data_cu_tca_i2_0m
_audit_creation_date               2023-11-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_shelx_SHELXL_version_number       '2018/3'
_audit_contact_author_address      ?
_audit_contact_author_email        ?
_audit_contact_author_name         ''
_audit_contact_author_phone        ?
_publ_contact_author_id_orcid      ?
_publ_section_references
;
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
 (2009), J. Appl. Cryst. 42, 339-341.

Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8.

Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common              ?
_chemical_name_systematic          ?
_chemical_formula_moiety          
 '2(C21 H12 N O6), 2(C21 H15 N O6), 6(H4 N), 1.5(H2 O2), 2(C H I3)'
_chemical_formula_sum              'C86 H83 I6 N10 O27'
_chemical_formula_weight           2450.02
_chemical_absolute_configuration   ?
_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        'cubic'
_space_group_IT_number             197
_space_group_name_H-M_alt          'I 2 3'
_space_group_name_Hall             'I 2 2 3'
loop_
  _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, z'
 '-x, y, -z'
 'x, -y, -z'
 'z, x, y'
 'z, -x, -y'
 '-z, -x, y'
 '-z, x, -y'
 'y, z, x'
 '-y, z, -x'
 'y, -z, -x'
 '-y, -z, x'
 'x+1/2, y+1/2, z+1/2'
 '-x+1/2, -y+1/2, z+1/2'
 '-x+1/2, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z+1/2'
 'z+1/2, x+1/2, y+1/2'
 'z+1/2, -x+1/2, -y+1/2'
 '-z+1/2, -x+1/2, y+1/2'
 '-z+1/2, x+1/2, -y+1/2'
 'y+1/2, z+1/2, x+1/2'
 '-y+1/2, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x+1/2'
 '-y+1/2, -z+1/2, x+1/2'

_cell_length_a                     20.95740(10)
_cell_length_b                     20.95740(10)
_cell_length_c                     20.95740(10)
_cell_angle_alpha                  90
_cell_angle_beta                   90
_cell_angle_gamma                  90
_cell_volume                       9204.75(13)
_cell_formula_units_Z              4
_cell_measurement_reflns_used      5986
_cell_measurement_temperature      301.00
_cell_measurement_theta_max        61.80
_cell_measurement_theta_min        5.17
_shelx_estimated_absorpt_T_max     0.241
_shelx_estimated_absorpt_T_min     0.115
_exptl_absorpt_coefficient_mu      16.597
_exptl_absorpt_correction_T_max    0.7522
_exptl_absorpt_correction_T_min    0.5589
_exptl_absorpt_correction_type     cylinder
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1375 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.7430.
The λ/2 correction factor is Not present.
;
_exptl_absorpt_special_details     ?
_exptl_crystal_colour              'clear light yellow'
_exptl_crystal_colour_lustre       clear
_exptl_crystal_colour_modifier     light
_exptl_crystal_colour_primary      yellow
_exptl_crystal_density_diffrn      1.768
_exptl_crystal_density_meas        ?
_exptl_crystal_density_method      ?
_exptl_crystal_description         block
_exptl_crystal_F_000               4812
_exptl_crystal_size_max            0.23
_exptl_crystal_size_mid            0.14
_exptl_crystal_size_min            0.12
_exptl_transmission_factor_max     ?
_exptl_transmission_factor_min     ?
_diffrn_reflns_av_R_equivalents    0.0932
_diffrn_reflns_av_unetI/netI       0.0403
_diffrn_reflns_Laue_measured_fraction_full  0.999
_diffrn_reflns_Laue_measured_fraction_max  0.999
_diffrn_reflns_limit_h_max         23
_diffrn_reflns_limit_h_min         -16
_diffrn_reflns_limit_k_max         20
_diffrn_reflns_limit_k_min         -24
_diffrn_reflns_limit_l_max         23
_diffrn_reflns_limit_l_min         -23
_diffrn_reflns_number              18013
_diffrn_reflns_point_group_measured_fraction_full  0.999
_diffrn_reflns_point_group_measured_fraction_max  0.999
_diffrn_reflns_theta_full          62.548
_diffrn_reflns_theta_max           62.548
_diffrn_reflns_theta_min           5.169
_diffrn_ambient_temperature        301.00
_diffrn_detector_area_resol_mean   ?
_diffrn_measured_fraction_theta_full  0.999
_diffrn_measured_fraction_theta_max  0.999
_diffrn_measurement_device_type    'Bruker APEX-II CCD'
_diffrn_measurement_method         'φ and ω scans'
_diffrn_radiation_type             CuK\a
_diffrn_radiation_wavelength       1.54178
_diffrn_source                     ?
_diffrn_source_current             1.2
_diffrn_source_power               0.06
_diffrn_source_voltage             50.0
_diffrn_standards_number           0
_reflns_Friedel_coverage           0.831
_reflns_Friedel_fraction_full      1.000
_reflns_Friedel_fraction_max       1.000
_reflns_number_gt                  2098
_reflns_number_total               2458
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression       'I > 2σ(I)'
_computing_cell_refinement         'SAINT V8.40B (?, 2016)'
_computing_data_collection         ?
_computing_data_reduction          'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics      'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement    'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution      'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max           0.431
_refine_diff_density_min           -0.461
_refine_diff_density_rms           0.113
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack     0.5
_refine_ls_extinction_coef         0.0012(3)
_refine_ls_extinction_expression  
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^'
_refine_ls_extinction_method       'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref     1.150
_refine_ls_hydrogen_treatment      constr
_refine_ls_matrix_type             full
_refine_ls_number_parameters       190
_refine_ls_number_reflns           2458
_refine_ls_number_restraints       2
_refine_ls_R_factor_all            0.0835
_refine_ls_R_factor_gt             0.0748
_refine_ls_restrained_S_all        1.153
_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)+(0.1487P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme        calc
_refine_ls_wR_factor_gt            0.2032
_refine_ls_wR_factor_ref           0.2104
_refine_special_details
;
 Refined as a 2-component perfect inversion twin.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 I1-C4
 1.89 with sigma of 0.02
 N00G-C4
 3.2 with sigma of 0.02
3. Rigid bond restraints
 C4, I1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: H00M(0.5)
5.a Riding coordinates:
 O003(H003), N006(H00B), N006(H00C,H00G,H00H), O00M(H00M)
5.b Ternary CH refined with riding coordinates:
 C4(H4)
5.c Aromatic/amide H refined with riding coordinates:
 C00A(H00A), C00D(H00D), C00E(H00E), C00F(H00F), C00I(H00I), C00J(H00J),
 C00K(H00K), C00L(H00L)
;
_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
 O001 O 0.60622(19) 0.02026(18) 0.2698(2) 0.0690(11) Uani 1 1 d . . . . .
 O002 O 0.5857(2) 0.0131(2) 0.1666(2) 0.0784(13) Uani 1 1 d . . . . .
 O003 O 0.51972(19) 0.10155(19) 0.2688(2) 0.0748(13) Uani 1 1 d . . . . .
 H003 H 0.545514 0.074632 0.270618 0.112 Uiso 1 1 d R U . . .
 O004 O 0.5113(3) 0.0875(2) 0.3737(2) 0.0956(17) Uani 1 1 d . . . . .
 N005 N 0.3266(4) 0.3266(4) 0.3266(4) 0.088(3) Uani 1 3 d S T P . .
 N006 N 0.4973(3) 0.0922(2) 0.1130(2) 0.0743(14) Uani 1 1 d . . . . .
 H00B H 0.458532 0.080229 0.125532 0.089 Uiso 1 1 d R U . . .
 H00C H 0.498872 0.092729 0.070532 0.089 Uiso 1 1 d R U . . .
 H00G H 0.505562 0.131109 0.127922 0.089 Uiso 1 1 d R U . . .
 H00H H 0.526092 0.064879 0.127922 0.089 Uiso 1 1 d R U . . .
 C007 C 0.6165(2) -0.0013(3) 0.2143(3) 0.0589(12) Uani 1 1 d . . . . .
 C008 C 0.4982(3) 0.1160(3) 0.3246(3) 0.0628(13) Uani 1 1 d . . . . .
 C009 C 0.6693(2) -0.0498(2) 0.2074(3) 0.0569(13) Uani 1 1 d . . . . .
 C00A C 0.4299(3) 0.1955(3) 0.2674(3) 0.0685(16) Uani 1 1 d . . . . .
 H00A H 0.442355 0.177389 0.228874 0.082 Uiso 1 1 calc R U . . .
 C00B C 0.4527(2) 0.1709(3) 0.3251(3) 0.0641(14) Uani 1 1 d . . . . .
 C00C C 0.3695(3) 0.2740(3) 0.3257(3) 0.077(2) Uani 1 1 d . . . . .
 C00D C 0.6961(3) -0.0783(3) 0.2596(3) 0.0646(14) Uani 1 1 d . . . . .
 H00D H 0.681525 -0.067634 0.300093 0.078 Uiso 1 1 calc R U . . .
 C00E C 0.7440(3) -0.1222(3) 0.2534(3) 0.0753(18) Uani 1 1 d . . . . .
 H00E H 0.761520 -0.141553 0.289299 0.090 Uiso 1 1 calc R U . . .
 C00F C 0.3889(3) 0.2465(3) 0.2683(3) 0.0761(19) Uani 1 1 d . . . . .
 H00F H 0.373821 0.263007 0.229962 0.091 Uiso 1 1 calc R U . . .
 N00G N 0.8147(4) -0.1853(4) 0.1853(4) 0.094(4) Uani 1 3 d DS T P . .
 C00H C 0.7666(3) -0.1379(3) 0.1921(3) 0.0736(18) Uani 1 1 d . . . . .
 C00I C 0.6914(3) -0.0651(3) 0.1475(3) 0.0738(18) Uani 1 1 d . . . . .
 H00I H 0.673215 -0.045900 0.111866 0.089 Uiso 1 1 calc R U . . .
 C00J C 0.3918(4) 0.2490(4) 0.3810(3) 0.096(3) Uani 1 1 d . . . . .
 H00J H 0.380011 0.267238 0.419729 0.116 Uiso 1 1 calc R U . . .
 C00K C 0.7405(3) -0.1087(4) 0.1398(3) 0.087(2) Uani 1 1 d . . . . .
 H00K H 0.755623 -0.118186 0.099172 0.104 Uiso 1 1 calc R U . . .
 C00L C 0.4314(4) 0.1973(3) 0.3805(3) 0.088(2) Uani 1 1 d . . . . .
 H00L H 0.444227 0.179565 0.419089 0.105 Uiso 1 1 calc R U . . .
 O00M O 0.500000 0.0545(8) 0.500000 0.200(6) Uani 1 2 d S T P . .
 H00M H 0.503770 0.065985 0.460370 0.300 Uiso 0.5 1 d R U P . .
 I1 I 0.8577(13) -0.094(2) 0.0151(14) 1.96(4) Uiso 1 1 d D . . . .
 C4 C 0.9035(9) -0.0965(9) 0.0965(9) 1.3(3) Uiso 1 3 d DS . P . .
 H4 H 0.876506 -0.123494 0.123493 1.607 Uiso 1 3 calc R U P . .


_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
 O001 C007 1.267(7) . ?
 O002 C007 1.226(6) . ?
 O003 H003 0.7822 . ?
 O003 C008 1.288(7) . ?
 O004 C008 1.222(7) . ?
 N005 C00C 1.422(5) 9 ?
 N005 C00C 1.422(5) 5 ?
 N005 C00C 1.422(5) . ?
 N006 H00B 0.8897 . ?
 N006 H00C 0.8903 . ?
 N006 H00G 0.8900 . ?
 N006 H00H 0.8896 . ?
 C007 C009 1.511(6) . ?
 C008 C00B 1.494(7) . ?
 C009 C00D 1.366(8) . ?
 C009 C00I 1.375(9) . ?
 C00A H00A 0.9300 . ?
 C00A C00B 1.397(8) . ?
 C00A C00F 1.372(7) . ?
 C00B C00L 1.362(9) . ?
 C00C C00F 1.394(9) . ?
 C00C C00J 1.357(9) . ?
 C00D H00D 0.9300 . ?
 C00D C00E 1.368(7) . ?
 C00E H00E 0.9300 . ?
 C00E C00H 1.407(9) . ?
 C00F H00F 0.9300 . ?
 N00G C00H 1.423(5) 8_645 ?
 N00G C00H 1.423(5) 11_656 ?
 N00G C00H 1.423(5) . ?
 C00H C00K 1.370(8) . ?
 C00I H00I 0.9300 . ?
 C00I C00K 1.386(8) . ?
 C00J H00J 0.9300 . ?
 C00J C00L 1.365(8) . ?
 C00K H00K 0.9300 . ?
 C00L H00L 0.9300 . ?
 O00M H00M 0.8681 . ?
 O00M H00M 0.8680 3_656 ?
 I1 C4 1.96(2) . ?
 C4 H4 0.9800 . ?

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
 C008 O003 H003 111.6 . . ?
 C00C N005 C00C 119.2(2) 5 . ?
 C00C N005 C00C 119.2(2) 9 5 ?
 C00C N005 C00C 119.2(2) 9 . ?
 H00B N006 H00C 109.5 . . ?
 H00B N006 H00G 109.4 . . ?
 H00B N006 H00H 109.5 . . ?
 H00C N006 H00G 109.5 . . ?
 H00C N006 H00H 109.5 . . ?
 H00G N006 H00H 109.5 . . ?
 O001 C007 C009 116.9(4) . . ?
 O002 C007 O001 124.8(4) . . ?
 O002 C007 C009 118.2(5) . . ?
 O003 C008 C00B 114.3(4) . . ?
 O004 C008 O003 124.8(4) . . ?
 O004 C008 C00B 120.9(5) . . ?
 C00D C009 C007 121.3(5) . . ?
 C00D C009 C00I 119.4(5) . . ?
 C00I C009 C007 119.4(5) . . ?
 C00B C00A H00A 120.3 . . ?
 C00F C00A H00A 120.3 . . ?
 C00F C00A C00B 119.4(5) . . ?
 C00A C00B C008 119.8(5) . . ?
 C00L C00B C008 121.9(5) . . ?
 C00L C00B C00A 118.3(5) . . ?
 C00F C00C N005 121.1(6) . . ?
 C00J C00C N005 120.4(6) . . ?
 C00J C00C C00F 118.5(5) . . ?
 C009 C00D H00D 119.3 . . ?
 C009 C00D C00E 121.3(5) . . ?
 C00E C00D H00D 119.3 . . ?
 C00D C00E H00E 120.3 . . ?
 C00D C00E C00H 119.3(5) . . ?
 C00H C00E H00E 120.3 . . ?
 C00A C00F C00C 121.1(5) . . ?
 C00A C00F H00F 119.5 . . ?
 C00C C00F H00F 119.5 . . ?
 C00H N00G C00H 119.59(14) 8_645 11_656 ?
 C00H N00G C00H 119.59(14) 11_656 . ?
 C00H N00G C00H 119.59(14) 8_645 . ?
 C00E C00H N00G 119.5(6) . . ?
 C00K C00H C00E 119.5(5) . . ?
 C00K C00H N00G 120.9(6) . . ?
 C009 C00I H00I 119.7 . . ?
 C009 C00I C00K 120.6(5) . . ?
 C00K C00I H00I 119.7 . . ?
 C00C C00J H00J 119.7 . . ?
 C00C C00J C00L 120.6(6) . . ?
 C00L C00J H00J 119.7 . . ?
 C00H C00K C00I 119.8(6) . . ?
 C00H C00K H00K 120.1 . . ?
 C00I C00K H00K 120.1 . . ?
 C00B C00L C00J 122.0(6) . . ?
 C00B C00L H00L 119.0 . . ?
 C00J C00L H00L 119.0 . . ?
 H00M O00M H00M 147.9 . 3_656 ?
 I1 C4 I1 114.8(7) . 8_645 ?
 I1 C4 I1 114.8(7) . 11_656 ?
 I1 C4 I1 114.8(7) 11_656 8_645 ?
 I1 C4 H4 103.4 . . ?
 I1 C4 H4 103.4 8_645 . ?
 I1 C4 H4 103.4 11_656 . ?

loop_
  _geom_torsion_atom_site_label_1
  _geom_torsion_atom_site_label_2
  _geom_torsion_atom_site_label_3
  _geom_torsion_atom_site_label_4
  _geom_torsion
  _geom_torsion_site_symmetry_1
  _geom_torsion_site_symmetry_2
  _geom_torsion_site_symmetry_3
  _geom_torsion_site_symmetry_4
  _geom_torsion_publ_flag
 O001 C007 C009 C00D 12.5(8) . . . . ?
 O001 C007 C009 C00I -166.7(6) . . . . ?
 O002 C007 C009 C00D -165.6(6) . . . . ?
 O002 C007 C009 C00I 15.1(8) . . . . ?
 O003 C008 C00B C00A 9.4(9) . . . . ?
 O003 C008 C00B C00L -172.0(7) . . . . ?
 O004 C008 C00B C00A -168.9(6) . . . . ?
 O004 C008 C00B C00L 9.8(10) . . . . ?
 N005 C00C C00F C00A -179.4(8) . . . . ?
 N005 C00C C00J C00L 177.9(9) . . . . ?
 C007 C009 C00D C00E -179.9(6) . . . . ?
 C007 C009 C00I C00K 179.0(7) . . . . ?
 C008 C00B C00L C00J 177.4(8) . . . . ?
 C009 C00D C00E C00H 0.7(10) . . . . ?
 C009 C00I C00K C00H 1.1(12) . . . . ?
 C00A C00B C00L C00J -4.0(12) . . . . ?
 C00B C00A C00F C00C -0.2(11) . . . . ?
 C00C N005 C00C C00F 133.4(8) 9 . . . ?
 C00C N005 C00C C00F -28.9(16) 5 . . . ?
 C00C N005 C00C C00J -45.7(17) 9 . . . ?
 C00C N005 C00C C00J 152.0(9) 5 . . . ?
 C00C C00J C00L C00B 3.4(14) . . . . ?
 C00D C009 C00I C00K -0.2(10) . . . . ?
 C00D C00E C00H N00G -177.6(7) . . . . ?
 C00D C00E C00H C00K 0.3(11) . . . . ?
 C00E C00H C00K C00I -1.2(12) . . . . ?
 C00F C00A C00B C008 -179.0(6) . . . . ?
 C00F C00A C00B C00L 2.3(10) . . . . ?
 C00F C00C C00J C00L -1.2(13) . . . . ?
 N00G C00H C00K C00I 176.7(8) . . . . ?
 C00H N00G C00H C00E -33.3(16) 11_656 . . . ?
 C00H N00G C00H C00E 133.9(8) 8_645 . . . ?
 C00H N00G C00H C00K 148.8(8) 11_656 . . . ?
 C00H N00G C00H C00K -44.0(16) 8_645 . . . ?
 C00I C009 C00D C00E -0.7(9) . . . . ?
 C00J C00C C00F C00A -0.4(12) . . . . ?

_olex2_submission_special_instructions  'No special instructions were received'
