Uani 1 1 d . . . . .
C6 C 0.5056(6) 0.5714(3) 0.5493(3) 0.0506(14) Uani 1 1 d . . . . .
H6 H 0.590003 0.565963 0.538503 0.061 Uiso 1 1 calc R U . . .
C7 C 0.4027(6) 0.5707(3) 0.5078(3) 0.0540(14) Uani 1 1 d . . . . .
H7 H 0.416982 0.565573 0.469099 0.065 Uiso 1 1 calc R U . . .
C8 C 0.2784(6) 0.5774(3) 0.5227(3) 0.0486(13) Uani 1 1 d . . . . .
H8 H 0.207717 0.576530 0.494073 0.058 Uiso 1 1 calc R U . . .
C9 C 0.2565(5) 0.5854(2) 0.5794(2) 0.0382(11) Uani 1 1 d . . . . .
C10 C 0.6063(5) 0.5811(2) 0.6502(3) 0.0438(12) Uani 1 1 d . . . . .
H10 H 0.575110 0.582791 0.688714 0.053 Uiso 1 1 calc R U . . .
C11 C 0.6889(5) 0.5217(3) 0.6468(3) 0.0568(16) Uani 1 1 d . . . . .
H11A H 0.635946 0.484718 0.651981 0.085 Uiso 1 1 calc R U . . .
H11B H 0.761063 0.522924 0.676677 0.085 Uiso 1 1 calc R U . . .
H11C H 0.722009 0.519706 0.609557 0.085 Uiso 1 1 calc R U . . .
C12 C 0.6891(5) 0.6390(3) 0.6430(3) 0.0559(15) Uani 1 1 d . . . . .
H12A H 0.716063 0.639624 0.604515 0.084 Uiso 1 1 calc R U . . .
H12B H 0.765265 0.637851 0.670806 0.084 Uiso 1 1 calc R U . . .
H12C H 0.638879 0.676718 0.648988 0.084 Uiso 1 1 calc R U . . .
C13 C 0.1215(4) 0.5981(3) 0.5944(2) 0.0438(12) Uani 1 1 d . . . . .
H13 H 0.119913 0.589277 0.635868 0.053 Uiso 1 1 calc R U . . .
C14 C 0.0882(5) 0.6674(3) 0.5845(3) 0.0600(17) Uani 1 1 d . . . . .
H14A H 0.090402 0.677413 0.544158 0.090 Uiso 1 1 calc R U . . .
H14B H 0.151098 0.693324 0.607371 0.090 Uiso 1 1 calc R U . . .
H14C H 0.001884 0.675666 0.595479 0.090 Uiso 1 1 calc R U . . .
C15 C 0.0198(5) 0.5568(3) 0.5619(3) 0.0512(14) Uani 1 1 d . . . . .
H15A H -0.063783 0.564003 0.576147 0.077 Uiso 1 1 calc R U . . .
H15B H 0.043995 0.512803 0.567189 0.077 Uiso 1 1 calc R U . . .
H15C H 0.013929 0.567216 0.521343 0.077 Uiso 1 1 calc R U . . .
C16 C 0.3499(5) 0.7317(2) 0.7733(2) 0.0406(12) Uani 1 1 d . . . . .
C17 C 0.4638(5) 0.7452(2) 0.8082(3) 0.0443(12) Uani 1 1 d . . . . .
C18 C 0.4675(6) 0.8006(3) 0.8384(3) 0.0543(15) Uani 1 1 d . . . . .
H18 H 0.541972 0.810425 0.863314 0.065 Uiso 1 1 calc R U . . .
C19 C 0.3664(6) 0.8415(3) 0.8334(3) 0.0615(17) Uani 1 1 d . . . . .
H19 H 0.372070 0.879239 0.854600 0.074 Uiso 1 1 calc R U . . .
C20 C 0.2571(6) 0.8288(3) 0.7983(3) 0.0577(16) Uani 1 1 d . . . . .
H20 H 0.188476 0.858162 0.794821 0.069 Uiso 1 1 calc R U . . .
C21 C 0.2455(5) 0.7727(2) 0.7673(3) 0.0484(14) Uani 1 1 d . . . . .
C22 C 0.5762(5) 0.6997(3) 0.8139(3) 0.0477(13) Uani 1 1 d . . . . .
H22 H 0.572757 0.674790 0.777969 0.057 Uiso 1 1 calc R U . . .
C23 C 0.5656(6) 0.6544(3) 0.8625(3) 0.0672(18) Uani 1 1 d . . . . .
H23A H 0.568266 0.677725 0.898282 0.101 Uiso 1 1 calc R U . . .
H23B H 0.637513 0.624839 0.864497 0.101 Uiso 1 1 calc R U . . .
H23C H 0.484136 0.631539 0.856198 0.101 Uiso 1 1 calc R U . . .
C24 C 0.7064(6) 0.7327(3) 0.8218(3) 0.0654(18) Uani 1 1 d . . . . .
H24A H 0.713902 0.761197 0.789888 0.098 Uiso 1 1 calc R U . . .
H24B H 0.775503 0.701558 0.823243 0.098 Uiso 1 1 calc R U . . .
H24C H 0.713425 0.756497 0.857361 0.098 Uiso 1 1 calc R U . . .
C25 C 0.1228(5) 0.7569(3) 0.7297(3) 0.0625(18) Uani 1 1 d . . . . .
H25 H 0.143735 0.723322 0.702678 0.075 Uiso 1 1 calc R U . . .
C26 C 0.0204(7) 0.7317(4) 0.7647(4) 0.086(3) Uani 1 1 d . . . . .
H26A H -0.013413 0.765881 0.786433 0.129 Uiso 1 1 calc R U . . .
H26B H 0.058197 0.699672 0.790932 0.129 Uiso 1 1 calc R U . . .
H26C H -0.049780 0.713295 0.739421 0.129 Uiso 1 1 calc R U . . .
C27 C 0.0663(7) 0.8115(4) 0.6949(4) 0.086(2) Uani 1 1 d . . . . .
H27A H -0.007206 0.797146 0.669108 0.129 Uiso 1 1 calc R U . . .
H27B H 0.131868 0.829162 0.672758 0.129 Uiso 1 1 calc R U . . .
H27C H 0.037609 0.843575 0.720371 0.129 Uiso 1 1 calc R U . . .
C28 C 0.1980(4) 0.4601(2) 0.6786(2) 0.0319(10) Uani 1 1 d . . . . .
C29 C 0.2864(4) 0.4423(2) 0.6413(2) 0.0358(11) Uani 1 1 d . . . . .
C30 C 0.2602(5) 0.4040(2) 0.5952(2) 0.0392(11) Uani 1 1 d . . . . .
C31 C 0.1388(5) 0.3793(2) 0.5837(2) 0.0439(12) Uani 1 1 d . . . . .
C32 C 0.0477(5) 0.3945(2) 0.6188(2) 0.0423(12) Uani 1 1 d . . . . .
C33 C 0.0773(4) 0.4336(2) 0.6648(2) 0.0365(11) Uani 1 1 d . . . . .
C34 C 0.3678(4) 0.4565(2) 0.7666(2) 0.0349(10) Uani 1 1 d . . . . .
C35 C 0.3421(4) 0.3946(2) 0.7793(2) 0.0396(11) Uani 1 1 d . . . . .
C36 C 0.4305(5) 0.3534(2) 0.8050(3) 0.0466(13) Uani 1 1 d . . . . .
C37 C 0.5541(5) 0.3728(3) 0.8192(3) 0.0526(15) Uani 1 1 d . . . . .
C38 C 0.5865(5) 0.4323(3) 0.8070(3) 0.0502(14) Uani 1 1 d . . . . .
C39 C 0.4943(5) 0.4729(2) 0.7814(2) 0.0417(12) Uani 1 1 d . . . . .
C40 C 0.1368(4) 0.5114(2) 0.7803(2) 0.0367(11) Uani 1 1 d . . . . .
C41 C 0.1437(5) 0.4948(3) 0.8367(3) 0.0512(14) Uani 1 1 d . . . . .
C42 C 0.0509(6) 0.5074(4) 0.8728(3) 0.0613(17) Uani 1 1 d . . . . .
C43 C -0.0572(5) 0.5402(3) 0.8524(3) 0.0552(15) Uani 1 1 d . . . . .
C44 C -0.0705(4) 0.5589(2) 0.7976(3) 0.0441(13) Uani 1 1 d . . . . .
C45 C 0.0262(4) 0.5448(2) 0.7632(2) 0.0400(12) Uani 1 1 d . . . . .
B1 B 0.2492(5) 0.5012(2) 0.7359(3) 0.0326(12) Uani 1 1 d . . . . .
Rb1 Rb 0.42195(7) 0.72951(4) 0.57710(3) 0.0757(3) Uani 1 1 d . . . . .
O1 O 0.2699(18) 0.7932(10) 0.4988(8) 0.098(5) Uani 0.394(3) 1 d D U P A 1
O2 O 0.6512(10) 0.7835(5) 0.5512(5) 0.070(3) Uani 0.515(12) 1 d D U P A 4
C46 C 0.198(3) 0.7731(11) 0.4437(10) 0.111(5) Uani 0.394(3) 1 d D U P A 1
H46A H 0.259637 0.765736 0.415395 0.134 Uiso 0.394(3) 1 calc R U P A 1
H46B H 0.152939 0.733184 0.449533 0.134 Uiso 0.394(3) 1 calc R U P A 1
C47 C 0.102(3) 0.8209(13) 0.4215(10) 0.122(6) Uani 0.394(3) 1 d D U P A 1
H47A H 0.013020 0.804484 0.419612 0.146 Uiso 0.394(3) 1 calc R U P A 1
H47B H 0.119153 0.835811 0.383361 0.146 Uiso 0.394(3) 1 calc R U P A 1
C48 C 0.125(3) 0.8721(10) 0.4659(10) 0.121(6) Uani 0.394(3) 1 d D U P A 1
H48A H 0.193563 0.901258 0.456862 0.145 Uiso 0.394(3) 1 calc R U P A 1
H48B H 0.045320 0.895899 0.470428 0.145 Uiso 0.394(3) 1 calc R U P A 1
C49 C 0.166(2) 0.8333(13) 0.5170(9) 0.112(5) Uani 0.394(3) 1 d D U P A 1
H49A H 0.198219 0.859978 0.549603 0.134 Uiso 0.394(3) 1 calc R U P A 1
H49B H 0.093440 0.807671 0.527993 0.134 Uiso 0.394(3) 1 calc R U P A 1
C50 C 0.7883(15) 0.7814(8) 0.5715(9) 0.105(5) Uani 0.515(12) 1 d D U P A 4
H50A H 0.830927 0.747245 0.552288 0.126 Uiso 0.515(12) 1 calc R U P A 4
H50B H 0.799625 0.773591 0.612921 0.126 Uiso 0.515(12) 1 calc R U P A 4
C51 C 0.8458(16) 0.8419(9) 0.5587(10) 0.117(5) Uani 0.515(12) 1 d D U P A 4
H51A H 0.930329 0.835893 0.543981 0.140 Uiso 0.515(12) 1 calc R U P A 4
H51B H 0.857407 0.868537 0.593014 0.140 Uiso 0.515(12) 1 calc R U P A 4
C52 C 0.7515(18) 0.8704(11) 0.5146(9) 0.124(5) Uani 0.515(12) 1 d D U P A 4
H52A H 0.761343 0.916377 0.513403 0.149 Uiso 0.515(12) 1 calc R U P A 4
H52B H 0.761043 0.852965 0.476454 0.149 Uiso 0.515(12) 1 calc R U P A 4
C53 C 0.6268(16) 0.8525(8) 0.5342(9) 0.102(5) Uani 0.515(12) 1 d D U P A 4
H53A H 0.555673 0.856475 0.503424 0.123 Uiso 0.515(12) 1 calc R U P A 4
H53B H 0.607136 0.878060 0.567112 0.123 Uiso 0.515(12) 1 calc R U P A 4
C54 C 0.253(4) 0.939(2) 0.548(2) 0.144(14) Uani 0.286(11) 1 d D U P B -1
H54A H 0.197469 0.936148 0.512277 0.216 Uiso 0.286(11) 1 calc R U P B -1
H54B H 0.208220 0.961403 0.576246 0.216 Uiso 0.286(11) 1 calc R U P B -1
H54C H 0.274312 0.896536 0.562148 0.216 Uiso 0.286(11) 1 calc R U P B -1
C55 C 0.358(4) 0.968(3) 0.5399(19) 0.142(13) Uani 0.286(11) 1 d D U P B -1
H55A H 0.337368 1.012308 0.547618 0.170 Uiso 0.286(11) 1 calc R U P B -1
H55B H 0.419061 0.954991 0.572496 0.170 Uiso 0.286(11) 1 calc R U P B -1
C56 C 0.428(4) 0.972(2) 0.4993(17) 0.115(11) Uani 0.286(11) 1 d D U P B -1
H56A H 0.365918 0.986034 0.467478 0.138 Uiso 0.286(11) 1 calc R U P B -1
H56B H 0.444314 0.927422 0.491098 0.138 Uiso 0.286(11) 1 calc R U P B -1
C57 C 0.532(4) 0.998(3) 0.488(2) 0.150(14) Uani 0.286(11) 1 d D U P B -1
H57A H 0.600141 0.975532 0.512059 0.180 Uiso 0.286(11) 1 calc R U P B -1
H57B H 0.528201 1.040193 0.504682 0.180 Uiso 0.286(11) 1 calc R U P B -1
C58 C 0.582(4) 1.0073(19) 0.4411(17) 0.114(11) Uani 0.286(11) 1 d D U P B -1
H58A H 0.514332 1.017148 0.410804 0.170 Uiso 0.286(11) 1 calc R U P B -1
H58B H 0.628187 0.969618 0.431049 0.170 Uiso 0.286(11) 1 calc R U P B -1
H58C H 0.642955 1.042374 0.446015 0.170 Uiso 0.286(11) 1 calc R U P B -1
C54A C 0.389(5) 0.902(2) 0.554(3) 0.126(13) Uani 0.214(11) 1 d D U P B -2
H54D H 0.314058 0.903322 0.525051 0.189 Uiso 0.214(11) 1 calc R U P B -2
H54E H 0.361586 0.911004 0.591153 0.189 Uiso 0.214(11) 1 calc R U P B -2
H54F H 0.426879 0.859778 0.554021 0.189 Uiso 0.214(11) 1 calc R U P B -2
C55A C 0.472(5) 0.9418(15) 0.542(2) 0.105(11) Uani 0.214(11) 1 d D U P B -2
H55C H 0.470218 0.937914 0.499805 0.126 Uiso 0.214(11) 1 calc R U P B -2
H55D H 0.554357 0.922658 0.557069 0.126 Uiso 0.214(11) 1 calc R U P B -2
C56A C 0.492(4) 1.0007(14) 0.5502(14) 0.075(9) Uani 0.214(11) 1 d D U P B -2
H56C H 0.404052 1.018679 0.549241 0.090 Uiso 0.214(11) 1 calc R U P B -2
H56D H 0.528234 1.003135 0.590423 0.090 Uiso 0.214(11) 1 calc R U P B -2
C57A C 0.555(4) 1.0419(16) 0.525(2) 0.101(11) Uani 0.214(11) 1 d D U P B -2
H57C H 0.644385 1.036700 0.542996 0.121 Uiso 0.214(11) 1 calc R U P B -2
H57D H 0.555995 1.024705 0.486122 0.121 Uiso 0.214(11) 1 calc R U P B -2
C58A C 0.546(6) 1.1005(18) 0.517(3) 0.130(15) Uani 0.214(11) 1 d D U P B -2
H58D H 0.615158 1.114566 0.494860 0.195 Uiso 0.214(11) 1 calc R U P B -2
H58E H 0.462394 1.109957 0.495524 0.195 Uiso 0.214(11) 1 calc R U P B -2
H58F H 0.552310 1.122160 0.553379 0.195 Uiso 0.214(11) 1 calc R U P B -2
O2A O 0.6191(15) 0.7944(8) 0.5290(8) 0.112(4) Uani 0.485(12) 1 d D U P A 5
C50A C 0.714(2) 0.8362(12) 0.5647(9) 0.129(6) Uani 0.485(12) 1 d D U P A 5
H50C H 0.670217 0.873447 0.578603 0.155 Uiso 0.485(12) 1 calc R U P A 5
H50D H 0.757349 0.813184 0.597474 0.155 Uiso 0.485(12) 1 calc R U P A 5
C51A C 0.805(3) 0.8536(9) 0.5232(12) 0.132(6) Uani 0.485(12) 1 d D U P A 5
H51C H 0.769388 0.887075 0.497342 0.159 Uiso 0.485(12) 1 calc R U P A 5
H51D H 0.888425 0.867897 0.542858 0.159 Uiso 0.485(12) 1 calc R U P A 5
C52A C 0.821(2) 0.7953(9) 0.4920(9) 0.116(5) Uani 0.485(12) 1 d D U P A 5
H52C H 0.905728 0.775944 0.504101 0.140 Uiso 0.485(12) 1 calc R U P A 5
H52D H 0.815020 0.803131 0.450606 0.140 Uiso 0.485(12) 1 calc R U P A 5
C53A C 0.7144(17) 0.7542(8) 0.5066(9) 0.098(5) Uani 0.485(12) 1 d D U P A 5
H53C H 0.675808 0.731933 0.472317 0.118 Uiso 0.485(12) 1 calc R U P A 5
H53D H 0.746718 0.722925 0.535351 0.118 Uiso 0.485(12) 1 calc R U P A 5
O1A O 0.227(3) 0.7859(14) 0.4999(12) 0.117(6) Uani 0.354(3) 1 d D U P C 2
C46A C 0.278(3) 0.7593(13) 0.4481(12) 0.120(6) Uani 0.354(3) 1 d D U P C 2
H46C H 0.372519 0.764214 0.448267 0.144 Uiso 0.354(3) 1 calc R U P C 2
H46D H 0.252389 0.715354 0.440416 0.144 Uiso 0.354(3) 1 calc R U P C 2
C47A C 0.203(3) 0.8050(14) 0.4109(11) 0.122(6) Uani 0.354(3) 1 d D U P C 2
H47C H 0.109326 0.797581 0.410534 0.146 Uiso 0.354(3) 1 calc R U P C 2
H47D H 0.226688 0.802972 0.371475 0.146 Uiso 0.354(3) 1 calc R U P C 2
C48A C 0.241(4) 0.8662(11) 0.4379(12) 0.132(7) Uani 0.354(3) 1 d D U P C 2
H48C H 0.184206 0.900345 0.421836 0.158 Uiso 0.354(3) 1 calc R U P C 2
H48D H 0.331237 0.876687 0.432967 0.158 Uiso 0.354(3) 1 calc R U P C 2
C49A C 0.224(4) 0.8554(14) 0.4993(11) 0.128(6) Uani 0.354(3) 1 d D U P C 2
H49C H 0.294783 0.873634 0.524875 0.154 Uiso 0.354(3) 1 calc R U P C 2
H49D H 0.140280 0.871922 0.509390 0.154 Uiso 0.354(3) 1 calc R U P C 2
O1B O 0.237(3) 0.7754(19) 0.4936(13) 0.102(7) Uani 0.252(3) 1 d D U P D 3
C46B C 0.263(3) 0.7920(19) 0.4348(15) 0.106(7) Uani 0.252(3) 1 d D U P D 3
H46E H 0.238889 0.756858 0.408617 0.127 Uiso 0.252(3) 1 calc R U P D 3
H46F H 0.355099 0.801366 0.433624 0.127 Uiso 0.252(3) 1 calc R U P D 3
C47B C 0.183(3) 0.8486(17) 0.4176(18) 0.102(7) Uani 0.252(3) 1 d D U P D 3
H47E H 0.221153 0.887119 0.435209 0.122 Uiso 0.252(3) 1 calc R U P D 3
H47F H 0.171224 0.853690 0.375808 0.122 Uiso 0.252(3) 1 calc R U P D 3
C48B C 0.058(3) 0.8326(19) 0.4406(19) 0.113(7) Uani 0.252(3) 1 d D U P D 3
H48E H 0.025429 0.868367 0.461381 0.135 Uiso 0.252(3) 1 calc R U P D 3
H48F H -0.007860 0.819822 0.409787 0.135 Uiso 0.252(3) 1 calc R U P D 3
C49B C 0.095(3) 0.7801(18) 0.4792(17) 0.109(7) Uani 0.252(3) 1 d D U P D 3
H49E H 0.062798 0.740609 0.461042 0.130 Uiso 0.252(3) 1 calc R U P D 3
H49F H 0.053229 0.785446 0.514577 0.130 Uiso 0.252(3) 1 calc R U P D 3
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'
Rb Rb -0.4688 1.6079 '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 -8 -12 0.0095
-7 -3 2 0.0458
0 8 12 0.0095
7 1 -5 0.0403
1 -13 2 0.0382
-1 14 0 0.0069
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
C36 F7 Rb1 114.8(3) . 2_646 ?
C37 F8 Rb1 125.1(4) . 2_646 ?
C1 N1 C2 113.6(4) . . ?
C1 N1 C4 113.7(4) . . ?
C2 N1 C4 132.6(4) . . ?
C1 N2 C3 111.4(4) . . ?
C1 N2 C16 123.5(4) . . ?
C3 N2 C16 125.0(5) . . ?
N2 C1 N1 102.7(4) . . ?
N2 C1 Rb1 148.1(3) . . ?
N1 C1 Rb1 107.7(3) . . ?
C3 C2 N1 102.2(4) . . ?
C3 C2 B1 122.2(5) . . ?
N1 C2 B1 135.6(4) . . ?
C2 C3 N2 110.1(5) . . ?
C9 C4 C5 121.4(5) . . ?
C9 C4 N1 119.3(4) . . ?
C5 C4 N1 118.5(4) . . ?
C9 C4 Rb1 87.7(3) . . ?
C5 C4 Rb1 78.9(3) . . ?
N1 C4 Rb1 94.9(2) . . ?
C6 C5 C4 117.5(5) . . ?
C6 C5 C10 120.0(5) . . ?
C4 C5 C10 122.5(5) . . ?
C6 C5 Rb1 88.2(3) . . ?
C4 C5 Rb1 76.5(3) . . ?
C10 C5 Rb1 105.1(3) . . ?
C7 C6 C5 122.0(5) . . ?
C7 C6 Rb1 87.4(4) . . ?
C5 C6 Rb1 69.0(3) . . ?
C6 C7 C8 120.0(6) . . ?
C7 C8 C9 120.5(5) . . ?
C8 C9 C4 118.6(5) . . ?
C8 C9 C13 119.8(5) . . ?
C4 C9 C13 121.3(5) . . ?
C8 C9 Rb1 87.9(3) . . ?
C4 C9 Rb1 69.0(3) . . ?
C13 C9 Rb1 108.4(3) . . ?
C5 C10 C12 111.2(5) . . ?
C5 C10 C11 111.2(5) . . ?
C12 C10 C11 109.7(4) . . ?
C10 C12 Rb1 93.5(3) . . ?
C9 C13 C15 113.2(5) . . ?
C9 C13 C14 109.8(5) . . ?
C15 C13 C14 110.2(4) . . ?
C21 C16 C17 122.3(5) . . ?
C21 C16 N2 119.2(5) . . ?
C17 C16 N2 118.5(4) . . ?
C18 C17 C16 117.2(5) . . ?
C18 C17 C22 121.5(5) . . ?
C16 C17 C22 121.2(5) . . ?
C19 C18 C17 121.5(6) . . ?
C18 C19 C20 121.0(5) . . ?
C19 C20 C21 120.5(5) . . ?
C16 C21 C20 117.4(5) . . ?
C16 C21 C25 121.5(5) . . ?
C20 C21 C25 121.2(5) . . ?
C23 C22 C17 111.1(5) . . ?
C23 C22 C24 109.6(5) . . ?
C17 C22 C24 112.6(5) . . ?
C27 C25 C26 108.3(6) . . ?
C27 C25 C21 113.8(6) . . ?
C26 C25 C21 110.9(6) . . ?
C33 C28 C29 112.4(4) . . ?
C33 C28 B1 128.2(4) . . ?
C29 C28 B1 119.0(4) . . ?
F1 C29 C30 115.6(4) . . ?
F1 C29 C28 119.1(4) . . ?
C30 C29 C28 125.3(4) . . ?
F2 C30 C29 121.2(5) . . ?
F2 C30 C31 119.2(5) . . ?
C29 C30 C31 119.5(5) . . ?
F3 C31 C32 121.4(5) . . ?
F3 C31 C30 120.3(5) . . ?
C32 C31 C30 118.3(5) . . ?
F4 C32 C31 118.6(5) . . ?
F4 C32 C33 120.7(5) . . ?
C31 C32 C33 120.6(5) . . ?
F5 C33 C32 114.8(4) . . ?
F5 C33 C28 121.3(4) . . ?
C32 C33 C28 123.9(5) . . ?
C39 C34 C35 112.9(4) . . ?
C39 C34 B1 127.9(4) . . ?
C35 C34 B1 119.2(4) . . ?
F6 C35 C36 115.5(4) . . ?
F6 C35 C34 119.6(4) . . ?
C36 C35 C34 124.8(4) . . ?
F7 C36 C37 119.2(5) . . ?
F7 C36 C35 121.4(5) . . ?
C37 C36 C35 119.4(5) . . ?
F8 C37 C38 121.0(5) . . ?
F8 C37 C36 120.1(5) . . ?
C38 C37 C36 118.9(5) . . ?
F9 C38 C37 119.8(5) . . ?
F9 C38 C39 120.0(5) . . ?
C37 C38 C39 120.3(5) . . ?
F10 C39 C34 120.9(4) . . ?
F10 C39 C38 115.4(4) . . ?
C34 C39 C38 123.7(5) . . ?
C41 C40 C45 112.1(5) . . ?
C41 C40 B1 127.3(4) . . ?
C45 C40 B1 120.3(5) . . ?
F11 C41 C40 121.5(5) . . ?
F11 C41 C42 113.2(5) . . ?
C40 C41 C42 125.3(5) . . ?
F12 C42 C43 119.6(6) . . ?
F12 C42 C41 121.3(6) . . ?
C43 C42 C41 119.0(6) . . ?
C44 C43 F13 120.7(5) . . ?
C44 C43 C42 119.3(5) . . ?
F13 C43 C42 120.0(6) . . ?
F14 C44 C43 120.5(5) . . ?
F14 C44 C45 120.4(5) . . ?
C43 C44 C45 119.1(5) . . ?
F15 C45 C40 119.9(5) . . ?
F15 C45 C44 115.0(4) . . ?
C40 C45 C44 125.1(5) . . ?
C2 B1 C28 115.6(4) . . ?
C2 B1 C40 102.7(4) . . ?
C28 B1 C40 113.3(4) . . ?
C2 B1 C34 113.2(4) . . ?
C28 B1 C34 102.4(4) . . ?
C40 B1 C34 109.9(4) . . ?
C49 O1 C46 95.8(17) . . ?
C49 O1 Rb1 119.5(13) . . ?
C46 O1 Rb1 131.5(14) . . ?
C50 O2 C53 104.2(12) . . ?
C50 O2 Rb1 138.6(9) . . ?
C53 O2 Rb1 109.4(8) . . ?
C47 C46 O1 111.7(15) . . ?
C46 C47 C48 101.4(11) . . ?
C49 C48 C47 99.9(11) . . ?
O1 C49 C48 104.1(18) . . ?
O1 C49 Rb1 39.8(9) . . ?
C48 C49 Rb1 142.3(17) . . ?
O2 C50 C51 108.2(11) . . ?
C50 C51 C52 104.5(11) . . ?
C53 C52 C51 102.3(11) . . ?
C52 C53 O2 101.7(12) . . ?
C52 C53 Rb1 147.8(12) . . ?
O2 C53 Rb1 46.8(6) . . ?
C56 C55 C54 135(4) . . ?
C55 C56 C57 139(4) . . ?
C56 C57 C58 133(4) . . ?
C55A C54A Rb1 130(3) . . ?
C54A C55A C56A 136(4) . . ?
C57A C56A C55A 133(3) . . ?
C58A C57A C56A 135(4) . . ?
C53A O2A C50A 96.9(15) . . ?
C53A O2A Rb1 114.3(11) . . ?
C50A O2A Rb1 121.6(12) . . ?
C51A C50A O2A 101.9(15) . . ?
C52A C51A C50A 103.4(11) . . ?
C51A C52A C53A 105.0(10) . . ?
O2A C53A C52A 107.0(13) . . ?
O2A C53A Rb1 44.5(8) . . ?
C52A C53A Rb1 150.5(10) . . ?
C49A O1A C46A 112(2) . . ?
C49A O1A Rb1 116(2) . . ?
C46A O1A Rb1 93.9(18) . . ?
C47A C46A O1A 91(2) . . ?
C47A C46A Rb1 146.4(15) . . ?
O1A C46A Rb1 59.3(16) . . ?
C46A C47A C48A 102.8(13) . . ?
C47A C48A C49A 103.1(13) . . ?
O1A C49A C48A 99(2) . . ?
C46B O1B C49B 92(2) . . ?
C46B O1B Rb1 124(2) . . ?
C49B O1B Rb1 142(2) . . ?
O1B C46B C47B 107(3) . . ?
C48B C47B C46B 101.3(13) . . ?
C49B C48B C47B 102.7(13) . . ?
C48B C49B O1B 112(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
F1 C29 1.352(5) . ?
F2 C30 1.348(6) . ?
F3 C31 1.349(6) . ?
F4 C32 1.355(6) . ?
F5 C33 1.350(6) . ?
F6 C35 1.362(5) . ?
F7 C36 1.355(6) . ?
F7 Rb1 3.278(4) 2_646 ?
F8 C37 1.355(6) . ?
F8 Rb1 2.980(4) 2_646 ?
F9 C38 1.355(6) . ?
F10 C39 1.354(6) . ?
F11 C41 1.367(7) . ?
F12 C42 1.339(8) . ?
F13 C43 1.355(7) . ?
F14 C44 1.346(6) . ?
F15 C45 1.352(6) . ?
N1 C1 1.372(6) . ?
N1 C2 1.425(6) . ?
N1 C4 1.446(7) . ?
N2 C1 1.352(7) . ?
N2 C3 1.383(6) . ?
N2 C16 1.431(6) . ?
C1 Rb1 3.067(6) . ?
C2 C3 1.348(7) . ?
C2 B1 1.643(7) . ?
C4 C9 1.398(7) . ?
C4 C5 1.416(7) . ?
C4 Rb1 3.307(5) . ?
C5 C6 1.382(8) . ?
C5 C10 1.523(7) . ?
C5 Rb1 3.336(5) . ?
C6 C7 1.378(9) . ?
C6 Rb1 3.572(6) . ?
C7 C8 1.387(8) . ?
C8 C9 1.394(8) . ?
C9 C13 1.514(7) . ?
C9 Rb1 3.538(5) . ?
C10 C12 1.530(8) . ?
C10 C11 1.543(7) . ?
C12 Rb1 3.615(6) . ?
C13 C15 1.527(7) . ?
C13 C14 1.536(8) . ?
C16 C21 1.396(7) . ?
C16 C17 1.407(7) . ?
C17 C18 1.383(8) . ?
C17 C22 1.521(8) . ?
C18 C19 1.367(9) . ?
C19 C20 1.369(9) . ?
C20 C21 1.405(8) . ?
C21 C25 1.522(8) . ?
C22 C23 1.517(10) . ?
C22 C24 1.526(8) . ?
C25 C27 1.513(11) . ?
C25 C26 1.518(11) . ?
C28 C33 1.391(6) . ?
C28 C29 1.395(7) . ?
C28 B1 1.658(7) . ?
C29 C30 1.369(7) . ?
C30 C31 1.375(8) . ?
C31 C32 1.365(8) . ?
C32 C33 1.381(8) . ?
C34 C39 1.377(7) . ?
C34 C35 1.391(7) . ?
C34 B1 1.670(7) . ?
C35 C36 1.372(7) . ?
C36 C37 1.364(8) . ?
C37 C38 1.356(8) . ?
C38 C39 1.389(7) . ?
C40 C41 1.376(8) . ?
C40 C45 1.382(7) . ?
C40 B1 1.668(7) . ?
C41 C42 1.381(9) . ?
C42 C43 1.374(9) . ?
C43 C44 1.349(9) . ?
C44 C45 1.394(8) . ?
Rb1 O1 2.685(19) . ?
Rb1 O2 2.783(10) . ?
O1 C49 1.484(16) . ?
O1 C46 1.500(16) . ?
O2 C50 1.463(14) . ?
O2 C53 1.544(14) . ?
C46 C47 1.489(16) . ?
C47 C48 1.521(16) . ?
C48 C49 1.494(16) . ?
C50 C51 1.471(15) . ?
C51 C52 1.490(15) . ?
C52 C53 1.478(15) . ?
C54 C55 1.29(2) . ?
C55 C56 1.268(19) . ?
C56 C57 1.28(2) . ?
C57 C58 1.29(2) . ?
C54A C55A 1.27(2) . ?
C55A C56A 1.29(2) . ?
C56A C57A 1.29(2) . ?
C57A C58A 1.27(2) . ?
O2A C53A 1.455(15) . ?
O2A C50A 1.521(15) . ?
C50A C51A 1.488(15) . ?
C51A C52A 1.468(15) . ?
C52A C53A 1.488(15) . ?
O1A C49A 1.487(17) . ?
O1A C46A 1.500(17) . ?
C46A C47A 1.487(17) . ?
C47A C48A 1.494(16) . ?
C48A C49A 1.500(17) . ?
O1B C46B 1.486(17) . ?
O1B C49B 1.488(18) . ?
C46B C47B 1.502(16) . ?
C47B C48B 1.498(16) . ?
C48B C49B 1.474(16) . ?
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 -1.9(5) . . . . ?
C16 N2 C1 N1 -177.8(4) . . . . ?
C3 N2 C1 Rb1 160.5(5) . . . . ?
C16 N2 C1 Rb1 -15.4(8) . . . . ?
C2 N1 C1 N2 1.3(5) . . . . ?
C4 N1 C1 N2 177.4(4) . . . . ?
C2 N1 C1 Rb1 -169.1(3) . . . . ?
C4 N1 C1 Rb1 7.0(4) . . . . ?
C1 N1 C2 C3 -0.1(5) . . . . ?
C4 N1 C2 C3 -175.3(4) . . . . ?
C1 N1 C2 B1 -178.9(5) . . . . ?
C4 N1 C2 B1 5.9(8) . . . . ?
N1 C2 C3 N2 -1.1(5) . . . . ?
B1 C2 C3 N2 177.9(4) . . . . ?
C1 N2 C3 C2 2.0(5) . . . . ?
C16 N2 C3 C2 177.9(4) . . . . ?
C1 N1 C4 C9 -96.3(5) . . . . ?
C2 N1 C4 C9 78.8(6) . . . . ?
C1 N1 C4 C5 73.8(5) . . . . ?
C2 N1 C4 C5 -111.1(5) . . . . ?
C1 N1 C4 Rb1 -6.2(4) . . . . ?
C2 N1 C4 Rb1 168.9(4) . . . . ?
C9 C4 C5 C6 -0.4(7) . . . . ?
N1 C4 C5 C6 -170.4(4) . . . . ?
Rb1 C4 C5 C6 -80.8(5) . . . . ?
C9 C4 C5 C10 179.8(5) . . . . ?
N1 C4 C5 C10 9.9(7) . . . . ?
Rb1 C4 C5 C10 99.5(4) . . . . ?
C9 C4 C5 Rb1 80.3(4) . . . . ?
N1 C4 C5 Rb1 -89.6(4) . . . . ?
C4 C5 C6 C7 1.1(8) . . . . ?
C10 C5 C6 C7 -179.2(5) . . . . ?
Rb1 C5 C6 C7 -72.7(6) . . . . ?
C4 C5 C6 Rb1 73.8(4) . . . . ?
C10 C5 C6 Rb1 -106.4(5) . . . . ?
C5 C6 C7 C8 -1.2(9) . . . . ?
Rb1 C6 C7 C8 -64.3(6) . . . . ?
C6 C7 C8 C9 0.5(9) . . . . ?
C7 C8 C9 C4 0.1(8) . . . . ?
C7 C8 C9 C13 174.9(5) . . . . ?
C7 C8 C9 Rb1 64.8(5) . . . . ?
C5 C4 C9 C8 -0.2(7) . . . . ?
N1 C4 C9 C8 169.7(4) . . . . ?
Rb1 C4 C9 C8 75.3(4) . . . . ?
C5 C4 C9 C13 -174.8(5) . . . . ?
N1 C4 C9 C13 -5.0(7) . . . . ?
Rb1 C4 C9 C13 -99.3(4) . . . . ?
C5 C4 C9 Rb1 -75.5(4) . . . . ?
N1 C4 C9 Rb1 94.4(4) . . . . ?
C6 C5 C10 C12 67.4(7) . . . . ?
C4 C5 C10 C12 -112.8(6) . . . . ?
Rb1 C5 C10 C12 -29.4(5) . . . . ?
C6 C5 C10 C11 -55.0(7) . . . . ?
C4 C5 C10 C11 124.7(5) . . . . ?
Rb1 C5 C10 C11 -151.9(4) . . . . ?
C5 C10 C12 Rb1 26.0(4) . . . . ?
C11 C10 C12 Rb1 149.4(4) . . . . ?
C8 C9 C13 C15 43.6(7) . . . . ?
C4 C9 C13 C15 -141.9(5) . . . . ?
Rb1 C9 C13 C15 142.0(4) . . . . ?
C8 C9 C13 C14 -80.1(6) . . . . ?
C4 C9 C13 C14 94.5(6) . . . . ?
Rb1 C9 C13 C14 18.3(5) . . . . ?
C1 N2 C16 C21 86.1(6) . . . . ?
C3 N2 C16 C21 -89.2(7) . . . . ?
C1 N2 C16 C17 -94.1(6) . . . . ?
C3 N2 C16 C17 90.6(6) . . . . ?
C21 C16 C17 C18 2.2(9) . . . . ?
N2 C16 C17 C18 -177.6(5) . . . . ?
C21 C16 C17 C22 -179.8(6) . . . . ?
N2 C16 C17 C22 0.4(8) . . . . ?
C16 C17 C18 C19 -2.0(10) . . . . ?
C22 C17 C18 C19 -179.9(6) . . . . ?
C17 C18 C19 C20 0.4(11) . . . . ?
C18 C19 C20 C21 1.2(11) . . . . ?
C17 C16 C21 C20 -0.8(9) . . . . ?
N2 C16 C21 C20 179.0(5) . . . . ?
C17 C16 C21 C25 -179.5(6) . . . . ?
N2 C16 C21 C25 0.3(9) . . . . ?
C19 C20 C21 C16 -0.9(10) . . . . ?
C19 C20 C21 C25 177.8(7) . . . . ?
C18 C17 C22 C23 87.6(7) . . . . ?
C16 C17 C22 C23 -90.3(7) . . . . ?
C18 C17 C22 C24 -35.8(8) . . . . ?
C16 C17 C22 C24 146.4(6) . . . . ?
C16 C21 C25 C27 -138.8(7) . . . . ?
C20 C21 C25 C27 42.5(9) . . . . ?
C16 C21 C25 C26 98.7(7) . . . . ?
C20 C21 C25 C26 -80.0(8) . . . . ?
C33 C28 C29 F1 -175.6(4) . . . . ?
B1 C28 C29 F1 -2.6(6) . . . . ?
C33 C28 C29 C30 1.1(7) . . . . ?
B1 C28 C29 C30 174.1(4) . . . . ?
F1 C29 C30 F2 -2.9(7) . . . . ?
C28 C29 C30 F2 -179.7(4) . . . . ?
F1 C29 C30 C31 175.6(4) . . . . ?
C28 C29 C30 C31 -1.2(8) . . . . ?
F2 C30 C31 F3 -0.6(7) . . . . ?
C29 C30 C31 F3 -179.1(4) . . . . ?
F2 C30 C31 C32 179.3(4) . . . . ?
C29 C30 C31 C32 0.7(7) . . . . ?
F3 C31 C32 F4 -1.7(7) . . . . ?
C30 C31 C32 F4 178.4(4) . . . . ?
F3 C31 C32 C33 179.4(5) . . . . ?
C30 C31 C32 C33 -0.4(8) . . . . ?
F4 C32 C33 F5 4.1(7) . . . . ?
C31 C32 C33 F5 -177.1(4) . . . . ?
F4 C32 C33 C28 -178.4(4) . . . . ?
C31 C32 C33 C28 0.4(8) . . . . ?
C29 C28 C33 F5 176.6(4) . . . . ?
B1 C28 C33 F5 4.5(7) . . . . ?
C29 C28 C33 C32 -0.7(7) . . . . ?
B1 C28 C33 C32 -172.9(5) . . . . ?
C39 C34 C35 F6 177.6(5) . . . . ?
B1 C34 C35 F6 -3.1(7) . . . . ?
C39 C34 C35 C36 1.5(8) . . . . ?
B1 C34 C35 C36 -179.2(5) . . . . ?
Rb1 F7 C36 C37 24.6(7) 2_646 . . . ?
Rb1 F7 C36 C35 -154.4(5) 2_646 . . . ?
F6 C35 C36 F7 1.9(8) . . . . ?
C34 C35 C36 F7 178.2(5) . . . . ?
F6 C35 C36 C37 -177.1(5) . . . . ?
C34 C35 C36 C37 -0.8(9) . . . . ?
Rb1 F8 C37 C38 150.4(5) 2_646 . . . ?
Rb1 F8 C37 C36 -27.4(8) 2_646 . . . ?
F7 C36 C37 F8 -1.8(10) . . . . ?
C35 C36 C37 F8 177.3(6) . . . . ?
F7 C36 C37 C38 -179.6(6) . . . . ?
C35 C36 C37 C38 -0.6(10) . . . . ?
F8 C37 C38 F9 3.2(10) . . . . ?
C36 C37 C38 F9 -178.9(6) . . . . ?
F8 C37 C38 C39 -176.6(6) . . . . ?
C36 C37 C38 C39 1.2(10) . . . . ?
C35 C34 C39 F10 -179.9(5) . . . . ?
B1 C34 C39 F10 0.8(9) . . . . ?
C35 C34 C39 C38 -0.8(8) . . . . ?
B1 C34 C39 C38 179.9(5) . . . . ?
F9 C38 C39 F10 -1.2(8) . . . . ?
C37 C38 C39 F10 178.6(6) . . . . ?
F9 C38 C39 C34 179.7(6) . . . . ?
C37 C38 C39 C34 -0.5(10) . . . . ?
C45 C40 C41 F11 -177.0(5) . . . . ?
B1 C40 C41 F11 -2.8(9) . . . . ?
C45 C40 C41 C42 2.0(9) . . . . ?
B1 C40 C41 C42 176.1(6) . . . . ?
F11 C41 C42 F12 -0.5(10) . . . . ?
C40 C41 C42 F12 -179.6(6) . . . . ?
F11 C41 C42 C43 177.6(6) . . . . ?
C40 C41 C42 C43 -1.4(11) . . . . ?
F12 C42 C43 C44 178.6(6) . . . . ?
C41 C42 C43 C44 0.4(10) . . . . ?
F12 C42 C43 F13 -0.5(10) . . . . ?
C41 C42 C43 F13 -178.7(6) . . . . ?
F13 C43 C44 F14 -0.8(9) . . . . ?
C42 C43 C44 F14 -179.9(6) . . . . ?
F13 C43 C44 C45 178.8(5) . . . . ?
C42 C43 C44 C45 -0.3(9) . . . . ?
C41 C40 C45 F15 178.1(5) . . . . ?
B1 C40 C45 F15 3.5(7) . . . . ?
C41 C40 C45 C44 -1.8(7) . . . . ?
B1 C40 C45 C44 -176.4(5) . . . . ?
F14 C44 C45 F15 0.8(7) . . . . ?
C43 C44 C45 F15 -178.9(5) . . . . ?
F14 C44 C45 C40 -179.3(5) . . . . ?
C43 C44 C45 C40 1.1(8) . . . . ?
C3 C2 B1 C28 155.4(4) . . . . ?
N1 C2 B1 C28 -25.9(7) . . . . ?
C3 C2 B1 C40 31.5(6) . . . . ?
N1 C2 B1 C40 -149.8(5) . . . . ?
C3 C2 B1 C34 -86.9(5) . . . . ?
N1 C2 B1 C34 91.7(6) . . . . ?
C33 C28 B1 C2 -119.4(5) . . . . ?
C29 C28 B1 C2 68.9(5) . . . . ?
C33 C28 B1 C40 -1.2(7) . . . . ?
C29 C28 B1 C40 -173.0(4) . . . . ?
C33 C28 B1 C34 117.1(5) . . . . ?
C29 C28 B1 C34 -54.6(5) . . . . ?
C41 C40 B1 C2 -111.7(6) . . . . ?
C45 C40 B1 C2 62.0(5) . . . . ?
C41 C40 B1 C28 123.0(5) . . . . ?
C45 C40 B1 C28 -63.4(6) . . . . ?
C41 C40 B1 C34 9.1(7) . . . . ?
C45 C40 B1 C34 -177.2(4) . . . . ?
C39 C34 B1 C2 -1.1(8) . . . . ?
C35 C34 B1 C2 179.7(5) . . . . ?
C39 C34 B1 C28 124.0(5) . . . . ?
C35 C34 B1 C28 -55.2(6) . . . . ?
C39 C34 B1 C40 -115.3(6) . . . . ?
C35 C34 B1 C40 65.5(6) . . . . ?
C49 O1 C46 C47 28(3) . . . . ?
Rb1 O1 C46 C47 166.4(19) . . . . ?
O1 C46 C47 C48 2(4) . . . . ?
C46 C47 C48 C49 -31(3) . . . . ?
C46 O1 C49 C48 -48(3) . . . . ?
Rb1 O1 C49 C48 166.7(15) . . . . ?
C46 O1 C49 Rb1 145(2) . . . . ?
C47 C48 C49 O1 52(3) . . . . ?
C47 C48 C49 Rb1 66(3) . . . . ?
C53 O2 C50 C51 -9(2) . . . . ?
Rb1 O2 C50 C51 -152.1(13) . . . . ?
O2 C50 C51 C52 -18(2) . . . . ?
C50 C51 C52 C53 39(2) . . . . ?
C51 C52 C53 O2 -43(2) . . . . ?
C51 C52 C53 Rb1 -54(3) . . . . ?
C50 O2 C53 C52 32.3(18) . . . . ?
Rb1 O2 C53 C52 -172.4(12) . . . . ?
C50 O2 C53 Rb1 -155.3(14) . . . . ?
C54 C55 C56 C57 -178(7) . . . . ?
C55 C56 C57 C58 -165(8) . . . . ?
Rb1 C54A C55A C56A -151(5) . . . . ?
C54A C55A C56A C57A -158(7) . . . . ?
C55A C56A C57A C58A 150(7) . . . . ?
C53A O2A C50A C51A 50(2) . . . . ?
Rb1 O2A C50A C51A 173.9(15) . . . . ?
O2A C50A C51A C52A -40(3) . . . . ?
C50A C51A C52A C53A 14(3) . . . . ?
C50A O2A C53A C52A -41(2) . . . . ?
Rb1 O2A C53A C52A -170.7(14) . . . . ?
C50A O2A C53A Rb1 129.3(18) . . . . ?
C51A C52A C53A O2A 18(3) . . . . ?
C51A C52A C53A Rb1 5(4) . . . . ?
C49A O1A C46A C47A -42(3) . . . . ?
Rb1 O1A C46A C47A -163.0(19) . . . . ?
C49A O1A C46A Rb1 120(3) . . . . ?
O1A C46A C47A C48A 53(3) . . . . ?
Rb1 C46A C47A C48A 26(5) . . . . ?
C46A C47A C48A C49A -49(3) . . . . ?
C46A O1A C49A C48A 15(4) . . . . ?
Rb1 O1A C49A C48A 122(2) . . . . ?
C47A C48A C49A O1A 20(3) . . . . ?
C49B O1B C46B C47B 48(4) . . . . ?
Rb1 O1B C46B C47B -143(3) . . . . ?
O1B C46B C47B C48B -42(4) . . . . ?
C46B C47B C48B C49B 14(5) . . . . ?
C47B C48B C49B O1B 17(5) . . . . ?
C46B O1B C49B C48B -39(4) . . . . ?
Rb1 O1B C49B C48B 156(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
0.1542 -8.1321 -12.4194 0.0018 0.0090 1.0000
-6.6155 -3.0141 1.9434 0.2323 0.9698 0.0739
-0.1542 8.1321 12.4194 -0.0018 -0.0090 -1.0000
6.6062 1.1732 -4.7114 -0.2303 -0.9614 0.1505
1.2645 -13.4554 2.2075 0.8739 -0.2090 0.4388
-1.2072 13.6568 -0.3395 -0.8143 0.1946 -0.5469
