# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 2173463'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2022-03-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C10 H18 Ag2 O4'
_chemical_formula_sum            'C10 H18 Ag2 O4'
_chemical_formula_weight         417.98
_chemical_melting_point          ?
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'
Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.7752(4)
_cell_length_b                   13.4830(10)
_cell_length_c                   16.9347(12)
_cell_angle_alpha                108.220(7)
_cell_angle_beta                 90.240(5)
_cell_angle_gamma                94.770(6)
_cell_volume                     1247.57(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2398
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.6360
_cell_measurement_theta_min      3.6450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    25.178
_exptl_absorpt_correction_T_max  0.829
_exptl_absorpt_correction_T_min  0.164
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             816
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -8 0 0.0246
0 8 0 0.0156
0 -7 8 0.0068
0 7 -8 0.0010
3 -5 4 0.0754
-3 5 -4 0.0836

_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.059
_exptl_crystal_size_min          0.008
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
0.2897 -8.2921 -0.0815 -0.9832 -0.1822 -0.0090
-0.2897 8.2921 0.0815 0.9832 0.1822 0.0090
0.0625 -7.4859 8.3345 -0.5883 -0.4036 0.7007
-0.0625 7.4859 -8.3345 0.5883 0.4036 -0.7007
3.0266 -5.3140 4.2701 -0.3336 -0.9422 0.0307
-3.0927 5.2160 -3.8585 0.3338 0.9426 0.0106

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0716
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8322
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.125
_diffrn_reflns_theta_min         3.465
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -14.00   1.00    1.00    --  -41.40 -57.00  90.00  101
  2  ω    -55.00  35.00   1.00    1.00    --  -41.40  77.00-150.00   90
  3  ω     28.00  97.00   1.00    1.00    --   41.40-125.00  60.00   69
  4  ω     14.00 115.00   1.00    1.00    --   41.40  57.00 -30.00  101
  5  ω     39.00 118.00   1.00    2.00    --  112.00 -45.00  60.00   79
  6  ω     40.00 140.00   1.00    2.00    --  112.00 -61.00-180.00  100
  7  ω     60.00 145.00   1.00    2.00    --  112.00 -77.00 -30.00   85
  8  ω     38.00 109.00   1.00    2.00    --  112.00-111.00   0.00   71
  9  ω     39.00 109.00   1.00    2.00    --  112.00-111.00 150.00   70
 10  ω     37.00 139.00   1.00    2.00    --  112.00 -30.00 -60.00  102
 11  ω    124.00 175.00   1.00    2.00    --  112.00  45.00   0.00   51
 12  ω     37.00 109.00   1.00    2.00    --  112.00-111.00-150.00   72
 13  ω     31.00 165.00   1.00    2.00    --  112.00 -15.00-180.00  134
;
_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      0.0484401000
_diffrn_orient_matrix_UB_12      0.1199043000
_diffrn_orient_matrix_UB_13      0.0367489000
_diffrn_orient_matrix_UB_21      -0.2386811000
_diffrn_orient_matrix_UB_22      0.0139712000
_diffrn_orient_matrix_UB_23      -0.0340886000
_diffrn_orient_matrix_UB_31      -0.1114056000
_diffrn_orient_matrix_UB_32      -0.0036137000
_diffrn_orient_matrix_UB_33      0.0816656000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3314
_reflns_number_total             4849
_reflns_odcompleteness_completeness 98.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.261
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.186
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         4849
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0371
_refine_ls_restrained_S_all      0.978
_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)+(0.0225P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0855
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ag1 Ag 0.94156(9) 0.92596(4) 0.91636(3) 0.01995(12) Uani 1 1 d . . . . .
Ag2 Ag 0.50837(9) 0.88637(4) 0.98766(3) 0.02034(12) Uani 1 1 d . . . . .
O11 O 1.0905(9) 0.8582(4) 1.0087(3) 0.0244(12) Uani 1 1 d . . . . .
O13 O 0.7412(8) 0.7987(4) 1.0372(3) 0.0227(12) Uani 1 1 d . . . . .
O21 O 0.3568(8) 0.9332(4) 0.8830(3) 0.0231(12) Uani 1 1 d . . . . .
O23 O 0.6949(9) 0.9295(4) 0.8198(3) 0.0214(11) Uani 1 1 d . . . . .
C12 C 0.9554(12) 0.8000(6) 1.0385(4) 0.0170(14) Uani 1 1 d . . . . .
C14 C 1.0662(12) 0.7258(6) 1.0782(4) 0.0171(14) Uani 1 1 d . . . . .
C15 C 1.2398(12) 0.7916(6) 1.1476(4) 0.0213(15) Uani 1 1 d . . . . .
H15A H 1.3587 0.8272 1.1244 0.032 Uiso 1 1 calc GR . . . .
H15B H 1.3092 0.7465 1.1731 0.032 Uiso 1 1 calc GR . . . .
H15C H 1.1597 0.8423 1.1886 0.032 Uiso 1 1 calc GR . . . .
C16 C 1.1951(13) 0.6482(6) 1.0103(5) 0.0236(16) Uani 1 1 d . . . . .
H16A H 1.0869 0.6090 0.9662 0.035 Uiso 1 1 calc GR . . . .
H16B H 1.2654 0.6011 1.0335 0.035 Uiso 1 1 calc GR . . . .
H16C H 1.3134 0.6861 0.9887 0.035 Uiso 1 1 calc GR . . . .
C17 C 0.8791(13) 0.6652(6) 1.1119(5) 0.0261(17) Uani 1 1 d . . . . .
H17A H 0.7980 0.7134 1.1545 0.039 Uiso 1 1 calc GR . . . .
H17B H 0.9499 0.6179 1.1349 0.039 Uiso 1 1 calc GR . . . .
H17C H 0.7714 0.6260 1.0676 0.039 Uiso 1 1 calc GR . . . .
C22 C 0.4783(12) 0.9277(5) 0.8188(4) 0.0155(14) Uani 1 1 d . . . . .
C24 C 0.3503(12) 0.9166(6) 0.7363(4) 0.0180(14) Uani 1 1 d . . . . .
C25 C 0.2193(13) 1.0143(6) 0.7486(5) 0.0266(17) Uani 1 1 d . . . . .
H25A H 0.1118 1.0200 0.7925 0.040 Uiso 1 1 calc GR . . . .
H25B H 0.1358 1.0086 0.6980 0.040 Uiso 1 1 calc GR . . . .
H25C H 0.3282 1.0754 0.7629 0.040 Uiso 1 1 calc GR . . . .
C26 C 0.1786(13) 0.8184(6) 0.7147(5) 0.0237(16) Uani 1 1 d . . . . .
H26A H 0.2619 0.7580 0.7094 0.035 Uiso 1 1 calc GR . . . .
H26B H 0.0978 0.8101 0.6631 0.035 Uiso 1 1 calc GR . . . .
H26C H 0.0687 0.8254 0.7580 0.035 Uiso 1 1 calc GR . . . .
C27 C 0.5225(13) 0.9060(8) 0.6677(5) 0.0297(19) Uani 1 1 d . . . . .
H27A H 0.6388 0.9644 0.6836 0.045 Uiso 1 1 calc GR . . . .
H27B H 0.4426 0.9049 0.6175 0.045 Uiso 1 1 calc GR . . . .
H27C H 0.5952 0.8420 0.6583 0.045 Uiso 1 1 calc GR . . . .
Ag3 Ag 0.58235(9) 0.61434(4) 0.50956(3) 0.01879(12) Uani 1 1 d . . . . .
Ag4 Ag 0.14190(9) 0.57169(4) 0.57452(3) 0.01738(12) Uani 1 1 d . . . . .
O31 O 0.3530(9) 0.6962(4) 0.4538(3) 0.0233(11) Uani 1 1 d . . . . .
O33 O 0.0029(9) 0.6537(4) 0.4942(3) 0.0223(11) Uani 1 1 d . . . . .
O41 O 0.3839(8) 0.5206(4) 0.6490(3) 0.0202(11) Uani 1 1 d . . . . .
O43 O 0.7305(8) 0.5901(4) 0.6243(3) 0.0202(11) Uani 1 1 d . . . . .
C32 C 0.1423(12) 0.7056(5) 0.4605(4) 0.0158(14) Uani 1 1 d . . . . .
C34 C 0.0385(12) 0.7864(5) 0.4263(4) 0.0174(14) Uani 1 1 d . . . . .
C35 C -0.1038(13) 0.8573(6) 0.4922(5) 0.0231(15) Uani 1 1 d . . . . .
H35A H -0.2375 0.8170 0.5032 0.035 Uiso 1 1 calc GR . . . .
H35B H -0.1533 0.9120 0.4727 0.035 Uiso 1 1 calc GR . . . .
H35C H -0.0105 0.8877 0.5423 0.035 Uiso 1 1 calc GR . . . .
C36 C 0.2319(12) 0.8526(6) 0.3997(5) 0.0234(16) Uani 1 1 d . . . . .
H36A H 0.3321 0.8898 0.4469 0.035 Uiso 1 1 calc GR . . . .
H36B H 0.1647 0.9019 0.3780 0.035 Uiso 1 1 calc GR . . . .
H36C H 0.3204 0.8077 0.3575 0.035 Uiso 1 1 calc GR . . . .
C37 C -0.1201(13) 0.7274(6) 0.3503(4) 0.0230(16) Uani 1 1 d . . . . .
H37A H -0.0304 0.6834 0.3080 0.034 Uiso 1 1 calc GR . . . .
H37B H -0.1879 0.7770 0.3291 0.034 Uiso 1 1 calc GR . . . .
H37C H -0.2412 0.6850 0.3663 0.034 Uiso 1 1 calc GR . . . .
C42 C 0.5935(11) 0.5544(5) 0.6679(4) 0.0146(13) Uani 1 1 d . . . . .
C44 C 0.6783(13) 0.5576(6) 0.7563(4) 0.0206(15) Uani 1 1 d . . . . .
C45 C 0.6018(14) 0.6585(6) 0.8160(5) 0.0265(17) Uani 1 1 d . . . . .
H45A H 0.6605 0.7168 0.7985 0.040 Uiso 1 1 calc GR . . . .
H45B H 0.6615 0.6676 0.8710 0.040 Uiso 1 1 calc GR . . . .
H45C H 0.4351 0.6549 0.8161 0.040 Uiso 1 1 calc GR . . . .
C46 C 0.9421(12) 0.5606(6) 0.7611(4) 0.0232(16) Uani 1 1 d . . . . .
H46A H 0.9924 0.5011 0.7189 0.035 Uiso 1 1 calc GR . . . .
H46B H 0.9908 0.5589 0.8149 0.035 Uiso 1 1 calc GR . . . .
H46C H 1.0094 0.6239 0.7525 0.035 Uiso 1 1 calc GR . . . .
C47 C 0.5703(13) 0.4615(6) 0.7774(5) 0.0245(16) Uani 1 1 d . . . . .
H47A H 0.4040 0.4589 0.7731 0.037 Uiso 1 1 calc GR . . . .
H47B H 0.6171 0.4665 0.8330 0.037 Uiso 1 1 calc GR . . . .
H47C H 0.6224 0.3990 0.7391 0.037 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ag1 Ag1 2.9478(11) 2_777 ?
Ag1 Ag2 2.8649(8) . ?
Ag1 O11 2.243(5) . ?
Ag1 O21 2.467(5) 1_655 ?
Ag1 O23 2.179(5) . ?
Ag2 Ag2 2.9701(11) 2_677 ?
Ag2 O11 2.457(5) 1_455 ?
Ag2 O13 2.188(5) . ?
Ag2 O21 2.255(5) . ?
O11 Ag2 2.457(5) 1_655 ?
O11 C12 1.277(9) . ?
O13 C12 1.235(8) . ?
O21 Ag1 2.467(5) 1_455 ?
O21 C22 1.282(9) . ?
O23 C22 1.249(8) . ?
C12 C14 1.543(9) . ?
C14 C15 1.537(10) . ?
C14 C16 1.535(10) . ?
C14 C17 1.520(9) . ?
C22 C24 1.537(9) . ?
C24 C25 1.531(10) . ?
C24 C26 1.532(10) . ?
C24 C27 1.513(10) . ?
Ag3 Ag3 3.0662(10) 2_666 ?
Ag3 Ag4 3.0504(7) 2_666 ?
Ag3 Ag4 2.8613(8) . ?
Ag3 O31 2.179(5) . ?
Ag3 O33 2.475(5) 1_655 ?
Ag3 O43 2.245(5) . ?
Ag4 Ag3 3.0503(7) 2_666 ?
Ag4 Ag4 3.0300(10) 2_566 ?
Ag4 O33 2.190(5) . ?
Ag4 O41 2.170(5) . ?
Ag4 O43 2.530(5) 1_455 ?
O31 C32 1.236(8) . ?
O33 Ag3 2.475(5) 1_455 ?
O33 C32 1.274(8) . ?
O41 C42 1.260(8) . ?
O43 Ag4 2.530(5) 1_655 ?
O43 C42 1.252(8) . ?
C32 C34 1.544(9) . ?
C34 C35 1.518(9) . ?
C34 C36 1.529(9) . ?
C34 C37 1.535(10) . ?
C42 C44 1.559(9) . ?
C44 C45 1.520(11) . ?
C44 C46 1.522(10) . ?
C44 C47 1.534(10) . ?

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
Ag2 Ag1 Ag1 84.18(3) . 2_777 ?
O11 Ag1 Ag1 63.87(15) . 2_777 ?
O11 Ag1 Ag2 83.83(13) . . ?
O11 Ag1 O21 79.14(18) . 1_655 ?
O21 Ag1 Ag1 89.63(13) 1_655 2_777 ?
O21 Ag1 Ag2 162.91(12) 1_655 . ?
O23 Ag1 Ag1 131.61(15) . 2_777 ?
O23 Ag1 Ag2 78.82(13) . . ?
O23 Ag1 O11 154.5(2) . . ?
O23 Ag1 O21 116.70(17) . 1_655 ?
Ag1 Ag2 Ag2 80.95(3) . 2_677 ?
O11 Ag2 Ag1 162.25(12) 1_455 . ?
O11 Ag2 Ag2 93.59(13) 1_455 2_677 ?
O13 Ag2 Ag1 77.87(13) . . ?
O13 Ag2 Ag2 132.69(15) . 2_677 ?
O13 Ag2 O11 117.17(18) . 1_455 ?
O13 Ag2 O21 152.5(2) . . ?
O21 Ag2 Ag1 83.39(13) . . ?
O21 Ag2 Ag2 62.22(15) . 2_677 ?
O21 Ag2 O11 79.15(17) . 1_455 ?
Ag1 O11 Ag2 100.73(19) . 1_655 ?
C12 O11 Ag1 118.5(4) . . ?
C12 O11 Ag2 138.0(5) . 1_655 ?
C12 O13 Ag2 131.2(4) . . ?
Ag2 O21 Ag1 100.08(18) . 1_455 ?
C22 O21 Ag1 137.5(4) . 1_455 ?
C22 O21 Ag2 118.9(4) . . ?
C22 O23 Ag1 131.1(4) . . ?
O11 C12 C14 118.0(6) . . ?
O13 C12 O11 124.1(6) . . ?
O13 C12 C14 117.9(6) . . ?
C15 C14 C12 108.6(6) . . ?
C16 C14 C12 107.9(5) . . ?
C16 C14 C15 109.8(6) . . ?
C17 C14 C12 110.3(6) . . ?
C17 C14 C15 111.1(6) . . ?
C17 C14 C16 109.1(6) . . ?
O21 C22 C24 118.3(6) . . ?
O23 C22 O21 123.3(6) . . ?
O23 C22 C24 118.5(6) . . ?
C25 C24 C22 108.0(6) . . ?
C25 C24 C26 110.2(6) . . ?
C26 C24 C22 108.4(6) . . ?
C27 C24 C22 110.1(6) . . ?
C27 C24 C25 110.6(7) . . ?
C27 C24 C26 109.5(6) . . ?
Ag4 Ag3 Ag3 55.78(2) 2_666 2_666 ?
Ag4 Ag3 Ag3 61.83(2) . 2_666 ?
Ag4 Ag3 Ag4 117.61(2) . 2_666 ?
O31 Ag3 Ag3 115.65(15) . 2_666 ?
O31 Ag3 Ag4 77.85(13) . . ?
O31 Ag3 Ag4 129.24(15) . 2_666 ?
O31 Ag3 O33 115.18(18) . 1_655 ?
O31 Ag3 O43 149.0(2) . . ?
O33 Ag3 Ag3 116.56(13) 1_655 2_666 ?
O33 Ag3 Ag4 63.30(13) 1_655 2_666 ?
O33 Ag3 Ag4 163.35(12) 1_655 . ?
O43 Ag3 Ag3 76.50(14) . 2_666 ?
O43 Ag3 Ag4 81.54(14) . 2_666 ?
O43 Ag3 Ag4 84.65(12) . . ?
O43 Ag3 O33 79.02(17) . 1_655 ?
Ag3 Ag4 Ag3 62.39(2) . 2_666 ?
Ag3 Ag4 Ag4 104.76(3) . 2_566 ?
Ag4 Ag4 Ag3 71.62(2) 2_566 2_666 ?
O33 Ag4 Ag3 85.14(13) . . ?
O33 Ag4 Ag3 116.67(14) . 2_666 ?
O33 Ag4 Ag4 66.32(14) . 2_566 ?
O33 Ag4 O43 78.83(17) . 1_455 ?
O41 Ag4 Ag3 77.16(12) . . ?
O41 Ag4 Ag3 60.86(15) . 2_666 ?
O41 Ag4 Ag4 124.99(15) . 2_566 ?
O41 Ag4 O33 160.91(18) . . ?
O41 Ag4 O43 117.13(17) . 1_455 ?
O43 Ag4 Ag3 161.20(12) 1_455 . ?
O43 Ag4 Ag3 134.23(12) 1_455 2_666 ?
O43 Ag4 Ag4 77.76(12) 1_455 2_566 ?
C32 O31 Ag3 130.9(4) . . ?
Ag4 O33 Ag3 99.21(18) . 1_455 ?
C32 O33 Ag3 141.2(5) . 1_455 ?
C32 O33 Ag4 119.5(5) . . ?
C42 O41 Ag4 127.9(4) . . ?
Ag3 O43 Ag4 96.13(17) . 1_655 ?
C42 O43 Ag3 117.6(4) . . ?
C42 O43 Ag4 138.8(5) . 1_655 ?
O31 C32 O33 124.9(6) . . ?
O31 C32 C34 118.1(6) . . ?
O33 C32 C34 117.0(6) . . ?
C35 C34 C32 110.1(6) . . ?
C35 C34 C36 109.6(6) . . ?
C35 C34 C37 109.1(6) . . ?
C36 C34 C32 110.4(6) . . ?
C36 C34 C37 108.9(6) . . ?
C37 C34 C32 108.7(6) . . ?
O41 C42 C44 115.4(6) . . ?
O43 C42 O41 125.7(6) . . ?
O43 C42 C44 118.7(6) . . ?
C45 C44 C42 105.9(6) . . ?
C45 C44 C46 109.2(6) . . ?
C45 C44 C47 111.2(6) . . ?
C46 C44 C42 110.6(6) . . ?
C46 C44 C47 109.6(6) . . ?
C47 C44 C42 110.4(6) . . ?


_ins_header                      
;
TITL OIS-016_numabs_ana1 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   5.775206  13.482956  16.934656 108.2203  90.2400  94.7698
ZERR    8.00   0.000367   0.001024   0.001184   0.0065   0.0055   0.0057
LATT  1
SFAC C H O Ag
UNIT 40.00 72.00 16.00 8.00
TREF
HKLF 4
END
;
_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 1.270
_oxdiff_exptl_absorpt_empirical_full_min 0.747
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/DIPE'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1c
_database_code_depnum_ccdc_archive 'CCDC 2173464'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2022-04-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        
;
 ? 
;
_chemical_formula_moiety         'C24 H38 Ag2 N4 O4'
_chemical_formula_sum            'C24 H38 Ag2 N4 O4'
_chemical_formula_weight         662.32
_chemical_melting_point          ?
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'
Ag Ag -0.8971 1.1015 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.8349(11)
_cell_length_b                   9.4356(18)
_cell_length_c                   11.4549(19)
_cell_angle_alpha                82.991(14)
_cell_angle_beta                 72.900(14)
_cell_angle_gamma                73.381(15)
_cell_volume                     676.0(2)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    1211
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      23.8550
_cell_measurement_theta_min      2.9650
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             336
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -11 -7 0.0264
0 11 7 0.0264
9 6 7 0.1283
-9 -6 -7 0.1283
0 -8 11 0.0602
0 6 14 0.0425
9 8 1 0.1181
6 -3 13 0.1132
0 10 -9 0.0295
0 13 -2 0.0246
-1 4 14 0.0315
-4 2 12 0.0487
-7 5 -8 0.1048
8 -5 5 0.1124
1 1 -15 0.0452

_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.053
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
0.4946 -11.2937 -6.9648 -0.0779 0.9881 0.1329
-0.4946 11.2937 6.9648 0.0779 -0.9881 -0.1329
9.3005 6.2711 7.2431 -0.8102 -0.3358 0.4804
-9.3005 -6.2711 -7.2431 0.8102 0.3358 -0.4804
-0.0973 -8.4144 11.1564 0.4601 0.1906 0.8672
-0.0134 5.9530 14.0070 0.3149 -0.8476 0.4378
8.9951 7.9986 1.0701 -0.9845 -0.2600 0.1020
5.9817 -3.0213 12.9906 -0.1730 -0.0204 0.9902
0.0119 10.0088 -8.9411 -0.4119 -0.3705 -0.8273
0.0052 12.9853 -1.9376 -0.2545 -0.7943 -0.6084
-1.0132 3.9546 13.9940 0.4443 -0.7489 0.4756
-4.0096 1.9585 11.9761 0.7141 -0.6525 0.3351
-6.9858 5.0032 -7.9927 0.3868 -0.3063 -0.8692
7.9884 -4.9936 5.0009 -0.5729 0.4364 0.7657
1.0155 1.0404 -14.9696 -0.5489 0.4508 -0.7207

_exptl_special_details           
;
 ? 
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.1168
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4536
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.864
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0107
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00   0.00   1.00    2.00    --  -18.29 -57.00  60.00   87
  2  ω    -48.00  41.00   1.00    2.00    --  -18.29  77.00-150.00   89
  3  ω    -22.00  10.00   1.00    2.00    --  -18.29 -77.00  90.00   32
  4  ω    -20.00  10.00   1.00    2.00    --  -18.29 -77.00 -30.00   30
  5  ω    -39.00  -6.00   1.00    2.00    --  -18.29  57.00 -30.00   33
  6  ω    -50.00  40.00   1.00    2.00    --   19.23 -37.00 -60.00   90
  7  ω      3.00  31.00   1.00    2.00    --   19.23  77.00 -60.00   28
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0993176000
_diffrn_orient_matrix_UB_12      -0.0152506000
_diffrn_orient_matrix_UB_13      0.0288682000
_diffrn_orient_matrix_UB_21      0.0336579000
_diffrn_orient_matrix_UB_22      -0.0660197000
_diffrn_orient_matrix_UB_23      -0.0324200000
_diffrn_orient_matrix_UB_31      0.0408966000
_diffrn_orient_matrix_UB_32      -0.0396794000
_diffrn_orient_matrix_UB_33      0.0481609000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1914
_reflns_number_total             2745
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.608
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         2745
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0821
_refine_ls_R_factor_gt           0.0538
_refine_ls_restrained_S_all      0.903
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0514P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1124
_refine_special_details          Twin
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ag1 Ag 0.18187(7) 0.44658(6) 0.54058(4) 0.02661(18) Uani 1 1 d . . . . .
O11 O -0.0267(6) 0.5584(4) 0.7107(3) 0.0275(10) Uani 1 1 d . . . . .
O13 O -0.2954(6) 0.6776(5) 0.6308(3) 0.0309(10) Uani 1 1 d . . . . .
N1 N 0.4887(7) 0.3537(5) 0.6080(4) 0.0216(11) Uani 1 1 d . . . . .
N7 N 1.0576(7) 0.1733(5) 0.7034(4) 0.0277(12) Uani 1 1 d . . . . .
C2 C 0.5029(9) 0.3666(6) 0.7180(5) 0.0257(14) Uani 1 1 d . . . . .
H2 H 0.3827 0.4183 0.7744 0.031 Uiso 1 1 calc R . . . .
C3 C 0.6858(9) 0.3079(6) 0.7544(5) 0.0218(13) Uani 1 1 d . . . . .
H3 H 0.6865 0.3209 0.8335 0.026 Uiso 1 1 calc R . . . .
C4 C 0.8731(9) 0.2279(6) 0.6721(5) 0.0217(13) Uani 1 1 d . . . . .
C5 C 0.8535(9) 0.2144(6) 0.5551(5) 0.0224(13) Uani 1 1 d . . . . .
H5 H 0.9690 0.1622 0.4963 0.027 Uiso 1 1 calc R . . . .
C6 C 0.6636(9) 0.2784(6) 0.5280(5) 0.0264(14) Uani 1 1 d . . . . .
H6 H 0.6558 0.2690 0.4497 0.032 Uiso 1 1 calc R . . . .
C8 C 1.0690(9) 0.1883(7) 0.8250(5) 0.0315(15) Uani 1 1 d . . . . .
H8A H 1.0195 0.2909 0.8443 0.047 Uiso 1 1 calc GR . . . .
H8B H 1.2134 0.1505 0.8287 0.047 Uiso 1 1 calc GR . . . .
H8C H 0.9819 0.1335 0.8828 0.047 Uiso 1 1 calc GR . . . .
C9 C 1.2372(9) 0.0746(7) 0.6206(5) 0.0305(15) Uani 1 1 d . . . . .
H9A H 1.2049 -0.0175 0.6188 0.046 Uiso 1 1 calc GR . . . .
H9B H 1.3613 0.0566 0.6491 0.046 Uiso 1 1 calc GR . . . .
H9C H 1.2629 0.1201 0.5399 0.046 Uiso 1 1 calc GR . . . .
C12 C -0.2029(9) 0.6480(6) 0.7154(5) 0.0233(13) Uani 1 1 d . . . . .
C14 C -0.3129(9) 0.7373(7) 0.8315(5) 0.0276(14) Uani 1 1 d . . . . .
C15 C -0.5546(9) 0.7592(7) 0.8630(5) 0.0363(17) Uani 1 1 d . . . . .
H15A H -0.6044 0.8034 0.7935 0.055 Uiso 1 1 calc GR . . . .
H15B H -0.6238 0.8228 0.9307 0.055 Uiso 1 1 calc GR . . . .
H15C H -0.5861 0.6650 0.8844 0.055 Uiso 1 1 calc GR . . . .
C16 C -0.2639(11) 0.8873(7) 0.8021(5) 0.0416(18) Uani 1 1 d . . . . .
H16A H -0.1139 0.8742 0.7858 0.062 Uiso 1 1 calc GR . . . .
H16B H -0.3376 0.9494 0.8705 0.062 Uiso 1 1 calc GR . . . .
H16C H -0.3093 0.9329 0.7315 0.062 Uiso 1 1 calc GR . . . .
C17 C -0.2290(11) 0.6595(8) 0.9388(5) 0.0445(19) Uani 1 1 d . . . . .
H17A H -0.2603 0.5649 0.9567 0.067 Uiso 1 1 calc GR . . . .
H17B H -0.2959 0.7189 1.0093 0.067 Uiso 1 1 calc GR . . . .
H17C H -0.0783 0.6456 0.9180 0.067 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ag1 Ag1 2.7853(10) 2_566 ?
Ag1 O11 2.225(4) . ?
Ag1 O13 2.231(4) 2_566 ?
Ag1 N1 2.345(5) . ?
O11 C12 1.248(6) . ?
O13 Ag1 2.231(4) 2_566 ?
O13 C12 1.269(6) . ?
N1 C2 1.315(7) . ?
N1 C6 1.343(7) . ?
N7 C4 1.354(7) . ?
N7 C8 1.444(7) . ?
N7 C9 1.466(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.378(7) . ?
C3 H3 0.9300 . ?
C3 C4 1.417(7) . ?
C4 C5 1.410(7) . ?
C5 H5 0.9300 . ?
C5 C6 1.375(8) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C12 C14 1.538(8) . ?
C14 C15 1.541(8) . ?
C14 C16 1.522(8) . ?
C14 C17 1.527(8) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

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
O11 Ag1 Ag1 83.33(10) . 2_566 ?
O11 Ag1 O13 162.00(14) . 2_566 ?
O11 Ag1 N1 97.16(14) . . ?
O13 Ag1 Ag1 81.79(10) 2_566 2_566 ?
O13 Ag1 N1 97.64(15) 2_566 . ?
N1 Ag1 Ag1 179.29(12) . 2_566 ?
C12 O11 Ag1 122.7(3) . . ?
C12 O13 Ag1 123.8(4) . 2_566 ?
C2 N1 Ag1 125.6(4) . . ?
C2 N1 C6 117.3(5) . . ?
C6 N1 Ag1 117.1(3) . . ?
C4 N7 C8 121.0(5) . . ?
C4 N7 C9 119.2(5) . . ?
C8 N7 C9 118.8(5) . . ?
N1 C2 H2 118.2 . . ?
N1 C2 C3 123.6(5) . . ?
C3 C2 H2 118.2 . . ?
C2 C3 H3 119.8 . . ?
C2 C3 C4 120.4(5) . . ?
C4 C3 H3 119.8 . . ?
N7 C4 C3 122.0(5) . . ?
N7 C4 C5 123.1(5) . . ?
C5 C4 C3 114.9(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 C4 120.0(5) . . ?
C6 C5 H5 120.0 . . ?
N1 C6 C5 123.8(5) . . ?
N1 C6 H6 118.1 . . ?
C5 C6 H6 118.1 . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7 C9 H9A 109.5 . . ?
N7 C9 H9B 109.5 . . ?
N7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O11 C12 O13 126.0(5) . . ?
O11 C12 C14 117.2(5) . . ?
O13 C12 C14 116.7(5) . . ?
C12 C14 C15 109.7(5) . . ?
C16 C14 C12 106.6(4) . . ?
C16 C14 C15 109.4(5) . . ?
C16 C14 C17 109.9(5) . . ?
C17 C14 C12 111.0(5) . . ?
C17 C14 C15 110.2(5) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?

_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 1.293
_oxdiff_exptl_absorpt_empirical_full_min 0.736
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.8867 3375 1473 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000
1.0000
2 0.1133 3564 1473 nmt 1.0399 -0.0566 -0.0470 0.1248 0.9738 -0.0314 0.1501
-0.0130 0.9728

_twin_special_details            
;
Component 2 rotated by 6.4240° 
around [0.09 -0.62 0.78] (reciprocal) or [0.20 -0.78 0.59] (direct)
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetone+DMSO'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2b
_database_code_depnum_ccdc_archive 'CCDC 2173465'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2021-10-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H16 I N O2'
_chemical_formula_sum            'C11 H16 I N O2'
_chemical_formula_weight         321.15
_chemical_melting_point          ?
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'
I I -0.4742 1.8119 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.6777(3)
_cell_length_b                   8.6359(5)
_cell_length_c                   13.1369(8)
_cell_angle_alpha                76.766(5)
_cell_angle_beta                 78.689(5)
_cell_angle_gamma                86.009(4)
_cell_volume                     614.64(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    2380
_cell_measurement_temperature    119.98(13)
_cell_measurement_theta_max      28.4710
_cell_measurement_theta_min      2.6050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.587
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             316
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 6 7 0.0684
0 -12 -8 0.0662
5 10 9 0.0733
-3 10 6 0.1026
-7 -6 -7 0.0736
1 -2 17 0.0165
5 10 2 0.0618
-4 9 -6 0.0904
0 12 0 0.0863
-1 1 -18 0.0068
6 7 -3 0.0525
0 2 18 0.0390
0 -5 -18 0.0279
2 6 -13 0.0207
2 4 -14 0.0135

_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.027
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
7.0292 6.3643 7.1905 -0.0841 0.2838 0.9552
0.4596 -11.6565 -8.2613 -0.2095 0.7068 -0.6756
4.5242 10.1588 9.0127 0.0483 -0.1630 0.9854
-3.4696 10.1937 6.0953 0.2668 -0.9003 0.3438
-7.0374 -6.3433 -7.1783 0.0847 -0.2857 -0.9546
0.6378 -2.1688 16.9092 0.9531 0.2825 0.1086
5.1515 9.5310 1.8188 -0.3642 -0.1078 0.9251
-4.1910 8.6822 -6.0144 -0.3326 -0.9396 0.0814
-0.0668 11.8766 0.2228 -0.2580 -0.7291 0.6339
-1.3366 0.9703 -17.6324 -0.9322 -0.2762 -0.2339
5.7826 6.8637 -3.4985 -0.6264 0.0825 0.7751
-0.3294 1.5423 17.9203 0.9695 -0.0253 0.2439
-0.1765 -5.2211 -17.7959 -0.8538 0.2048 -0.4786
1.6864 5.7808 -12.6602 -0.9123 -0.2703 0.3076
1.8567 4.3963 -13.8826 -0.9560 -0.1773 0.2337

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0688
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4129
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.424
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.98(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -38.00  49.00   1.00    2.50    --  -18.45  57.00   0.00   87
  2  ω    -35.00  47.00   1.00    2.50    --  -18.45  57.00-120.00   82
  3  ω    -37.00  48.00   1.00    2.50    --  -18.45  57.00 120.00   85
  4  ω     -2.00  26.00   1.00    2.50    --   19.23  77.00  90.00   28
  5  ω    -10.00  24.00   1.00    2.50    --   19.23  77.00 -30.00   34
  6  ω     -8.00  29.00   1.00    2.50    --   19.23  77.00-150.00   37
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0475852000
_diffrn_orient_matrix_UB_12      -0.0230304000
_diffrn_orient_matrix_UB_13      0.0552069000
_diffrn_orient_matrix_UB_21      0.0899687000
_diffrn_orient_matrix_UB_22      -0.0609834000
_diffrn_orient_matrix_UB_23      0.0054915000
_diffrn_orient_matrix_UB_31      0.0767043000
_diffrn_orient_matrix_UB_32      0.0536136000
_diffrn_orient_matrix_UB_33      0.0104040000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2254
_reflns_number_total             2509
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2509
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0355
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0124P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0655
_refine_special_details          ?
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.29764(5) 0.22168(3) 0.61834(2) 0.01576(9) Uani 1 1 d . . . . .
O11 O 0.4643(5) 0.1940(3) 0.7565(2) 0.0214(7) Uani 1 1 d . . . . .
O13 O 0.6313(5) 0.4322(3) 0.6931(2) 0.0220(7) Uani 1 1 d . . . . .
N1 N 0.1181(6) 0.2260(4) 0.4767(3) 0.0133(7) Uani 1 1 d . . . . .
C2 C -0.0819(7) 0.3131(5) 0.4623(3) 0.0167(9) Uani 1 1 d . . . . .
H2 H -0.1503 0.3733 0.5114 0.020 Uiso 1 1 calc R . . . .
C3 C -0.1892(7) 0.3156(5) 0.3762(3) 0.0168(9) Uani 1 1 d . . . . .
H3 H -0.3281 0.3771 0.3679 0.020 Uiso 1 1 calc R . . . .
C4 C -0.0904(8) 0.2267(5) 0.3021(3) 0.0174(9) Uani 1 1 d . . . . .
C5 C 0.1174(7) 0.1361(5) 0.3186(4) 0.0192(10) Uani 1 1 d . . . . .
H5 H 0.1891 0.0741 0.2711 0.023 Uiso 1 1 calc R . . . .
C6 C 0.2149(8) 0.1394(5) 0.4057(3) 0.0195(10) Uani 1 1 d . . . . .
H6 H 0.3540 0.0790 0.4159 0.023 Uiso 1 1 calc R . . . .
C7 C -0.2019(8) 0.2283(5) 0.2071(3) 0.0256(11) Uani 1 1 d . . . . .
H7A H -0.2749 0.1280 0.2158 0.038 Uiso 1 1 calc GR . . . .
H7B H -0.0800 0.2458 0.1440 0.038 Uiso 1 1 calc GR . . . .
H7C H -0.3220 0.3121 0.2009 0.038 Uiso 1 1 calc GR . . . .
C12 C 0.5898(7) 0.3123(5) 0.7640(3) 0.0137(9) Uani 1 1 d . . . . .
C14 C 0.6685(7) 0.2889(4) 0.8709(3) 0.0142(9) Uani 1 1 d . . . . .
C15 C 0.7861(8) 0.1234(5) 0.9011(3) 0.0203(10) Uani 1 1 d . . . . .
H15A H 0.6730 0.0433 0.9058 0.030 Uiso 1 1 calc GR . . . .
H15B H 0.8343 0.1112 0.9687 0.030 Uiso 1 1 calc GR . . . .
H15C H 0.9245 0.1123 0.8478 0.030 Uiso 1 1 calc GR . . . .
C16 C 0.8451(7) 0.4173(5) 0.8660(3) 0.0199(10) Uani 1 1 d . . . . .
H16A H 0.9872 0.4062 0.8146 0.030 Uiso 1 1 calc GR . . . .
H16B H 0.8874 0.4058 0.9347 0.030 Uiso 1 1 calc GR . . . .
H16C H 0.7717 0.5204 0.8457 0.030 Uiso 1 1 calc GR . . . .
C17 C 0.4423(7) 0.3042(5) 0.9544(3) 0.0213(10) Uani 1 1 d . . . . .
H17A H 0.3731 0.4095 0.9378 0.032 Uiso 1 1 calc GR . . . .
H17B H 0.4845 0.2849 1.0236 0.032 Uiso 1 1 calc GR . . . .
H17C H 0.3277 0.2277 0.9541 0.032 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O11 2.166(3) . ?
I1 N1 2.283(3) . ?
O11 C12 1.317(4) . ?
O13 C12 1.225(5) . ?
N1 C2 1.338(5) . ?
N1 C6 1.338(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.381(5) . ?
C3 H3 0.9300 . ?
C3 C4 1.385(6) . ?
C4 C5 1.395(6) . ?
C4 C7 1.503(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.372(6) . ?
C6 H6 0.9300 . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C12 C14 1.522(5) . ?
C14 C15 1.535(5) . ?
C14 C16 1.528(5) . ?
C14 C17 1.536(5) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?

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
O11 I1 N1 174.71(10) . . ?
C12 O11 I1 118.4(2) . . ?
C2 N1 I1 121.8(3) . . ?
C6 N1 I1 119.4(3) . . ?
C6 N1 C2 118.8(4) . . ?
N1 C2 H2 119.2 . . ?
N1 C2 C3 121.6(4) . . ?
C3 C2 H2 119.2 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.1(4) . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 117.5(4) . . ?
C3 C4 C7 121.3(4) . . ?
C5 C4 C7 121.1(4) . . ?
C4 C5 H5 120.4 . . ?
C6 C5 C4 119.3(4) . . ?
C6 C5 H5 120.4 . . ?
N1 C6 C5 122.7(4) . . ?
N1 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O11 C12 C14 113.6(3) . . ?
O13 C12 O11 123.1(4) . . ?
O13 C12 C14 123.3(3) . . ?
C12 C14 C15 110.8(3) . . ?
C12 C14 C16 109.7(3) . . ?
C12 C14 C17 107.3(3) . . ?
C15 C14 C17 109.3(3) . . ?
C16 C14 C15 109.9(3) . . ?
C16 C14 C17 109.8(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?


_ins_header                      
;
TITL OIK053_scale2 in P-1 
REM P-1 (#2 in standard setting)
CELL 0.71073   5.677672   8.635945  13.136891  76.7655  78.6890  86.0091
ZERR    2.00   0.000297   0.000451   0.000810   0.0049   0.0048   0.0043
LATT  1
SFAC C H N O I
UNIT 22.00 32.00 2.00 4.00 2.00
TREF
HKLF 4
END
;
_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 1.109
_oxdiff_exptl_absorpt_empirical_full_min 0.863
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene/pentane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2c
_database_code_depnum_ccdc_archive 'CCDC 2173466'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2021-02-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C12 H19 I N2 O2'
_chemical_formula_sum            'C12 H19 I N2 O2'
_chemical_formula_weight         350.19
_chemical_melting_point          ?
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4936(5)
_cell_length_b                   14.6196(7)
_cell_length_c                   14.9627(7)
_cell_angle_alpha                95.341(4)
_cell_angle_beta                 91.077(4)
_cell_angle_gamma                107.447(4)
_cell_volume                     2177.71(19)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    8187
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.6050
_cell_measurement_theta_min      3.1450
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    17.287
_exptl_absorpt_correction_T_max  0.505
_exptl_absorpt_correction_T_min  0.040
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 0 10 0.0197
1 0 -10 0.0217
-7 1 0 0.1016
7 -1 0 0.1076
0 -9 1 0.1036
0 9 -1 0.0996
-2 -7 -2 0.1140
0 -8 -4 0.0986
0 8 5 0.0835

_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.041
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
-0.7009 0.3293 9.6220 0.0785 -0.9969 0.0090
0.7009 -0.3293 -9.6220 -0.0785 0.9969 -0.0090
-6.5782 0.5571 -0.4867 0.7822 0.0621 0.6199
6.5782 -0.5571 0.4867 -0.7822 -0.0621 -0.6199
0.1709 -9.1209 1.1357 -0.4342 -0.0334 0.9002
-0.1709 9.1209 -1.1357 0.4342 0.0334 -0.9002
-1.9899 -6.9988 -1.9988 -0.0843 0.2768 0.9171
0.0105 -7.9995 -3.9979 -0.3559 0.4878 0.8192
-0.0112 8.0000 4.9971 0.3543 -0.5912 -0.8223

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14919
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.115
_diffrn_reflns_theta_min         2.970
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.989
_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 -20.00   1.00    1.00    --  -41.65 -37.00-150.00   96
  2  ω    -74.00  33.00   1.00    1.00    --  -41.65  77.00   0.00  107
  3  ω     14.00 115.00   1.00    1.00    --   41.65  57.00 120.00  101
  4  ω     27.00  98.00   1.00    1.00    --   41.65-125.00-120.00   71
  5  ω     40.00 109.00   1.00    1.00    --  112.00-111.00 -60.00   69
  6  ω     37.00 109.00   1.00    1.00    --  112.00-111.00 150.00   72
  7  ω     36.00 137.00   1.00    1.00    --  112.00 -77.00 -30.00  101
  8  ω     37.00 140.00   1.00    1.00    --  112.00 -30.00 -30.00  103
  9  ω    124.00 178.00   1.00    1.00    --  112.00  77.00 150.00   54
 10  ω     40.00  90.00   1.00    1.00    --  112.00 -61.00-180.00   50
 11  ω    106.00 140.00   1.00    1.00    --  112.00 -61.00-180.00   34
 12  ω     99.00 177.00   1.00    1.00    --  112.00  45.00 -30.00   78
 13  ω    120.00 156.00   1.00    1.00    --  112.00 111.00 -90.00   36
 14  ω     36.00 106.00   1.00    1.00    --  112.00 -94.00-180.00   70
 15  ω     32.00 151.00   1.00    1.00    --  112.00 -15.00 150.00  119
;
_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      -0.1149525000
_diffrn_orient_matrix_UB_12      0.0452291000
_diffrn_orient_matrix_UB_13      -0.0017675000
_diffrn_orient_matrix_UB_21      -0.0025652000
_diffrn_orient_matrix_UB_22      -0.0092681000
_diffrn_orient_matrix_UB_23      -0.1034736000
_diffrn_orient_matrix_UB_31      -0.1025603000
_diffrn_orient_matrix_UB_32      -0.1010024000
_diffrn_orient_matrix_UB_33      -0.0030784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7561
_reflns_number_total             8483
_reflns_odcompleteness_completeness 98.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         8483
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0362
_refine_ls_restrained_S_all      1.035
_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)+(0.0523P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0969
_refine_special_details          ?
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C22(H22), C23(H23), C25(H25), C26(H26),
 C42(H42), C43(H43), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C35(H35A,H35B,
 H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C48(H48A,H48B,H48C), C49(H49A,
 H49B,H49C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.88441(2) 0.90284(2) 0.60126(2) 0.02485(8) Uani 1 1 d . . . . .
I2 I 0.82722(3) 0.41202(2) 0.40203(2) 0.02714(8) Uani 1 1 d . . . . .
I3 I 0.42926(2) 0.82304(2) 0.32969(2) 0.02377(7) Uani 1 1 d . . . . .
O11 O 0.8946(3) 1.0061(2) 0.7169(2) 0.0366(7) Uani 1 1 d . . . . .
O13 O 0.7260(3) 0.9034(2) 0.7797(2) 0.0359(7) Uani 1 1 d . . . . .
O31 O 0.9453(3) 0.3527(3) 0.30912(19) 0.0350(7) Uani 1 1 d . . . . .
O33 O 0.8344(4) 0.3817(3) 0.1908(2) 0.0423(8) Uani 1 1 d . . . . .
O51 O 0.4327(4) 0.7808(3) 0.1867(2) 0.0428(9) Uani 1 1 d . . . . .
O53 O 0.5842(4) 0.7055(3) 0.2013(2) 0.0458(9) Uani 1 1 d . . . . .
N1 N 0.9018(3) 0.8042(3) 0.4787(2) 0.0256(7) Uani 1 1 d . . . . .
N7 N 0.9670(4) 0.6398(3) 0.2510(2) 0.0315(8) Uani 1 1 d . . . . .
N21 N 0.7131(4) 0.4723(3) 0.5074(2) 0.0273(7) Uani 1 1 d . . . . .
N27 N 0.5076(4) 0.5821(2) 0.7035(2) 0.0271(7) Uani 1 1 d . . . . .
N41 N 0.4047(3) 0.8722(2) 0.4739(2) 0.0230(6) Uani 1 1 d . . . . .
N47 N 0.3408(3) 0.9578(3) 0.7389(2) 0.0258(7) Uani 1 1 d . . . . .
C2 C 0.8303(4) 0.7944(3) 0.4003(3) 0.0297(9) Uani 1 1 d . . . . .
H2 H 0.7656 0.8260 0.3985 0.036 Uiso 1 1 calc R . . . .
C3 C 0.8464(4) 0.7419(3) 0.3244(3) 0.0302(9) Uani 1 1 d . . . . .
H3 H 0.7933 0.7377 0.2728 0.036 Uiso 1 1 calc R . . . .
C4 C 0.9447(4) 0.6935(3) 0.3243(3) 0.0263(8) Uani 1 1 d . . . . .
C5 C 1.0202(4) 0.7033(3) 0.4064(3) 0.0271(8) Uani 1 1 d . . . . .
H5 H 1.0864 0.6733 0.4100 0.033 Uiso 1 1 calc R . . . .
C6 C 0.9952(4) 0.7572(3) 0.4801(3) 0.0270(8) Uani 1 1 d . . . . .
H6 H 1.0447 0.7618 0.5335 0.032 Uiso 1 1 calc R . . . .
C8 C 0.8892(6) 0.6268(4) 0.1662(3) 0.0427(12) Uani 1 1 d . . . . .
H8A H 0.8050 0.6376 0.1776 0.064 Uiso 1 1 calc GR . . . .
H8B H 0.8740 0.5622 0.1385 0.064 Uiso 1 1 calc GR . . . .
H8C H 0.9376 0.6718 0.1269 0.064 Uiso 1 1 calc GR . . . .
C9 C 1.0780(5) 0.5988(4) 0.2522(3) 0.0404(11) Uani 1 1 d . . . . .
H9A H 1.1606 0.6497 0.2649 0.061 Uiso 1 1 calc GR . . . .
H9B H 1.0804 0.5644 0.1947 0.061 Uiso 1 1 calc GR . . . .
H9C H 1.0658 0.5553 0.2978 0.061 Uiso 1 1 calc GR . . . .
C12 C 0.8167(4) 0.9774(3) 0.7831(3) 0.0234(8) Uani 1 1 d . . . . .
C14 C 0.8543(4) 1.0506(3) 0.8682(2) 0.0249(8) Uani 1 1 d . . . . .
C15 C 0.8262(5) 1.1437(3) 0.8476(3) 0.0312(9) Uani 1 1 d . . . . .
H15A H 0.8741 1.1674 0.7963 0.047 Uiso 1 1 calc GR . . . .
H15B H 0.8548 1.1912 0.8986 0.047 Uiso 1 1 calc GR . . . .
H15C H 0.7320 1.1308 0.8351 0.047 Uiso 1 1 calc GR . . . .
C16 C 1.0037(4) 1.0729(3) 0.8931(3) 0.0316(9) Uani 1 1 d . . . . .
H16A H 1.0222 1.0145 0.9047 0.047 Uiso 1 1 calc GR . . . .
H16B H 1.0272 1.1182 0.9459 0.047 Uiso 1 1 calc GR . . . .
H16C H 1.0552 1.0999 0.8443 0.047 Uiso 1 1 calc GR . . . .
C17 C 0.7718(5) 1.0084(4) 0.9457(3) 0.0339(10) Uani 1 1 d . . . . .
H17A H 0.6785 0.9959 0.9303 0.051 Uiso 1 1 calc GR . . . .
H17B H 0.7966 1.0535 0.9986 0.051 Uiso 1 1 calc GR . . . .
H17C H 0.7884 0.9493 0.9571 0.051 Uiso 1 1 calc GR . . . .
C22 C 0.7134(4) 0.5649(3) 0.5127(3) 0.0298(9) Uani 1 1 d . . . . .
H22 H 0.7597 0.6041 0.4710 0.036 Uiso 1 1 calc R . . . .
C23 C 0.6485(4) 0.6032(3) 0.5767(3) 0.0293(9) Uani 1 1 d . . . . .
H23 H 0.6535 0.6679 0.5787 0.035 Uiso 1 1 calc R . . . .
C24 C 0.5742(4) 0.5468(3) 0.6399(3) 0.0237(8) Uani 1 1 d . . . . .
C25 C 0.5748(4) 0.4493(3) 0.6337(3) 0.0264(8) Uani 1 1 d . . . . .
H25 H 0.5288 0.4082 0.6742 0.032 Uiso 1 1 calc R . . . .
C26 C 0.6436(4) 0.4166(3) 0.5678(3) 0.0282(8) Uani 1 1 d . . . . .
H26 H 0.6425 0.3526 0.5645 0.034 Uiso 1 1 calc R . . . .
C28 C 0.5193(5) 0.6852(3) 0.7144(3) 0.0360(10) Uani 1 1 d . . . . .
H28A H 0.6111 0.7222 0.7278 0.054 Uiso 1 1 calc GR . . . .
H28B H 0.4660 0.6979 0.7627 0.054 Uiso 1 1 calc GR . . . .
H28C H 0.4882 0.7030 0.6597 0.054 Uiso 1 1 calc GR . . . .
C29 C 0.4242(5) 0.5209(3) 0.7637(3) 0.0355(10) Uani 1 1 d . . . . .
H29A H 0.3694 0.4629 0.7300 0.053 Uiso 1 1 calc GR . . . .
H29B H 0.3681 0.5542 0.7933 0.053 Uiso 1 1 calc GR . . . .
H29C H 0.4796 0.5050 0.8077 0.053 Uiso 1 1 calc GR . . . .
C32 C 0.9220(4) 0.3534(3) 0.2238(3) 0.0264(8) Uani 1 1 d . . . . .
C34 C 1.0163(5) 0.3138(3) 0.1646(3) 0.0295(9) Uani 1 1 d . . . . .
C35 C 0.9703(6) 0.2046(4) 0.1650(4) 0.0493(13) Uani 1 1 d . . . . .
H35A H 0.9786 0.1886 0.2252 0.074 Uiso 1 1 calc GR . . . .
H35B H 1.0249 0.1771 0.1269 0.074 Uiso 1 1 calc GR . . . .
H35C H 0.8786 0.1793 0.1433 0.074 Uiso 1 1 calc GR . . . .
C36 C 1.1592(5) 0.3535(4) 0.2039(3) 0.0464(13) Uani 1 1 d . . . . .
H36A H 1.1874 0.4226 0.2067 0.070 Uiso 1 1 calc GR . . . .
H36B H 1.2170 0.3286 0.1664 0.070 Uiso 1 1 calc GR . . . .
H36C H 1.1635 0.3344 0.2632 0.070 Uiso 1 1 calc GR . . . .
C37 C 1.0089(6) 0.3402(4) 0.0694(3) 0.0448(12) Uani 1 1 d . . . . .
H37A H 0.9197 0.3111 0.0438 0.067 Uiso 1 1 calc GR . . . .
H37B H 1.0704 0.3172 0.0339 0.067 Uiso 1 1 calc GR . . . .
H37C H 1.0319 0.4090 0.0703 0.067 Uiso 1 1 calc GR . . . .
C42 C 0.3081(4) 0.9136(3) 0.4938(3) 0.0258(8) Uani 1 1 d . . . . .
H42 H 0.2549 0.9224 0.4469 0.031 Uiso 1 1 calc R . . . .
C43 C 0.2850(4) 0.9433(3) 0.5801(3) 0.0251(8) Uani 1 1 d . . . . .
H43 H 0.2170 0.9712 0.5905 0.030 Uiso 1 1 calc R . . . .
C44 C 0.3637(4) 0.9318(3) 0.6531(3) 0.0235(8) Uani 1 1 d . . . . .
C45 C 0.4681(4) 0.8921(3) 0.6307(3) 0.0252(8) Uani 1 1 d . . . . .
H45 H 0.5262 0.8853 0.6756 0.030 Uiso 1 1 calc R . . . .
C46 C 0.4830(4) 0.8640(3) 0.5427(3) 0.0243(8) Uani 1 1 d . . . . .
H46 H 0.5516 0.8375 0.5298 0.029 Uiso 1 1 calc R . . . .
C48 C 0.2465(4) 1.0113(3) 0.7589(3) 0.0299(9) Uani 1 1 d . . . . .
H48A H 0.2806 1.0747 0.7399 0.045 Uiso 1 1 calc GR . . . .
H48B H 0.2345 1.0163 0.8224 0.045 Uiso 1 1 calc GR . . . .
H48C H 0.1622 0.9782 0.7276 0.045 Uiso 1 1 calc GR . . . .
C49 C 0.4287(5) 0.9510(4) 0.8131(3) 0.0350(10) Uani 1 1 d . . . . .
H49A H 0.4396 0.8879 0.8081 0.053 Uiso 1 1 calc GR . . . .
H49B H 0.3901 0.9623 0.8691 0.053 Uiso 1 1 calc GR . . . .
H49C H 0.5144 0.9984 0.8107 0.053 Uiso 1 1 calc GR . . . .
C52 C 0.5060(4) 0.7300(3) 0.1564(3) 0.0260(8) Uani 1 1 d . . . . .
C54 C 0.4823(5) 0.6989(4) 0.0536(3) 0.0336(10) Uani 1 1 d . . . . .
C55 C 0.3507(6) 0.6161(5) 0.0415(3) 0.0525(14) Uani 1 1 d . . . . .
H55A H 0.3574 0.5650 0.0753 0.079 Uiso 1 1 calc GR . . . .
H55B H 0.3335 0.5926 -0.0210 0.079 Uiso 1 1 calc GR . . . .
H55C H 0.2789 0.6390 0.0626 0.079 Uiso 1 1 calc GR . . . .
C56 C 0.4680(8) 0.7821(5) 0.0043(3) 0.0596(17) Uani 1 1 d . . . . .
H56A H 0.3982 0.8048 0.0295 0.089 Uiso 1 1 calc GR . . . .
H56B H 0.4461 0.7604 -0.0583 0.089 Uiso 1 1 calc GR . . . .
H56C H 0.5508 0.8336 0.0105 0.089 Uiso 1 1 calc GR . . . .
C57 C 0.5946(6) 0.6629(5) 0.0174(4) 0.0562(16) Uani 1 1 d . . . . .
H57A H 0.6767 0.7151 0.0227 0.084 Uiso 1 1 calc GR . . . .
H57B H 0.5741 0.6383 -0.0446 0.084 Uiso 1 1 calc GR . . . .
H57C H 0.6042 0.6125 0.0513 0.084 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O11 2.166(3) . ?
I1 N1 2.270(3) . ?
I2 O31 2.169(3) . ?
I2 N21 2.267(3) . ?
I3 O51 2.175(3) . ?
I3 N41 2.255(3) . ?
O11 C12 1.314(5) . ?
O13 C12 1.204(5) . ?
O31 C32 1.297(5) . ?
O33 C32 1.228(5) . ?
O51 C52 1.280(5) . ?
O53 C52 1.206(5) . ?
N1 C2 1.353(5) . ?
N1 C6 1.356(5) . ?
N7 C4 1.355(5) . ?
N7 C8 1.460(5) . ?
N7 C9 1.461(6) . ?
N21 C22 1.348(6) . ?
N21 C26 1.349(5) . ?
N27 C24 1.345(5) . ?
N27 C28 1.468(5) . ?
N27 C29 1.445(6) . ?
N41 C42 1.352(5) . ?
N41 C46 1.342(5) . ?
N47 C44 1.351(5) . ?
N47 C48 1.453(5) . ?
N47 C49 1.459(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.353(6) . ?
C3 H3 0.9300 . ?
C3 C4 1.415(6) . ?
C4 C5 1.421(5) . ?
C5 H5 0.9300 . ?
C5 C6 1.371(5) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C12 C14 1.548(5) . ?
C14 C15 1.534(6) . ?
C14 C16 1.533(5) . ?
C14 C17 1.525(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C22 H22 0.9300 . ?
C22 C23 1.359(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.404(6) . ?
C24 C25 1.421(6) . ?
C25 H25 0.9300 . ?
C25 C26 1.367(6) . ?
C26 H26 0.9300 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C32 C34 1.542(6) . ?
C34 C35 1.524(7) . ?
C34 C36 1.520(6) . ?
C34 C37 1.516(6) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C42 H42 0.9300 . ?
C42 C43 1.374(5) . ?
C43 H43 0.9300 . ?
C43 C44 1.410(5) . ?
C44 C45 1.417(6) . ?
C45 H45 0.9300 . ?
C45 C46 1.369(5) . ?
C46 H46 0.9300 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C52 C54 1.557(5) . ?
C54 C55 1.533(7) . ?
C54 C56 1.523(7) . ?
C54 C57 1.518(7) . ?
C55 H55A 0.9600 . ?
C55 H55B 0.9600 . ?
C55 H55C 0.9600 . ?
C56 H56A 0.9600 . ?
C56 H56B 0.9600 . ?
C56 H56C 0.9600 . ?
C57 H57A 0.9600 . ?
C57 H57B 0.9600 . ?
C57 H57C 0.9600 . ?

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
O11 I1 N1 172.73(13) . . ?
O31 I2 N21 175.86(12) . . ?
O51 I3 N41 173.32(12) . . ?
C12 O11 I1 117.8(3) . . ?
C32 O31 I2 118.0(3) . . ?
C52 O51 I3 121.7(3) . . ?
C2 N1 I1 123.6(3) . . ?
C2 N1 C6 116.8(3) . . ?
C6 N1 I1 119.4(2) . . ?
C4 N7 C8 121.9(4) . . ?
C4 N7 C9 120.5(4) . . ?
C8 N7 C9 117.4(4) . . ?
C22 N21 I2 121.5(3) . . ?
C22 N21 C26 117.6(4) . . ?
C26 N21 I2 120.9(3) . . ?
C24 N27 C28 120.5(4) . . ?
C24 N27 C29 121.6(4) . . ?
C29 N27 C28 117.9(4) . . ?
C42 N41 I3 119.6(2) . . ?
C46 N41 I3 123.4(3) . . ?
C46 N41 C42 117.1(3) . . ?
C44 N47 C48 120.9(3) . . ?
C44 N47 C49 120.8(4) . . ?
C48 N47 C49 117.1(3) . . ?
N1 C2 H2 117.7 . . ?
C3 C2 N1 124.6(4) . . ?
C3 C2 H2 117.7 . . ?
C2 C3 H3 120.3 . . ?
C2 C3 C4 119.4(4) . . ?
C4 C3 H3 120.3 . . ?
N7 C4 C3 122.9(4) . . ?
N7 C4 C5 120.7(4) . . ?
C3 C4 C5 116.4(4) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 C4 119.8(4) . . ?
C6 C5 H5 120.1 . . ?
N1 C6 C5 123.0(4) . . ?
N1 C6 H6 118.5 . . ?
C5 C6 H6 118.5 . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
N7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N7 C9 H9A 109.5 . . ?
N7 C9 H9B 109.5 . . ?
N7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O11 C12 C14 112.1(3) . . ?
O13 C12 O11 125.2(4) . . ?
O13 C12 C14 122.7(4) . . ?
C15 C14 C12 108.7(3) . . ?
C16 C14 C12 109.3(3) . . ?
C16 C14 C15 109.1(4) . . ?
C17 C14 C12 109.7(4) . . ?
C17 C14 C15 110.1(4) . . ?
C17 C14 C16 109.8(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N21 C22 H22 118.8 . . ?
N21 C22 C23 122.5(4) . . ?
C23 C22 H22 118.8 . . ?
C22 C23 H23 119.4 . . ?
C22 C23 C24 121.2(4) . . ?
C24 C23 H23 119.4 . . ?
N27 C24 C23 122.7(4) . . ?
N27 C24 C25 121.5(4) . . ?
C23 C24 C25 115.8(4) . . ?
C24 C25 H25 120.3 . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 H25 120.3 . . ?
N21 C26 C25 123.5(4) . . ?
N21 C26 H26 118.2 . . ?
C25 C26 H26 118.2 . . ?
N27 C28 H28A 109.5 . . ?
N27 C28 H28B 109.5 . . ?
N27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N27 C29 H29A 109.5 . . ?
N27 C29 H29B 109.5 . . ?
N27 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
O31 C32 C34 113.3(4) . . ?
O33 C32 O31 125.1(4) . . ?
O33 C32 C34 121.6(4) . . ?
C35 C34 C32 107.1(4) . . ?
C36 C34 C32 110.2(3) . . ?
C36 C34 C35 108.9(4) . . ?
C37 C34 C32 110.4(4) . . ?
C37 C34 C35 110.1(4) . . ?
C37 C34 C36 110.1(4) . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N41 C42 H42 118.5 . . ?
N41 C42 C43 122.9(4) . . ?
C43 C42 H42 118.5 . . ?
C42 C43 H43 119.8 . . ?
C42 C43 C44 120.4(4) . . ?
C44 C43 H43 119.8 . . ?
N47 C44 C43 121.7(4) . . ?
N47 C44 C45 122.4(4) . . ?
C43 C44 C45 115.9(4) . . ?
C44 C45 H45 120.2 . . ?
C46 C45 C44 119.6(4) . . ?
C46 C45 H45 120.2 . . ?
N41 C46 C45 124.1(4) . . ?
N41 C46 H46 118.0 . . ?
C45 C46 H46 118.0 . . ?
N47 C48 H48A 109.5 . . ?
N47 C48 H48B 109.5 . . ?
N47 C48 H48C 109.5 . . ?
H48A C48 H48B 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N47 C49 H49A 109.5 . . ?
N47 C49 H49B 109.5 . . ?
N47 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
O51 C52 C54 113.3(4) . . ?
O53 C52 O51 125.1(4) . . ?
O53 C52 C54 121.6(4) . . ?
C55 C54 C52 106.3(4) . . ?
C56 C54 C52 110.4(4) . . ?
C56 C54 C55 109.2(5) . . ?
C57 C54 C52 110.6(4) . . ?
C57 C54 C55 109.1(5) . . ?
C57 C54 C56 111.1(5) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55B 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?


_ins_header                      
;
TITL OIE003_numabs_ana in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.493586  14.619594  14.962680  95.3409  91.0769 107.4465
ZERR    6.00   0.000494   0.000683   0.000676   0.0038   0.0038   0.0042
LATT  1
SFAC C H N O S I
UNIT 84.00 120.00 6.00 18.00 6.00 6.00
TREF
HKLF 4
END
;
_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 1.506
_oxdiff_exptl_absorpt_empirical_full_min 0.638
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/pentane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2d
_database_code_depnum_ccdc_archive 'CCDC 2173467'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2021-10-06
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H21 I N2 O3'
_chemical_formula_sum            'C14 H21 I N2 O3'
_chemical_formula_weight         392.23
_chemical_melting_point          ?
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.6593(3)
_cell_length_b                   12.9198(4)
_cell_length_c                   13.3925(5)
_cell_angle_alpha                83.712(3)
_cell_angle_beta                 71.291(3)
_cell_angle_gamma                65.959(3)
_cell_volume                     1594.89(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8335
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      76.5610
_cell_measurement_theta_min      3.4640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    15.858
_exptl_absorpt_correction_T_max  0.457
_exptl_absorpt_correction_T_min  0.082
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             784
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 6 6 0.0624
-1 -5 -6 0.0475
5 3 -3 0.1089
-5 -3 3 0.1235
6 0 -1 0.0371
-6 0 1 0.0278
0 6 -5 0.2036
0 -7 4 0.2155
5 -1 6 0.1647
-1 -5 6 0.2144
6 5 6 0.0695
3 2 9 0.1524
-4 -5 4 0.1598
4 7 -2 0.1775

_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.065
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
1.0493 5.6181 6.3017 -0.9565 -0.2833 0.0698
-0.7910 -5.3826 -6.3590 0.9585 0.2839 -0.0255
5.2631 3.3658 -3.1787 0.3379 0.1009 0.9358
-5.2329 -3.2888 3.2413 -0.3479 -0.1038 -0.9318
5.7206 -0.4232 -0.6513 0.6080 -0.3733 0.7007
-5.7206 0.4232 0.6513 -0.6080 0.3733 -0.7007
0.4542 6.0307 -5.3100 -0.2321 0.7818 0.5787
-0.3870 -7.1069 3.5326 0.4799 -0.6975 -0.5322
5.3393 -0.9410 5.7989 0.1724 -0.9317 0.3196
-1.3655 -5.4805 5.7756 0.0576 -0.7249 -0.6864
5.9609 5.4446 5.5368 -0.4403 -0.5748 0.6897
2.5663 2.1495 8.5964 -0.6087 -0.7933 -0.0125
-4.0322 -4.6565 4.4898 -0.1807 -0.3771 -0.9084
4.1785 7.2107 -1.9783 -0.2590 0.3021 0.9174

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0271
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10718
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.129
_diffrn_reflns_theta_min         3.485
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -106.00 -25.00   1.00    1.00    --  -41.90 -37.00-180.00   81
  2  ω    -77.00 -10.00   1.00    1.00    --  -41.90 125.00 -30.00   67
  3  ω    -61.00  24.00   1.00    1.00    --  -41.90  57.00 -30.00   85
  4  ω   -113.00 -18.00   1.00    1.00    --  -41.90 -37.00  90.00   95
  5  ω     53.00  92.00   1.00    1.00    --   41.90-125.00-180.00   39
  6  ω     44.00 109.00   1.00    1.00    --  112.00-111.00  90.00   65
  7  ω     88.00 132.00   1.00    1.00    --  112.00  45.00-150.00   44
  8  ω     92.00 144.00   1.00    1.00    --  112.00 -77.00 -90.00   52
  9  ω     36.00 109.00   1.00    1.00    --  112.00-111.00 -30.00   73
 10  ω     36.00 132.00   1.00    1.00    --  112.00 -30.00 -90.00   96
 11  ω     38.00 140.00   1.00    1.00    --  112.00 -30.00  30.00  102
 12  ω     44.00 109.00   1.00    1.00    --  112.00-111.00 -90.00   65
 13  ω    152.00 178.00   1.00    1.00    --  112.00  45.00-150.00   26
 14  ω     62.00 159.00   1.00    1.00    --  112.00  15.00 -60.00   97
 15  ω     36.00  71.00   1.00    1.00    --  112.00 -77.00 -90.00   35
 16  ω     52.00 145.00   1.00    1.00    --  112.00 -77.00  90.00   93
;
_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      0.0902576000
_diffrn_orient_matrix_UB_12      -0.1076508000
_diffrn_orient_matrix_UB_13      -0.0708397000
_diffrn_orient_matrix_UB_21      -0.0706594000
_diffrn_orient_matrix_UB_22      0.0592427000
_diffrn_orient_matrix_UB_23      -0.0860003000
_diffrn_orient_matrix_UB_31      0.1202469000
_diffrn_orient_matrix_UB_32      0.0442673000
_diffrn_orient_matrix_UB_33      -0.0484175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5820
_reflns_number_total             6221
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.424
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         6221
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0300
_refine_ls_restrained_S_all      1.033
_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)+(0.0547P)²+0.1801P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0821
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C48(H48A,H48B),
 C49(H49A,H49B), C51(H51A,H51B), C52(H52A,H52B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C42(H42), C43(H43), C45(H45), C46(H46)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 0.74864(2) 0.64597(2) 0.95577(2) 0.01707(7) Uani 1 1 d . . . . .
I2 I 0.74784(2) 0.16204(2) 0.36438(2) 0.02026(7) Uani 1 1 d . . . . .
O10 O 0.2093(2) 0.4386(2) 0.65030(19) 0.0317(5) Uani 1 1 d . . . . .
O21 O 0.8953(2) 0.68720(19) 1.00699(18) 0.0231(4) Uani 1 1 d . . . . .
O23 O 0.7167(2) 0.8452(2) 1.0880(2) 0.0351(6) Uani 1 1 d . . . . .
O50 O 0.3080(3) -0.1682(2) 0.12341(19) 0.0334(5) Uani 1 1 d . . . . .
O61 O 0.9115(2) 0.2069(2) 0.38849(19) 0.0300(5) Uani 1 1 d . . . . .
O63 O 0.7597(2) 0.3055(2) 0.53715(18) 0.0263(5) Uani 1 1 d . . . . .
N1 N 0.6121(2) 0.5935(2) 0.88628(19) 0.0176(5) Uani 1 1 d . . . . .
N7 N 0.3687(2) 0.5083(2) 0.74403(19) 0.0182(5) Uani 1 1 d . . . . .
N41 N 0.5945(3) 0.1037(2) 0.3251(2) 0.0200(5) Uani 1 1 d . . . . .
N47 N 0.3233(3) -0.0104(2) 0.2462(2) 0.0252(5) Uani 1 1 d . . . . .
C2 C 0.6715(3) 0.5403(2) 0.7911(2) 0.0198(6) Uani 1 1 d . . . . .
H2 H 0.7691 0.5221 0.7575 0.024 Uiso 1 1 calc R . . . .
C3 C 0.5962(3) 0.5116(2) 0.7410(2) 0.0188(5) Uani 1 1 d . . . . .
H3 H 0.6428 0.4757 0.6749 0.023 Uiso 1 1 calc R . . . .
C4 C 0.4471(3) 0.5366(2) 0.7897(2) 0.0163(5) Uani 1 1 d . . . . .
C5 C 0.3873(3) 0.5919(2) 0.8901(2) 0.0188(5) Uani 1 1 d . . . . .
H5 H 0.2902 0.6106 0.9264 0.023 Uiso 1 1 calc R . . . .
C6 C 0.4705(3) 0.6181(2) 0.9344(2) 0.0191(5) Uani 1 1 d . . . . .
H6 H 0.4276 0.6544 1.0003 0.023 Uiso 1 1 calc R . . . .
C8 C 0.4203(3) 0.4778(3) 0.6315(2) 0.0211(6) Uani 1 1 d . . . . .
H8A H 0.5249 0.4439 0.6079 0.025 Uiso 1 1 calc R . . . .
H8B H 0.3889 0.5456 0.5914 0.025 Uiso 1 1 calc R . . . .
C9 C 0.3626(3) 0.3948(3) 0.6117(3) 0.0295(7) Uani 1 1 d . . . . .
H9A H 0.3938 0.3787 0.5366 0.035 Uiso 1 1 calc R . . . .
H9B H 0.4021 0.3243 0.6462 0.035 Uiso 1 1 calc R . . . .
C11 C 0.1649(3) 0.4599(3) 0.7609(3) 0.0272(6) Uani 1 1 d . . . . .
H11A H 0.2060 0.3896 0.7952 0.033 Uiso 1 1 calc R . . . .
H11B H 0.0608 0.4864 0.7881 0.033 Uiso 1 1 calc R . . . .
C12 C 0.2110(3) 0.5473(3) 0.7878(2) 0.0208(6) Uani 1 1 d . . . . .
H12A H 0.1648 0.6197 0.7582 0.025 Uiso 1 1 calc R . . . .
H12B H 0.1820 0.5574 0.8637 0.025 Uiso 1 1 calc R . . . .
C22 C 0.8437(3) 0.7814(2) 1.0611(2) 0.0179(5) Uani 1 1 d . . . . .
C24 C 0.9603(3) 0.8072(2) 1.0848(2) 0.0186(5) Uani 1 1 d . . . . .
C25 C 1.0465(3) 0.8408(3) 0.9796(2) 0.0217(6) Uani 1 1 d . . . . .
H25A H 1.0821 0.7821 0.9273 0.032 Uiso 1 1 calc GR . . . .
H25B H 1.1261 0.8511 0.9893 0.032 Uiso 1 1 calc GR . . . .
H25C H 0.9848 0.9104 0.9566 0.032 Uiso 1 1 calc GR . . . .
C26 C 1.0605(3) 0.7014(3) 1.1278(2) 0.0215(6) Uani 1 1 d . . . . .
H26A H 1.0067 0.6833 1.1948 0.032 Uiso 1 1 calc GR . . . .
H26B H 1.1377 0.7164 1.1362 0.032 Uiso 1 1 calc GR . . . .
H26C H 1.0996 0.6387 1.0791 0.032 Uiso 1 1 calc GR . . . .
C27 C 0.8920(3) 0.9037(3) 1.1651(3) 0.0282(7) Uani 1 1 d . . . . .
H27A H 0.8269 0.9691 1.1398 0.042 Uiso 1 1 calc GR . . . .
H27B H 0.9660 0.9215 1.1758 0.042 Uiso 1 1 calc GR . . . .
H27C H 0.8399 0.8816 1.2306 0.042 Uiso 1 1 calc GR . . . .
C42 C 0.5697(3) 0.0138(3) 0.3715(2) 0.0203(6) Uani 1 1 d . . . . .
H42 H 0.6136 -0.0222 0.4227 0.024 Uiso 1 1 calc R . . . .
C43 C 0.4833(3) -0.0282(3) 0.3475(2) 0.0204(6) Uani 1 1 d . . . . .
H43 H 0.4694 -0.0908 0.3825 0.024 Uiso 1 1 calc R . . . .
C44 C 0.4151(3) 0.0238(2) 0.2696(2) 0.0183(5) Uani 1 1 d . . . . .
C45 C 0.4465(3) 0.1163(2) 0.2201(2) 0.0220(6) Uani 1 1 d . . . . .
H45 H 0.4080 0.1526 0.1664 0.026 Uiso 1 1 calc R . . . .
C46 C 0.5324(3) 0.1535(2) 0.2497(2) 0.0230(6) Uani 1 1 d . . . . .
H46 H 0.5487 0.2158 0.2164 0.028 Uiso 1 1 calc R . . . .
C48 C 0.2884(3) -0.1061(3) 0.2947(3) 0.0272(6) Uani 1 1 d . . . . .
H48A H 0.1846 -0.0832 0.3195 0.033 Uiso 1 1 calc R . . . .
H48B H 0.3245 -0.1308 0.3548 0.033 Uiso 1 1 calc R . . . .
C49 C 0.3561(4) -0.2030(3) 0.2145(3) 0.0331(7) Uani 1 1 d . . . . .
H49A H 0.4603 -0.2290 0.1936 0.040 Uiso 1 1 calc R . . . .
H49B H 0.3308 -0.2657 0.2464 0.040 Uiso 1 1 calc R . . . .
C51 C 0.3435(4) -0.0753(3) 0.0761(3) 0.0295(7) Uani 1 1 d . . . . .
H51A H 0.3110 -0.0528 0.0142 0.035 Uiso 1 1 calc R . . . .
H51B H 0.4474 -0.0989 0.0536 0.035 Uiso 1 1 calc R . . . .
C52 C 0.2744(4) 0.0249(3) 0.1523(3) 0.0287(7) Uani 1 1 d . . . . .
H52A H 0.3014 0.0865 0.1190 0.034 Uiso 1 1 calc R . . . .
H52B H 0.1702 0.0516 0.1725 0.034 Uiso 1 1 calc R . . . .
C62 C 0.8795(3) 0.2665(2) 0.4724(2) 0.0181(5) Uani 1 1 d . . . . .
C64 C 1.0105(3) 0.2800(3) 0.4843(2) 0.0196(6) Uani 1 1 d . . . . .
C65 C 1.0947(3) 0.3139(3) 0.3795(3) 0.0281(7) Uani 1 1 d . . . . .
H65A H 1.1214 0.2591 0.3255 0.042 Uiso 1 1 calc GR . . . .
H65B H 1.1801 0.3166 0.3867 0.042 Uiso 1 1 calc GR . . . .
H65C H 1.0355 0.3871 0.3606 0.042 Uiso 1 1 calc GR . . . .
C66 C 1.1063(4) 0.1651(3) 0.5174(3) 0.0348(8) Uani 1 1 d . . . . .
H66A H 1.0506 0.1413 0.5800 0.052 Uiso 1 1 calc GR . . . .
H66B H 1.1855 0.1721 0.5312 0.052 Uiso 1 1 calc GR . . . .
H66C H 1.1428 0.1098 0.4617 0.052 Uiso 1 1 calc GR . . . .
C67 C 0.9608(3) 0.3697(3) 0.5699(3) 0.0278(7) Uani 1 1 d . . . . .
H67A H 0.8980 0.4410 0.5505 0.042 Uiso 1 1 calc GR . . . .
H67B H 1.0432 0.3774 0.5774 0.042 Uiso 1 1 calc GR . . . .
H67C H 0.9100 0.3469 0.6357 0.042 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O21 2.155(2) . ?
I1 N1 2.292(2) . ?
I2 O61 2.171(2) . ?
I2 N41 2.271(2) . ?
O10 C9 1.423(4) . ?
O10 C11 1.424(4) . ?
O21 C22 1.305(4) . ?
O23 C22 1.219(4) . ?
O50 C49 1.431(4) . ?
O50 C51 1.426(4) . ?
O61 C62 1.304(4) . ?
O63 C62 1.223(4) . ?
N1 C2 1.348(4) . ?
N1 C6 1.351(3) . ?
N7 C4 1.354(3) . ?
N7 C8 1.466(3) . ?
N7 C12 1.472(3) . ?
N41 C42 1.339(4) . ?
N41 C46 1.346(4) . ?
N47 C44 1.353(4) . ?
N47 C48 1.461(4) . ?
N47 C52 1.471(4) . ?
C2 H2 0.9300 . ?
C2 C3 1.369(4) . ?
C3 H3 0.9300 . ?
C3 C4 1.421(4) . ?
C4 C5 1.419(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.371(4) . ?
C6 H6 0.9300 . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C8 C9 1.517(4) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C12 1.517(4) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C22 C24 1.539(4) . ?
C24 C25 1.543(4) . ?
C24 C26 1.540(4) . ?
C24 C27 1.514(4) . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C42 H42 0.9300 . ?
C42 C43 1.372(4) . ?
C43 H43 0.9300 . ?
C43 C44 1.416(4) . ?
C44 C45 1.411(4) . ?
C45 H45 0.9300 . ?
C45 C46 1.363(4) . ?
C46 H46 0.9300 . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C48 C49 1.517(5) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C51 H51A 0.9700 . ?
C51 H51B 0.9700 . ?
C51 C52 1.514(5) . ?
C52 H52A 0.9700 . ?
C52 H52B 0.9700 . ?
C62 C64 1.534(4) . ?
C64 C65 1.531(4) . ?
C64 C66 1.535(4) . ?
C64 C67 1.530(4) . ?
C65 H65A 0.9600 . ?
C65 H65B 0.9600 . ?
C65 H65C 0.9600 . ?
C66 H66A 0.9600 . ?
C66 H66B 0.9600 . ?
C66 H66C 0.9600 . ?
C67 H67A 0.9600 . ?
C67 H67B 0.9600 . ?
C67 H67C 0.9600 . ?

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
O21 I1 N1 174.12(8) . . ?
O61 I2 N41 174.17(8) . . ?
C9 O10 C11 108.8(2) . . ?
C22 O21 I1 117.96(17) . . ?
C51 O50 C49 110.1(2) . . ?
C62 O61 I2 118.96(18) . . ?
C2 N1 I1 119.78(18) . . ?
C2 N1 C6 117.3(2) . . ?
C6 N1 I1 122.83(19) . . ?
C4 N7 C8 121.6(2) . . ?
C4 N7 C12 122.0(2) . . ?
C8 N7 C12 112.2(2) . . ?
C42 N41 I2 121.11(19) . . ?
C42 N41 C46 117.4(3) . . ?
C46 N41 I2 121.4(2) . . ?
C44 N47 C48 124.3(3) . . ?
C44 N47 C52 123.7(3) . . ?
C48 N47 C52 110.4(2) . . ?
N1 C2 H2 118.1 . . ?
N1 C2 C3 123.8(3) . . ?
C3 C2 H2 118.1 . . ?
C2 C3 H3 119.9 . . ?
C2 C3 C4 120.1(3) . . ?
C4 C3 H3 119.9 . . ?
N7 C4 C3 122.3(3) . . ?
N7 C4 C5 122.6(2) . . ?
C5 C4 C3 115.1(2) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 C4 121.0(2) . . ?
C6 C5 H5 119.5 . . ?
N1 C6 C5 122.7(3) . . ?
N1 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
N7 C8 H8A 109.5 . . ?
N7 C8 H8B 109.5 . . ?
N7 C8 C9 110.5(2) . . ?
H8A C8 H8B 108.1 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
O10 C9 C8 111.6(3) . . ?
O10 C9 H9A 109.3 . . ?
O10 C9 H9B 109.3 . . ?
C8 C9 H9A 109.3 . . ?
C8 C9 H9B 109.3 . . ?
H9A C9 H9B 108.0 . . ?
O10 C11 H11A 109.1 . . ?
O10 C11 H11B 109.1 . . ?
O10 C11 C12 112.4(2) . . ?
H11A C11 H11B 107.9 . . ?
C12 C11 H11A 109.1 . . ?
C12 C11 H11B 109.1 . . ?
N7 C12 C11 109.0(2) . . ?
N7 C12 H12A 109.9 . . ?
N7 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
O21 C22 C24 113.3(2) . . ?
O23 C22 O21 123.9(3) . . ?
O23 C22 C24 122.7(3) . . ?
C22 C24 C25 106.6(2) . . ?
C22 C24 C26 110.3(2) . . ?
C26 C24 C25 110.2(2) . . ?
C27 C24 C22 110.6(2) . . ?
C27 C24 C25 110.0(2) . . ?
C27 C24 C26 109.1(3) . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N41 C42 H42 118.2 . . ?
N41 C42 C43 123.6(3) . . ?
C43 C42 H42 118.2 . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 120.0(3) . . ?
C44 C43 H43 120.0 . . ?
N47 C44 C43 122.6(3) . . ?
N47 C44 C45 122.4(3) . . ?
C45 C44 C43 115.0(3) . . ?
C44 C45 H45 119.4 . . ?
C46 C45 C44 121.1(3) . . ?
C46 C45 H45 119.4 . . ?
N41 C46 C45 122.8(3) . . ?
N41 C46 H46 118.6 . . ?
C45 C46 H46 118.6 . . ?
N47 C48 H48A 109.8 . . ?
N47 C48 H48B 109.8 . . ?
N47 C48 C49 109.6(3) . . ?
H48A C48 H48B 108.2 . . ?
C49 C48 H48A 109.8 . . ?
C49 C48 H48B 109.8 . . ?
O50 C49 C48 111.0(3) . . ?
O50 C49 H49A 109.4 . . ?
O50 C49 H49B 109.4 . . ?
C48 C49 H49A 109.4 . . ?
C48 C49 H49B 109.4 . . ?
H49A C49 H49B 108.0 . . ?
O50 C51 H51A 109.4 . . ?
O50 C51 H51B 109.4 . . ?
O50 C51 C52 111.3(3) . . ?
H51A C51 H51B 108.0 . . ?
C52 C51 H51A 109.4 . . ?
C52 C51 H51B 109.4 . . ?
N47 C52 C51 108.9(3) . . ?
N47 C52 H52A 109.9 . . ?
N47 C52 H52B 109.9 . . ?
C51 C52 H52A 109.9 . . ?
C51 C52 H52B 109.9 . . ?
H52A C52 H52B 108.3 . . ?
O61 C62 C64 112.6(2) . . ?
O63 C62 O61 124.7(3) . . ?
O63 C62 C64 122.6(3) . . ?
C62 C64 C66 107.3(2) . . ?
C65 C64 C62 110.4(2) . . ?
C65 C64 C66 109.9(3) . . ?
C67 C64 C62 109.8(2) . . ?
C67 C64 C65 110.0(3) . . ?
C67 C64 C66 109.4(3) . . ?
C64 C65 H65A 109.5 . . ?
C64 C65 H65B 109.5 . . ?
C64 C65 H65C 109.5 . . ?
H65A C65 H65B 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C64 C66 H66A 109.5 . . ?
C64 C66 H66B 109.5 . . ?
C64 C66 H66C 109.5 . . ?
H66A C66 H66B 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?


_ins_header                      
;
TITL OIK019_numabs_ana1 in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184  10.659345  12.919778  13.392520  83.7115  71.2915  65.9585
ZERR    4.00   0.000313   0.000376   0.000463   0.0026   0.0030   0.0028
LATT  1
SFAC C H N O I
UNIT 56.00 84.00 8.00 12.00 4.00
TREF
HKLF 4
END
;
_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 1.700
_oxdiff_exptl_absorpt_empirical_full_min 0.629
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/DIPE'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4b
_database_code_depnum_ccdc_archive 'CCDC 2173470'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2021-09-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C27 H24 I3 N3 O6'
_chemical_formula_sum            'C27 H24 I3 N3 O6'
_chemical_formula_weight         867.19
_chemical_melting_point          ?
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   15.6502(4)
_cell_length_b                   9.9201(2)
_cell_length_c                   19.5464(5)
_cell_angle_alpha                90
_cell_angle_beta                 109.522(3)
_cell_angle_gamma                90
_cell_volume                     2860.16(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5135
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      76.4410
_cell_measurement_theta_min      3.1180
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    26.136
_exptl_absorpt_correction_T_max  0.420
_exptl_absorpt_correction_T_min  0.130
_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_absorpt_special_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.014
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1656
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 0 7 0.0229
9 -1 -9 0.0370
10 0 -7 0.0361
8 2 3 0.0501
-2 1 -11 0.0600
-1 -6 0 0.0396
0 6 -3 0.0370
1 6 5 0.0400
1 -6 5 0.0426
-6 4 9 0.0371
-9 0 -1 0.0441
-5 5 -1 0.0393
7 4 -9 0.0328
7 5 -4 0.0256
-7 -5 3 0.0396
-7 -3 10 0.0429
7 -5 -2 0.0396
3 -6 -6 0.0453

_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.059
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
-9.8484 0.2898 6.9968 -0.9588 -0.2840 -0.0090
9.0723 -0.9229 -8.8849 0.9330 0.2765 0.2304
9.9471 -0.1583 -6.5670 0.9582 0.2838 -0.0364
7.9924 2.0853 2.9524 0.6020 0.1777 -0.7784
-2.2953 0.8757 -10.5739 0.1614 -0.5426 0.8244
-0.5088 -6.4288 -0.1949 -0.2474 0.8369 0.4883
-0.1985 6.2341 -2.9128 0.2773 -0.9369 -0.2128
1.4638 5.6906 4.7155 0.1643 -0.5571 -0.8140
0.8127 -5.6080 5.4627 -0.2837 0.9577 -0.0474
-5.5206 3.8377 9.3693 -0.5751 -0.4904 -0.6548
-9.3758 0.2021 -0.6815 -0.6998 -0.4815 0.5276
-5.4667 5.2042 -0.5877 -0.2334 -0.9718 -0.0326
6.8422 3.6262 -8.5827 0.9025 -0.4305 0.0090
7.1774 4.5507 -3.5196 0.8107 -0.3871 -0.4392
-7.1139 -4.5988 2.8401 -0.7875 0.3761 0.4883
-6.5261 -3.2672 9.5916 -0.8957 0.4271 -0.1235
6.7564 -4.7954 -2.1294 0.4266 0.8946 0.1329
3.2773 -5.5223 -6.1572 0.2510 0.7103 0.6576

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10773
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.128
_diffrn_reflns_theta_min         3.151
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -82.00  -6.00   1.00    1.50    --  -42.03 125.00  30.00   76
  2  ω    -86.00 -53.00   1.00    1.50    --  -42.03 125.00-180.00   33
  3  ω    -49.00  -9.00   1.00    1.50    --  -42.03 125.00-180.00   40
  4  ω     47.00  74.00   1.00    1.50    --   42.03 -99.00 -60.00   27
  5  ω     26.00 115.00   1.00    1.50    --   42.03  37.00  60.00   89
  6  ω     87.00 178.00   1.00    6.00    --  112.00  45.00  60.00   91
  7  ω     83.00 178.00   1.00    6.00    --  112.00  61.00   0.00   95
  8  ω     41.00 135.00   1.00    6.00    --  112.00 -61.00-150.00   94
  9  ω     83.00 169.00   1.00    6.00    --  112.00  61.00  90.00   86
 10  ω    110.00 145.00   1.00    6.00    --  112.00  77.00 -60.00   35
;
_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      0.0774903000
_diffrn_orient_matrix_UB_12      0.0332454000
_diffrn_orient_matrix_UB_13      -0.0293366000
_diffrn_orient_matrix_UB_21      0.0462632000
_diffrn_orient_matrix_UB_22      -0.1347460000
_diffrn_orient_matrix_UB_23      0.0301097000
_diffrn_orient_matrix_UB_31      -0.0525207000
_diffrn_orient_matrix_UB_32      -0.0696074000
_diffrn_orient_matrix_UB_33      -0.0723250000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4760
_reflns_number_total             5592
_reflns_odcompleteness_completeness 99.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.297
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5592
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0351
_refine_ls_restrained_S_all      1.049
_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)+(0.0535P)²+1.2425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0995
_refine_special_details          ?
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C22(H22), C23(H23), C25(H25), C26(H26), C32(H32),
 C33(H33), C35(H35), C36(H36), C42(H42), C43(H43), C45(H45), C46(H46)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 1.05770(2) -0.07663(3) 0.85149(2) 0.03065(10) Uani 1 1 d . . . . .
I2 I 1.05698(2) 0.94420(3) 0.63650(2) 0.03003(10) Uani 1 1 d . . . . .
I3 I 0.57714(2) 0.25972(4) 0.51427(2) 0.03509(10) Uani 1 1 d . . . . .
O8 O 0.9854(3) 0.0940(4) 0.7877(2) 0.0324(8) Uani 1 1 d . . . . .
O9 O 1.1168(3) 0.2065(4) 0.8147(2) 0.0402(9) Uani 1 1 d . . . . .
O11 O 0.9928(3) 0.7482(4) 0.6381(2) 0.0362(9) Uani 1 1 d . . . . .
O12 O 1.1186(3) 0.6687(4) 0.7230(2) 0.0370(9) Uani 1 1 d . . . . .
O14 O 0.7086(3) 0.2809(4) 0.6030(2) 0.0356(8) Uani 1 1 d . . . . .
O15 O 0.7223(3) 0.4734(4) 0.5490(3) 0.0483(11) Uani 1 1 d . . . . .
N21 N 1.1304(3) -0.2626(4) 0.9122(3) 0.0309(9) Uani 1 1 d . . . . .
N31 N 1.1067(3) 1.1547(4) 0.6225(2) 0.0294(9) Uani 1 1 d . . . . .
N41 N 0.4430(3) 0.2179(5) 0.4262(3) 0.0380(10) Uani 1 1 d . . . . .
C1 C 0.9841(3) 0.3062(5) 0.7326(3) 0.0280(10) Uani 1 1 d . . . . .
C2 C 1.0306(4) 0.4228(5) 0.7279(3) 0.0297(10) Uani 1 1 d . . . . .
H2 H 1.0919 0.4295 0.7549 0.036 Uiso 1 1 calc R . . . .
C3 C 0.9881(4) 0.5302(5) 0.6838(3) 0.0290(10) Uani 1 1 d . . . . .
C4 C 0.8968(4) 0.5151(5) 0.6411(3) 0.0309(10) Uani 1 1 d . . . . .
H4 H 0.8673 0.5848 0.6104 0.037 Uiso 1 1 calc R . . . .
C5 C 0.8494(4) 0.3973(5) 0.6438(3) 0.0303(10) Uani 1 1 d . . . . .
C6 C 0.8934(4) 0.2929(5) 0.6903(3) 0.0291(10) Uani 1 1 d . . . . .
H6 H 0.8620 0.2146 0.6929 0.035 Uiso 1 1 calc R . . . .
C7 C 1.0359(4) 0.1957(5) 0.7837(3) 0.0291(10) Uani 1 1 d . . . . .
C10 C 1.0398(4) 0.6573(6) 0.6833(3) 0.0350(11) Uani 1 1 d . . . . .
C13 C 0.7530(4) 0.3859(6) 0.5945(3) 0.0337(11) Uani 1 1 d . . . . .
C22 C 1.1099(4) -0.3856(6) 0.8826(3) 0.0352(11) Uani 1 1 d . . . . .
H22 H 1.0584 -0.3965 0.8420 0.042 Uiso 1 1 calc R . . . .
C23 C 1.1634(4) -0.4964(6) 0.9109(3) 0.0362(12) Uani 1 1 d . . . . .
H23 H 1.1477 -0.5806 0.8894 0.043 Uiso 1 1 calc R . . . .
C24 C 1.2409(4) -0.4822(6) 0.9717(3) 0.0327(11) Uani 1 1 d . . . . .
C25 C 1.2599(4) -0.3552(6) 1.0025(3) 0.0348(11) Uani 1 1 d . . . . .
H25 H 1.3099 -0.3422 1.0441 0.042 Uiso 1 1 calc R . . . .
C26 C 1.2046(4) -0.2483(5) 0.9713(3) 0.0350(11) Uani 1 1 d . . . . .
H26 H 1.2191 -0.1632 0.9918 0.042 Uiso 1 1 calc R . . . .
C27 C 1.3025(4) -0.5987(7) 1.0028(4) 0.0435(14) Uani 1 1 d . . . . .
H27A H 1.2742 -0.6809 0.9805 0.065 Uiso 1 1 calc GR . . . .
H27B H 1.3142 -0.6033 1.0542 0.065 Uiso 1 1 calc GR . . . .
H27C H 1.3587 -0.5866 0.9938 0.065 Uiso 1 1 calc GR . . . .
C32 C 1.1801(4) 1.2135(6) 0.6712(3) 0.0332(11) Uani 1 1 d . . . . .
H32 H 1.2139 1.1651 0.7120 0.040 Uiso 1 1 calc R . . . .
C33 C 1.2056(4) 1.3412(6) 0.6620(3) 0.0348(11) Uani 1 1 d . . . . .
H33 H 1.2554 1.3792 0.6971 0.042 Uiso 1 1 calc R . . . .
C34 C 1.1584(4) 1.4163(6) 0.6008(3) 0.0344(11) Uani 1 1 d . . . . .
C35 C 1.0840(4) 1.3530(6) 0.5503(3) 0.0362(12) Uani 1 1 d . . . . .
H35 H 1.0503 1.3983 0.5083 0.043 Uiso 1 1 calc R . . . .
C36 C 1.0605(4) 1.2249(6) 0.5624(3) 0.0343(11) Uani 1 1 d . . . . .
H36 H 1.0109 1.1846 0.5281 0.041 Uiso 1 1 calc R . . . .
C37 C 1.1861(4) 1.5556(6) 0.5879(4) 0.0427(14) Uani 1 1 d . . . . .
H37A H 1.1563 1.6200 0.6088 0.064 Uiso 1 1 calc GR . . . .
H37B H 1.1693 1.5714 0.5366 0.064 Uiso 1 1 calc GR . . . .
H37C H 1.2506 1.5648 0.6099 0.064 Uiso 1 1 calc GR . . . .
C42 C 0.3872(4) 0.3185(6) 0.3957(4) 0.0422(13) Uani 1 1 d . . . . .
H42 H 0.4047 0.4067 0.4094 0.051 Uiso 1 1 calc R . . . .
C43 C 0.3026(4) 0.2942(7) 0.3435(4) 0.0420(13) Uani 1 1 d . . . . .
H43 H 0.2654 0.3661 0.3217 0.050 Uiso 1 1 calc R . . . .
C44 C 0.2742(4) 0.1633(7) 0.3241(3) 0.0417(13) Uani 1 1 d . . . . .
C45 C 0.3334(5) 0.0615(7) 0.3552(4) 0.0469(15) Uani 1 1 d . . . . .
H45 H 0.3174 -0.0277 0.3426 0.056 Uiso 1 1 calc R . . . .
C46 C 0.4177(5) 0.0919(7) 0.4059(4) 0.0468(15) Uani 1 1 d . . . . .
H46 H 0.4577 0.0219 0.4261 0.056 Uiso 1 1 calc R . . . .
C47 C 0.1822(5) 0.1355(8) 0.2714(4) 0.0515(16) Uani 1 1 d . . . . .
H47A H 0.1779 0.0422 0.2575 0.077 Uiso 1 1 calc GR . . . .
H47B H 0.1720 0.1910 0.2292 0.077 Uiso 1 1 calc GR . . . .
H47C H 0.1373 0.1553 0.2935 0.077 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O8 2.181(4) . ?
I1 N21 2.281(4) . ?
I2 O11 2.193(4) . ?
I2 N31 2.277(4) . ?
I3 O14 2.214(4) . ?
I3 N41 2.264(5) . ?
O8 C7 1.300(7) . ?
O9 C7 1.212(7) . ?
O11 C10 1.304(7) . ?
O12 C10 1.222(7) . ?
O14 C13 1.293(7) . ?
O15 C13 1.221(7) . ?
N21 C22 1.343(7) . ?
N21 C26 1.344(8) . ?
N31 C32 1.353(7) . ?
N31 C36 1.349(7) . ?
N41 C42 1.329(9) . ?
N41 C46 1.331(9) . ?
C1 C2 1.386(7) . ?
C1 C6 1.390(7) . ?
C1 C7 1.522(7) . ?
C2 H2 0.9300 . ?
C2 C3 1.392(7) . ?
C3 C4 1.401(7) . ?
C3 C10 1.501(7) . ?
C4 H4 0.9300 . ?
C4 C5 1.396(7) . ?
C5 C6 1.397(7) . ?
C5 C13 1.498(7) . ?
C6 H6 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.381(8) . ?
C23 H23 0.9300 . ?
C23 C24 1.391(8) . ?
C24 C25 1.386(8) . ?
C24 C27 1.498(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.375(8) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C32 H32 0.9300 . ?
C32 C33 1.358(8) . ?
C33 H33 0.9300 . ?
C33 C34 1.393(8) . ?
C34 C35 1.399(8) . ?
C34 C37 1.495(8) . ?
C35 H35 0.9300 . ?
C35 C36 1.365(8) . ?
C36 H36 0.9300 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C42 H42 0.9300 . ?
C42 C43 1.395(9) . ?
C43 H43 0.9300 . ?
C43 C44 1.383(10) . ?
C44 C45 1.369(10) . ?
C44 C47 1.490(9) . ?
C45 H45 0.9300 . ?
C45 C46 1.392(9) . ?
C46 H46 0.9300 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?

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
O8 I1 N21 176.66(16) . . ?
O11 I2 N31 172.45(15) . . ?
O14 I3 N41 174.77(17) . . ?
C7 O8 I1 115.3(3) . . ?
C10 O11 I2 117.7(3) . . ?
C13 O14 I3 112.0(3) . . ?
C22 N21 I1 120.3(4) . . ?
C22 N21 C26 118.6(5) . . ?
C26 N21 I1 120.0(4) . . ?
C32 N31 I2 123.7(4) . . ?
C36 N31 I2 118.2(4) . . ?
C36 N31 C32 118.1(5) . . ?
C42 N41 I3 120.5(4) . . ?
C42 N41 C46 119.1(6) . . ?
C46 N41 I3 120.4(4) . . ?
C2 C1 C6 119.7(5) . . ?
C2 C1 C7 117.9(5) . . ?
C6 C1 C7 122.4(5) . . ?
C1 C2 H2 119.1 . . ?
C1 C2 C3 121.7(5) . . ?
C3 C2 H2 119.1 . . ?
C2 C3 C4 118.0(5) . . ?
C2 C3 C10 119.9(5) . . ?
C4 C3 C10 122.1(5) . . ?
C3 C4 H4 119.5 . . ?
C5 C4 C3 121.1(5) . . ?
C5 C4 H4 119.5 . . ?
C4 C5 C6 119.5(5) . . ?
C4 C5 C13 118.2(5) . . ?
C6 C5 C13 122.3(5) . . ?
C1 C6 C5 120.0(5) . . ?
C1 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
O8 C7 C1 113.4(5) . . ?
O9 C7 O8 126.3(5) . . ?
O9 C7 C1 120.2(5) . . ?
O11 C10 C3 113.7(5) . . ?
O12 C10 O11 126.0(5) . . ?
O12 C10 C3 120.4(5) . . ?
O14 C13 C5 116.5(5) . . ?
O15 C13 O14 124.7(5) . . ?
O15 C13 C5 118.8(5) . . ?
N21 C22 H22 119.2 . . ?
N21 C22 C23 121.7(5) . . ?
C23 C22 H22 119.2 . . ?
C22 C23 H23 120.0 . . ?
C22 C23 C24 120.0(5) . . ?
C24 C23 H23 120.0 . . ?
C23 C24 C27 121.9(6) . . ?
C25 C24 C23 117.5(5) . . ?
C25 C24 C27 120.6(6) . . ?
C24 C25 H25 120.1 . . ?
C26 C25 C24 119.7(5) . . ?
C26 C25 H25 120.1 . . ?
N21 C26 C25 122.3(5) . . ?
N21 C26 H26 118.8 . . ?
C25 C26 H26 118.8 . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N31 C32 H32 119.1 . . ?
N31 C32 C33 121.8(5) . . ?
C33 C32 H32 119.1 . . ?
C32 C33 H33 119.4 . . ?
C32 C33 C34 121.2(5) . . ?
C34 C33 H33 119.4 . . ?
C33 C34 C35 116.3(5) . . ?
C33 C34 C37 122.6(5) . . ?
C35 C34 C37 121.1(5) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 C34 120.3(5) . . ?
C36 C35 H35 119.9 . . ?
N31 C36 C35 122.3(5) . . ?
N31 C36 H36 118.8 . . ?
C35 C36 H36 118.8 . . ?
C34 C37 H37A 109.5 . . ?
C34 C37 H37B 109.5 . . ?
C34 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N41 C42 H42 119.4 . . ?
N41 C42 C43 121.2(6) . . ?
C43 C42 H42 119.4 . . ?
C42 C43 H43 119.9 . . ?
C44 C43 C42 120.1(6) . . ?
C44 C43 H43 119.9 . . ?
C43 C44 C47 120.8(6) . . ?
C45 C44 C43 117.6(6) . . ?
C45 C44 C47 121.7(7) . . ?
C44 C45 H45 120.1 . . ?
C44 C45 C46 119.7(6) . . ?
C46 C45 H45 120.1 . . ?
N41 C46 C45 122.1(6) . . ?
N41 C46 H46 118.9 . . ?
C45 C46 H46 118.9 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?


_ins_header                      
;
TITL OIK009_numabs in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184  15.650236   9.920134  19.546389  90.0000 109.5225  90.0000
ZERR    4.00   0.000378   0.000178   0.000536   0.0000   0.0028   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O I
UNIT 108.00 96.00 12.00 24.00 12.00
TREF
HKLF 4
END
;
_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 1.215
_oxdiff_exptl_absorpt_empirical_full_min 0.800

#===END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/TBME'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4a
_database_code_depnum_ccdc_archive 'CCDC 2173469'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2021-09-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C24 H18 I3 N3 O6, H2 O'
_chemical_formula_sum            'C24 H20 I3 N3 O7'
_chemical_formula_weight         843.13
_chemical_melting_point          ?
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   9.7621(2)
_cell_length_b                   24.2101(5)
_cell_length_c                   11.4785(2)
_cell_angle_alpha                90
_cell_angle_beta                 91.437(2)
_cell_angle_gamma                90
_cell_volume                     2711.99(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4914
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      75.4470
_cell_measurement_theta_min      4.2400
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    27.569
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.088
_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_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -3 -3 0.0167
5 3 3 0.0135
2 0 -7 0.0910
1 -15 1 0.0164
-1 15 -1 0.0164
-5 -11 -1 0.0223
5 2 4 0.0140
-6 -2 -2 0.0197
-3 6 6 0.0839
-5 4 -3 0.0132
1 -12 -5 0.0665
-1 10 -6 0.0521

_exptl_crystal_size_max          0.187
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.033
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
-5.6099 -2.6146 -3.0662 0.0487 0.1991 0.9788
5.4705 2.6221 3.3844 -0.0595 -0.2441 -0.9679
2.4967 -0.3595 -6.9146 0.2306 0.9610 -0.1529
0.6856 -15.3591 1.3592 -0.9914 0.1305 0.0090
-0.6856 15.3591 -1.3592 0.9914 -0.1305 -0.0090
-4.5068 -10.9638 -0.5118 -0.5760 0.0752 0.8140
5.1867 2.0869 4.0091 -0.1137 -0.3233 -0.9394
-5.9359 -2.4678 -2.1492 0.0240 0.0701 0.9973
-3.1317 6.2525 5.8450 0.1778 -0.9583 0.2236
-5.2359 4.3989 -3.4869 0.4834 0.1424 0.8637
0.6123 -12.2830 -4.6077 -0.5571 0.8104 0.1813
-1.0129 10.1421 -5.5391 0.8554 0.4646 0.2290

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10193
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.110
_diffrn_reflns_theta_min         3.651
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  29.00   1.00    2.50    --  -42.03  57.00 150.00   99
  2  ω    -29.00  69.00   1.00    2.50    --   42.03 -57.00 -90.00   98
  3  ω     75.00 140.00   1.00   10.00    --  112.00 -30.00-150.00   65
  4  ω     51.00 102.00   1.00   10.00    --  112.00 -30.00 -60.00   51
  5  ω     86.00 173.00   1.00   10.00    --  112.00  30.00-150.00   87
  6  ω     36.00 109.00   1.00   10.00    --  112.00-111.00 -90.00   73
  7  ω     51.00 141.00   1.00   10.00    --  112.00 -77.00 -60.00   90
  8  ω    106.00 140.00   1.00   10.00    --  112.00 -30.00 -60.00   34
  9  ω     36.00  73.00   1.00   10.00    --  112.00 -30.00-150.00   37
;
_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      -0.0140428000
_diffrn_orient_matrix_UB_12      0.0602446000
_diffrn_orient_matrix_UB_13      -0.0415498000
_diffrn_orient_matrix_UB_21      0.0402470000
_diffrn_orient_matrix_UB_22      -0.0176329000
_diffrn_orient_matrix_UB_23      -0.1235276000
_diffrn_orient_matrix_UB_31      -0.1520661000
_diffrn_orient_matrix_UB_32      -0.0102317000
_diffrn_orient_matrix_UB_33      -0.0322700000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4622
_reflns_number_total             5294
_reflns_odcompleteness_completeness 99.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0260
_refine_ls_restrained_S_all      1.008
_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)+(0.0302P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0622
_refine_ls_wR_factor_ref         0.0662
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Free rotating group:
 O101(H10A,H10B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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 -0.26613(2) 0.11881(2) 0.39745(2) 0.02589(7) Uani 1 1 d . . . . .
I2 I 0.77492(2) 0.19680(2) 0.73098(2) 0.02486(7) Uani 1 1 d . . . . .
I3 I 0.27322(2) 0.46303(2) 0.47239(2) 0.02443(7) Uani 1 1 d . . . . .
O8 O -0.0955(3) 0.17525(13) 0.4336(3) 0.0273(6) Uani 1 1 d . . . . .
O9 O 0.0271(3) 0.10437(13) 0.5069(3) 0.0349(7) Uani 1 1 d . . . . .
O11 O 0.5770(3) 0.22610(13) 0.6656(3) 0.0325(7) Uani 1 1 d . . . . .
O12 O 0.4973(3) 0.13930(14) 0.6570(3) 0.0379(8) Uani 1 1 d . . . . .
O14 O 0.2849(3) 0.37978(12) 0.5419(3) 0.0303(6) Uani 1 1 d . . . . .
O15 O 0.0634(3) 0.36676(14) 0.4951(3) 0.0355(7) Uani 1 1 d . . . . .
N21 N -0.4419(3) 0.06038(15) 0.3607(3) 0.0263(7) Uani 1 1 d . . . . .
N31 N 0.9903(3) 0.17683(16) 0.8028(3) 0.0264(7) Uani 1 1 d . . . . .
N41 N 0.2857(3) 0.54847(14) 0.3905(3) 0.0245(7) Uani 1 1 d . . . . .
C1 C 0.1186(4) 0.19539(17) 0.5241(3) 0.0217(7) Uani 1 1 d . . . . .
C2 C 0.2447(4) 0.17564(17) 0.5676(4) 0.0246(8) Uani 1 1 d . . . . .
H2 H 0.2589 0.1378 0.5755 0.029 Uiso 1 1 calc R . . . .
C3 C 0.3485(4) 0.21243(18) 0.5990(4) 0.0243(8) Uani 1 1 d . . . . .
C4 C 0.3271(4) 0.26939(17) 0.5874(3) 0.0235(8) Uani 1 1 d . . . . .
H4 H 0.3969 0.2940 0.6074 0.028 Uiso 1 1 calc R . . . .
C5 C 0.2008(4) 0.28913(17) 0.5459(3) 0.0214(7) Uani 1 1 d . . . . .
C6 C 0.0971(4) 0.25181(18) 0.5134(3) 0.0243(8) Uani 1 1 d . . . . .
H6 H 0.0133 0.2649 0.4846 0.029 Uiso 1 1 calc R . . . .
C7 C 0.0110(4) 0.15351(18) 0.4876(4) 0.0267(8) Uani 1 1 d . . . . .
C10 C 0.4837(4) 0.18900(18) 0.6449(4) 0.0259(8) Uani 1 1 d . . . . .
C13 C 0.1764(4) 0.34970(18) 0.5261(4) 0.0245(8) Uani 1 1 d . . . . .
C22 C -0.4235(4) 0.01752(19) 0.2883(4) 0.0309(9) Uani 1 1 d . . . . .
H22 H -0.3429 0.0153 0.2470 0.037 Uiso 1 1 calc R . . . .
C23 C -0.5213(5) -0.0234(2) 0.2737(4) 0.0351(10) Uani 1 1 d . . . . .
H23 H -0.5074 -0.0527 0.2230 0.042 Uiso 1 1 calc R . . . .
C24 C -0.6398(5) -0.0197(2) 0.3358(4) 0.0365(11) Uani 1 1 d . . . . .
H24 H -0.7062 -0.0471 0.3286 0.044 Uiso 1 1 calc R . . . .
C25 C -0.6599(5) 0.0245(2) 0.4087(4) 0.0392(11) Uani 1 1 d . . . . .
H25 H -0.7408 0.0278 0.4493 0.047 Uiso 1 1 calc R . . . .
C26 C -0.5576(4) 0.0643(2) 0.4206(4) 0.0325(9) Uani 1 1 d . . . . .
H26 H -0.5696 0.0940 0.4708 0.039 Uiso 1 1 calc R . . . .
C32 C 1.0392(4) 0.12548(19) 0.7975(4) 0.0293(9) Uani 1 1 d . . . . .
H32 H 0.9830 0.0972 0.7692 0.035 Uiso 1 1 calc R . . . .
C33 C 1.1723(5) 0.1136(2) 0.8335(4) 0.0342(10) Uani 1 1 d . . . . .
H33 H 1.2053 0.0777 0.8298 0.041 Uiso 1 1 calc R . . . .
C34 C 1.2555(4) 0.1556(2) 0.8747(4) 0.0354(10) Uani 1 1 d . . . . .
H34 H 1.3459 0.1485 0.8975 0.042 Uiso 1 1 calc R . . . .
C35 C 1.2030(5) 0.2087(2) 0.8819(4) 0.0384(11) Uani 1 1 d . . . . .
H35 H 1.2563 0.2375 0.9116 0.046 Uiso 1 1 calc R . . . .
C36 C 1.0690(5) 0.2177(2) 0.8439(4) 0.0335(9) Uani 1 1 d . . . . .
H36 H 1.0330 0.2533 0.8471 0.040 Uiso 1 1 calc R . . . .
C42 C 0.4047(4) 0.5633(2) 0.3439(4) 0.0326(9) Uani 1 1 d . . . . .
H42 H 0.4789 0.5392 0.3490 0.039 Uiso 1 1 calc R . . . .
C43 C 0.4197(5) 0.6133(2) 0.2887(4) 0.0348(10) Uani 1 1 d . . . . .
H43 H 0.5031 0.6229 0.2569 0.042 Uiso 1 1 calc R . . . .
C44 C 0.3103(5) 0.6488(2) 0.2810(4) 0.0371(10) Uani 1 1 d . . . . .
H44 H 0.3187 0.6829 0.2445 0.044 Uiso 1 1 calc R . . . .
C45 C 0.1869(5) 0.63303(19) 0.3285(4) 0.0335(9) Uani 1 1 d . . . . .
H45 H 0.1109 0.6562 0.3229 0.040 Uiso 1 1 calc R . . . .
C46 C 0.1782(4) 0.58267(18) 0.3842(4) 0.0286(8) Uani 1 1 d . . . . .
H46 H 0.0964 0.5724 0.4178 0.034 Uiso 1 1 calc R . . . .
O101 O 0.0536(9) 0.0079(2) 0.6465(5) 0.092(2) Uani 1 1 d . . . . .
H10A H 0.0472 0.0397 0.6154 0.138 Uiso 1 1 d G . . . .
H10B H 0.0455 -0.0167 0.5941 0.138 Uiso 1 1 d G . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 O8 2.186(3) . ?
I1 N21 2.256(3) . ?
I2 O11 2.174(3) . ?
I2 N31 2.291(3) . ?
I3 O14 2.170(3) . ?
I3 N41 2.277(3) . ?
O8 C7 1.308(5) . ?
O9 C7 1.220(6) . ?
O11 C10 1.297(5) . ?
O12 C10 1.218(6) . ?
O14 C13 1.295(5) . ?
O15 C13 1.222(5) . ?
N21 C22 1.344(6) . ?
N21 C26 1.340(6) . ?
N31 C32 1.333(6) . ?
N31 C36 1.332(6) . ?
N41 C42 1.340(6) . ?
N41 C46 1.337(5) . ?
C1 C2 1.401(5) . ?
C1 C6 1.387(6) . ?
C1 C7 1.512(5) . ?
C2 H2 0.9300 . ?
C2 C3 1.390(6) . ?
C3 C4 1.401(6) . ?
C3 C10 1.518(5) . ?
C4 H4 0.9300 . ?
C4 C5 1.394(5) . ?
C5 C6 1.401(5) . ?
C5 C13 1.502(5) . ?
C6 H6 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.383(6) . ?
C23 H23 0.9300 . ?
C23 C24 1.377(7) . ?
C24 H24 0.9300 . ?
C24 C25 1.375(8) . ?
C25 H25 0.9300 . ?
C25 C26 1.393(6) . ?
C26 H26 0.9300 . ?
C32 H32 0.9300 . ?
C32 C33 1.383(6) . ?
C33 H33 0.9300 . ?
C33 C34 1.378(7) . ?
C34 H34 0.9300 . ?
C34 C35 1.387(7) . ?
C35 H35 0.9300 . ?
C35 C36 1.386(6) . ?
C36 H36 0.9300 . ?
C42 H42 0.9300 . ?
C42 C43 1.376(7) . ?
C43 H43 0.9300 . ?
C43 C44 1.373(7) . ?
C44 H44 0.9300 . ?
C44 C45 1.388(7) . ?
C45 H45 0.9300 . ?
C45 C46 1.380(6) . ?
C46 H46 0.9300 . ?
O101 H10A 0.8501 . ?
O101 H10B 0.8499 . ?

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
O8 I1 N21 179.81(13) . . ?
O11 I2 N31 173.13(13) . . ?
O14 I3 N41 173.24(13) . . ?
C7 O8 I1 115.5(3) . . ?
C10 O11 I2 116.8(3) . . ?
C13 O14 I3 115.8(2) . . ?
C22 N21 I1 119.1(3) . . ?
C26 N21 I1 120.4(3) . . ?
C26 N21 C22 120.0(4) . . ?
C32 N31 I2 120.4(3) . . ?
C36 N31 I2 119.1(3) . . ?
C36 N31 C32 120.4(4) . . ?
C42 N41 I3 117.6(3) . . ?
C46 N41 I3 122.4(3) . . ?
C46 N41 C42 120.0(4) . . ?
C2 C1 C7 117.9(4) . . ?
C6 C1 C2 119.9(4) . . ?
C6 C1 C7 122.2(3) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.2(4) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 C10 118.2(4) . . ?
C4 C3 C10 121.8(4) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 C3 119.9(4) . . ?
C5 C4 H4 120.0 . . ?
C4 C5 C6 119.8(4) . . ?
C4 C5 C13 121.5(4) . . ?
C6 C5 C13 118.6(3) . . ?
C1 C6 C5 120.3(3) . . ?
C1 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
O8 C7 C1 113.6(4) . . ?
O9 C7 O8 125.2(4) . . ?
O9 C7 C1 121.2(4) . . ?
O11 C10 C3 113.9(4) . . ?
O12 C10 O11 126.0(4) . . ?
O12 C10 C3 120.0(4) . . ?
O14 C13 C5 113.7(3) . . ?
O15 C13 O14 125.5(4) . . ?
O15 C13 C5 120.9(4) . . ?
N21 C22 H22 119.2 . . ?
N21 C22 C23 121.6(4) . . ?
C23 C22 H22 119.2 . . ?
C22 C23 H23 120.7 . . ?
C24 C23 C22 118.5(5) . . ?
C24 C23 H23 120.7 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.0(4) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 120.5 . . ?
C24 C25 C26 119.0(5) . . ?
C26 C25 H25 120.5 . . ?
N21 C26 C25 120.8(5) . . ?
N21 C26 H26 119.6 . . ?
C25 C26 H26 119.6 . . ?
N31 C32 H32 119.5 . . ?
N31 C32 C33 120.9(4) . . ?
C33 C32 H32 119.5 . . ?
C32 C33 H33 120.3 . . ?
C34 C33 C32 119.4(4) . . ?
C34 C33 H33 120.3 . . ?
C33 C34 H34 120.4 . . ?
C33 C34 C35 119.2(4) . . ?
C35 C34 H34 120.4 . . ?
C34 C35 H35 120.8 . . ?
C36 C35 C34 118.4(4) . . ?
C36 C35 H35 120.8 . . ?
N31 C36 C35 121.7(5) . . ?
N31 C36 H36 119.2 . . ?
C35 C36 H36 119.2 . . ?
N41 C42 H42 119.3 . . ?
N41 C42 C43 121.5(4) . . ?
C43 C42 H42 119.3 . . ?
C42 C43 H43 120.4 . . ?
C44 C43 C42 119.3(4) . . ?
C44 C43 H43 120.4 . . ?
C43 C44 H44 120.5 . . ?
C43 C44 C45 119.0(4) . . ?
C45 C44 H44 120.5 . . ?
C44 C45 H45 120.4 . . ?
C46 C45 C44 119.2(4) . . ?
C46 C45 H45 120.4 . . ?
N41 C46 C45 121.0(4) . . ?
N41 C46 H46 119.5 . . ?
C45 C46 H46 119.5 . . ?
H10A O101 H10B 109.5 . . ?


_ins_header                      
;
TITL OIK008_numabs_ana2 in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 1.54184   9.762113  24.210092  11.478524  90.0000  91.4366  90.0000
ZERR    4.00   0.000152   0.000477   0.000206   0.0000   0.0017   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H N O I
UNIT 96.00 72.00 12.00 24.00 12.00
TREF
HKLF 4
END
;
_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 1.341
_oxdiff_exptl_absorpt_empirical_full_min 0.707
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/pentane'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3a_py_4
_database_code_depnum_ccdc_archive 'CCDC 2173468'
loop_
_audit_author_name
_audit_author_address
'Jas Ward'
;University of Jyvaskyla
Finland
;
_audit_update_record             
;
2022-05-18 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;
_audit_creation_date             2021-11-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2014/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C44 H38 Ag3 N7 O6'
_chemical_formula_sum            'C44 H38 Ag3 N7 O6'
_chemical_formula_weight         1084.42
_chemical_melting_point          ?
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'
Ag Ag -0.8971 1.1015 '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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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'

_cell_length_a                   20.8504(9)
_cell_length_b                   10.5290(3)
_cell_length_c                   19.2520(4)
_cell_angle_alpha                90
_cell_angle_beta                 91.048(3)
_cell_angle_gamma                90
_cell_volume                     4225.8(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    6022
_cell_measurement_temperature    119.96(19)
_cell_measurement_theta_max      27.2700
_cell_measurement_theta_min      2.7410
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2160
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 7 24 0.0426
-1 -7 -24 0.0426
6 -13 11 0.0384
-6 13 -11 0.0844
29 3 -2 0.0073
-29 -3 2 0.0020
-6 12 -14 0.0800

_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.009
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
1.1056 7.0428 23.8458 0.1574 -0.2294 0.9605
-1.1056 -7.0428 -23.8458 -0.1574 0.2294 -0.9605
5.6416 -13.3621 10.5385 0.5308 -0.7718 -0.3501
-5.6416 13.3621 -10.5385 -0.5308 0.7718 0.3501
28.5572 3.4423 -1.7098 0.8189 0.5630 0.1111
-28.5572 -3.4423 1.7098 -0.8189 -0.5630 -0.1111
-5.9847 11.9846 -14.0194 -0.5531 0.7873 0.1935

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43231
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.116
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.96(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0053
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -42.00  12.00   1.00   50.00    --  -18.29 -77.00  90.00   54
  2  ω    -42.00  12.00   1.00   50.00    --  -18.29 -77.00 -60.00   54
  3  ω    -53.00  45.00   1.00   50.00    --   19.23 -37.00 -60.00   98
  4  ω    -50.00  41.00   1.00   50.00    --   19.23 -57.00  30.00   91
  5  ω     39.00  95.00   1.00   50.00    --   19.23 178.00   0.00   56
  6  ω    -50.00  41.00   1.00   50.00    --   19.23 -57.00 150.00   91
  7  ω    -11.00  42.00   1.00   50.00    --   19.23  77.00 -90.00   53
  8  ω     15.00  92.00   1.00   50.00    --   19.23  37.00 120.00   77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0314925000
_diffrn_orient_matrix_UB_12      -0.0181438000
_diffrn_orient_matrix_UB_13      0.0104991000
_diffrn_orient_matrix_UB_21      0.0129206000
_diffrn_orient_matrix_UB_22      0.0447381000
_diffrn_orient_matrix_UB_23      -0.0234317000
_diffrn_orient_matrix_UB_31      -0.0001891000
_diffrn_orient_matrix_UB_32      0.0469579000
_diffrn_orient_matrix_UB_33      0.0264205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6802
_reflns_number_total             8637
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_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)'
_refine_diff_density_max         2.161
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.1071
_refine_ls_R_factor_gt           0.0794
_refine_ls_restrained_S_all      1.209
_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)+(0.0312P)²+16.7942P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1319
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 N51, C52, C53, C54, C55, C56
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
 C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
  C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
 C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74),
  C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ag1 Ag 0.85511(3) 0.61370(6) 0.56486(3) 0.02388(15) Uani 1 1 d . . . . .
Ag2 Ag 0.88294(3) 0.87523(6) 0.62228(3) 0.02410(15) Uani 1 1 d . . . . .
Ag3 Ag 0.53265(3) 0.26648(6) 0.79748(3) 0.02835(16) Uani 1 1 d . . . . .
O8 O 0.7941(2) 0.6133(5) 0.6648(2) 0.0247(12) Uani 1 1 d . . . . .
O9 O 0.8436(2) 0.7746(5) 0.7203(2) 0.0228(11) Uani 1 1 d . . . . .
O11 O 0.8036(2) 0.5894(5) 1.0324(2) 0.0243(12) Uani 1 1 d . . . . .
O12 O 0.8633(2) 0.7323(5) 0.9770(2) 0.0248(12) Uani 1 1 d . . . . .
O14 O 0.6173(2) 0.4043(5) 0.7853(2) 0.0267(12) Uani 1 1 d . . . . .
O15 O 0.6158(2) 0.3990(5) 0.9014(2) 0.0286(12) Uani 1 1 d . . . . .
N21 N 0.7960(3) 0.4838(6) 0.4869(3) 0.0306(16) Uani 1 1 d . . . . .
N31 N 0.9461(3) 0.5314(6) 0.6167(3) 0.0248(14) Uani 1 1 d . . . . .
N41 N 0.9890(3) 0.8579(6) 0.5948(3) 0.0296(15) Uani 1 1 d . . . . .
N51 N 0.8377(4) 1.0768(7) 0.6639(3) 0.0421(15) Uani 1 1 d . U . . .
N61 N 0.5286(3) 0.2333(6) 0.6750(3) 0.0246(14) Uani 1 1 d . . . . .
N71 N 0.5684(3) 0.0518(6) 0.8283(3) 0.0300(15) Uani 1 1 d . . . . .
N81 N 0.4410(3) 0.2568(6) 0.8588(3) 0.0259(14) Uani 1 1 d . . . . .
C1 C 0.7797(3) 0.6339(6) 0.7854(3) 0.0136(14) Uani 1 1 d . . . . .
C2 C 0.8098(3) 0.6635(6) 0.8487(3) 0.0155(14) Uani 1 1 d . . . . .
H2 H 0.8456 0.7161 0.8496 0.019 Uiso 1 1 calc R . . . .
C3 C 0.7863(3) 0.6147(6) 0.9104(3) 0.0155(14) Uani 1 1 d . . . . .
C4 C 0.7318(3) 0.5405(6) 0.9098(3) 0.0157(15) Uani 1 1 d . . . . .
H4 H 0.7159 0.5094 0.9513 0.019 Uiso 1 1 calc R . . . .
C5 C 0.7002(3) 0.5117(6) 0.8469(3) 0.0151(14) Uani 1 1 d . . . . .
C6 C 0.7253(3) 0.5586(6) 0.7857(3) 0.0166(15) Uani 1 1 d . . . . .
H6 H 0.7050 0.5389 0.7437 0.020 Uiso 1 1 calc R . . . .
C7 C 0.8082(3) 0.6798(7) 0.7181(3) 0.0170(15) Uani 1 1 d . . . . .
C10 C 0.8207(3) 0.6479(7) 0.9792(3) 0.0173(15) Uani 1 1 d . . . . .
C13 C 0.6396(3) 0.4314(7) 0.8452(4) 0.0191(15) Uani 1 1 d . . . . .
C22 C 0.7582(4) 0.3883(8) 0.5023(4) 0.036(2) Uani 1 1 d . . . . .
H22 H 0.7527 0.3707 0.5491 0.043 Uiso 1 1 calc R . . . .
C23 C 0.7257(4) 0.3112(8) 0.4546(5) 0.038(2) Uani 1 1 d . . . . .
H23 H 0.7002 0.2437 0.4687 0.046 Uiso 1 1 calc R . . . .
C24 C 0.7331(4) 0.3403(9) 0.3852(4) 0.042(2) Uani 1 1 d . . . . .
H24 H 0.7116 0.2939 0.3509 0.051 Uiso 1 1 calc R . . . .
C25 C 0.7726(4) 0.4376(8) 0.3678(4) 0.042(2) Uani 1 1 d . . . . .
H25 H 0.7797 0.4563 0.3214 0.050 Uiso 1 1 calc R . . . .
C26 C 0.8016(4) 0.5080(8) 0.4191(4) 0.038(2) Uani 1 1 d . . . . .
H26 H 0.8268 0.5766 0.4060 0.046 Uiso 1 1 calc R . . . .
C32 C 0.9655(4) 0.5690(8) 0.6793(4) 0.036(2) Uani 1 1 d . . . . .
H32 H 0.9414 0.6311 0.7011 0.043 Uiso 1 1 calc R . . . .
C33 C 1.0182(4) 0.5235(9) 0.7143(4) 0.044(2) Uani 1 1 d . . . . .
H33 H 1.0299 0.5548 0.7579 0.052 Uiso 1 1 calc R . . . .
C34 C 1.0537(4) 0.4295(9) 0.6831(4) 0.047(2) Uani 1 1 d . . . . .
H34 H 1.0899 0.3953 0.7050 0.056 Uiso 1 1 calc R . . . .
C35 C 1.0338(4) 0.3877(9) 0.6179(4) 0.047(3) Uani 1 1 d . . . . .
H35 H 1.0559 0.3239 0.5951 0.057 Uiso 1 1 calc R . . . .
C36 C 0.9807(4) 0.4427(9) 0.5881(4) 0.037(2) Uani 1 1 d . . . . .
H36 H 0.9683 0.4150 0.5440 0.045 Uiso 1 1 calc R . . . .
C42 C 1.0047(5) 0.8522(10) 0.5282(4) 0.053(3) Uani 1 1 d . . . . .
H42 H 0.9717 0.8491 0.4951 0.064 Uiso 1 1 calc R . . . .
C43 C 1.0663(4) 0.8505(10) 0.5058(5) 0.055(3) Uani 1 1 d . . . . .
H43 H 1.0744 0.8505 0.4585 0.066 Uiso 1 1 calc R . . . .
C44 C 1.1161(5) 0.8490(9) 0.5529(5) 0.051(3) Uani 1 1 d . . . . .
H44 H 1.1584 0.8471 0.5385 0.061 Uiso 1 1 calc R . . . .
C45 C 1.1020(4) 0.8502(11) 0.6213(5) 0.056(3) Uani 1 1 d . . . . .
H45 H 1.1342 0.8481 0.6554 0.067 Uiso 1 1 calc R . . . .
C46 C 1.0389(4) 0.8546(10) 0.6383(5) 0.052(3) Uani 1 1 d . . . . .
H46 H 1.0299 0.8555 0.6854 0.063 Uiso 1 1 calc R . . . .
C52 C 0.8533(5) 1.1921(9) 0.6705(5) 0.056(2) Uani 1 1 d . U . . .
H52 H 0.8955 1.2121 0.6603 0.067 Uiso 1 1 calc R . . . .
C53 C 0.8146(5) 1.2936(9) 0.6912(4) 0.050(2) Uani 1 1 d . U . . .
H53 H 0.8315 1.3736 0.7008 0.060 Uiso 1 1 calc R . . . .
C54 C 0.7507(5) 1.2684(9) 0.6964(5) 0.054(2) Uani 1 1 d . U . . .
H54 H 0.7221 1.3322 0.7083 0.065 Uiso 1 1 calc R . . . .
C55 C 0.7295(5) 1.1470(9) 0.6838(5) 0.055(2) Uani 1 1 d . U . . .
H55 H 0.6860 1.1281 0.6860 0.066 Uiso 1 1 calc R . . . .
C56 C 0.7715(5) 1.0562(9) 0.6684(4) 0.0485(19) Uani 1 1 d . U . . .
H56 H 0.7559 0.9747 0.6602 0.058 Uiso 1 1 calc R . . . .
C62 C 0.5713(4) 0.2946(8) 0.6371(4) 0.0288(18) Uani 1 1 d . . . . .
H62 H 0.6000 0.3493 0.6595 0.035 Uiso 1 1 calc R . . . .
C63 C 0.5750(4) 0.2804(8) 0.5656(4) 0.035(2) Uani 1 1 d . . . . .
H63 H 0.6049 0.3264 0.5407 0.042 Uiso 1 1 calc R . . . .
C64 C 0.5345(4) 0.1989(8) 0.5325(4) 0.037(2) Uani 1 1 d . . . . .
H64 H 0.5370 0.1860 0.4848 0.044 Uiso 1 1 calc R . . . .
C65 C 0.4895(4) 0.1353(8) 0.5710(4) 0.035(2) Uani 1 1 d . . . . .
H65 H 0.4605 0.0802 0.5497 0.042 Uiso 1 1 calc R . . . .
C66 C 0.4884(4) 0.1551(7) 0.6422(4) 0.0290(18) Uani 1 1 d . . . . .
H66 H 0.4582 0.1117 0.6680 0.035 Uiso 1 1 calc R . . . .
C72 C 0.5992(4) -0.0197(9) 0.7830(4) 0.042(2) Uani 1 1 d . . . . .
H72 H 0.5955 0.0007 0.7361 0.050 Uiso 1 1 calc R . . . .
C73 C 0.6358(5) -0.1210(9) 0.8018(5) 0.054(3) Uani 1 1 d . . . . .
H73 H 0.6567 -0.1679 0.7681 0.064 Uiso 1 1 calc R . . . .
C74 C 0.6417(5) -0.1540(9) 0.8697(6) 0.063(3) Uani 1 1 d . . . . .
H74 H 0.6675 -0.2219 0.8835 0.076 Uiso 1 1 calc R . . . .
C75 C 0.6081(5) -0.0831(9) 0.9184(5) 0.053(3) Uani 1 1 d . . . . .
H75 H 0.6097 -0.1043 0.9653 0.063 Uiso 1 1 calc R . . . .
C76 C 0.5725(4) 0.0188(9) 0.8952(4) 0.039(2) Uani 1 1 d . . . . .
H76 H 0.5503 0.0668 0.9274 0.047 Uiso 1 1 calc R . . . .
C82 C 0.4158(5) 0.3544(8) 0.8933(4) 0.042(2) Uani 1 1 d . . . . .
H82 H 0.4387 0.4299 0.8963 0.050 Uiso 1 1 calc R . . . .
C83 C 0.3563(5) 0.3470(10) 0.9249(4) 0.055(3) Uani 1 1 d . . . . .
H83 H 0.3399 0.4169 0.9481 0.066 Uiso 1 1 calc R . . . .
C84 C 0.3228(4) 0.2375(12) 0.9214(4) 0.055(3) Uani 1 1 d . . . . .
H84 H 0.2831 0.2308 0.9423 0.066 Uiso 1 1 calc R . . . .
C85 C 0.3479(4) 0.1369(10) 0.8866(4) 0.041(2) Uani 1 1 d . . . . .
H85 H 0.3257 0.0605 0.8837 0.049 Uiso 1 1 calc R . . . .
C86 C 0.4061(4) 0.1496(8) 0.8562(4) 0.0277(18) Uani 1 1 d . . . . .
H86 H 0.4225 0.0804 0.8324 0.033 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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
Ag1 Ag2 3.0195(8) . ?
Ag1 O8 2.326(4) . ?
Ag1 O12 2.351(5) 4_575 ?
Ag1 N21 2.361(6) . ?
Ag1 N31 2.296(6) . ?
Ag2 O9 2.326(4) . ?
Ag2 O11 2.402(5) 4_575 ?
Ag2 N41 2.292(6) . ?
Ag2 N51 2.463(7) . ?
Ag3 O14 2.301(5) . ?
Ag3 N61 2.384(5) . ?
Ag3 N71 2.450(6) . ?
Ag3 N81 2.267(6) . ?
O8 C7 1.272(8) . ?
O9 C7 1.243(8) . ?
O11 Ag2 2.402(5) 4_576 ?
O11 C10 1.253(8) . ?
O12 Ag1 2.351(5) 4_576 ?
O12 C10 1.256(8) . ?
O14 C13 1.268(8) . ?
O15 C13 1.246(8) . ?
N21 C22 1.315(10) . ?
N21 C26 1.338(9) . ?
N31 C32 1.326(9) . ?
N31 C36 1.308(10) . ?
N41 C42 1.329(10) . ?
N41 C46 1.323(10) . ?
N51 C52 1.263(11) . ?
N51 C56 1.401(12) . ?
N61 C62 1.328(9) . ?
N61 C66 1.327(9) . ?
N71 C72 1.326(10) . ?
N71 C76 1.334(9) . ?
N81 C82 1.337(10) . ?
N81 C86 1.343(9) . ?
C1 C2 1.395(8) . ?
C1 C6 1.384(9) . ?
C1 C7 1.514(9) . ?
C2 H2 0.9300 . ?
C2 C3 1.393(9) . ?
C3 C4 1.379(9) . ?
C3 C10 1.535(8) . ?
C4 H4 0.9300 . ?
C4 C5 1.400(9) . ?
C5 C6 1.389(9) . ?
C5 C13 1.521(9) . ?
C6 H6 0.9300 . ?
C22 H22 0.9300 . ?
C22 C23 1.392(11) . ?
C23 H23 0.9300 . ?
C23 C24 1.382(12) . ?
C24 H24 0.9300 . ?
C24 C25 1.359(12) . ?
C25 H25 0.9300 . ?
C25 C26 1.366(11) . ?
C26 H26 0.9300 . ?
C32 H32 0.9300 . ?
C32 C33 1.366(11) . ?
C33 H33 0.9300 . ?
C33 C34 1.380(12) . ?
C34 H34 0.9300 . ?
C34 C35 1.386(12) . ?
C35 H35 0.9300 . ?
C35 C36 1.365(11) . ?
C36 H36 0.9300 . ?
C42 H42 0.9300 . ?
C42 C43 1.363(12) . ?
C43 H43 0.9300 . ?
C43 C44 1.366(13) . ?
C44 H44 0.9300 . ?
C44 C45 1.355(13) . ?
C45 H45 0.9300 . ?
C45 C46 1.362(12) . ?
C46 H46 0.9300 . ?
C52 H52 0.9300 . ?
C52 C53 1.401(12) . ?
C53 H53 0.9300 . ?
C53 C54 1.364(13) . ?
C54 H54 0.9300 . ?
C54 C55 1.373(13) . ?
C55 H55 0.9300 . ?
C55 C56 1.332(12) . ?
C56 H56 0.9300 . ?
C62 H62 0.9300 . ?
C62 C63 1.389(10) . ?
C63 H63 0.9300 . ?
C63 C64 1.355(11) . ?
C64 H64 0.9300 . ?
C64 C65 1.380(11) . ?
C65 H65 0.9300 . ?
C65 C66 1.386(10) . ?
C66 H66 0.9300 . ?
C72 H72 0.9300 . ?
C72 C73 1.356(12) . ?
C73 H73 0.9300 . ?
C73 C74 1.356(14) . ?
C74 H74 0.9300 . ?
C74 C75 1.398(14) . ?
C75 H75 0.9300 . ?
C75 C76 1.375(12) . ?
C76 H76 0.9300 . ?
C82 H82 0.9300 . ?
C82 C83 1.393(13) . ?
C83 H83 0.9300 . ?
C83 C84 1.349(14) . ?
C84 H84 0.9300 . ?
C84 C85 1.363(13) . ?
C85 H85 0.9300 . ?
C85 C86 1.363(10) . ?
C86 H86 0.9300 . ?

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
O8 Ag1 Ag2 78.65(12) . . ?
O8 Ag1 O12 130.11(17) . 4_575 ?
O8 Ag1 N21 103.75(19) . . ?
O12 Ag1 Ag2 67.57(12) 4_575 . ?
O12 Ag1 N21 89.20(19) 4_575 . ?
N21 Ag1 Ag2 148.82(16) . . ?
N31 Ag1 Ag2 91.91(16) . . ?
N31 Ag1 O8 95.73(19) . . ?
N31 Ag1 O12 120.2(2) . 4_575 ?
N31 Ag1 N21 118.4(2) . . ?
O9 Ag2 Ag1 79.24(12) . . ?
O9 Ag2 O11 114.00(17) . 4_575 ?
O9 Ag2 N51 89.2(2) . . ?
O11 Ag2 Ag1 75.66(12) 4_575 . ?
O11 Ag2 N51 80.7(2) 4_575 . ?
N41 Ag2 Ag1 91.30(16) . . ?
N41 Ag2 O9 120.46(19) . . ?
N41 Ag2 O11 120.10(19) . 4_575 ?
N41 Ag2 N51 121.4(3) . . ?
N51 Ag2 Ag1 146.38(19) . . ?
O14 Ag3 N61 90.28(18) . . ?
O14 Ag3 N71 112.1(2) . . ?
N61 Ag3 N71 96.3(2) . . ?
N81 Ag3 O14 137.5(2) . . ?
N81 Ag3 N61 119.6(2) . . ?
N81 Ag3 N71 95.0(2) . . ?
C7 O8 Ag1 123.0(4) . . ?
C7 O9 Ag2 123.8(4) . . ?
C10 O11 Ag2 108.0(4) . 4_576 ?
C10 O12 Ag1 113.8(4) . 4_576 ?
C13 O14 Ag3 108.5(4) . . ?
C22 N21 Ag1 127.5(5) . . ?
C22 N21 C26 115.4(7) . . ?
C26 N21 Ag1 117.1(5) . . ?
C32 N31 Ag1 121.3(5) . . ?
C36 N31 Ag1 123.0(5) . . ?
C36 N31 C32 115.7(7) . . ?
C42 N41 Ag2 118.7(6) . . ?
C46 N41 Ag2 127.3(6) . . ?
C46 N41 C42 113.9(8) . . ?
C52 N51 Ag2 139.6(7) . . ?
C52 N51 C56 113.2(9) . . ?
C56 N51 Ag2 105.7(5) . . ?
C62 N61 Ag3 117.4(5) . . ?
C66 N61 Ag3 124.9(5) . . ?
C66 N61 C62 117.7(6) . . ?
C72 N71 Ag3 120.9(5) . . ?
C72 N71 C76 117.6(7) . . ?
C76 N71 Ag3 119.2(5) . . ?
C82 N81 Ag3 124.6(6) . . ?
C82 N81 C86 116.5(7) . . ?
C86 N81 Ag3 118.7(5) . . ?
C2 C1 C7 120.0(6) . . ?
C6 C1 C2 118.6(6) . . ?
C6 C1 C7 121.4(6) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.3(6) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 C10 119.1(6) . . ?
C4 C3 C2 120.3(6) . . ?
C4 C3 C10 120.6(6) . . ?
C3 C4 H4 119.8 . . ?
C3 C4 C5 120.3(6) . . ?
C5 C4 H4 119.8 . . ?
C4 C5 C13 121.1(6) . . ?
C6 C5 C4 118.5(6) . . ?
C6 C5 C13 120.4(6) . . ?
C1 C6 C5 122.0(6) . . ?
C1 C6 H6 119.0 . . ?
C5 C6 H6 119.0 . . ?
O8 C7 C1 115.2(6) . . ?
O9 C7 O8 126.8(6) . . ?
O9 C7 C1 118.0(6) . . ?
O11 C10 O12 126.0(6) . . ?
O11 C10 C3 117.2(6) . . ?
O12 C10 C3 116.8(6) . . ?
O14 C13 C5 115.8(6) . . ?
O15 C13 O14 125.7(7) . . ?
O15 C13 C5 118.5(6) . . ?
N21 C22 H22 117.1 . . ?
N21 C22 C23 125.8(8) . . ?
C23 C22 H22 117.1 . . ?
C22 C23 H23 121.8 . . ?
C24 C23 C22 116.5(8) . . ?
C24 C23 H23 121.8 . . ?
C23 C24 H24 120.5 . . ?
C25 C24 C23 119.0(8) . . ?
C25 C24 H24 120.5 . . ?
C24 C25 H25 120.2 . . ?
C24 C25 C26 119.6(8) . . ?
C26 C25 H25 120.2 . . ?
N21 C26 C25 123.8(8) . . ?
N21 C26 H26 118.1 . . ?
C25 C26 H26 118.1 . . ?
N31 C32 H32 117.5 . . ?
N31 C32 C33 125.0(8) . . ?
C33 C32 H32 117.5 . . ?
C32 C33 H33 121.0 . . ?
C32 C33 C34 118.0(8) . . ?
C34 C33 H33 121.0 . . ?
C33 C34 H34 121.1 . . ?
C33 C34 C35 117.8(8) . . ?
C35 C34 H34 121.1 . . ?
C34 C35 H35 120.9 . . ?
C36 C35 C34 118.3(8) . . ?
C36 C35 H35 120.9 . . ?
N31 C36 C35 125.1(7) . . ?
N31 C36 H36 117.4 . . ?
C35 C36 H36 117.4 . . ?
N41 C42 H42 118.1 . . ?
N41 C42 C43 123.7(9) . . ?
C43 C42 H42 118.1 . . ?
C42 C43 H43 120.0 . . ?
C42 C43 C44 120.0(9) . . ?
C44 C43 H43 120.0 . . ?
C43 C44 H44 121.0 . . ?
C45 C44 C43 118.0(9) . . ?
C45 C44 H44 121.0 . . ?
C44 C45 H45 121.3 . . ?
C44 C45 C46 117.4(9) . . ?
C46 C45 H45 121.3 . . ?
N41 C46 C45 126.9(8) . . ?
N41 C46 H46 116.6 . . ?
C45 C46 H46 116.6 . . ?
N51 C52 H52 116.1 . . ?
N51 C52 C53 127.8(11) . . ?
C53 C52 H52 116.1 . . ?
C52 C53 H53 121.9 . . ?
C54 C53 C52 116.2(10) . . ?
C54 C53 H53 121.9 . . ?
C53 C54 H54 120.7 . . ?
C53 C54 C55 118.7(10) . . ?
C55 C54 H54 120.7 . . ?
C54 C55 H55 120.1 . . ?
C56 C55 C54 119.8(11) . . ?
C56 C55 H55 120.1 . . ?
N51 C56 H56 118.2 . . ?
C55 C56 N51 123.7(9) . . ?
C55 C56 H56 118.2 . . ?
N61 C62 H62 118.6 . . ?
N61 C62 C63 122.8(7) . . ?
C63 C62 H62 118.6 . . ?
C62 C63 H63 120.3 . . ?
C64 C63 C62 119.3(7) . . ?
C64 C63 H63 120.3 . . ?
C63 C64 H64 120.7 . . ?
C63 C64 C65 118.5(7) . . ?
C65 C64 H64 120.7 . . ?
C64 C65 H65 120.6 . . ?
C64 C65 C66 118.9(8) . . ?
C66 C65 H65 120.6 . . ?
N61 C66 C65 122.8(7) . . ?
N61 C66 H66 118.6 . . ?
C65 C66 H66 118.6 . . ?
N71 C72 H72 118.4 . . ?
N71 C72 C73 123.2(8) . . ?
C73 C72 H72 118.4 . . ?
C72 C73 H73 120.0 . . ?
C72 C73 C74 119.9(9) . . ?
C74 C73 H73 120.0 . . ?
C73 C74 H74 120.9 . . ?
C73 C74 C75 118.2(9) . . ?
C75 C74 H74 120.9 . . ?
C74 C75 H75 120.9 . . ?
C76 C75 C74 118.2(9) . . ?
C76 C75 H75 120.9 . . ?
N71 C76 C75 122.8(9) . . ?
N71 C76 H76 118.6 . . ?
C75 C76 H76 118.6 . . ?
N81 C82 H82 118.8 . . ?
N81 C82 C83 122.4(9) . . ?
C83 C82 H82 118.8 . . ?
C82 C83 H83 120.3 . . ?
C84 C83 C82 119.4(9) . . ?
C84 C83 H83 120.3 . . ?
C83 C84 H84 120.5 . . ?
C83 C84 C85 119.0(8) . . ?
C85 C84 H84 120.5 . . ?
C84 C85 H85 120.4 . . ?
C86 C85 C84 119.2(9) . . ?
C86 C85 H85 120.4 . . ?
N81 C86 C85 123.6(8) . . ?
N81 C86 H86 118.2 . . ?
C85 C86 H86 118.2 . . ?


_ins_header                      
;
TITL OIK096_scale1 in P2(1)/c 
REM P2(1)/c (#14 in standard setting)
CELL 0.71073  20.850443  10.528970  19.251987  90.0000  91.0477  90.0000
ZERR    4.00   0.000931   0.000340   0.000442   0.0000   0.0029   0.0000
LATT  1
SYMM -x, y+1/2,-z+1/2 
SFAC C H N O Ag
UNIT 176.00 152.00 28.00 24.00 12.00
TREF
HKLF 4
END
;
_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 1.164
_oxdiff_exptl_absorpt_empirical_full_min 0.887
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pyridine+DMSO/TBME'
