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_7716855
_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
'C32 H34 In N6 O7, 2(F3 P0.5), 2(C H4 O), 0.25[C4H10O], 0.5[CH4O]'
_chemical_formula_sum            'C34 H42 F6 In N6 O9 P'
_chemical_formula_weight         938.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.11.27 svn.r5f609507 for Rigaku Oxford Diffraction, GUI svn.r6214)
;
_audit_update_record
;
2024-07-25 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.5693(2)
_cell_length_b                   10.51590(10)
_cell_length_c                   16.23520(10)
_cell_measurement_reflns_used    34077
_cell_measurement_temperature    100.3(8)
_cell_measurement_theta_max      77.6810
_cell_measurement_theta_min      3.8170
_cell_volume                     3936.37(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.3(8)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_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   -116.00 -37.00   0.50    0.33    --  -48.30 -27.00-154.00  158
  2  \w    -23.00  20.00   0.50    0.33    --  -48.30  27.00   8.00   86
  3  \w    -21.00   4.00   0.50    0.33    --   48.30 -27.00-154.00   50
  4  \w     56.00  81.00   0.50    0.33    --   48.30  27.00   8.00   50
  5  \w   -141.00-115.00   0.50    1.32    --  -86.25 -27.00-154.00   52
  6  \w    105.00 135.00   0.50    1.32    --  107.75  27.00   8.00   60
  7  \w   -119.00 -74.00   0.50    0.33    --  -48.30-125.00 -90.00   90
  8  \w   -116.00 -74.00   0.50    0.33    --  -48.30-125.00-180.00   84
  9  \w    -10.00  16.00   0.50    0.33    --   48.30 -19.00   0.00   52
 10  \w    -22.00  26.00   0.50    0.33    --   48.30 -19.00  60.00   96
 11  \w    -49.00 -14.00   0.50    1.32    --  -86.25  45.00-180.00   70
 12  \w     36.00  69.00   0.50    1.32    --  107.75 -78.00 -51.72   66
 13  \w     36.00  61.00   0.50    1.32    --  107.75 -61.00 -60.00   50
 14  \w     36.00  71.00   0.50    1.32    --  107.75 -61.00   0.00   70
 15  \w     56.00  94.00   0.50    1.32    --  107.75 -77.00 120.00   76
 16  \w     97.00 136.00   0.50    1.32    --  107.75  15.00 -90.00   78
 17  \w     36.00  73.00   0.50    1.32    --  107.75 -73.00 -83.38   74
 18  \w    141.00 173.00   0.50    1.32    --  107.75  45.00  30.00   64
 19  \w    126.00 177.00   0.50    1.32    --  107.75  45.00 150.00  102
 20  \w     86.00 111.00   0.50    1.32    --  107.75 -78.00 -51.72   50
 21  \w     39.00  70.00   0.50    1.32    --  107.75 -61.00 120.00   62
 22  \w     66.00 103.00   0.50    1.32    --  107.75-125.00 -90.00   74
 23  \w     59.00 102.00   0.50    1.32    --  107.75 -77.00   0.00   86
 24  \w     37.00  70.00   0.50    1.32    --  107.75 -61.00 -30.00   66
 25  \w    117.00 143.00   0.50    1.32    --  107.75  62.00 156.27   52
 26  \w    139.00 165.00   0.50    1.32    --  107.75  15.00 -90.00   52
 27  \w     38.00  63.00   0.50    1.32    --  107.75-104.00  -7.42   50
 28  \w     81.00 107.00   0.50    1.32    --  107.75-104.00  -7.42   52
 29  \w     39.00  85.00   0.50    1.32    --  107.75-125.00  60.00   92
 30  \w    101.00 134.00   0.50    1.32    --  107.75  30.00-120.00   66
 31  \w    149.00 176.00   0.50    1.32    --  107.75  30.00-120.00   54
 32  \w     77.00 102.00   0.50    1.32    --  107.75 -77.00  60.00   50
 33  \w    146.00 171.00   0.50    1.32    --  107.75  15.00 150.00   50
 34  \w    111.00 157.00   0.50    1.32    --  107.75  61.00 120.00   92
 35  \w     98.00 144.00   0.50    1.32    --  107.75  15.00 150.00   92
 36  \w    122.00 167.00   0.50    1.32    --  107.75  45.00 -60.00   90
 37  \w     36.00  63.00   0.50    1.32    --  107.75 -77.00  60.00   54
 38  \w     59.00  97.00   0.50    1.32    --  107.75 -97.00-113.92   76
 39  \w     86.00 127.00   0.50    1.32    --  107.75-146.00 111.20   82
 40  \w     43.00  72.00   0.50    1.32    --  107.75 -94.00  90.00   58
 41  \w     36.00  61.00   0.50    1.32    --  107.75-109.00 174.15   50
 42  \w     76.00 103.00   0.50    1.32    --  107.75-109.00 174.15   54
 43  \w     37.00  70.00   0.50    1.32    --  107.75 -61.00 -90.00   66
 44  \w     38.00  63.00   0.50    1.32    --  107.75-125.00 -60.00   50
 45  \w     40.00  67.00   0.50    1.32    --  107.75 -61.00-120.00   54
 46  \w     99.00 177.00   0.50    1.32    --  107.75  77.00-180.00  156
 47  \w     38.00  64.00   0.50    1.32    --  107.75 -68.00-140.91   52
 48  \w     61.00  86.00   0.50    1.32    --  107.75 -77.00  90.00   50
 49  \w     57.00  99.00   0.50    1.32    --  107.75 -90.00  60.20   84
 50  \w    132.00 157.00   0.50    1.32    --  107.75  45.00-180.00   50
 51  \w    126.00 152.00   0.50    1.32    --  107.75  45.00 -30.00   52
 52  \w     89.00 131.00   0.50    1.32    --  107.75  77.00  90.00   84
 53  \w     86.00 111.00   0.50    1.32    --  107.75  77.00 111.80   50
 54  \w     52.00  78.00   0.50    1.32    --  107.75 -79.00  90.16   52
 55  \w     81.00 107.00   0.50    1.32    --  107.75 -79.00  90.16   52
 56  \w     37.00  71.00   0.50    1.32    --  107.75 -61.00  90.00   68
;
_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      0.0664841000
_diffrn_orient_matrix_UB_12      -0.0148837000
_diffrn_orient_matrix_UB_13      0.0215096000
_diffrn_orient_matrix_UB_21      0.0032865000
_diffrn_orient_matrix_UB_22      0.0494807000
_diffrn_orient_matrix_UB_23      -0.0882036000
_diffrn_orient_matrix_UB_31      0.0059950000
_diffrn_orient_matrix_UB_32      0.1370609000
_diffrn_orient_matrix_UB_33      0.0341230000
_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  0.0442
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53708
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.047
_diffrn_reflns_theta_min         3.834
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.968
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021)
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    1.584
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.263
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.855
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         8361
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0380P)^2^+3.7356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0793
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7888
_reflns_number_total             8361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02146k3.cif
_cod_data_source_block           rah28_abs
_cod_depositor_comments
'Adding full bibliography for 7716855--7716856.cif.'
_cod_database_code               7716855
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C34H43F6InN6O9P
_chemical_oxdiff_usercomment     'Crystallized from methanol/ether.'
_shelx_estimated_absorpt_t_max   0.701
_shelx_estimated_absorpt_t_min   0.303
_reflns_odcompleteness_completeness 97.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     78.89
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O7-H7B = O7-H7A = O2S-H2S = O1S-H1S
 0.84 with sigma of 0.02
 H1S-C1S
 1.8 with sigma of 0.04
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7C,H7D), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C16(H16A,
 H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C26(H26A,H26B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C21(H21), C22(H22),
 C23(H23), C28(H28), C29(H29), C30(H30)
3.c Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              68176
_shelx_fab_checksum              81273
_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 1.502
_oxdiff_exptl_absorpt_empirical_full_min 0.701