#------------------------------------------------------------------------------
#$Date: 2022-02-16 01:59:30 +0200 (Wed, 16 Feb 2022) $
#$Revision: 272982 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/95/7709518.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_7709518
loop_
_publ_author_name
'Saab, Marina'
'Nelson, David J.'
'Leech, Matthew C.'
'Lam, Kevin'
'Nolan, Steven P.'
'Nahra, Fady'
'Van Hecke, Kristof'
_publ_section_title
;
 Reactions of N-heterocyclic carbene-based chalcogenoureas with halogens:
 a diverse range of outcomes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00010E
_journal_year                    2022
_chemical_formula_moiety         'C69 H56 I2 N2 S'
_chemical_formula_sum            'C69 H56 I2 N2 S'
_chemical_formula_weight         1199.02
_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     dual
_audit_creation_date             2021-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-11-12 deposited with the CCDC.	2022-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.0680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.00810(10)
_cell_length_b                   17.9100(2)
_cell_length_c                   24.2237(2)
_cell_measurement_reflns_used    15440
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7110
_cell_measurement_theta_min      3.0500
_cell_volume                     5635.43(9)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    1.00    --  -41.68 -38.00-120.00   99
  2  ω    -74.00  34.00   1.00    1.00    --  -41.68  77.00  30.00  108
  3  ω      9.00  42.00   1.00    1.00    --   41.68  77.00 141.04   33
  4  ω     30.00 134.00   1.00    4.00    --  106.01 -30.00 -30.00  104
  5  ω    103.00 178.00   1.00    4.00    --  106.01  82.00  -9.00   75
  6  ω     30.00 139.00   1.00    4.00    --  106.01 -77.00   0.00  109
  7  ω    103.00 178.00   1.00    4.00    --  106.01  77.00  90.00   75
  8  ω     23.00 107.00   1.00    4.00    --  106.01 -94.00  30.00   84
  9  ω     33.00 112.00   1.00    4.00    --  106.01-125.00   0.00   79
 10  ω    103.00 178.00   1.00    4.00    --  106.01  77.00  30.00   75
 11  ω    -87.00  -6.00   1.00    1.00    --  -41.68 125.00 150.00   81
 12  ω   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00   0.00  101
 13  ω   -115.00 -14.00   1.00    1.00    --  -41.68 -57.00 120.00  101
 14  ω     77.00 178.00   1.00    4.00    --  106.01  61.00-120.00  101
 15  ω     78.00 178.00   1.00    4.00    --  106.01  30.00-180.00  100
 16  ω     53.00 178.00   1.00    4.00    --  106.01  15.00  60.00  125
 17  ω     77.00 178.00   1.00    4.00    --  106.01  61.00 -60.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0281510000
_diffrn_orient_matrix_UB_12      -0.0799756000
_diffrn_orient_matrix_UB_13      -0.0187357000
_diffrn_orient_matrix_UB_21      0.0584564000
_diffrn_orient_matrix_UB_22      -0.0314319000
_diffrn_orient_matrix_UB_23      0.0518949000
_diffrn_orient_matrix_UB_31      -0.0992532000
_diffrn_orient_matrix_UB_32      0.0041494000
_diffrn_orient_matrix_UB_33      0.0318170000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            54281
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.913
_diffrn_reflns_theta_min         3.070
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.437
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.754
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         11204
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0487P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8825
_reflns_number_total             11204
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt00010e2.cif
_cod_data_source_block           ms360
_cod_database_code               7709518
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C69 H56 I2 N2 S'
_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   0.519
_shelx_estimated_absorpt_t_min   0.352
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Ternary CH refined with riding coordinates:
 C11(H11), C24(H24), C44(H44), C56(H56)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C9(H9), C13(H13), C14(H14), C15(H15), C16(H16),
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C39(H39), C42(H42), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50),
  C52(H52), C53(H53), C54(H54), C55(H55), C58(H58), C59(H59), C60(H60),
 C61(H61), C62(H62), C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C41(H41A,H41B,H41C)
;
_olex2_date_sample_data_collection 2021-07-22
_olex2_exptl_crystal_mounting_method 'mounted on a LithoLoop'
_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.854
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
I1 I 0.40972(2) 0.73814(2) 0.73925(2) 0.02413(6) Uani 1 1 d . . . . .
I2 I 0.19696(2) 0.73647(2) 0.72479(2) 0.04108(7) Uani 1 1 d . . . . .
S1 S 0.62628(6) 0.75209(3) 0.75709(3) 0.02526(16) Uani 1 1 d . . . . .
N1 N 0.66838(18) 0.60017(12) 0.75915(9) 0.0165(4) Uani 1 1 d . . . . .
N2 N 0.80217(18) 0.67219(11) 0.76126(9) 0.0153(4) Uani 1 1 d . . . . .
C1 C 0.6979(2) 0.67319(14) 0.75853(11) 0.0162(5) Uani 1 1 d . . . . .
C2 C 0.7544(2) 0.55427(14) 0.76258(11) 0.0182(5) Uani 1 1 d . . . . .
H2 H 0.754434 0.501250 0.763653 0.022 Uiso 1 1 calc R . . . .
C3 C 0.8379(2) 0.59893(14) 0.76411(11) 0.0186(5) Uani 1 1 d . . . . .
H3 H 0.907831 0.583383 0.766638 0.022 Uiso 1 1 calc R . . . .
C4 C 0.8655(2) 0.73744(14) 0.75608(11) 0.0153(5) Uani 1 1 d . . . . .
C5 C 0.8988(2) 0.77551(14) 0.80448(11) 0.0176(5) Uani 1 1 d . . . . .
C6 C 0.9570(2) 0.83962(15) 0.79863(12) 0.0219(6) Uani 1 1 d . . . . .
H6 H 0.980379 0.866455 0.830719 0.026 Uiso 1 1 calc R . . . .
C7 C 0.9820(2) 0.86565(15) 0.74682(12) 0.0238(6) Uani 1 1 d . . . . .
C8 C 1.0442(3) 0.93589(19) 0.74150(15) 0.0384(8) Uani 1 1 d . . . . .
H8A H 1.089937 0.930488 0.710895 0.058 Uiso 1 1 calc GR . . . .
H8B H 1.085391 0.944678 0.775945 0.058 Uiso 1 1 calc GR . . . .
H8C H 0.997739 0.978250 0.734193 0.058 Uiso 1 1 calc GR . . . .
C9 C 0.9494(2) 0.82506(15) 0.70016(12) 0.0217(6) Uani 1 1 d . . . . .
H9 H 0.967946 0.841949 0.664880 0.026 Uiso 1 1 calc R . . . .
C10 C 0.8907(2) 0.76088(14) 0.70345(11) 0.0174(5) Uani 1 1 d . . . . .
C11 C 0.8559(2) 0.71859(14) 0.65083(11) 0.0182(5) Uani 1 1 d . . . . .
H11 H 0.816033 0.674220 0.662742 0.022 Uiso 1 1 calc R . . . .
C12 C 0.9504(2) 0.68842(15) 0.62289(12) 0.0205(6) Uani 1 1 d . . . . .
C13 C 0.9857(3) 0.61644(17) 0.63586(13) 0.0267(7) Uani 1 1 d . . . . .
H13 H 0.949112 0.586421 0.660492 0.032 Uiso 1 1 calc R . . . .
C14 C 1.0736(3) 0.5882(2) 0.61325(15) 0.0381(8) Uani 1 1 d . . . . .
H14 H 1.096303 0.539058 0.622170 0.046 Uiso 1 1 calc R . . . .
C15 C 1.1282(3) 0.6318(2) 0.57762(17) 0.0437(9) Uani 1 1 d . . . . .
H15 H 1.189442 0.613220 0.562906 0.052 Uiso 1 1 calc R . . . .
C16 C 1.0928(3) 0.7032(2) 0.56357(16) 0.0385(8) Uani 1 1 d . . . . .
H16 H 1.129313 0.732871 0.538692 0.046 Uiso 1 1 calc R . . . .
C17 C 1.0042(3) 0.73108(17) 0.58578(13) 0.0278(6) Uani 1 1 d . . . . .
H17 H 0.980043 0.779497 0.575623 0.033 Uiso 1 1 calc R . . . .
C18 C 0.7836(2) 0.76390(15) 0.61196(11) 0.0203(6) Uani 1 1 d . . . . .
C19 C 0.7607(3) 0.73787(17) 0.55822(12) 0.0257(6) Uani 1 1 d . . . . .
H19 H 0.793631 0.694129 0.545709 0.031 Uiso 1 1 calc R . . . .
C20 C 0.6902(3) 0.77544(19) 0.52281(13) 0.0314(7) Uani 1 1 d . . . . .
H20 H 0.674648 0.756527 0.486680 0.038 Uiso 1 1 calc R . . . .
C21 C 0.6430(3) 0.8394(2) 0.53963(14) 0.0386(8) Uani 1 1 d . . . . .
H21 H 0.596241 0.865558 0.515150 0.046 Uiso 1 1 calc R . . . .
C22 C 0.6647(3) 0.8652(2) 0.59285(15) 0.0431(9) Uani 1 1 d . . . . .
H22 H 0.631846 0.909195 0.605033 0.052 Uiso 1 1 calc R . . . .
C23 C 0.7338(3) 0.82771(18) 0.62866(13) 0.0315(7) Uani 1 1 d . . . . .
H23 H 0.747202 0.846092 0.665126 0.038 Uiso 1 1 calc R . . . .
C24 C 0.8727(2) 0.74755(14) 0.86153(11) 0.0199(6) Uani 1 1 d . . . . .
H24 H 0.805963 0.720050 0.856341 0.024 Uiso 1 1 calc R . . . .
C25 C 0.9510(2) 0.69155(15) 0.88640(12) 0.0228(6) Uani 1 1 d . . . . .
C26 C 1.0360(3) 0.66878(19) 0.85941(14) 0.0316(7) Uani 1 1 d . . . . .
H26 H 1.049292 0.689777 0.824493 0.038 Uiso 1 1 calc R . . . .
C27 C 1.1033(3) 0.6147(2) 0.88301(18) 0.0445(9) Uani 1 1 d . . . . .
H27 H 1.160569 0.598253 0.863510 0.053 Uiso 1 1 calc R . . . .
C28 C 1.0863(3) 0.5856(2) 0.93441(17) 0.0458(10) Uani 1 1 d . . . . .
H28 H 1.132076 0.549363 0.950477 0.055 Uiso 1 1 calc R . . . .
C29 C 1.0028(3) 0.60929(19) 0.96242(16) 0.0392(9) Uani 1 1 d . . . . .
H29 H 0.991218 0.589534 0.997957 0.047 Uiso 1 1 calc R . . . .
C30 C 0.9352(3) 0.66207(16) 0.93878(13) 0.0287(7) Uani 1 1 d . . . . .
H30 H 0.877931 0.678211 0.958378 0.034 Uiso 1 1 calc R . . . .
C31 C 0.8530(3) 0.81294(15) 0.89987(12) 0.0241(6) Uani 1 1 d . . . . .
C32 C 0.9294(3) 0.84050(17) 0.93742(13) 0.0284(7) Uani 1 1 d . . . . .
H32 H 0.994866 0.816952 0.940690 0.034 Uiso 1 1 calc R . . . .
C33 C 0.9094(3) 0.90245(18) 0.96999(13) 0.0370(8) Uani 1 1 d . . . . .
H33 H 0.961767 0.921293 0.995091 0.044 Uiso 1 1 calc R . . . .
C34 C 0.8150(4) 0.93633(18) 0.96607(14) 0.0419(10) Uani 1 1 d . . . . .
H34 H 0.801628 0.978402 0.988463 0.050 Uiso 1 1 calc R . . . .
C35 C 0.7392(4) 0.9089(2) 0.92928(15) 0.0457(10) Uani 1 1 d . . . . .
H35 H 0.673491 0.932232 0.926534 0.055 Uiso 1 1 calc R . . . .
C36 C 0.7584(3) 0.84734(19) 0.89626(14) 0.0345(8) Uani 1 1 d . . . . .
H36 H 0.705790 0.829004 0.871092 0.041 Uiso 1 1 calc R . . . .
C37 C 0.5636(2) 0.57344(14) 0.75394(11) 0.0178(5) Uani 1 1 d . . . . .
C38 C 0.5105(2) 0.56228(14) 0.80128(11) 0.0191(5) Uani 1 1 d . . . . .
C39 C 0.4103(2) 0.53531(15) 0.79517(12) 0.0218(6) Uani 1 1 d . . . . .
H39 H 0.372172 0.527773 0.827078 0.026 Uiso 1 1 calc R . . . .
C40 C 0.3645(2) 0.51906(16) 0.74301(12) 0.0236(6) Uani 1 1 d . . . . .
C41 C 0.2559(3) 0.4904(2) 0.73731(13) 0.0351(8) Uani 1 1 d . . . . .
H41A H 0.237076 0.468543 0.772482 0.053 Uiso 1 1 calc GR . . . .
H41B H 0.250626 0.452144 0.708337 0.053 Uiso 1 1 calc GR . . . .
H41C H 0.209031 0.531663 0.727399 0.053 Uiso 1 1 calc GR . . . .
C42 C 0.4203(2) 0.53175(16) 0.69660(12) 0.0234(6) Uani 1 1 d . . . . .
H42 H 0.388917 0.521921 0.661042 0.028 Uiso 1 1 calc R . . . .
C43 C 0.5212(2) 0.55853(15) 0.70068(11) 0.0196(6) Uani 1 1 d . . . . .
C44 C 0.5847(2) 0.57161(15) 0.65030(11) 0.0202(6) Uani 1 1 d . . . . .
H44 H 0.632283 0.613979 0.660115 0.024 Uiso 1 1 calc R . . . .
C45 C 0.6529(2) 0.50459(16) 0.63894(11) 0.0211(6) Uani 1 1 d . . . . .
C46 C 0.7417(2) 0.51621(16) 0.60997(12) 0.0236(6) Uani 1 1 d . . . . .
H46 H 0.756609 0.564801 0.596847 0.028 Uiso 1 1 calc R . . . .
C47 C 0.8082(3) 0.45783(18) 0.60015(13) 0.0276(6) Uani 1 1 d . . . . .
H47 H 0.868601 0.466860 0.580819 0.033 Uiso 1 1 calc R . . . .
C48 C 0.7870(3) 0.38598(18) 0.61843(13) 0.0297(7) Uani 1 1 d . . . . .
H48 H 0.832470 0.345892 0.611677 0.036 Uiso 1 1 calc R . . . .
C49 C 0.6988(3) 0.37393(17) 0.64654(13) 0.0308(7) Uani 1 1 d . . . . .
H49 H 0.683462 0.325111 0.659066 0.037 Uiso 1 1 calc R . . . .
C50 C 0.6322(3) 0.43252(16) 0.65669(13) 0.0267(6) Uani 1 1 d . . . . .
H50 H 0.571829 0.423217 0.675989 0.032 Uiso 1 1 calc R . . . .
C51 C 0.5172(2) 0.59745(16) 0.60075(11) 0.0226(6) Uani 1 1 d . . . . .
C52 C 0.4974(3) 0.67318(18) 0.59384(13) 0.0304(7) Uani 1 1 d . . . . .
H52 H 0.529476 0.708168 0.618688 0.036 Uiso 1 1 calc R . . . .
C53 C 0.4313(3) 0.6981(2) 0.55112(15) 0.0401(9) Uani 1 1 d . . . . .
H53 H 0.417810 0.749975 0.546750 0.048 Uiso 1 1 calc R . . . .
C54 C 0.3847(3) 0.6468(2) 0.51458(14) 0.0401(8) Uani 1 1 d . . . . .
H54 H 0.338873 0.663774 0.485384 0.048 Uiso 1 1 calc R . . . .
C55 C 0.4047(3) 0.5717(2) 0.52051(13) 0.0332(7) Uani 1 1 d . . . . .
H55 H 0.373097 0.536921 0.495299 0.040 Uiso 1 1 calc R . . . .
C56 C 0.5630(2) 0.57847(15) 0.85794(11) 0.0205(6) Uani 1 1 d . . . . .
H56 H 0.605701 0.624219 0.853232 0.025 Uiso 1 1 calc R . . . .
C57 C 0.6378(2) 0.51659(16) 0.87487(11) 0.0224(6) Uani 1 1 d . . . . .
C58 C 0.7327(3) 0.53466(18) 0.90092(13) 0.0290(7) Uani 1 1 d . . . . .
H58 H 0.747500 0.585174 0.910269 0.035 Uiso 1 1 calc R . . . .
C59 C 0.8059(3) 0.4799(2) 0.91339(14) 0.0358(8) Uani 1 1 d . . . . .
H59 H 0.870612 0.493220 0.930580 0.043 Uiso 1 1 calc R . . . .
C60 C 0.7845(3) 0.4056(2) 0.90079(14) 0.0343(7) Uani 1 1 d . . . . .
H60 H 0.834654 0.368095 0.908901 0.041 Uiso 1 1 calc R . . . .
C61 C 0.6892(3) 0.38684(18) 0.87621(13) 0.0327(7) Uani 1 1 d . . . . .
H61 H 0.673557 0.336037 0.868189 0.039 Uiso 1 1 calc R . . . .
C62 C 0.6164(3) 0.44180(17) 0.86324(12) 0.0273(7) Uani 1 1 d . . . . .
H62 H 0.551459 0.428259 0.846313 0.033 Uiso 1 1 calc R . . . .
C63 C 0.4850(2) 0.59857(16) 0.89994(11) 0.0223(6) Uani 1 1 d . . . . .
C64 C 0.4527(2) 0.54930(16) 0.93948(12) 0.0219(6) Uani 1 1 d . . . . .
H64 H 0.483223 0.501186 0.942582 0.026 Uiso 1 1 calc R . . . .
C65 C 0.3761(3) 0.56916(17) 0.97485(12) 0.0266(6) Uani 1 1 d . . . . .
H65 H 0.355100 0.534837 1.001937 0.032 Uiso 1 1 calc R . . . .
C66 C 0.3310(3) 0.63858(19) 0.97045(13) 0.0339(8) Uani 1 1 d . . . . .
H66 H 0.278838 0.652379 0.994467 0.041 Uiso 1 1 calc R . . . .
C67 C 0.3622(4) 0.6883(2) 0.93072(14) 0.0433(10) Uani 1 1 d . . . . .
H67 H 0.330458 0.735929 0.927166 0.052 Uiso 1 1 calc R . . . .
C68 C 0.4390(3) 0.66886(17) 0.89638(13) 0.0363(8) Uani 1 1 d . . . . .
H68 H 0.460929 0.703821 0.869949 0.044 Uiso 1 1 calc R . . . .
C69 C 0.4711(2) 0.54680(18) 0.56349(12) 0.0264(6) Uani 1 1 d . . . . .
H69 H 0.485222 0.494975 0.567438 0.032 Uiso 1 1 calc R . . . .
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'
I I -0.3257 6.8362 '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'
S S 0.3331 0.5567 '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
-6 -2 12 0.0207
7 -5 2 0.0394
5 2 -13 0.0564
-5 7 -9 0.0817
-8 -3 5 0.0286
2 -8 -11 0.0486
8 4 -4 0.0498
2 10 8 0.0592
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
I2 I1 S1 175.313(16) . . ?
C1 S1 I1 118.06(9) . . ?
C1 N1 C2 110.0(2) . . ?
C1 N1 C37 125.6(2) . . ?
C2 N1 C37 124.3(2) . . ?
C1 N2 C3 110.2(2) . . ?
C1 N2 C4 124.1(2) . . ?
C3 N2 C4 125.3(2) . . ?
N1 C1 S1 130.3(2) . . ?
N2 C1 S1 124.10(19) . . ?
N2 C1 N1 105.6(2) . . ?
C3 C2 N1 107.2(2) . . ?
C2 C3 N2 106.9(2) . . ?
C5 C4 N2 118.3(2) . . ?
C10 C4 N2 119.1(2) . . ?
C10 C4 C5 122.6(2) . . ?
C4 C5 C24 121.5(2) . . ?
C6 C5 C4 117.6(3) . . ?
C6 C5 C24 120.9(2) . . ?
C5 C6 C7 121.6(3) . . ?
C6 C7 C8 120.6(3) . . ?
C9 C7 C6 118.8(3) . . ?
C9 C7 C8 120.6(3) . . ?
C10 C9 C7 122.2(3) . . ?
C4 C10 C11 122.5(2) . . ?
C9 C10 C4 117.3(2) . . ?
C9 C10 C11 120.2(3) . . ?
C10 C11 C12 109.5(2) . . ?
C18 C11 C10 113.3(2) . . ?
C18 C11 C12 113.4(2) . . ?
C13 C12 C11 119.2(3) . . ?
C17 C12 C11 122.2(3) . . ?
C17 C12 C13 118.7(3) . . ?
C14 C13 C12 120.9(3) . . ?
C15 C14 C13 120.0(3) . . ?
C14 C15 C16 119.6(4) . . ?
C17 C16 C15 120.3(4) . . ?
C16 C17 C12 120.4(3) . . ?
C19 C18 C11 119.3(3) . . ?
C23 C18 C11 122.7(3) . . ?
C23 C18 C19 117.9(3) . . ?
C20 C19 C18 120.7(3) . . ?
C21 C20 C19 120.7(3) . . ?
C20 C21 C22 118.9(3) . . ?
C21 C22 C23 120.8(3) . . ?
C18 C23 C22 120.9(3) . . ?
C5 C24 C25 113.3(3) . . ?
C31 C24 C5 110.6(2) . . ?
C31 C24 C25 113.2(2) . . ?
C26 C25 C24 122.8(3) . . ?
C26 C25 C30 118.7(3) . . ?
C30 C25 C24 118.5(3) . . ?
C25 C26 C27 120.6(3) . . ?
C28 C27 C26 120.1(4) . . ?
C27 C28 C29 119.8(3) . . ?
C28 C29 C30 120.2(3) . . ?
C29 C30 C25 120.6(4) . . ?
C32 C31 C24 122.0(3) . . ?
C36 C31 C24 119.0(3) . . ?
C36 C31 C32 119.0(3) . . ?
C33 C32 C31 120.1(3) . . ?
C34 C33 C32 120.5(3) . . ?
C33 C34 C35 119.6(3) . . ?
C34 C35 C36 120.5(4) . . ?
C31 C36 C35 120.4(3) . . ?
C38 C37 N1 119.1(2) . . ?
C38 C37 C43 123.1(3) . . ?
C43 C37 N1 117.8(3) . . ?
C37 C38 C39 117.9(2) . . ?
C37 C38 C56 119.8(3) . . ?
C39 C38 C56 122.2(3) . . ?
C38 C39 C40 121.3(3) . . ?
C39 C40 C41 120.4(3) . . ?
C42 C40 C39 118.8(3) . . ?
C42 C40 C41 120.7(3) . . ?
C40 C42 C43 121.9(3) . . ?
C37 C43 C44 120.2(3) . . ?
C42 C43 C37 116.9(3) . . ?
C42 C43 C44 122.8(2) . . ?
C45 C44 C43 111.6(2) . . ?
C51 C44 C43 111.3(2) . . ?
C51 C44 C45 114.4(2) . . ?
C46 C45 C44 118.5(3) . . ?
C50 C45 C44 123.3(3) . . ?
C50 C45 C46 118.1(3) . . ?
C47 C46 C45 120.9(3) . . ?
C46 C47 C48 120.4(3) . . ?
C49 C48 C47 119.0(3) . . ?
C48 C49 C50 120.7(3) . . ?
C49 C50 C45 120.9(3) . . ?
C52 C51 C44 119.2(3) . . ?
C52 C51 C69 119.2(3) . . ?
C69 C51 C44 121.6(3) . . ?
C53 C52 C51 120.6(3) . . ?
C52 C53 C54 119.6(3) . . ?
C55 C54 C53 120.4(3) . . ?
C54 C55 C69 119.8(3) . . ?
C57 C56 C38 110.7(2) . . ?
C57 C56 C63 115.7(2) . . ?
C63 C56 C38 111.4(2) . . ?
C58 C57 C56 119.5(3) . . ?
C62 C57 C56 122.0(3) . . ?
C62 C57 C58 118.5(3) . . ?
C59 C58 C57 121.0(3) . . ?
C58 C59 C60 120.1(3) . . ?
C61 C60 C59 119.3(3) . . ?
C60 C61 C62 120.5(3) . . ?
C61 C62 C57 120.6(3) . . ?
C64 C63 C56 123.5(3) . . ?
C64 C63 C68 118.2(3) . . ?
C68 C63 C56 118.2(3) . . ?
C63 C64 C65 121.1(3) . . ?
C66 C65 C64 119.9(3) . . ?
C65 C66 C67 119.6(3) . . ?
C68 C67 C66 120.3(3) . . ?
C67 C68 C63 120.9(3) . . ?
C55 C69 C51 120.3(3) . . ?
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
I1 I2 2.7711(3) . ?
I1 S1 2.8381(8) . ?
S1 C1 1.692(3) . ?
N1 C1 1.363(3) . ?
N1 C2 1.387(3) . ?
N1 C37 1.444(4) . ?
N2 C1 1.355(4) . ?
N2 C3 1.393(3) . ?
N2 C4 1.439(3) . ?
C2 C3 1.348(4) . ?
C4 C5 1.405(4) . ?
C4 C10 1.398(4) . ?
C5 C6 1.387(4) . ?
C5 C24 1.525(4) . ?
C6 C7 1.393(4) . ?
C7 C8 1.505(4) . ?
C7 C9 1.391(4) . ?
C9 C10 1.384(4) . ?
C10 C11 1.530(3) . ?
C11 C12 1.533(4) . ?
C11 C18 1.528(4) . ?
C12 C13 1.399(4) . ?
C12 C17 1.396(5) . ?
C13 C14 1.389(5) . ?
C14 C15 1.388(6) . ?
C15 C16 1.394(6) . ?
C16 C17 1.391(5) . ?
C18 C19 1.400(4) . ?
C18 C23 1.384(4) . ?
C19 C20 1.395(4) . ?
C20 C21 1.372(5) . ?
C21 C22 1.384(5) . ?
C22 C23 1.389(4) . ?
C24 C25 1.530(4) . ?
C24 C31 1.525(4) . ?
C25 C26 1.376(5) . ?
C25 C30 1.399(4) . ?
C26 C27 1.406(5) . ?
C27 C28 1.378(6) . ?
C28 C29 1.379(6) . ?
C29 C30 1.393(5) . ?
C31 C32 1.400(4) . ?
C31 C36 1.375(5) . ?
C32 C33 1.394(5) . ?
C33 C34 1.369(6) . ?
C34 C35 1.384(6) . ?
C35 C36 1.393(5) . ?
C37 C38 1.385(4) . ?
C37 C43 1.401(4) . ?
C38 C39 1.390(4) . ?
C38 C56 1.528(3) . ?
C39 C40 1.398(4) . ?
C40 C41 1.504(4) . ?
C40 C42 1.389(4) . ?
C42 C43 1.396(4) . ?
C43 C44 1.527(4) . ?
C44 C45 1.527(4) . ?
C44 C51 1.521(4) . ?
C45 C46 1.399(4) . ?
C45 C50 1.391(4) . ?
C46 C47 1.386(4) . ?
C47 C48 1.393(5) . ?
C48 C49 1.382(5) . ?
C49 C50 1.391(5) . ?
C51 C52 1.389(4) . ?
C51 C69 1.392(4) . ?
C52 C53 1.383(5) . ?
C53 C54 1.392(5) . ?
C54 C55 1.377(5) . ?
C55 C69 1.391(4) . ?
C56 C57 1.517(4) . ?
C56 C63 1.517(4) . ?
C57 C58 1.394(4) . ?
C57 C62 1.394(4) . ?
C58 C59 1.389(5) . ?
C59 C60 1.389(5) . ?
C60 C61 1.388(5) . ?
C61 C62 1.390(5) . ?
C63 C64 1.384(4) . ?
C63 C68 1.395(4) . ?
C64 C65 1.395(5) . ?
C65 C66 1.377(5) . ?
C66 C67 1.387(5) . ?
C67 C68 1.379(6) . ?
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
-5.8468 -1.6187 11.6971 0.0749 0.3161 0.9458
7.4954 -5.0643 1.6166 0.1637 0.6812 -0.7135
5.0968 2.4372 -12.5842 -0.1026 -0.4317 -0.8961
-4.5868 6.6341 -9.2143 -0.2288 -0.9548 0.1896
-7.7698 -3.3877 4.8809 0.3982 -0.0944 0.9124
1.7257 -8.2749 -10.7233 0.8141 -0.1955 -0.5468
7.7188 3.9677 -4.2058 -0.4558 0.1082 -0.8835
2.0222 9.5303 7.9645 -0.9683 0.2320 0.0922
