Chelation of [<sup>111</sup>In]In<sup>3+</sup> with the dual-size-selective macrocycles py-macrodipa and py<sub>2</sub>-macrodipa.
Lee, Kevin K.; Chakraborty, Mou; Hu, Aohan; Kanagasundaram, Thines; Thorek, Daniel L. J.; Wilson, Justin J.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14634–14647; doi:10.1039/d4dt02146k

data_7716856
_publ_section_title
;
 Chelation of [<sup>111</sup>In]In<sup>3+</sup> with the
 dual-size-selective macrocycles py-macrodipa and
 py<sub>2</sub>-macrodipa.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14634
_journal_page_last               14647
_journal_paper_doi               10.1039/d4dt02146k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C29 H33 In N5 O7, F6 P, C3 H7 N O'
_chemical_formula_sum            'C32 H40 F6 In N6 O8 P'
_chemical_formula_weight         896.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-27
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2024-07-25 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                65.421(2)
_cell_angle_beta                 85.7740(10)
_cell_angle_gamma                74.083(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2106(2)
_cell_length_b                   14.4787(3)
_cell_length_c                   14.7558(2)
_cell_measurement_reflns_used    22778
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      76.5200
_cell_measurement_theta_min      3.2790
_cell_volume                     1719.05(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.81a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(4)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -23.00  17.00   0.50    0.31    --  -50.09  59.00 -82.00   80
  2  \w    -26.00  21.00   0.50    0.31    --  -50.09  19.00 -90.00   94
  3  \w    -19.00  21.00   0.50    0.31    --  -50.09  19.00-150.00   80
  4  \w    -52.00 -25.00   0.50    1.23    --  -82.50  59.00 -82.00   54
  5  \w   -121.00 -38.00   0.50    0.31    --  -50.09 -59.00 136.00  166
  6  \w     55.00 119.00   0.50    0.31    --   50.09  59.00 -82.00  128
  7  \w    142.00 167.00   0.50    1.23    --  104.00  59.00 -82.00   50
  8  \w    146.00 174.00   0.50    1.23    --  104.00  15.00-120.00   56
  9  \w    150.00 176.00   0.50    1.23    --  104.00  61.00-180.00   52
 10  \w    125.00 151.00   0.50    1.23    --  104.00 125.00 -90.00   52
 11  \w    134.00 165.00   0.50    1.23    --  104.00 125.00 -30.00   62
 12  \w    121.00 147.00   0.50    1.23    --  104.00  77.00 -60.00   52
 13  \w    138.00 164.00   0.50    1.23    --  104.00  30.00 -60.00   52
 14  \w    108.00 175.00   0.50    1.23    --  104.00  80.00-160.28  134
 15  \w    116.00 142.00   0.50    1.23    --  104.00  61.00-180.00   52
 16  \w    102.00 140.00   0.50    1.23    --  104.00  15.00-120.00   76
 17  \w    100.00 140.00   0.50    1.23    --  104.00  15.00 -30.00   80
 18  \w    120.00 150.00   0.50    1.23    --  104.00  77.00  30.00   60
 19  \w    132.00 176.00   0.50    1.23    --  104.00  77.00  90.00   88
 20  \w    139.00 165.00   0.50    1.23    --  104.00  30.00  90.00   52
 21  \w    108.00 173.00   0.50    1.23    --  104.00  61.00 150.00  130
 22  \w    120.00 146.00   0.50    1.23    --  104.00  15.00 120.00   52
 23  \w    103.00 129.00   0.50    1.23    --  104.00  15.00 150.00   52
 24  \w    100.00 155.00   0.50    1.23    --  104.00  30.00 150.00  110
 25  \w     91.00 120.00   0.50    1.23    --  104.00 -84.00  65.44   58
 26  \w     81.00 106.00   0.50    1.23    --  104.00 -94.00 150.00   50
 27  \w     76.00 111.00   0.50    1.23    --  104.00-125.00 120.00   70
 28  \w     85.00 111.00   0.50    1.23    --  104.00-125.00 150.00   52
 29  \w     74.00 126.00   0.50    1.23    --  104.00-144.00 172.72  104
 30  \w     74.00  99.00   0.50    1.23    --  104.00 -77.00 150.00   50
 31  \w     52.00  78.00   0.50    1.23    --  104.00 -94.00  60.00   52
 32  \w     66.00 107.00   0.50    1.23    --  104.00-102.00  42.63   82
 33  \w     79.00 112.00   0.50    1.23    --  104.00-125.00  30.00   66
 34  \w     77.00 107.00   0.50    1.23    --  104.00-125.00  60.00   60
 35  \w     52.00  91.00   0.50    1.23    --  104.00-125.00 -30.00   78
 36  \w     81.00 110.00   0.50    1.23    --  104.00-125.00 -90.00   58
 37  \w     81.00 107.00   0.50    1.23    --  104.00-106.00-151.44   52
 38  \w     78.00 104.00   0.50    1.23    --  104.00 -94.00-150.00   52
 39  \w     73.00  98.00   0.50    1.23    --  104.00-125.00-150.00   50
 40  \w     70.00 100.00   0.50    1.23    --  104.00 -94.00-180.00   60
 41  \w     60.00  87.00   0.50    1.23    --  104.00 -77.00-150.00   54
 42  \w     55.00 110.00   0.50    1.23    --  104.00-125.00-180.00  110
 43  \w     79.00 124.00   0.50    1.23    --  104.00 -79.00 -65.37   90
 44  \w     63.00 106.00   0.50    1.23    --  104.00 -94.00 -60.00   86
 45  \w     60.00 108.00   0.50    1.23    --  104.00-109.00 -56.82   96
 46  \w     39.00  76.00   0.50    1.23    --  104.00-125.00 -60.00   74
 47  \w     32.00  66.00   0.50    1.23    --  104.00 -94.00   0.00   68
 48  \w     37.00  62.00   0.50    1.23    --  104.00-125.00  30.00   50
 49  \w     37.00  91.00   0.50    1.23    --  104.00 -81.00  32.84  108
 50  \w     36.00  80.00   0.50    0.31    --   50.09-125.00   0.00   88
 51  \w     32.00  71.00   0.50    1.23    --  104.00 -61.00 -30.00   78
 52  \w     42.00  67.00   0.50    1.23    --  104.00 -61.00  30.00   50
 53  \w     34.00  60.00   0.50    1.23    --  104.00 -61.00   0.00   52
 54  \w     42.00  94.00   0.50    1.23    --  104.00 -91.00 -88.03  104
 55  \w     32.00  72.00   0.50    1.23    --  104.00 -94.00-150.00   80
 56  \w     32.00  67.00   0.50    1.23    --  104.00 -94.00 -90.00   70
 57  \w     33.00  78.00   0.50    1.23    --  104.00 -77.00-120.00   90
 58  \w     33.00  58.00   0.50    1.23    --  104.00 -77.00-180.00   50
 59  \w     64.00 102.00   0.50    1.23    --  104.00   0.00 -90.00   76
 60  \w     93.00 133.00   0.50    1.23    --  104.00  61.00 -90.00   80
 61  \w    107.00 136.00   0.50    1.23    --  104.00 117.00 -73.23   58
 62  \w     95.00 132.00   0.50    1.23    --  104.00 125.00   0.00   74
 63  \w     97.00 127.00   0.50    1.23    --  104.00 125.00 -30.00   60
 64  \w     98.00 176.00   0.50    1.23    --  104.00 125.00-150.00  156
 65  \w     32.00  66.00   0.50    1.23    --  104.00 -59.00 136.00   68
 66  \w     40.00  66.00   0.50    1.23    --  104.00 -94.00 150.00   52
 67  \w     38.00  72.00   0.50    1.23    --  104.00-125.00 120.00   68
 68  \w     45.00  70.00   0.50    1.23    --  104.00-125.00 150.00   50
 69  \w     42.00  68.00   0.50    1.23    --  104.00 -77.00 120.00   52
 70  \w     33.00  70.00   0.50    1.23    --  104.00 -61.00  90.00   74
 71  \w     34.00  59.00   0.50    1.23    --  104.00 -61.00 150.00   50
 72  \w    -19.00  59.00   0.50    0.31    --   50.09 -59.00 136.00  156
 73  \w    -18.00  25.00   0.50    0.31    --   50.09 -19.00  30.00   86
 74  \w     33.00  78.00   0.50    1.23    --  104.00 -65.00 -65.18   90
 75  \w   -101.00 -76.00   0.50    0.31    --  -50.09-125.00  60.00   50
 76  \w   -136.00-111.00   0.50    1.23    --  -82.50 -59.00 136.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1195771000
_diffrn_orient_matrix_UB_12      0.0060141000
_diffrn_orient_matrix_UB_13      -0.0714189000
_diffrn_orient_matrix_UB_21      -0.0524742000
_diffrn_orient_matrix_UB_22      0.1207302000
_diffrn_orient_matrix_UB_23      -0.0360001000
_diffrn_orient_matrix_UB_31      0.1151658000
_diffrn_orient_matrix_UB_32      0.0119290000
_diffrn_orient_matrix_UB_33      -0.0825352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37369
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.286
_diffrn_reflns_theta_min         3.297
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.776
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.411
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.81a (Rigaku Oxford Diffraction, 2020)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_description       block
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.929
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         7224
_refine_ls_number_restraints     298
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+1.8272P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6930
_reflns_number_total             7224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02146k3.cif
_cod_data_source_block           rah22_abs
_cod_depositor_comments
'Adding full bibliography for 7716855--7716856.cif.'
_cod_original_cell_volume        1719.05(6)
_cod_database_code               7716856
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C32H40F6InN6O8P
_chemical_oxdiff_usercomment     'Crystallized from DMF/ether.'
_reflns_odcompleteness_completeness 98.07
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.83
_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. Restrained distances
 F5A-F4A \\sim F5A-F6A \\sim F4A-F3A \\sim F3A-F6A \\sim F3B-F4B \\sim F3B-F6B
\\sim F4B-F5B \\sim F5B-F6B
 with sigma of 0.04
 P-F1 \\sim P-F2 \\sim P-F5A \\sim P-F4A \\sim P-F3A \\sim P-F6A \\sim P-F3B
\\sim P-F4B \\sim P-F5B \\sim P-F6B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P \\sim F1 \\sim F2 \\sim F3A \\sim F4A \\sim F5A \\sim F6A \\sim F3B \\sim F4B
\\sim F5B \\sim F6B: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
4. Rigid body (RIGU) restrains
 P, F1, F2, F5A, F4A, F3A, F6A, F3B, F4B, F5B, F6B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F3B)=Sof(F4B)=Sof(F5B)=Sof(F6B)=1-FVAR(1)
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,
 H11B), C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B),
 C16(H16A,H16B), C23(H23A,H23B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26),
 C27(H27), C1S(H1S)
6.c Idealised Me refined as rotating group:
 C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              18905
_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 1.242
_oxdiff_exptl_absorpt_empirical_full_min 0.840