#------------------------------------------------------------------------------
#$Date: 2021-02-05 01:24:50 +0200 (Fri, 05 Feb 2021) $
#$Revision: 261723 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/01/7060152.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_7060152
loop_
_publ_author_name
'O’Toole, Niall'
'Lecourt, Constance'
'Suffren, Yan'
'Toche, François'
'Chiriac, Rodica'
'Gilon, Nicole'
'Bessueille, François'
'Brioude, Arnaud'
'Jeanneau, Erwann'
'Luneau, Dominique'
'Desroches, Cédric'
_publ_section_title
;
 Intercalation of a manganese(ii)-thiacalixarene luminescent complex in
 layered double hydroxides: synthesis and photophysical characterization
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              343
_journal_page_last               350
_journal_paper_doi               10.1039/D0NJ04890A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C92 H120 Al4 N4 O32 S8'
_chemical_formula_sum            'C92 H120 Al4 N4 O32 S8'
_chemical_formula_weight         2158.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-03
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.421(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9486(4)
_cell_length_b                   22.9133(7)
_cell_length_c                   20.0205(6)
_cell_measurement_reflns_used    13198
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      24.6920
_cell_measurement_theta_min      3.0500
_cell_volume                     6197.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.2634
_diffrn_detector_type            Onyx
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -62.00  31.00   1.00   90.00    --    9.08 -57.00 -60.00   93
  2  ω    -19.00   7.00   1.00   90.00    --    9.08 -57.00 150.00   26
  3  ω    -17.00  76.00   1.00   90.00    --    9.08  57.00  90.00   93
  4  ω     32.00  98.00   1.00   90.00    --    9.08-178.00 150.00   66
  5  ω    -83.00  11.00   1.00   90.00    --  -10.64 -57.00-150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Onyx'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0122848000
_diffrn_orient_matrix_UB_12      0.0045392000
_diffrn_orient_matrix_UB_13      -0.0361824000
_diffrn_orient_matrix_UB_21      0.0345264000
_diffrn_orient_matrix_UB_22      0.0232784000
_diffrn_orient_matrix_UB_23      0.0043846000
_diffrn_orient_matrix_UB_31      0.0376020000
_diffrn_orient_matrix_UB_32      -0.0198884000
_diffrn_orient_matrix_UB_33      -0.0031397000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.891
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            68248
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.891
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.266
_diffrn_reflns_theta_min         2.752
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.240
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.157
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     717
_refine_ls_number_reflns         15063
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.0653
_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)+(0.0663P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1327
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8109
_reflns_number_total             15063
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj04890a2.cif
_cod_data_source_block           28af2
_cod_depositor_comments          'Adding full bibliography for 7060152.cif.'
_cod_database_code               7060152
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C92 H120 Al4 N4 O32 S8'
_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   0.970
_shelx_estimated_absorpt_t_min   0.923
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O13-H13
 0.95 with sigma of 0.01
 O14-H14
 0.95 with sigma of 0.01
 C30A-C27 \\sim C30B-C27 \\sim C28A-C27 \\sim C28B-C27 \\sim C29A-C27 \\sim
C29B-C27
 with sigma of 0.01
 C19B-C17 \\sim C19A-C17 \\sim C18B-C17 \\sim C18A-C17 \\sim C20B-C17 \\sim
C20A-C17
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C27 \\sim C28A \\sim C28B \\sim C29A \\sim C29B \\sim C30A \\sim C30B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C18A \\sim C18B \\sim C19A \\sim C19B \\sim C20A \\sim C20B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C37 \\sim C38 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C18B)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19B)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C20B)=Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(2)
 Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=Sof(C20A)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C13(H13A), C15(H15), C24(H24), C26(H26), C33(H33), C35(H35),
 C41(H41), C44(H44)
5.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C18A(H18A,H18B,H18C),
 C18B(H18D,H18E,H18F), C19A(H19A,H19B,H19C), C19B(H19D,H19E,H19F), C20A(H20A,
 H20B,H20C), C20B(H20D,H20E,H20F), C28A(H28A,H28B,H28C), C28B(H28D,H28E,H28F),
 C29A(H29A,H29B,H29C), C29B(H29D,H29E,H29F), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_date_sample_data_collection 2014-01-30
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id 28AF2
_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 1.214
_oxdiff_exptl_absorpt_empirical_full_min 0.825
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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
S1 S 0.27630(5) 0.32554(3) 0.88127(4) 0.03431(18) Uani 1 1 d . . . . .
S2 S 0.07540(5) 0.53312(3) 0.81553(4) 0.03818(19) Uani 1 1 d . . . . .
S3 S 0.41572(5) 0.63866(3) 0.77590(4) 0.03690(19) Uani 1 1 d . . . . .
S4 S 0.61371(5) 0.43131(3) 0.83605(4) 0.03492(18) Uani 1 1 d . . . . .
Al1 Al 0.35784(6) 0.43754(4) 0.95955(4) 0.0310(2) Uani 1 1 d . . . . .
Al2 Al 0.42091(6) 0.57359(4) 0.91219(4) 0.0337(2) Uani 1 1 d . . . . .
O1 O 0.31229(13) 0.35138(8) 0.94987(9) 0.0364(5) Uani 1 1 d . . . . .
O2 O 0.24984(14) 0.26521(8) 0.87957(10) 0.0433(5) Uani 1 1 d . . . . .
O3 O 0.10434(14) 0.55317(9) 0.88568(10) 0.0432(5) Uani 1 1 d . . . . .
O4 O -0.02481(14) 0.54509(9) 0.77804(11) 0.0466(5) Uani 1 1 d . . . . .
O5 O 0.43933(13) 0.64551(8) 0.85095(10) 0.0385(5) Uani 1 1 d . . . . .
O6 O 0.42261(15) 0.68978(9) 0.73651(11) 0.0480(5) Uani 1 1 d . . . . .
O7 O 0.63800(13) 0.44751(9) 0.90721(10) 0.0389(5) Uani 1 1 d . . . . .
O8 O 0.69129(14) 0.40457(9) 0.81062(11) 0.0461(5) Uani 1 1 d . . . . .
O9 O 0.44345(13) 0.41731(8) 0.90696(9) 0.0347(5) Uani 1 1 d . . . . .
O10 O 0.25373(13) 0.45437(8) 0.88222(10) 0.0365(5) Uani 1 1 d . . . . .
O11 O 0.29150(13) 0.57521(8) 0.86069(10) 0.0362(5) Uani 1 1 d . . . . .
O12 O 0.46021(13) 0.52631(8) 0.84691(9) 0.0359(5) Uani 1 1 d . . . . .
O13 O 0.39693(13) 0.51482(8) 0.96757(9) 0.0323(4) Uani 1 1 d D . . . .
H13 H 0.410(3) 0.5194(16) 1.0152(6) 0.076(12) Uiso 1 1 d D . . . .
O14 O 0.55118(14) 0.58576(9) 0.95945(10) 0.0388(5) Uani 1 1 d D . . . .
H14 H 0.579(4) 0.610(2) 0.932(2) 0.17(2) Uiso 1 1 d D . . . .
O15 O 0.38742(15) 0.63449(9) 0.96877(10) 0.0452(5) Uani 1 1 d . . . . .
O16 O 0.26617(14) 0.44151(9) 1.01730(10) 0.0407(5) Uani 1 1 d . . . . .
N1 N 0.2960(2) 0.68999(14) 1.02067(16) 0.0650(8) Uani 1 1 d . . . . .
N2 N 0.15744(19) 0.48659(13) 1.06589(15) 0.0546(7) Uani 1 1 d . . . . .
C1 C 0.17295(19) 0.36543(12) 0.83839(14) 0.0351(7) Uani 1 1 d . . . . .
C2 C 0.17616(19) 0.42704(12) 0.84663(14) 0.0326(6) Uani 1 1 d . . . . .
C3 C 0.08891(19) 0.45609(12) 0.81168(15) 0.0355(7) Uani 1 1 d . . . . .
C4 C 0.0091(2) 0.42616(14) 0.77090(16) 0.0422(7) Uani 1 1 d . . . . .
H4 H -0.046100 0.447436 0.748017 0.051 Uiso 1 1 calc R U . . .
C5 C 0.0076(2) 0.36620(14) 0.76258(15) 0.0416(7) Uani 1 1 d . . . . .
C6 C 0.0923(2) 0.33660(13) 0.79785(15) 0.0401(7) Uani 1 1 d . . . . .
H6 H 0.094574 0.296201 0.793985 0.048 Uiso 1 1 calc R U . . .
C7 C -0.0808(2) 0.33323(15) 0.71688(18) 0.0521(9) Uani 1 1 d . . . . .
C8 C -0.1646(3) 0.37461(18) 0.6837(2) 0.0820(13) Uani 1 1 d . . . . .
H8A H -0.185351 0.395814 0.718993 0.123 Uiso 1 1 calc R U . . .
H8B H -0.219321 0.352569 0.656917 0.123 Uiso 1 1 calc R U . . .
H8C H -0.141879 0.401537 0.654231 0.123 Uiso 1 1 calc R U . . .
C9 C -0.0450(3) 0.30251(19) 0.6592(2) 0.0778(12) Uani 1 1 d . . . . .
H9A H -0.020148 0.331043 0.632677 0.117 Uiso 1 1 calc R U . . .
H9B H -0.099270 0.281891 0.629746 0.117 Uiso 1 1 calc R U . . .
H9C H 0.006687 0.275431 0.679196 0.117 Uiso 1 1 calc R U . . .
C10 C -0.1191(3) 0.28834(19) 0.7599(2) 0.0803(13) Uani 1 1 d . . . . .
H10A H -0.066887 0.261640 0.780102 0.120 Uiso 1 1 calc R U . . .
H10B H -0.173189 0.267233 0.730908 0.120 Uiso 1 1 calc R U . . .
H10C H -0.141359 0.307814 0.795702 0.120 Uiso 1 1 calc R U . . .
C11 C 0.2505(2) 0.58196(12) 0.79606(15) 0.0332(6) Uani 1 1 d . . . . .
C12 C 0.2960(2) 0.61011(12) 0.74877(15) 0.0354(7) Uani 1 1 d . . . . .
C13 C 0.2498(2) 0.61743(13) 0.67921(16) 0.0445(8) Uani 1 1 d . . . . .
H13A H 0.283425 0.636379 0.650830 0.053 Uiso 1 1 calc R U . . .
C14 C 0.1542(2) 0.59703(14) 0.65118(16) 0.0461(8) Uani 1 1 d . . . . .
C15 C 0.1077(2) 0.57110(13) 0.69677(16) 0.0441(8) Uani 1 1 d . . . . .
H15 H 0.043123 0.557920 0.679935 0.053 Uiso 1 1 calc R U . . .
C16 C 0.1519(2) 0.56365(12) 0.76617(15) 0.0352(7) Uani 1 1 d . . . . .
C17 C 0.1040(3) 0.60438(16) 0.57411(17) 0.0610(10) Uani 1 1 d D . . . .
C18A C -0.0022(6) 0.5800(6) 0.5562(5) 0.100(4) Uani 0.540(8) 1 d D U P A 1
H18A H -0.032027 0.585890 0.508082 0.150 Uiso 0.540(8) 1 calc R U P A 1
H18B H -0.040358 0.599793 0.583100 0.150 Uiso 0.540(8) 1 calc R U P A 1
H18C H -0.000375 0.538972 0.566413 0.150 Uiso 0.540(8) 1 calc R U P A 1
C18B C 0.0553(13) 0.5483(4) 0.5448(6) 0.107(4) Uani 0.460(8) 1 d D U P A 2
H18D H 0.012596 0.534882 0.572478 0.160 Uiso 0.460(8) 1 calc R U P A 2
H18E H 0.105079 0.519446 0.544650 0.160 Uiso 0.460(8) 1 calc R U P A 2
H18F H 0.017016 0.554852 0.498411 0.160 Uiso 0.460(8) 1 calc R U P A 2
C19A C 0.1594(8) 0.5676(5) 0.5317(4) 0.110(4) Uani 0.540(8) 1 d D U P A 1
H19A H 0.162409 0.527784 0.546930 0.165 Uiso 0.540(8) 1 calc R U P A 1
H19B H 0.225362 0.582514 0.537764 0.165 Uiso 0.540(8) 1 calc R U P A 1
H19C H 0.125161 0.569553 0.483771 0.165 Uiso 0.540(8) 1 calc R U P A 1
C19B C 0.1778(7) 0.6273(6) 0.5349(4) 0.089(4) Uani 0.460(8) 1 d D U P A 2
H19D H 0.227532 0.598239 0.535295 0.134 Uiso 0.460(8) 1 calc R U P A 2
H19E H 0.208647 0.662201 0.556723 0.134 Uiso 0.460(8) 1 calc R U P A 2
H19F H 0.143477 0.635824 0.488088 0.134 Uiso 0.460(8) 1 calc R U P A 2
C20A C 0.0942(11) 0.6680(3) 0.5544(6) 0.110(4) Uani 0.540(8) 1 d D U P A 1
H20A H 0.058660 0.671582 0.506901 0.165 Uiso 0.540(8) 1 calc R U P A 1
H20B H 0.158903 0.684805 0.560725 0.165 Uiso 0.540(8) 1 calc R U P A 1
H20C H 0.058915 0.688058 0.582944 0.165 Uiso 0.540(8) 1 calc R U P A 1
C20B C 0.0286(9) 0.6537(5) 0.5695(7) 0.109(5) Uani 0.460(8) 1 d D U P A 2
H20D H 0.009178 0.667906 0.522947 0.163 Uiso 0.460(8) 1 calc R U P A 2
H20E H 0.057967 0.684881 0.599752 0.163 Uiso 0.460(8) 1 calc R U P A 2
H20F H -0.028463 0.639257 0.582833 0.163 Uiso 0.460(8) 1 calc R U P A 2
C21 C 0.4965(2) 0.58589(13) 0.75900(15) 0.0375(7) Uani 1 1 d . . . . .
C22 C 0.50940(19) 0.53453(12) 0.80027(14) 0.0323(6) Uani 1 1 d . . . . .
C23 C 0.5765(2) 0.49419(12) 0.78466(15) 0.0352(7) Uani 1 1 d . . . . .
C24 C 0.6219(2) 0.50369(14) 0.73095(15) 0.0438(8) Uani 1 1 d . . . . .
H24 H 0.664485 0.475253 0.721826 0.053 Uiso 1 1 calc R U . . .
C25 C 0.6065(2) 0.55358(16) 0.69057(17) 0.0504(8) Uani 1 1 d . . . . .
C26 C 0.5421(2) 0.59444(15) 0.70610(16) 0.0494(8) Uani 1 1 d . . . . .
H26 H 0.529343 0.628523 0.680172 0.059 Uiso 1 1 calc R U . . .
C27 C 0.6590(3) 0.56465(19) 0.6327(2) 0.0770(12) Uani 1 1 d D U . . .
C28A C 0.7175(7) 0.6227(3) 0.6486(5) 0.117(3) Uani 0.644(6) 1 d D U P B 1
H28A H 0.671927 0.654791 0.642326 0.175 Uiso 0.644(6) 1 calc R U P B 1
H28B H 0.759992 0.626896 0.617844 0.175 Uiso 0.644(6) 1 calc R U P B 1
H28C H 0.756691 0.622201 0.695358 0.175 Uiso 0.644(6) 1 calc R U P B 1
C28B C 0.6236(13) 0.6162(6) 0.5874(9) 0.108(4) Uani 0.356(6) 1 d D U P B 2
H28D H 0.552627 0.617847 0.576480 0.161 Uiso 0.356(6) 1 calc R U P B 2
H28E H 0.645052 0.612589 0.545552 0.161 Uiso 0.356(6) 1 calc R U P B 2
H28F H 0.650469 0.651313 0.610942 0.161 Uiso 0.356(6) 1 calc R U P B 2
C29A C 0.5787(6) 0.5730(5) 0.5668(3) 0.112(3) Uani 0.644(6) 1 d D U P B 1
H29A H 0.538624 0.538505 0.557423 0.169 Uiso 0.644(6) 1 calc R U P B 1
H29B H 0.608574 0.580201 0.529233 0.169 Uiso 0.644(6) 1 calc R U P B 1
H29C H 0.538074 0.605725 0.571910 0.169 Uiso 0.644(6) 1 calc R U P B 1
C29B C 0.6427(12) 0.5085(5) 0.5890(7) 0.110(4) Uani 0.356(6) 1 d D U P B 2
H29D H 0.660122 0.475185 0.618709 0.164 Uiso 0.356(6) 1 calc R U P B 2
H29E H 0.683431 0.509450 0.556828 0.164 Uiso 0.356(6) 1 calc R U P B 2
H29F H 0.574374 0.505749 0.564332 0.164 Uiso 0.356(6) 1 calc R U P B 2
C30A C 0.7365(7) 0.5205(4) 0.6290(5) 0.099(3) Uani 0.644(6) 1 d D U P B 1
H30A H 0.780722 0.515827 0.673845 0.148 Uiso 0.644(6) 1 calc R U P B 1
H30B H 0.773082 0.533552 0.597066 0.148 Uiso 0.644(6) 1 calc R U P B 1
H30C H 0.705453 0.483818 0.613775 0.148 Uiso 0.644(6) 1 calc R U P B 1
C30B C 0.7689(6) 0.5624(9) 0.6622(8) 0.108(4) Uani 0.356(6) 1 d D U P B 2
H30D H 0.789852 0.596326 0.690093 0.161 Uiso 0.356(6) 1 calc R U P B 2
H30E H 0.801608 0.561393 0.625275 0.161 Uiso 0.356(6) 1 calc R U P B 2
H30F H 0.785657 0.527955 0.689968 0.161 Uiso 0.356(6) 1 calc R U P B 2
C31 C 0.44100(19) 0.38071(12) 0.85792(14) 0.0310(6) Uani 1 1 d . . . . .
C32 C 0.5139(2) 0.38153(12) 0.81862(14) 0.0341(7) Uani 1 1 d . . . . .
C33 C 0.5138(2) 0.34120(13) 0.76681(16) 0.0423(7) Uani 1 1 d . . . . .
H33 H 0.563030 0.343694 0.743037 0.051 Uiso 1 1 calc R U . . .
C34 C 0.4433(2) 0.29727(13) 0.74891(17) 0.0469(8) Uani 1 1 d . . . . .
C35 C 0.3716(2) 0.29550(13) 0.78586(16) 0.0434(8) Uani 1 1 d . . . . .
H35 H 0.323297 0.266610 0.775788 0.052 Uiso 1 1 calc R U . . .
C36 C 0.36965(19) 0.33572(12) 0.83764(14) 0.0334(6) Uani 1 1 d . . . . .
C37 C 0.4515(3) 0.25044(17) 0.6960(2) 0.0686(11) Uani 1 1 d . U . . .
C38 C 0.4800(4) 0.2784(2) 0.6339(2) 0.1208(19) Uani 1 1 d . U . . .
H38A H 0.485275 0.248696 0.601275 0.181 Uiso 1 1 calc R U . . .
H38B H 0.542475 0.298046 0.649300 0.181 Uiso 1 1 calc R U . . .
H38C H 0.430139 0.306100 0.612466 0.181 Uiso 1 1 calc R U . . .
C39 C 0.5322(5) 0.2080(2) 0.7307(3) 0.145(2) Uani 1 1 d . U . . .
H39A H 0.539551 0.178488 0.698321 0.218 Uiso 1 1 calc R U . . .
H39B H 0.514463 0.190011 0.769274 0.218 Uiso 1 1 calc R U . . .
H39C H 0.593546 0.228642 0.746538 0.218 Uiso 1 1 calc R U . . .
C40 C 0.3556(4) 0.2177(2) 0.6691(2) 0.1080(18) Uani 1 1 d . U . . .
H40A H 0.306094 0.244015 0.643837 0.162 Uiso 1 1 calc R U . . .
H40B H 0.334042 0.201543 0.707107 0.162 Uiso 1 1 calc R U . . .
H40C H 0.365752 0.186811 0.639197 0.162 Uiso 1 1 calc R U . . .
C41 C 0.3092(3) 0.64438(15) 0.98387(18) 0.0531(9) Uani 1 1 d . . . . .
H41 H 0.256864 0.618581 0.968712 0.064 Uiso 1 1 calc R U . . .
C42 C 0.3736(4) 0.7311(2) 1.0448(3) 0.0986(16) Uani 1 1 d . . . . .
H42A H 0.394112 0.729789 1.094233 0.148 Uiso 1 1 calc R U . . .
H42B H 0.350297 0.769650 1.030274 0.148 Uiso 1 1 calc R U . . .
H42C H 0.428760 0.721701 1.026089 0.148 Uiso 1 1 calc R U . . .
C43 C 0.2027(4) 0.6972(3) 1.0390(3) 0.121(2) Uani 1 1 d . . . . .
H43A H 0.158588 0.666131 1.019045 0.181 Uiso 1 1 calc R U . . .
H43B H 0.173755 0.733962 1.021819 0.181 Uiso 1 1 calc R U . . .
H43C H 0.213725 0.696256 1.088266 0.181 Uiso 1 1 calc R U . . .
C44 C 0.2077(2) 0.48243(14) 1.01863(16) 0.0425(7) Uani 1 1 d . . . . .
H44 H 0.199310 0.511127 0.984815 0.051 Uiso 1 1 calc R U . . .
C45 C 0.0935(3) 0.53669(19) 1.0671(2) 0.0775(12) Uani 1 1 d . . . . .
H45A H 0.122537 0.560993 1.105933 0.116 Uiso 1 1 calc R U . . .
H45B H 0.029767 0.523366 1.070903 0.116 Uiso 1 1 calc R U . . .
H45C H 0.085928 0.558691 1.025322 0.116 Uiso 1 1 calc R U . . .
C46 C 0.1734(3) 0.4457(2) 1.1228(2) 0.0818(13) Uani 1 1 d . . . . .
H46A H 0.117010 0.420432 1.117025 0.123 Uiso 1 1 calc R U . . .
H46B H 0.182484 0.466743 1.165404 0.123 Uiso 1 1 calc R U . . .
H46C H 0.231360 0.422750 1.123797 0.123 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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 -1 0 0.0932
2 0 -1 0.1643
-2 0 1 0.1563
0 -1 -1 0.0880
0 1 1 0.0410
1 -1 0 0.1659
-17 16 0 0.1416
-1 -22 20 0.0737
1 22 -20 0.0648
-16 9 20 0.1064
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
O1 S1 C1 107.36(12) . . ?
O1 S1 C36 106.83(12) . . ?
O2 S1 O1 116.07(12) . . ?
O2 S1 C1 108.58(13) . . ?
O2 S1 C36 109.63(13) . . ?
C1 S1 C36 108.10(13) . . ?
O3 S2 O4 116.68(13) . . ?
O3 S2 C3 110.65(13) . . ?
O3 S2 C16 110.97(13) . . ?
O4 S2 C3 105.45(13) . . ?
O4 S2 C16 106.01(13) . . ?
C16 S2 C3 106.44(13) . . ?
O5 S3 C12 108.18(13) . . ?
O5 S3 C21 106.42(12) . . ?
O6 S3 O5 116.73(13) . . ?
O6 S3 C12 108.99(13) . . ?
O6 S3 C21 109.03(13) . . ?
C21 S3 C12 107.09(14) . . ?
O7 S4 O8 116.74(12) . . ?
O7 S4 C23 109.28(13) . . ?
O7 S4 C32 110.13(13) . . ?
O8 S4 C23 106.13(13) . . ?
O8 S4 C32 106.24(13) . . ?
C32 S4 C23 107.92(13) . . ?
O9 Al1 O1 86.21(8) . . ?
O9 Al1 O10 93.38(9) . . ?
O9 Al1 O13 94.11(9) . . ?
O9 Al1 O14 91.57(9) . 3_667 ?
O9 Al1 O16 168.08(10) . . ?
O10 Al1 O1 87.84(8) . . ?
O10 Al1 O16 89.57(9) . . ?
O13 Al1 O1 179.26(9) . . ?
O13 Al1 O10 91.48(9) . . ?
O13 Al1 O14 94.38(9) . 3_667 ?
O13 Al1 O16 97.36(9) . . ?
O14 Al1 O1 86.27(9) 3_667 . ?
O14 Al1 O10 172.05(10) 3_667 . ?
O14 Al1 O16 84.36(9) 3_667 . ?
O16 Al1 O1 82.36(9) . . ?
O11 Al2 O5 84.44(8) . . ?
O11 Al2 O12 92.13(9) . . ?
O11 Al2 O14 169.81(10) . . ?
O11 Al2 O15 88.13(9) . . ?
O12 Al2 O5 86.98(8) . . ?
O12 Al2 O15 168.76(10) . . ?
O13 Al2 O5 175.16(9) . . ?
O13 Al2 O11 93.01(9) . . ?
O13 Al2 O12 97.25(9) . . ?
O13 Al2 O14 96.06(9) . . ?
O13 Al2 O15 93.97(9) . . ?
O14 Al2 O5 86.17(9) . . ?
O14 Al2 O12 91.32(9) . . ?
O14 Al2 O15 86.63(10) . . ?
O15 Al2 O5 81.85(9) . . ?
S1 O1 Al1 119.95(11) . . ?
S3 O5 Al2 118.97(11) . . ?
C31 O9 Al1 134.83(17) . . ?
C2 O10 Al1 136.06(18) . . ?
C11 O11 Al2 133.88(18) . . ?
C22 O12 Al2 135.34(18) . . ?
Al1 O13 H13 100(2) . . ?
Al2 O13 Al1 138.42(11) . . ?
Al2 O13 H13 121(2) . . ?
Al1 O14 H14 113(4) 3_667 . ?
Al2 O14 Al1 140.23(12) . 3_667 ?
Al2 O14 H14 107(3) . . ?
C41 O15 Al2 129.9(2) . . ?
C44 O16 Al1 125.7(2) . . ?
C41 N1 C42 120.9(3) . . ?
C41 N1 C43 119.5(4) . . ?
C42 N1 C43 119.6(4) . . ?
C44 N2 C45 120.5(3) . . ?
C44 N2 C46 121.0(3) . . ?
C46 N2 C45 118.1(3) . . ?
C2 C1 S1 117.8(2) . . ?
C6 C1 S1 119.5(2) . . ?
C6 C1 C2 122.8(3) . . ?
O10 C2 C1 122.7(2) . . ?
O10 C2 C3 122.9(3) . . ?
C3 C2 C1 114.4(2) . . ?
C2 C3 S2 122.3(2) . . ?
C4 C3 S2 116.0(2) . . ?
C4 C3 C2 121.7(3) . . ?
C3 C4 H4 118.4 . . ?
C5 C4 C3 123.2(3) . . ?
C5 C4 H4 118.4 . . ?
C4 C5 C6 115.9(3) . . ?
C4 C5 C7 123.0(3) . . ?
C6 C5 C7 121.0(3) . . ?
C1 C6 C5 122.0(3) . . ?
C1 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
C8 C7 C5 111.6(3) . . ?
C8 C7 C9 108.3(3) . . ?
C9 C7 C5 108.0(3) . . ?
C10 C7 C5 109.8(3) . . ?
C10 C7 C8 109.2(3) . . ?
C10 C7 C9 109.9(3) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O11 C11 C12 124.4(3) . . ?
O11 C11 C16 122.0(3) . . ?
C12 C11 C16 113.6(3) . . ?
C11 C12 S3 120.9(2) . . ?
C13 C12 S3 115.8(2) . . ?
C13 C12 C11 123.3(3) . . ?
C12 C13 H13A 119.3 . . ?
C14 C13 C12 121.5(3) . . ?
C14 C13 H13A 119.3 . . ?
C13 C14 C17 121.3(3) . . ?
C15 C14 C13 116.0(3) . . ?
C15 C14 C17 122.6(3) . . ?
C14 C15 H15 118.2 . . ?
C14 C15 C16 123.5(3) . . ?
C16 C15 H15 118.2 . . ?
C11 C16 S2 122.5(2) . . ?
C15 C16 S2 115.5(2) . . ?
C15 C16 C11 122.0(3) . . ?
C14 C17 C18A 111.4(4) . . ?
C18B C17 C14 110.4(5) . . ?
C18B C17 C19B 112.8(7) . . ?
C18B C17 C20B 111.8(8) . . ?
C19A C17 C14 109.2(4) . . ?
C19A C17 C18A 105.1(6) . . ?
C19B C17 C14 110.8(4) . . ?
C20A C17 C14 111.0(5) . . ?
C20A C17 C18A 105.8(7) . . ?
C20A C17 C19A 114.2(7) . . ?
C20B C17 C14 106.1(5) . . ?
C20B C17 C19B 104.7(7) . . ?
C17 C18A H18A 109.5 . . ?
C17 C18A H18B 109.5 . . ?
C17 C18A H18C 109.5 . . ?
H18A C18A H18B 109.5 . . ?
H18A C18A H18C 109.5 . . ?
H18B C18A H18C 109.5 . . ?
C17 C18B H18D 109.5 . . ?
C17 C18B H18E 109.5 . . ?
C17 C18B H18F 109.5 . . ?
H18D C18B H18E 109.5 . . ?
H18D C18B H18F 109.5 . . ?
H18E C18B H18F 109.5 . . ?
C17 C19A H19A 109.5 . . ?
C17 C19A H19B 109.5 . . ?
C17 C19A H19C 109.5 . . ?
H19A C19A H19B 109.5 . . ?
H19A C19A H19C 109.5 . . ?
H19B C19A H19C 109.5 . . ?
C17 C19B H19D 109.5 . . ?
C17 C19B H19E 109.5 . . ?
C17 C19B H19F 109.5 . . ?
H19D C19B H19E 109.5 . . ?
H19D C19B H19F 109.5 . . ?
H19E C19B H19F 109.5 . . ?
C17 C20A H20A 109.5 . . ?
C17 C20A H20B 109.5 . . ?
C17 C20A H20C 109.5 . . ?
H20A C20A H20B 109.5 . . ?
H20A C20A H20C 109.5 . . ?
H20B C20A H20C 109.5 . . ?
C17 C20B H20D 109.5 . . ?
C17 C20B H20E 109.5 . . ?
C17 C20B H20F 109.5 . . ?
H20D C20B H20E 109.5 . . ?
H20D C20B H20F 109.5 . . ?
H20E C20B H20F 109.5 . . ?
C22 C21 S3 117.1(2) . . ?
C26 C21 S3 119.7(2) . . ?
C26 C21 C22 123.2(3) . . ?
O12 C22 C21 121.5(3) . . ?
O12 C22 C23 124.3(3) . . ?
C23 C22 C21 114.2(3) . . ?
C22 C23 S4 121.4(2) . . ?
C24 C23 S4 116.8(2) . . ?
C24 C23 C22 121.6(3) . . ?
C23 C24 H24 118.5 . . ?
C25 C24 C23 123.0(3) . . ?
C25 C24 H24 118.5 . . ?
C24 C25 C27 122.8(3) . . ?
C26 C25 C24 116.2(3) . . ?
C26 C25 C27 121.0(3) . . ?
C21 C26 C25 121.7(3) . . ?
C21 C26 H26 119.2 . . ?
C25 C26 H26 119.2 . . ?
C25 C27 C28A 108.2(4) . . ?
C25 C27 C29B 105.0(5) . . ?
C28B C27 C25 116.1(6) . . ?
C28B C27 C29B 109.6(10) . . ?
C28B C27 C30B 114.6(10) . . ?
C29A C27 C25 106.9(4) . . ?
C29A C27 C28A 107.8(6) . . ?
C30A C27 C25 114.3(4) . . ?
C30A C27 C28A 103.9(6) . . ?
C30A C27 C29A 115.4(6) . . ?
C30B C27 C25 109.3(6) . . ?
C30B C27 C29B 100.7(10) . . ?
C27 C28A H28A 109.5 . . ?
C27 C28A H28B 109.5 . . ?
C27 C28A H28C 109.5 . . ?
H28A C28A H28B 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
C27 C28B H28D 109.5 . . ?
C27 C28B H28E 109.5 . . ?
C27 C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
C27 C29A H29A 109.5 . . ?
C27 C29A H29B 109.5 . . ?
C27 C29A H29C 109.5 . . ?
H29A C29A H29B 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
C27 C29B H29D 109.5 . . ?
C27 C29B H29E 109.5 . . ?
C27 C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?
C27 C30A H30A 109.5 . . ?
C27 C30A H30B 109.5 . . ?
C27 C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C27 C30B H30D 109.5 . . ?
C27 C30B H30E 109.5 . . ?
C27 C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
O9 C31 C32 121.6(2) . . ?
O9 C31 C36 125.1(2) . . ?
C36 C31 C32 113.3(2) . . ?
C31 C32 S4 122.2(2) . . ?
C33 C32 S4 115.6(2) . . ?
C33 C32 C31 122.2(3) . . ?
C32 C33 H33 118.5 . . ?
C32 C33 C34 122.9(3) . . ?
C34 C33 H33 118.5 . . ?
C33 C34 C37 121.0(3) . . ?
C35 C34 C33 116.2(3) . . ?
C35 C34 C37 122.5(3) . . ?
C34 C35 H35 119.0 . . ?
C34 C35 C36 121.9(3) . . ?
C36 C35 H35 119.0 . . ?
C31 C36 S1 120.5(2) . . ?
C35 C36 S1 115.9(2) . . ?
C35 C36 C31 123.4(3) . . ?
C34 C37 C38 110.2(3) . . ?
C39 C37 C34 107.8(3) . . ?
C39 C37 C38 109.1(4) . . ?
C40 C37 C34 112.5(3) . . ?
C40 C37 C38 107.7(4) . . ?
C40 C37 C39 109.6(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
O15 C41 N1 122.9(3) . . ?
O15 C41 H41 118.6 . . ?
N1 C41 H41 118.6 . . ?
N1 C42 H42A 109.5 . . ?
N1 C42 H42B 109.5 . . ?
N1 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N1 C43 H43A 109.5 . . ?
N1 C43 H43B 109.5 . . ?
N1 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O16 C44 N2 122.6(3) . . ?
O16 C44 H44 118.7 . . ?
N2 C44 H44 118.7 . . ?
N2 C45 H45A 109.5 . . ?
N2 C45 H45B 109.5 . . ?
N2 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
N2 C46 H46A 109.5 . . ?
N2 C46 H46B 109.5 . . ?
N2 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
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
S1 O1 1.4648(19) . ?
S1 O2 1.429(2) . ?
S1 C1 1.742(3) . ?
S1 C36 1.755(3) . ?
S2 O3 1.437(2) . ?
S2 O4 1.439(2) . ?
S2 C3 1.779(3) . ?
S2 C16 1.769(3) . ?
S3 O5 1.464(2) . ?
S3 O6 1.429(2) . ?
S3 C12 1.749(3) . ?
S3 C21 1.743(3) . ?
S4 O7 1.429(2) . ?
S4 O8 1.442(2) . ?
S4 C23 1.772(3) . ?
S4 C32 1.766(3) . ?
Al1 O1 2.068(2) . ?
Al1 O9 1.837(2) . ?
Al1 O10 1.8799(19) . ?
Al1 O13 1.848(2) . ?
Al1 O14 1.871(2) 3_667 ?
Al1 O16 1.928(2) . ?
Al2 O5 2.107(2) . ?
Al2 O11 1.8428(19) . ?
Al2 O12 1.881(2) . ?
Al2 O13 1.827(2) . ?
Al2 O14 1.849(2) . ?
Al2 O15 1.927(2) . ?
O9 C31 1.285(3) . ?
O10 C2 1.299(3) . ?
O11 C11 1.287(3) . ?
O12 C22 1.303(3) . ?
O13 H13 0.932(10) . ?
O14 H14 0.942(10) . ?
O15 C41 1.223(4) . ?
O16 C44 1.247(3) . ?
N1 C41 1.318(4) . ?
N1 C42 1.427(5) . ?
N1 C43 1.447(5) . ?
N2 C44 1.314(4) . ?
N2 C45 1.458(4) . ?
N2 C46 1.450(5) . ?
C1 C2 1.421(4) . ?
C1 C6 1.381(4) . ?
C2 C3 1.411(4) . ?
C3 C4 1.387(4) . ?
C4 H4 0.9300 . ?
C4 C5 1.384(4) . ?
C5 C6 1.392(4) . ?
C5 C7 1.538(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.523(5) . ?
C7 C9 1.537(5) . ?
C7 C10 1.521(5) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.420(4) . ?
C11 C16 1.420(4) . ?
C12 C13 1.391(4) . ?
C13 H13A 0.9300 . ?
C13 C14 1.391(4) . ?
C14 C15 1.379(4) . ?
C14 C17 1.537(4) . ?
C15 H15 0.9300 . ?
C15 C16 1.383(4) . ?
C17 C18A 1.539(6) . ?
C17 C18B 1.502(7) . ?
C17 C19A 1.536(6) . ?
C17 C19B 1.536(6) . ?
C17 C20A 1.507(6) . ?
C17 C20B 1.530(7) . ?
C18A H18A 0.9600 . ?
C18A H18B 0.9600 . ?
C18A H18C 0.9600 . ?
C18B H18D 0.9600 . ?
C18B H18E 0.9600 . ?
C18B H18F 0.9600 . ?
C19A H19A 0.9600 . ?
C19A H19B 0.9600 . ?
C19A H19C 0.9600 . ?
C19B H19D 0.9600 . ?
C19B H19E 0.9600 . ?
C19B H19F 0.9600 . ?
C20A H20A 0.9600 . ?
C20A H20B 0.9600 . ?
C20A H20C 0.9600 . ?
C20B H20D 0.9600 . ?
C20B H20E 0.9600 . ?
C20B H20F 0.9600 . ?
C21 C22 1.423(4) . ?
C21 C26 1.378(4) . ?
C22 C23 1.405(4) . ?
C23 C24 1.395(4) . ?
C24 H24 0.9300 . ?
C24 C25 1.386(4) . ?
C25 C26 1.385(4) . ?
C25 C27 1.537(5) . ?
C26 H26 0.9300 . ?
C27 C28A 1.551(6) . ?
C27 C28B 1.497(7) . ?
C27 C29A 1.516(6) . ?
C27 C29B 1.541(7) . ?
C27 C30A 1.496(6) . ?
C27 C30B 1.501(7) . ?
C28A H28A 0.9600 . ?
C28A H28B 0.9600 . ?
C28A H28C 0.9600 . ?
C28B H28D 0.9600 . ?
C28B H28E 0.9600 . ?
C28B H28F 0.9600 . ?
C29A H29A 0.9600 . ?
C29A H29B 0.9600 . ?
C29A H29C 0.9600 . ?
C29B H29D 0.9600 . ?
C29B H29E 0.9600 . ?
C29B H29F 0.9600 . ?
C30A H30A 0.9600 . ?
C30A H30B 0.9600 . ?
C30A H30C 0.9600 . ?
C30B H30D 0.9600 . ?
C30B H30E 0.9600 . ?
C30B H30F 0.9600 . ?
C31 C32 1.432(4) . ?
C31 C36 1.420(4) . ?
C32 C33 1.389(4) . ?
C33 H33 0.9300 . ?
C33 C34 1.390(4) . ?
C34 C35 1.385(4) . ?
C34 C37 1.532(4) . ?
C35 H35 0.9300 . ?
C35 C36 1.392(4) . ?
C37 C38 1.536(6) . ?
C37 C39 1.518(6) . ?
C37 C40 1.511(5) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41 0.9300 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44 0.9300 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
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
S1 C1 C2 O10 2.8(4) . . . . ?
S1 C1 C2 C3 -178.6(2) . . . . ?
S1 C1 C6 C5 179.8(2) . . . . ?
S2 C3 C4 C5 -179.8(3) . . . . ?
S3 C12 C13 C14 -179.6(2) . . . . ?
S3 C21 C22 O12 2.5(4) . . . . ?
S3 C21 C22 C23 -179.2(2) . . . . ?
S3 C21 C26 C25 -179.7(3) . . . . ?
S4 C23 C24 C25 -174.2(3) . . . . ?
S4 C32 C33 C34 176.8(2) . . . . ?
Al1 O9 C31 C32 169.40(19) . . . . ?
Al1 O9 C31 C36 -11.7(4) . . . . ?
Al1 O10 C2 C1 -30.7(4) . . . . ?
Al1 O10 C2 C3 150.8(2) . . . . ?
Al1 O16 C44 N2 -169.9(2) . . . . ?
Al2 O11 C11 C12 -23.1(4) . . . . ?
Al2 O11 C11 C16 159.8(2) . . . . ?
Al2 O12 C22 C21 -39.7(4) . . . . ?
Al2 O12 C22 C23 142.1(2) . . . . ?
Al2 O15 C41 N1 -176.4(2) . . . . ?
O1 S1 C1 C2 40.4(3) . . . . ?
O1 S1 C1 C6 -140.0(2) . . . . ?
O1 S1 C36 C31 -22.7(2) . . . . ?
O1 S1 C36 C35 154.0(2) . . . . ?
O1 Al1 O9 C31 32.5(2) . . . . ?
O1 Al1 O10 C2 11.7(3) . . . . ?
O2 S1 O1 Al1 177.79(11) . . . . ?
O2 S1 C1 C2 166.6(2) . . . . ?
O2 S1 C1 C6 -13.8(3) . . . . ?
O2 S1 C36 C31 -149.2(2) . . . . ?
O2 S1 C36 C35 27.4(3) . . . . ?
O3 S2 C3 C2 -48.9(3) . . . . ?
O3 S2 C3 C4 132.5(2) . . . . ?
O3 S2 C16 C11 26.4(3) . . . . ?
O3 S2 C16 C15 -150.7(2) . . . . ?
O4 S2 C3 C2 -175.9(2) . . . . ?
O4 S2 C3 C4 5.5(3) . . . . ?
O4 S2 C16 C11 154.0(2) . . . . ?
O4 S2 C16 C15 -23.1(3) . . . . ?
O5 S3 C12 C11 -18.6(3) . . . . ?
O5 S3 C12 C13 160.8(2) . . . . ?
O5 S3 C21 C22 45.4(2) . . . . ?
O5 S3 C21 C26 -136.5(2) . . . . ?
O5 Al2 O11 C11 43.1(2) . . . . ?
O5 Al2 O12 C22 21.1(2) . . . . ?
O5 Al2 O14 Al1 167.89(19) . . . 3_667 ?
O6 S3 O5 Al2 175.60(12) . . . . ?
O6 S3 C12 C11 -146.5(2) . . . . ?
O6 S3 C12 C13 33.0(3) . . . . ?
O6 S3 C21 C22 172.1(2) . . . . ?
O6 S3 C21 C26 -9.8(3) . . . . ?
O7 S4 C23 C22 -46.0(3) . . . . ?
O7 S4 C23 C24 129.8(2) . . . . ?
O7 S4 C32 C31 27.8(3) . . . . ?
O7 S4 C32 C33 -148.8(2) . . . . ?
O8 S4 C23 C22 -172.7(2) . . . . ?
O8 S4 C23 C24 3.1(3) . . . . ?
O8 S4 C32 C31 155.1(2) . . . . ?
O8 S4 C32 C33 -21.5(3) . . . . ?
O9 Al1 O10 C2 97.7(3) . . . . ?
O9 Al1 O13 Al2 46.14(17) . . . . ?
O9 C31 C32 S4 1.7(4) . . . . ?
O9 C31 C32 C33 178.1(3) . . . . ?
O9 C31 C36 S1 -1.2(4) . . . . ?
O9 C31 C36 C35 -177.5(3) . . . . ?
O10 Al1 O9 C31 -55.1(3) . . . . ?
O10 Al1 O13 Al2 -47.35(17) . . . . ?
O10 C2 C3 S2 -2.2(4) . . . . ?
O10 C2 C3 C4 176.4(3) . . . . ?
O11 Al2 O12 C22 105.4(2) . . . . ?
O11 Al2 O13 Al1 63.53(17) . . . . ?
O11 Al2 O14 Al1 145.0(5) . . . 3_667 ?
O11 C11 C12 S3 0.1(4) . . . . ?
O11 C11 C12 C13 -179.3(3) . . . . ?
O11 C11 C16 S2 2.9(4) . . . . ?
O11 C11 C16 C15 179.8(3) . . . . ?
O12 Al2 O11 C11 -43.6(3) . . . . ?
O12 Al2 O13 Al1 -29.00(17) . . . . ?
O12 Al2 O14 Al1 -105.23(19) . . . 3_667 ?
O12 C22 C23 S4 -8.9(4) . . . . ?
O12 C22 C23 C24 175.6(3) . . . . ?
O13 Al1 O9 C31 -146.8(2) . . . . ?
O13 Al1 O10 C2 -168.1(3) . . . . ?
O13 Al2 O11 C11 -141.0(2) . . . . ?
O13 Al2 O12 C22 -161.3(2) . . . . ?
O13 Al2 O14 Al1 -7.8(2) . . . 3_667 ?
O14 Al1 O9 C31 118.6(2) 3_667 . . . ?
O14 Al1 O13 Al2 138.03(16) 3_667 . . . ?
O14 Al2 O11 C11 66.1(7) . . . . ?
O14 Al2 O12 C22 -65.0(3) . . . . ?
O14 Al2 O13 Al1 -121.12(16) . . . . ?
O15 Al2 O11 C11 125.1(3) . . . . ?
O15 Al2 O12 C22 14.3(6) . . . . ?
O15 Al2 O13 Al1 151.86(16) . . . . ?
O15 Al2 O14 Al1 85.8(2) . . . 3_667 ?
O16 Al1 O9 C31 48.9(6) . . . . ?
O16 Al1 O10 C2 -70.7(3) . . . . ?
O16 Al1 O13 Al2 -137.11(16) . . . . ?
C1 S1 O1 Al1 -60.57(16) . . . . ?
C1 S1 C36 C31 92.6(2) . . . . ?
C1 S1 C36 C35 -90.8(2) . . . . ?
C1 C2 C3 S2 179.1(2) . . . . ?
C1 C2 C3 C4 -2.3(4) . . . . ?
C2 C1 C6 C5 -0.6(5) . . . . ?
C2 C3 C4 C5 1.6(5) . . . . ?
C3 S2 C16 C11 -94.1(2) . . . . ?
C3 S2 C16 C15 88.9(2) . . . . ?
C3 C4 C5 C6 -0.2(5) . . . . ?
C3 C4 C5 C7 -179.6(3) . . . . ?
C4 C5 C6 C1 -0.3(4) . . . . ?
C4 C5 C7 C8 -0.7(5) . . . . ?
C4 C5 C7 C9 118.3(3) . . . . ?
C4 C5 C7 C10 -121.8(4) . . . . ?
C6 C1 C2 O10 -176.8(3) . . . . ?
C6 C1 C2 C3 1.9(4) . . . . ?
C6 C5 C7 C8 180.0(3) . . . . ?
C6 C5 C7 C9 -61.0(4) . . . . ?
C6 C5 C7 C10 58.8(4) . . . . ?
C7 C5 C6 C1 179.1(3) . . . . ?
C11 C12 C13 C14 -0.2(5) . . . . ?
C12 S3 O5 Al2 52.32(16) . . . . ?
C12 S3 C21 C22 -70.1(2) . . . . ?
C12 S3 C21 C26 108.0(3) . . . . ?
C12 C11 C16 S2 -174.5(2) . . . . ?
C12 C11 C16 C15 2.4(4) . . . . ?
C12 C13 C14 C15 2.1(5) . . . . ?
C12 C13 C14 C17 -179.1(3) . . . . ?
C13 C14 C15 C16 -1.7(5) . . . . ?
C13 C14 C17 C18A -178.3(6) . . . . ?
C13 C14 C17 C18B 134.2(8) . . . . ?
C13 C14 C17 C19A 66.1(7) . . . . ?
C13 C14 C17 C19B 8.5(7) . . . . ?
C13 C14 C17 C20A -60.7(8) . . . . ?
C13 C14 C17 C20B -104.6(7) . . . . ?
C14 C15 C16 S2 176.5(3) . . . . ?
C14 C15 C16 C11 -0.6(5) . . . . ?
C15 C14 C17 C18A 0.5(7) . . . . ?
C15 C14 C17 C18B -47.0(9) . . . . ?
C15 C14 C17 C19A -115.1(6) . . . . ?
C15 C14 C17 C19B -172.7(6) . . . . ?
C15 C14 C17 C20A 118.1(7) . . . . ?
C15 C14 C17 C20B 74.2(7) . . . . ?
C16 S2 C3 C2 71.8(3) . . . . ?
C16 S2 C3 C4 -106.9(2) . . . . ?
C16 C11 C12 S3 177.4(2) . . . . ?
C16 C11 C12 C13 -2.0(4) . . . . ?
C17 C14 C15 C16 179.5(3) . . . . ?
C21 S3 O5 Al2 -62.46(15) . . . . ?
C21 S3 C12 C11 95.7(2) . . . . ?
C21 S3 C12 C13 -84.9(2) . . . . ?
C21 C22 C23 S4 172.8(2) . . . . ?
C21 C22 C23 C24 -2.7(4) . . . . ?
C22 C21 C26 C25 -1.7(5) . . . . ?
C22 C23 C24 C25 1.6(5) . . . . ?
C23 S4 C32 C31 -91.4(2) . . . . ?
C23 S4 C32 C33 91.9(2) . . . . ?
C23 C24 C25 C26 -0.3(5) . . . . ?
C23 C24 C25 C27 178.3(3) . . . . ?
C24 C25 C26 C21 0.3(5) . . . . ?
C24 C25 C27 C28A -121.8(5) . . . . ?
C24 C25 C27 C28B 171.5(10) . . . . ?
C24 C25 C27 C29A 122.3(6) . . . . ?
C24 C25 C27 C29B 50.3(8) . . . . ?
C24 C25 C27 C30A -6.7(7) . . . . ?
C24 C25 C27 C30B -57.0(10) . . . . ?
C26 C21 C22 O12 -175.5(3) . . . . ?
C26 C21 C22 C23 2.8(4) . . . . ?
C26 C25 C27 C28A 56.6(6) . . . . ?
C26 C25 C27 C28B -10.1(11) . . . . ?
C26 C25 C27 C29A -59.3(6) . . . . ?
C26 C25 C27 C29B -131.3(7) . . . . ?
C26 C25 C27 C30A 171.8(6) . . . . ?
C26 C25 C27 C30B 121.4(9) . . . . ?
C27 C25 C26 C21 -178.2(3) . . . . ?
C31 C32 C33 C34 0.2(5) . . . . ?
C32 S4 C23 C22 73.7(3) . . . . ?
C32 S4 C23 C24 -110.5(2) . . . . ?
C32 C31 C36 S1 177.80(19) . . . . ?
C32 C31 C36 C35 1.5(4) . . . . ?
C32 C33 C34 C35 0.0(5) . . . . ?
C32 C33 C34 C37 -174.4(3) . . . . ?
C33 C34 C35 C36 0.5(5) . . . . ?
C33 C34 C37 C38 -43.7(5) . . . . ?
C33 C34 C37 C39 75.2(5) . . . . ?
C33 C34 C37 C40 -163.9(4) . . . . ?
C34 C35 C36 S1 -177.8(2) . . . . ?
C34 C35 C36 C31 -1.3(5) . . . . ?
C35 C34 C37 C38 142.2(4) . . . . ?
C35 C34 C37 C39 -98.8(5) . . . . ?
C35 C34 C37 C40 22.0(5) . . . . ?
C36 S1 O1 Al1 55.19(15) . . . . ?
C36 S1 C1 C2 -74.5(2) . . . . ?
C36 S1 C1 C6 105.1(2) . . . . ?
C36 C31 C32 S4 -177.3(2) . . . . ?
C36 C31 C32 C33 -0.9(4) . . . . ?
C37 C34 C35 C36 174.8(3) . . . . ?
C42 N1 C41 O15 0.5(6) . . . . ?
C43 N1 C41 O15 -177.2(4) . . . . ?
C45 N2 C44 O16 177.1(3) . . . . ?
C46 N2 C44 O16 4.9(5) . . . . ?
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 -1.0000 -0.0000 -0.0045 -0.0233 0.0199
2.0000 0.0000 -1.0000 0.0116 0.0647 0.0783
-2.0000 -0.0000 1.0000 -0.0116 -0.0647 -0.0783
0.0000 -1.0000 -1.0000 0.0316 -0.0277 0.0230
-0.0000 1.0000 1.0000 -0.0316 0.0277 -0.0230
1.0000 -1.0000 0.0000 -0.0168 0.0112 0.0575
-17.0000 16.0000 -0.0000 0.2815 -0.2145 -0.9574
-1.0000 -22.0000 20.0000 -0.8112 -0.4590 0.3371
1.0000 22.0000 -20.0000 0.8112 0.4590 -0.3371
-16.0000 9.0000 20.0000 -0.4862 -0.2552 -0.8434
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.384 0.000 0.000 788.6 147.3 ?
2 -0.519 0.500 0.500 788.6 147.3 ?
