#------------------------------------------------------------------------------
#$Date: 2022-09-05 09:17:02 +0300 (Mon, 05 Sep 2022) $
#$Revision: 277625 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/75/1567581.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_1567581
loop_
_publ_author_name
'Théry, Valentin'
'Molton, Florian'
'Sirach, Selim'
'Tillet, Neven'
'Pécaut, Jacques'
'Tomás-Mendivil, Eder'
'Martin, David'
_publ_section_title
;
 The curious case of a sterically crowded Stenhouse salt
;
_journal_issue                   33
_journal_name_full               'Chemical Science'
_journal_page_first              9755
_journal_page_last               9760
_journal_paper_doi               10.1039/D2SC01895K
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'Cl, C53 H77 N2 O, H2 O'
_chemical_formula_sum            'C53 H79 Cl N2 O2'
_chemical_formula_weight         811.63
_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   mixed
_audit_creation_date             2022-02-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-07-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.607(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0058(6)
_cell_length_b                   18.6532(8)
_cell_length_c                   20.2559(8)
_cell_measurement_reflns_used    2088
_cell_measurement_temperature    150.3(5)
_cell_measurement_theta_max      24.4110
_cell_measurement_theta_min      2.4990
_cell_volume                     4683.9(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.3(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9653
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00 101.00   1.00  120.00    --   25.25 178.00 -30.00   62
  2  ω    -48.00  69.00   1.00  120.00    --   25.25 -19.00 -30.00  117
  3  ω   -103.00 -39.00   1.00  120.00    --  -27.12-178.00 -90.00   64
  4  ω      4.00  29.00   1.00  120.00    --   25.25  57.00   0.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0185569000
_diffrn_orient_matrix_UB_12      0.0353530000
_diffrn_orient_matrix_UB_13      0.0024136000
_diffrn_orient_matrix_UB_21      -0.0426662000
_diffrn_orient_matrix_UB_22      -0.0053110000
_diffrn_orient_matrix_UB_23      -0.0311415000
_diffrn_orient_matrix_UB_31      -0.0333100000
_diffrn_orient_matrix_UB_32      -0.0129191000
_diffrn_orient_matrix_UB_33      0.0193822000
_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  0.1072
_diffrn_reflns_av_unetI/netI     0.1931
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22574
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.972
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.123
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.997
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
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            'translucent intense violet'
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       needle
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         9580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.1626
_refine_ls_R_factor_gt           0.0640
_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)+(0.0141P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4449
_reflns_number_total             9580
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2sc01895k2.cif
_cod_data_source_block           1HCl
_cod_database_code               1567581
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C50 H70 N4 O1 Cl'
_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   0.994
_shelx_estimated_absorpt_t_min   0.968
_reflns_odcompleteness_completeness 67.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1.a Free rotating group:
 O1W(H1WA,H1WB)
1.b Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C48(H48), C51(H51)
1.c Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C10(H10A,H10B), C26(H26A,H26B), C28(H28A,H28B), C36(H36A,H36B),
 C38(H38A,H38B)
1.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C14(H14), C15(H15), C16(H16), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C44(H44), C45(H45), C46(H46)
1.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,
 H29B,H29C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C)
;
_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 1.128
_oxdiff_exptl_absorpt_empirical_full_min 0.902
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
Cl1 Cl 0.65081(7) 0.83897(5) 0.75927(4) 0.0287(2) Uani 1 1 d . . . . .
O1 O 0.76673(18) 0.69147(13) 0.76089(11) 0.0213(6) Uani 1 1 d . . . . .
H1 H 0.727(3) 0.7319(18) 0.7578(16) 0.030(11) Uiso 1 1 d . . . . .
N1 N 0.4992(2) 0.77384(14) 0.54803(12) 0.0155(6) Uani 1 1 d . . . . .
N2 N 0.9551(2) 0.63348(15) 0.74790(13) 0.0198(7) Uani 1 1 d . . . . .
C1 C 0.4894(3) 0.72772(17) 0.59818(15) 0.0151(7) Uani 1 1 d . . . . .
C2 C 0.5706(2) 0.68705(17) 0.64226(15) 0.0154(7) Uani 1 1 d . . . . .
C3 C 0.6789(2) 0.68080(17) 0.63928(16) 0.0174(8) Uani 1 1 d . . . . .
H3 H 0.689570 0.682817 0.594940 0.021 Uiso 1 1 calc R U . . .
C4 C 0.7693(3) 0.67202(18) 0.69632(15) 0.0178(8) Uani 1 1 d . . . . .
C5 C 0.8683(3) 0.64262(18) 0.69288(16) 0.0193(8) Uani 1 1 d . . . . .
C6 C 0.3717(2) 0.73333(18) 0.60234(15) 0.0181(8) Uani 1 1 d . . . . .
C7 C 0.3176(3) 0.77664(19) 0.53709(15) 0.0213(8) Uani 1 1 d . . . . .
H7A H 0.285800 0.744111 0.497551 0.026 Uiso 1 1 calc R U . . .
H7B H 0.259343 0.806872 0.544308 0.026 Uiso 1 1 calc R U . . .
C8 C 0.4032(3) 0.82286(19) 0.52267(15) 0.0209(8) Uani 1 1 d . . . . .
C9 C 0.8896(3) 0.61428(19) 0.62716(16) 0.0230(8) Uani 1 1 d . . . . .
C10 C 0.9991(3) 0.5757(2) 0.65587(17) 0.0312(10) Uani 1 1 d . . . . .
H10A H 0.987988 0.523191 0.654590 0.037 Uiso 1 1 calc R U . . .
H10B H 1.046277 0.587465 0.627127 0.037 Uiso 1 1 calc R U . . .
C11 C 1.0519(3) 0.6002(2) 0.73031(17) 0.0231(8) Uani 1 1 d . . . . .
C12 C 0.5821(3) 0.77397(18) 0.51380(15) 0.0167(8) Uani 1 1 d . . . . .
C13 C 0.6643(3) 0.82553(18) 0.53052(15) 0.0205(8) Uani 1 1 d . . . . .
C14 C 0.7335(3) 0.8288(2) 0.48949(16) 0.0272(9) Uani 1 1 d . . . . .
H14 H 0.788072 0.864515 0.498980 0.033 Uiso 1 1 calc R U . . .
C15 C 0.7248(3) 0.7817(2) 0.43586(16) 0.0256(9) Uani 1 1 d . . . . .
H15 H 0.772459 0.785231 0.408519 0.031 Uiso 1 1 calc R U . . .
C16 C 0.6468(3) 0.72982(19) 0.42221(16) 0.0240(8) Uani 1 1 d . . . . .
H16 H 0.643256 0.696040 0.386483 0.029 Uiso 1 1 calc R U . . .
C17 C 0.5721(3) 0.72504(18) 0.45941(15) 0.0188(8) Uani 1 1 d . . . . .
C18 C 0.6858(3) 0.87607(19) 0.59144(16) 0.0258(9) Uani 1 1 d . . . . .
H18 H 0.629490 0.867826 0.614999 0.031 Uiso 1 1 calc R U . . .
C19 C 0.6803(3) 0.95476(19) 0.56917(18) 0.0353(10) Uani 1 1 d . . . . .
H19A H 0.680382 0.985489 0.608422 0.053 Uiso 1 1 calc R U . . .
H19B H 0.614075 0.962941 0.531014 0.053 Uiso 1 1 calc R U . . .
H19C H 0.743025 0.966213 0.553826 0.053 Uiso 1 1 calc R U . . .
C20 C 0.7962(3) 0.8604(2) 0.64343(16) 0.0302(9) Uani 1 1 d . . . . .
H20A H 0.852800 0.869586 0.621726 0.045 Uiso 1 1 calc R U . . .
H20B H 0.799251 0.810088 0.657865 0.045 Uiso 1 1 calc R U . . .
H20C H 0.807251 0.891446 0.684010 0.045 Uiso 1 1 calc R U . . .
C21 C 0.4858(3) 0.66807(18) 0.43807(15) 0.0196(8) Uani 1 1 d . . . . .
H21 H 0.429779 0.679088 0.461241 0.024 Uiso 1 1 calc R U . . .
C22 C 0.5299(3) 0.59322(18) 0.46104(16) 0.0282(9) Uani 1 1 d . . . . .
H22A H 0.587131 0.581766 0.440475 0.042 Uiso 1 1 calc R U . . .
H22B H 0.471641 0.557978 0.445729 0.042 Uiso 1 1 calc R U . . .
H22C H 0.559274 0.591885 0.511644 0.042 Uiso 1 1 calc R U . . .
C23 C 0.4299(3) 0.66778(19) 0.35925(15) 0.0260(9) Uani 1 1 d . . . . .
H23A H 0.404022 0.716156 0.343964 0.039 Uiso 1 1 calc R U . . .
H23B H 0.368694 0.634536 0.348285 0.039 Uiso 1 1 calc R U . . .
H23C H 0.481419 0.652456 0.335389 0.039 Uiso 1 1 calc R U . . .
C24 C 0.4196(3) 0.89320(18) 0.56311(16) 0.0277(9) Uani 1 1 d . . . . .
H24A H 0.447238 0.883039 0.612830 0.042 Uiso 1 1 calc R U . . .
H24B H 0.350591 0.918545 0.553140 0.042 Uiso 1 1 calc R U . . .
H24C H 0.471526 0.923159 0.549313 0.042 Uiso 1 1 calc R U . . .
C25 C 0.3776(3) 0.84134(19) 0.44604(15) 0.0286(9) Uani 1 1 d . . . . .
H25A H 0.435766 0.870933 0.439088 0.043 Uiso 1 1 calc R U . . .
H25B H 0.309502 0.867887 0.430779 0.043 Uiso 1 1 calc R U . . .
H25C H 0.371225 0.797081 0.419030 0.043 Uiso 1 1 calc R U . . .
C26 C 0.3111(3) 0.66224(18) 0.60091(16) 0.0228(8) Uani 1 1 d . . . . .
H26A H 0.343865 0.637647 0.645667 0.027 Uiso 1 1 calc R U . . .
H26B H 0.235701 0.673823 0.598295 0.027 Uiso 1 1 calc R U . . .
C27 C 0.3081(3) 0.60889(19) 0.54283(16) 0.0319(9) Uani 1 1 d . . . . .
H27A H 0.273874 0.631474 0.497858 0.048 Uiso 1 1 calc R U . . .
H27B H 0.266731 0.566420 0.547793 0.048 Uiso 1 1 calc R U . . .
H27C H 0.381898 0.594659 0.545709 0.048 Uiso 1 1 calc R U . . .
C28 C 0.3709(2) 0.77326(18) 0.66998(15) 0.0215(8) Uani 1 1 d . . . . .
H28A H 0.382188 0.737480 0.707607 0.026 Uiso 1 1 calc R U . . .
H28B H 0.432909 0.806711 0.683090 0.026 Uiso 1 1 calc R U . . .
C29 C 0.2692(3) 0.8153(2) 0.66572(17) 0.0314(10) Uani 1 1 d . . . . .
H29A H 0.265911 0.857967 0.636969 0.047 Uiso 1 1 calc R U . . .
H29B H 0.269969 0.829846 0.712357 0.047 Uiso 1 1 calc R U . . .
H29C H 0.205869 0.785115 0.645079 0.047 Uiso 1 1 calc R U . . .
C30 C 0.5458(2) 0.63853(18) 0.69526(15) 0.0164(8) Uani 1 1 d . . . . .
C31 C 0.5283(3) 0.56614(19) 0.67943(17) 0.0242(9) Uani 1 1 d . . . . .
H31 H 0.536568 0.548578 0.637316 0.029 Uiso 1 1 calc R U . . .
C32 C 0.4991(3) 0.5190(2) 0.72341(18) 0.0308(9) Uani 1 1 d . . . . .
H32 H 0.486643 0.469917 0.711109 0.037 Uiso 1 1 calc R U . . .
C33 C 0.4881(3) 0.5435(2) 0.78496(19) 0.0360(10) Uani 1 1 d . . . . .
H33 H 0.465270 0.511933 0.814581 0.043 Uiso 1 1 calc R U . . .
C34 C 0.5105(3) 0.6140(2) 0.80320(17) 0.0303(10) Uani 1 1 d . . . . .
H34 H 0.506311 0.630516 0.846686 0.036 Uiso 1 1 calc R U . . .
C35 C 0.5392(2) 0.66168(19) 0.75906(15) 0.0211(8) Uani 1 1 d . . . . .
H35 H 0.554373 0.710271 0.772546 0.025 Uiso 1 1 calc R U . . .
C36 C 0.8060(3) 0.55949(19) 0.58613(16) 0.0281(9) Uani 1 1 d . . . . .
H36A H 0.740666 0.585893 0.559313 0.034 Uiso 1 1 calc R U . . .
H36B H 0.835824 0.535241 0.552479 0.034 Uiso 1 1 calc R U . . .
C37 C 0.7721(3) 0.5021(2) 0.62934(19) 0.0398(10) Uani 1 1 d . . . . .
H37A H 0.722839 0.468100 0.598465 0.060 Uiso 1 1 calc R U . . .
H37B H 0.735636 0.524820 0.659707 0.060 Uiso 1 1 calc R U . . .
H37C H 0.836174 0.476445 0.657517 0.060 Uiso 1 1 calc R U . . .
C38 C 0.8988(3) 0.6788(2) 0.58072(17) 0.0330(10) Uani 1 1 d . . . . .
H38A H 0.830021 0.705845 0.567720 0.040 Uiso 1 1 calc R U . . .
H38B H 0.956375 0.711419 0.607571 0.040 Uiso 1 1 calc R U . . .
C39 C 0.9242(3) 0.6553(3) 0.51416(19) 0.0622(15) Uani 1 1 d . . . . .
H39A H 0.931988 0.697846 0.487631 0.093 Uiso 1 1 calc R U . . .
H39B H 0.865301 0.625415 0.485964 0.093 Uiso 1 1 calc R U . . .
H39C H 0.991607 0.627839 0.526678 0.093 Uiso 1 1 calc R U . . .
C40 C 1.1386(3) 0.6562(2) 0.73593(19) 0.0404(11) Uani 1 1 d . . . . .
H40A H 1.107594 0.697261 0.706450 0.061 Uiso 1 1 calc R U . . .
H40B H 1.196949 0.635424 0.720837 0.061 Uiso 1 1 calc R U . . .
H40C H 1.167242 0.672071 0.784151 0.061 Uiso 1 1 calc R U . . .
C41 C 1.1008(3) 0.5382(2) 0.77759(18) 0.0389(11) Uani 1 1 d . . . . .
H41A H 1.128635 0.555494 0.825401 0.058 Uiso 1 1 calc R U . . .
H41B H 1.159886 0.517389 0.763318 0.058 Uiso 1 1 calc R U . . .
H41C H 1.045446 0.501690 0.774674 0.058 Uiso 1 1 calc R U . . .
C42 C 0.9695(3) 0.64764(19) 0.82093(16) 0.0203(8) Uani 1 1 d . . . . .
C43 C 0.9448(3) 0.59273(19) 0.86065(17) 0.0223(8) Uani 1 1 d . . . . .
C44 C 0.9733(3) 0.6025(2) 0.93195(17) 0.0299(9) Uani 1 1 d . . . . .
H44 H 0.957542 0.565987 0.960100 0.036 Uiso 1 1 calc R U . . .
C45 C 1.0238(3) 0.6641(2) 0.96245(17) 0.0316(10) Uani 1 1 d . . . . .
H45 H 1.045192 0.669090 1.011410 0.038 Uiso 1 1 calc R U . . .
C46 C 1.0435(3) 0.7185(2) 0.92231(16) 0.0266(9) Uani 1 1 d . . . . .
H46 H 1.077013 0.761232 0.943906 0.032 Uiso 1 1 calc R U . . .
C47 C 1.0153(3) 0.71225(19) 0.85032(16) 0.0214(8) Uani 1 1 d . . . . .
C48 C 0.8842(3) 0.52489(19) 0.83052(17) 0.0263(9) Uani 1 1 d . . . . .
H48 H 0.883248 0.521399 0.781070 0.032 Uiso 1 1 calc R U . . .
C49 C 0.7675(3) 0.5286(2) 0.83152(18) 0.0363(10) Uani 1 1 d . . . . .
H49A H 0.728533 0.485839 0.808954 0.054 Uiso 1 1 calc R U . . .
H49B H 0.732932 0.571516 0.806668 0.054 Uiso 1 1 calc R U . . .
H49C H 0.766006 0.530683 0.879562 0.054 Uiso 1 1 calc R U . . .
C50 C 0.9381(3) 0.45682(19) 0.86782(18) 0.0331(10) Uani 1 1 d . . . . .
H50A H 1.015821 0.458764 0.874165 0.050 Uiso 1 1 calc R U . . .
H50B H 0.907145 0.414685 0.839988 0.050 Uiso 1 1 calc R U . . .
H50C H 0.925830 0.453528 0.913127 0.050 Uiso 1 1 calc R U . . .
C51 C 1.0264(3) 0.77906(19) 0.80914(17) 0.0261(9) Uani 1 1 d . . . . .
H51 H 1.004906 0.766202 0.758875 0.031 Uiso 1 1 calc R U . . .
C52 C 0.9500(3) 0.83704(19) 0.81941(17) 0.0339(9) Uani 1 1 d . . . . .
H52A H 0.970070 0.850377 0.868465 0.051 Uiso 1 1 calc R U . . .
H52B H 0.875847 0.818765 0.804675 0.051 Uiso 1 1 calc R U . . .
H52C H 0.954864 0.879235 0.791694 0.051 Uiso 1 1 calc R U . . .
C53 C 1.1415(3) 0.8084(2) 0.83002(18) 0.0372(10) Uani 1 1 d . . . . .
H53A H 1.146271 0.847038 0.798312 0.056 Uiso 1 1 calc R U . . .
H53B H 1.191503 0.769866 0.827721 0.056 Uiso 1 1 calc R U . . .
H53C H 1.160401 0.827066 0.877403 0.056 Uiso 1 1 calc R U . . .
O1W O 0.7670(3) 0.97602(18) 0.84409(19) 0.0835(12) Uani 1 1 d G . . . .
H1WA H 0.812488 0.970173 0.885143 0.125 Uiso 1 1 d G U . . .
H1WB H 0.737929 0.934982 0.828443 0.125 Uiso 1 1 d G 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'
Cl Cl 0.1484 0.1585 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 1 0 0.0211
1 -1 0 0.0311
-1 -1 0 0.0197
1 1 0 0.0267
0 0 -1 0.1251
0 0 1 0.1181
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
C4 O1 H1 109.5(19) . . ?
C1 N1 C8 112.4(2) . . ?
C1 N1 C12 127.4(3) . . ?
C12 N1 C8 119.7(2) . . ?
C5 N2 C11 113.7(2) . . ?
C5 N2 C42 129.8(3) . . ?
C42 N2 C11 116.4(2) . . ?
N1 C1 C2 126.8(3) . . ?
N1 C1 C6 108.1(3) . . ?
C2 C1 C6 124.8(3) . . ?
C1 C2 C3 125.8(3) . . ?
C1 C2 C30 120.1(3) . . ?
C3 C2 C30 113.9(3) . . ?
C2 C3 H3 117.6 . . ?
C4 C3 C2 124.8(3) . . ?
C4 C3 H3 117.6 . . ?
O1 C4 C3 120.4(3) . . ?
O1 C4 C5 115.7(3) . . ?
C3 C4 C5 123.9(3) . . ?
N2 C5 C4 123.9(3) . . ?
N2 C5 C9 110.6(3) . . ?
C4 C5 C9 125.5(3) . . ?
C1 C6 C28 110.2(3) . . ?
C7 C6 C1 101.0(2) . . ?
C7 C6 C26 109.9(3) . . ?
C7 C6 C28 112.6(3) . . ?
C26 C6 C1 116.5(3) . . ?
C26 C6 C28 106.8(2) . . ?
C6 C7 H7A 110.3 . . ?
C6 C7 H7B 110.3 . . ?
H7A C7 H7B 108.5 . . ?
C8 C7 C6 107.3(3) . . ?
C8 C7 H7A 110.3 . . ?
C8 C7 H7B 110.3 . . ?
N1 C8 C24 111.8(3) . . ?
N1 C8 C25 112.8(2) . . ?
C7 C8 N1 99.9(2) . . ?
C7 C8 C24 112.3(3) . . ?
C7 C8 C25 112.4(3) . . ?
C25 C8 C24 107.7(3) . . ?
C5 C9 C10 102.8(3) . . ?
C5 C9 C36 114.4(3) . . ?
C5 C9 C38 109.0(3) . . ?
C10 C9 C38 111.0(3) . . ?
C36 C9 C10 108.3(3) . . ?
C36 C9 C38 111.0(3) . . ?
C9 C10 H10A 109.9 . . ?
C9 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
C11 C10 C9 108.7(3) . . ?
C11 C10 H10A 109.9 . . ?
C11 C10 H10B 109.9 . . ?
C10 C11 N2 101.2(2) . . ?
C40 C11 N2 110.3(3) . . ?
C40 C11 C10 112.5(3) . . ?
C41 C11 N2 112.2(3) . . ?
C41 C11 C10 112.0(3) . . ?
C41 C11 C40 108.6(3) . . ?
C13 C12 N1 120.6(3) . . ?
C13 C12 C17 121.2(3) . . ?
C17 C12 N1 117.9(3) . . ?
C12 C13 C18 124.4(3) . . ?
C14 C13 C12 117.8(3) . . ?
C14 C13 C18 117.7(3) . . ?
C13 C14 H14 119.1 . . ?
C15 C14 C13 121.9(3) . . ?
C15 C14 H14 119.1 . . ?
C14 C15 H15 120.3 . . ?
C16 C15 C14 119.3(3) . . ?
C16 C15 H15 120.3 . . ?
C15 C16 H16 119.0 . . ?
C15 C16 C17 121.9(3) . . ?
C17 C16 H16 119.0 . . ?
C12 C17 C21 124.5(3) . . ?
C16 C17 C12 117.7(3) . . ?
C16 C17 C21 117.8(3) . . ?
C13 C18 H18 108.2 . . ?
C13 C18 C19 112.2(3) . . ?
C13 C18 C20 110.3(3) . . ?
C19 C18 H18 108.2 . . ?
C20 C18 H18 108.2 . . ?
C20 C18 C19 109.7(3) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C17 C21 H21 107.7 . . ?
C17 C21 C22 112.2(3) . . ?
C17 C21 C23 112.1(3) . . ?
C22 C21 H21 107.7 . . ?
C22 C21 C23 109.2(3) . . ?
C23 C21 H21 107.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C8 C24 H24A 109.5 . . ?
C8 C24 H24B 109.5 . . ?
C8 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C8 C25 H25A 109.5 . . ?
C8 C25 H25B 109.5 . . ?
C8 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C6 C26 H26A 107.8 . . ?
C6 C26 H26B 107.8 . . ?
H26A C26 H26B 107.2 . . ?
C27 C26 C6 117.9(2) . . ?
C27 C26 H26A 107.8 . . ?
C27 C26 H26B 107.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C6 C28 H28A 108.4 . . ?
C6 C28 H28B 108.4 . . ?
H28A C28 H28B 107.4 . . ?
C29 C28 C6 115.6(3) . . ?
C29 C28 H28A 108.4 . . ?
C29 C28 H28B 108.4 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 C2 118.2(3) . . ?
C35 C30 C2 124.1(3) . . ?
C35 C30 C31 117.7(3) . . ?
C30 C31 H31 119.1 . . ?
C32 C31 C30 121.8(3) . . ?
C32 C31 H31 119.1 . . ?
C31 C32 H32 120.1 . . ?
C33 C32 C31 119.8(4) . . ?
C33 C32 H32 120.1 . . ?
C32 C33 H33 120.3 . . ?
C34 C33 C32 119.3(3) . . ?
C34 C33 H33 120.3 . . ?
C33 C34 H34 119.5 . . ?
C33 C34 C35 121.1(3) . . ?
C35 C34 H34 119.5 . . ?
C30 C35 H35 119.9 . . ?
C34 C35 C30 120.3(3) . . ?
C34 C35 H35 119.9 . . ?
C9 C36 H36A 108.3 . . ?
C9 C36 H36B 108.3 . . ?
H36A C36 H36B 107.4 . . ?
C37 C36 C9 115.8(3) . . ?
C37 C36 H36A 108.3 . . ?
C37 C36 H36B 108.3 . . ?
C36 C37 H37A 109.5 . . ?
C36 C37 H37B 109.5 . . ?
C36 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C9 C38 H38A 109.1 . . ?
C9 C38 H38B 109.1 . . ?
H38A C38 H38B 107.8 . . ?
C39 C38 C9 112.6(3) . . ?
C39 C38 H38A 109.1 . . ?
C39 C38 H38B 109.1 . . ?
C38 C39 H39A 109.5 . . ?
C38 C39 H39B 109.5 . . ?
C38 C39 H39C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C11 C40 H40A 109.5 . . ?
C11 C40 H40B 109.5 . . ?
C11 C40 H40C 109.5 . . ?
H40A C40 H40B 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C11 C41 H41A 109.5 . . ?
C11 C41 H41B 109.5 . . ?
C11 C41 H41C 109.5 . . ?
H41A C41 H41B 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 N2 118.0(3) . . ?
C47 C42 N2 119.8(3) . . ?
C47 C42 C43 122.0(3) . . ?
C42 C43 C48 124.1(3) . . ?
C44 C43 C42 117.8(3) . . ?
C44 C43 C48 118.1(3) . . ?
C43 C44 H44 119.4 . . ?
C45 C44 C43 121.2(3) . . ?
C45 C44 H44 119.4 . . ?
C44 C45 H45 120.0 . . ?
C46 C45 C44 120.1(3) . . ?
C46 C45 H45 120.0 . . ?
C45 C46 H46 119.3 . . ?
C45 C46 C47 121.4(4) . . ?
C47 C46 H46 119.3 . . ?
C42 C47 C46 117.4(3) . . ?
C42 C47 C51 124.7(3) . . ?
C46 C47 C51 117.6(3) . . ?
C43 C48 H48 107.7 . . ?
C43 C48 C49 110.8(3) . . ?
C43 C48 C50 112.8(3) . . ?
C49 C48 H48 107.7 . . ?
C49 C48 C50 109.8(3) . . ?
C50 C48 H48 107.7 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C48 C50 H50A 109.5 . . ?
C48 C50 H50B 109.5 . . ?
C48 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C47 C51 H51 108.4 . . ?
C52 C51 C47 109.3(3) . . ?
C52 C51 H51 108.4 . . ?
C52 C51 C53 109.4(3) . . ?
C53 C51 C47 112.7(3) . . ?
C53 C51 H51 108.4 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52B 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53B 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
H1WA O1W H1WB 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
O1 H1 0.91(3) . ?
O1 C4 1.368(3) . ?
N1 C1 1.366(4) . ?
N1 C8 1.507(4) . ?
N1 C12 1.447(4) . ?
N2 C5 1.336(4) . ?
N2 C11 1.539(4) . ?
N2 C42 1.458(4) . ?
C1 C2 1.385(4) . ?
C1 C6 1.562(4) . ?
C2 C3 1.433(4) . ?
C2 C30 1.512(4) . ?
C3 H3 0.9500 . ?
C3 C4 1.387(4) . ?
C4 C5 1.420(4) . ?
C5 C9 1.534(4) . ?
C6 C7 1.527(4) . ?
C6 C26 1.538(4) . ?
C6 C28 1.562(4) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 C8 1.505(4) . ?
C8 C24 1.527(4) . ?
C8 C25 1.525(4) . ?
C9 C10 1.543(4) . ?
C9 C36 1.540(5) . ?
C9 C38 1.555(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.526(4) . ?
C11 C40 1.515(5) . ?
C11 C41 1.513(5) . ?
C12 C13 1.401(4) . ?
C12 C17 1.406(4) . ?
C13 C14 1.399(4) . ?
C13 C18 1.510(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.374(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.369(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.401(4) . ?
C17 C21 1.511(4) . ?
C18 H18 1.0000 . ?
C18 C19 1.531(5) . ?
C18 C20 1.530(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21 1.0000 . ?
C21 C22 1.528(4) . ?
C21 C23 1.541(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.532(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.518(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.391(5) . ?
C30 C35 1.390(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.384(4) . ?
C32 H32 0.9500 . ?
C32 C33 1.375(5) . ?
C33 H33 0.9500 . ?
C33 C34 1.374(5) . ?
C34 H34 0.9500 . ?
C34 C35 1.389(4) . ?
C35 H35 0.9500 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.530(5) . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.546(4) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.399(4) . ?
C42 C47 1.395(5) . ?
C43 C44 1.390(4) . ?
C43 C48 1.518(5) . ?
C44 H44 0.9500 . ?
C44 C45 1.374(5) . ?
C45 H45 0.9500 . ?
C45 C46 1.371(5) . ?
C46 H46 0.9500 . ?
C46 C47 1.397(4) . ?
C47 C51 1.531(5) . ?
C48 H48 1.0000 . ?
C48 C49 1.526(4) . ?
C48 C50 1.534(5) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51 1.0000 . ?
C51 C52 1.525(5) . ?
C51 C53 1.528(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
O1W H1WA 0.8694 . ?
O1W H1WB 0.8700 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O1 H1 Cl1 0.91(3) 2.23(3) 3.133(3) 171(3) . yes
C35 H35 Cl1 0.95 2.76 3.611(4) 149.7 . yes
O1W H1WB Cl1 0.87 2.34 3.194(4) 165.5 . yes
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
O1 C4 C5 N2 0.1(5) . . . . ?
O1 C4 C5 C9 177.5(3) . . . . ?
N1 C1 C2 C3 -6.1(5) . . . . ?
N1 C1 C2 C30 179.9(3) . . . . ?
N1 C1 C6 C7 11.5(3) . . . . ?
N1 C1 C6 C26 130.5(3) . . . . ?
N1 C1 C6 C28 -107.7(3) . . . . ?
N1 C12 C13 C14 -171.7(3) . . . . ?
N1 C12 C13 C18 10.6(5) . . . . ?
N1 C12 C17 C16 174.2(3) . . . . ?
N1 C12 C17 C21 -5.4(5) . . . . ?
N2 C5 C9 C10 8.8(4) . . . . ?
N2 C5 C9 C36 126.0(3) . . . . ?
N2 C5 C9 C38 -109.1(3) . . . . ?
N2 C42 C43 C44 170.8(3) . . . . ?
N2 C42 C43 C48 -12.2(5) . . . . ?
N2 C42 C47 C46 -169.8(3) . . . . ?
N2 C42 C47 C51 16.6(5) . . . . ?
C1 N1 C8 C7 -27.0(3) . . . . ?
C1 N1 C8 C24 92.0(3) . . . . ?
C1 N1 C8 C25 -146.5(3) . . . . ?
C1 N1 C12 C13 -105.2(4) . . . . ?
C1 N1 C12 C17 80.3(4) . . . . ?
C1 C2 C3 C4 146.8(4) . . . . ?
C1 C2 C30 C31 98.0(4) . . . . ?
C1 C2 C30 C35 -81.9(4) . . . . ?
C1 C6 C7 C8 -28.5(3) . . . . ?
C1 C6 C26 C27 -51.2(4) . . . . ?
C1 C6 C28 C29 150.2(3) . . . . ?
C2 C1 C6 C7 -173.4(3) . . . . ?
C2 C1 C6 C26 -54.4(4) . . . . ?
C2 C1 C6 C28 67.4(4) . . . . ?
C2 C3 C4 O1 -21.3(5) . . . . ?
C2 C3 C4 C5 158.1(3) . . . . ?
C2 C30 C31 C32 -176.2(3) . . . . ?
C2 C30 C35 C34 176.7(3) . . . . ?
C3 C2 C30 C31 -76.7(4) . . . . ?
C3 C2 C30 C35 103.4(4) . . . . ?
C3 C4 C5 N2 -179.3(3) . . . . ?
C3 C4 C5 C9 -1.9(6) . . . . ?
C4 C5 C9 C10 -168.9(3) . . . . ?
C4 C5 C9 C36 -51.7(5) . . . . ?
C4 C5 C9 C38 73.3(4) . . . . ?
C5 N2 C11 C10 -11.9(4) . . . . ?
C5 N2 C11 C40 107.4(3) . . . . ?
C5 N2 C11 C41 -131.4(3) . . . . ?
C5 N2 C42 C43 89.1(4) . . . . ?
C5 N2 C42 C47 -96.1(4) . . . . ?
C5 C9 C10 C11 -16.2(4) . . . . ?
C5 C9 C36 C37 -43.6(4) . . . . ?
C5 C9 C38 C39 178.0(3) . . . . ?
C6 C1 C2 C3 179.7(3) . . . . ?
C6 C1 C2 C30 5.7(5) . . . . ?
C6 C7 C8 N1 33.5(3) . . . . ?
C6 C7 C8 C24 -85.1(3) . . . . ?
C6 C7 C8 C25 153.3(3) . . . . ?
C7 C6 C26 C27 62.9(4) . . . . ?
C7 C6 C28 C29 38.2(4) . . . . ?
C8 N1 C1 C2 -165.2(3) . . . . ?
C8 N1 C1 C6 9.8(4) . . . . ?
C8 N1 C12 C13 82.8(4) . . . . ?
C8 N1 C12 C17 -91.8(4) . . . . ?
C9 C10 C11 N2 16.9(4) . . . . ?
C9 C10 C11 C40 -100.9(3) . . . . ?
C9 C10 C11 C41 136.5(3) . . . . ?
C10 C9 C36 C37 70.4(4) . . . . ?
C10 C9 C38 C39 65.5(4) . . . . ?
C11 N2 C5 C4 179.7(3) . . . . ?
C11 N2 C5 C9 2.0(4) . . . . ?
C11 N2 C42 C43 -88.3(4) . . . . ?
C11 N2 C42 C47 86.5(4) . . . . ?
C12 N1 C1 C2 22.3(5) . . . . ?
C12 N1 C1 C6 -162.7(3) . . . . ?
C12 N1 C8 C7 146.2(3) . . . . ?
C12 N1 C8 C24 -94.8(3) . . . . ?
C12 N1 C8 C25 26.7(4) . . . . ?
C12 C13 C14 C15 -2.3(5) . . . . ?
C12 C13 C18 C19 -122.4(4) . . . . ?
C12 C13 C18 C20 115.1(4) . . . . ?
C12 C17 C21 C22 -105.5(4) . . . . ?
C12 C17 C21 C23 131.3(3) . . . . ?
C13 C12 C17 C16 -0.3(5) . . . . ?
C13 C12 C17 C21 -179.9(3) . . . . ?
C13 C14 C15 C16 -0.4(5) . . . . ?
C14 C13 C18 C19 59.9(4) . . . . ?
C14 C13 C18 C20 -62.6(4) . . . . ?
C14 C15 C16 C17 2.9(5) . . . . ?
C15 C16 C17 C12 -2.5(5) . . . . ?
C15 C16 C17 C21 177.1(3) . . . . ?
C16 C17 C21 C22 75.0(4) . . . . ?
C16 C17 C21 C23 -48.2(4) . . . . ?
C17 C12 C13 C14 2.6(5) . . . . ?
C17 C12 C13 C18 -175.0(3) . . . . ?
C18 C13 C14 C15 175.5(3) . . . . ?
C26 C6 C7 C8 -152.1(3) . . . . ?
C26 C6 C28 C29 -82.4(3) . . . . ?
C28 C6 C7 C8 89.0(3) . . . . ?
C28 C6 C26 C27 -174.7(3) . . . . ?
C30 C2 C3 C4 -38.9(5) . . . . ?
C30 C31 C32 C33 -0.8(6) . . . . ?
C31 C30 C35 C34 -3.2(5) . . . . ?
C31 C32 C33 C34 -2.5(6) . . . . ?
C32 C33 C34 C35 3.0(6) . . . . ?
C33 C34 C35 C30 0.0(5) . . . . ?
C35 C30 C31 C32 3.7(5) . . . . ?
C36 C9 C10 C11 -137.7(3) . . . . ?
C36 C9 C38 C39 -55.1(4) . . . . ?
C38 C9 C10 C11 100.2(3) . . . . ?
C38 C9 C36 C37 -167.5(3) . . . . ?
C42 N2 C5 C4 2.3(6) . . . . ?
C42 N2 C5 C9 -175.4(3) . . . . ?
C42 N2 C11 C10 165.9(3) . . . . ?
C42 N2 C11 C40 -74.8(4) . . . . ?
C42 N2 C11 C41 46.4(4) . . . . ?
C42 C43 C44 C45 0.2(5) . . . . ?
C42 C43 C48 C49 -103.3(4) . . . . ?
C42 C43 C48 C50 133.1(3) . . . . ?
C42 C47 C51 C52 110.5(4) . . . . ?
C42 C47 C51 C53 -127.6(3) . . . . ?
C43 C42 C47 C46 4.8(5) . . . . ?
C43 C42 C47 C51 -168.9(3) . . . . ?
C43 C44 C45 C46 2.4(6) . . . . ?
C44 C43 C48 C49 73.6(4) . . . . ?
C44 C43 C48 C50 -49.9(4) . . . . ?
C44 C45 C46 C47 -1.4(5) . . . . ?
C45 C46 C47 C42 -2.1(5) . . . . ?
C45 C46 C47 C51 172.0(3) . . . . ?
C46 C47 C51 C52 -63.1(4) . . . . ?
C46 C47 C51 C53 58.8(4) . . . . ?
C47 C42 C43 C44 -3.8(5) . . . . ?
C47 C42 C43 C48 173.1(3) . . . . ?
C48 C43 C44 C45 -177.0(3) . . . . ?
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
-0.9994 1.0009 0.0033 0.0539 0.0372 0.0204
0.9994 -1.0009 -0.0033 -0.0539 -0.0372 -0.0204
-0.9998 -0.9982 0.0028 -0.0167 0.0479 0.0463
0.9998 0.9982 -0.0028 0.0167 -0.0479 -0.0463
-0.0005 0.0008 -0.9986 -0.0024 0.0311 -0.0193
0.0005 -0.0008 0.9986 0.0024 -0.0311 0.0193
