An Isoindoline Bridged [M(η6-arene)2]+ (M = Re, 99mTc) ansa-Arenophane and its Dinuclear Macrocycles with Axial Chirality
Alberto, Roger; Csucker, Joshua; Jo, Da Kyung; Nadeem, Qaisar; Blacque, Olivier; Fox, Thomas; Braband, Henrik; Dalton Transactions  (2022) –; doi:10.1039/D2DT00743F

data_7710395
_publ_section_title
;
 An Isoindoline Bridged [M(\h6-arene)2]+ (M = Re, 99mTc) ansa-Arenophane
 and its Dinuclear Macrocycles with Axial Chirality
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00743F
_journal_year                    2022
_chemical_formula_moiety         'C40 H32 N4 Re2, 2(C2 F3 O2), H2 O'
_chemical_formula_sum            'C44 H34 F6 N4 O5 Re2'
_chemical_formula_weight         1185.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.278(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3233(1)
_cell_length_b                   16.7762(1)
_cell_length_c                   15.1091(1)
_cell_measurement_reflns_used    32336
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      78.9
_cell_measurement_theta_min      3.0
_cell_volume                     3809.05(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -125.00 -38.00   0.50    0.46    --  -51.79 -53.00   0.00  174
  2  \w    -66.00  22.00   0.50    0.46    --  -51.79  53.00 144.00  176
  3  \w    -22.00  66.00   0.50    0.46    --   51.79 -53.00   0.00  176
  4  \w     38.00 126.00   0.50    0.46    --   51.79  53.00 144.00  176
  5  \w   -100.00 -12.00   0.50    1.59    --  -86.25  53.00 144.00  176
  6  \w   -160.00 -72.00   0.50    1.59    --  -86.25 -53.00   0.00  176
  7  \w     94.00 178.00   0.50    1.59    --  107.75  53.00 144.00  168
  8  \w     34.00 122.00   0.50    1.59    --  107.75 -53.00   0.00  176
  9  \w   -124.00 -37.00   0.50    0.46    --  -51.79 -57.00-150.00  174
 10  \w   -125.00 -29.00   0.50    0.46    --  -51.79 -77.00 -90.00  192
 11  \w   -126.00 -73.00   0.50    0.46    --  -51.79-125.00  90.00  106
 12  \w   -126.00 -73.00   0.50    0.46    --  -51.79-125.00 150.00  106
 13  \w   -128.00 -40.00   0.50    0.46    --  -51.79 -37.00 -60.00  176
 14  \w     80.00 106.00   0.50    0.46    --   51.79  57.00 -60.00   52
 15  \w   -104.00 -74.00   0.50    1.59    --  -86.25 -45.00 -90.00   60
 16  \w   -156.00 -68.00   0.50    1.59    --  -86.25 -67.00-122.57  176
 17  \w    -95.00 -70.00   0.50    1.59    --  -86.25 -62.00-102.42   50
 18  \w   -120.00 -83.00   0.50    1.59    --  -86.25 -94.00 120.00   74
 19  \w     92.00 145.00   0.50    1.59    --  107.75  61.00 -90.00  106
 20  \w     35.00 109.00   0.50    1.59    --  107.75 -15.00 120.00  148
 21  \w     86.00 111.00   0.50    1.59    --  107.75  77.00-150.00   50
 22  \w     35.00  68.00   0.50    1.59    --  107.75 -45.00 -30.00   66
 23  \w     86.00 175.00   0.50    1.59    --  107.75  77.00 -90.00  178
 24  \w     76.00 106.00   0.50    1.59    --  107.75 -94.00 120.00   60
 25  \w     39.00  76.00   0.50    1.59    --  107.75 -45.00 150.00   74
 26  \w    101.00 177.00   0.50    1.59    --  107.75  45.00-150.00  152
 27  \w     95.00 178.00   0.50    1.59    --  107.75  45.00  90.00  166
 28  \w     34.00  60.00   0.50    1.59    --  107.75 -94.00 120.00   52
 29  \w     32.00 104.00   0.50    1.59    --  107.75 -94.00-150.00  144
 30  \w    107.00 177.00   0.50    1.59    --  107.75  61.00-180.00  140
 31  \w    132.00 174.00   0.50    1.59    --  107.75  15.00 -60.00   84
 32  \w     70.00  96.00   0.50    1.59    --  107.75 -45.00 -30.00   52
 33  \w     90.00 178.00   0.50    1.59    --  107.75  77.00-120.00  176
 34  \w     32.00  69.00   0.50    1.59    --  107.75 -30.00 150.00   74
 35  \w     73.00 106.00   0.50    1.59    --  107.75 -30.00 150.00   66
 36  \w    149.00 176.00   0.50    1.59    --  107.75  61.00 -60.00   54
 37  \w    153.00 178.00   0.50    1.59    --  107.75  61.00  30.00   50
 38  \w     94.00 123.00   0.50    1.59    --  107.75  61.00 -60.00   58
 39  \w     92.00 145.00   0.50    1.59    --  107.75  61.00  30.00  106
 40  \w     95.00 177.00   0.50    1.59    --  107.75  45.00  60.00  164
 41  \w     96.00 145.00   0.50    1.59    --  107.75  45.00-120.00   98
 42  \w     92.00 135.00   0.50    1.59    --  107.75  61.00 150.00   86
 43  \w    144.00 169.00   0.50    1.59    --  107.75  61.00 150.00   50
 44  \w     32.00 111.00   0.50    1.59    --  107.75 -45.00  30.00  158
 45  \w    139.00 165.00   0.50    1.59    --  107.75  30.00 120.00   52
 46  \w     92.00 119.00   0.50    1.59    --  107.75  66.00-122.66   54
 47  \w    128.00 176.00   0.50    1.59    --  107.75  77.00-150.00   96
 48  \w     44.00  96.00   0.50    1.59    --  107.75 -94.00-120.00  104
 49  \w     97.00 124.00   0.50    1.59    --  107.75  15.00   0.00   54
 50  \w    147.00 177.00   0.50    1.59    --  107.75  15.00  60.00   60
 51  \w    132.00 177.00   0.50    1.59    --  107.75 111.00  60.00   90
 52  \w    104.00 130.00   0.50    1.59    --  107.75 111.00  60.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0163621000
_diffrn_orient_matrix_UB_12      -0.0176860000
_diffrn_orient_matrix_UB_13      0.1020030000
_diffrn_orient_matrix_UB_21      0.0768027000
_diffrn_orient_matrix_UB_22      -0.0565684000
_diffrn_orient_matrix_UB_23      -0.0098195000
_diffrn_orient_matrix_UB_31      0.0659412000
_diffrn_orient_matrix_UB_32      0.0700850000
_diffrn_orient_matrix_UB_33      0.0176619000
_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  0.0233
_diffrn_reflns_av_unetI/netI     0.0090
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            39299
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.495
_diffrn_reflns_theta_min         3.949
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.977
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.252
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
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_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.067
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.892
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.107
_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     348
_refine_ls_number_reflns         3889
_refine_ls_number_restraints     474
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0355
_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/[\s^2^(Fo^2^)+(0.0429P)^2^+28.6503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3868
_reflns_number_total             3889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00743f2.cif
_cod_data_source_block           '[6a][TFA]2H2O'
_cod_database_code               7710395
_shelx_estimated_absorpt_t_max   0.423
_shelx_estimated_absorpt_t_min   0.264
_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 O(H,H) groups
2. Restrained distances
 C22B-O1B
 2.3 with sigma of 0.01
 C22B-O2B
 2.3 with sigma of 0.01
 C22A-C21A \\sim C21B-C22B
 with sigma of 0.005
 F1B-C22B \\sim F2B-C22B \\sim F3B-C22B \\sim F1A-C22A \\sim F3A-C22A \\sim
F2A-C22A
 with sigma of 0.005
 O1A-C21A \\sim O2A-C21A \\sim O1B-C21B \\sim O2B-C21B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
F1A \\sim F2A \\sim F3A \\sim O1A \\sim O2A \\sim C21A \\sim C22A \\sim F1B
\\sim F2B \\sim F3B \\sim O1B \\sim O2B \\sim C21B \\sim C22B: within 3A with
sigma of 0.05 and sigma for terminal atoms of 0.01 within 3A
4. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=Sof(C21B)=Sof(C22B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(C21A)=Sof(C22A)=FVAR(1)
 Fixed Sof: O1(0.5) H1A(0.5) H1B(0.5)
5.a Free rotating group:
 O1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11), C12(H12),
 C16(H16), C17(H17), C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              15619