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_7710396
_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), 2(H2 O)'
_chemical_formula_sum            'C44 H36 F6 N4 O6 Re2'
_chemical_formula_weight         1203.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.432(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9702(2)
_cell_length_b                   11.4817(1)
_cell_length_c                   16.7301(1)
_cell_measurement_reflns_used    29602
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      79.0020
_cell_measurement_theta_min      2.6730
_cell_volume                     3948.25(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5'
_computing_structure_refinement  'SHELXL 2018/3 (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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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   -108.00 -28.00   0.50    1.41    --  -52.02 156.00 178.00  160
  2  \w   -128.00 -76.00   0.50    1.41    --  -52.02-119.00 -62.00  104
  3  \w    -84.00  -8.00   0.50    1.41    --  -52.02 119.00  22.00  152
  4  \w   -126.00 -51.00   0.50    1.41    --  -52.02-156.00 142.00  150
  5  \w     60.00  85.00   0.50    1.41    --   52.02-156.00 142.00   50
  6  \w     39.00  64.00   0.50    1.41    --   52.02-119.00 -62.00   50
  7  \w   -107.00 -31.00   0.50    3.00    --  -86.25 156.00 178.00  152
  8  \w     74.00 128.00   0.50    3.00    --  107.75 156.00 178.00  108
  9  \w     58.00  98.00   0.50    3.00    --  107.75-119.00 -62.00   80
 10  \w     92.00 117.00   0.50    3.00    --  107.75-156.00 142.00   50
 11  \w   -124.00 -75.00   0.50    1.41    --  -52.02-125.00 120.00   98
 12  \w    -98.00 -72.00   0.50    1.41    --  -52.02 -54.00-177.59   52
 13  \w   -125.00 -30.00   0.50    1.41    --  -52.02 -77.00-120.00  190
 14  \w   -126.00 -74.00   0.50    1.41    --  -52.02-125.00  60.00  104
 15  \w     32.00  99.00   0.50    3.00    --  107.75 -94.00 -30.00  134
 16  \w     41.00 106.00   0.50    3.00    --  107.75 -94.00  60.00  130
 17  \w     59.00 117.00   0.50    3.00    --  107.75 -45.00 -90.00  116
 18  \w     32.00 102.00   0.50    3.00    --  107.75-111.00 -60.00  140
 19  \w     93.00 177.00   0.50    3.00    --  107.75  61.00  90.00  168
 20  \w     43.00  77.00   0.50    3.00    --  107.75-111.00  30.00   68
 21  \w     82.00 109.00   0.50    3.00    --  107.75-111.00  30.00   54
 22  \w    142.00 178.00   0.50    3.00    --  107.75  45.00 -60.00   72
 23  \w     47.00 109.00   0.50    3.00    --  107.75-111.00 -30.00  124
 24  \w     35.00  93.00   0.50    3.00    --  107.75 -94.00-180.00  116
 25  \w     95.00 121.00   0.50    3.00    --  107.75  45.00 -60.00   52
 26  \w     40.00  67.00   0.50    3.00    --  107.75-111.00-180.00   54
 27  \w     43.00 106.00   0.50    3.00    --  107.75 -15.00  30.00  126
 28  \w     40.00 102.50   0.50    3.00    --  107.75 -94.00  30.00  125
;
_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      0.0198822000
_diffrn_orient_matrix_UB_12      -0.1253115000
_diffrn_orient_matrix_UB_13      -0.0176132000
_diffrn_orient_matrix_UB_21      0.0308533000
_diffrn_orient_matrix_UB_22      0.0452937000
_diffrn_orient_matrix_UB_23      -0.0703052000
_diffrn_orient_matrix_UB_31      0.0654277000
_diffrn_orient_matrix_UB_32      0.0164657000
_diffrn_orient_matrix_UB_33      0.0594452000
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41009
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.472
_diffrn_reflns_theta_min         4.302
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.551
_exptl_absorpt_correction_T_max  0.782
_exptl_absorpt_correction_T_min  0.502
_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    2.024
_exptl_crystal_description       plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.443
_refine_diff_density_min         -1.274
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         8059
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+9.2198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0597
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7555
_reflns_number_total             8059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00743f2.cif
_cod_data_source_block           '[6b][TFA]2(H2O)2'
_cod_database_code               7710396
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.398
_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
 C43-C44A = C44B-C43
 1.54 with sigma of 0.01
 F6B-F5B = F4B-F5B = F6B-F4B
 2.13 with sigma of 0.01
 F6A-F5A = F5A-F4A = F4A-F6A
 2.13 with sigma of 0.01
 O3A-C44A \\sim O3B-C44B \\sim O4A-C44A \\sim O4B-C44B
 with sigma of 0.005
 C43-C44A \\sim C44B-C43
 with sigma of 0.005
 F5B-C43 \\sim F5A-C43 \\sim F6B-C43 \\sim F6A-C43 \\sim F4B-C43 \\sim F4A-C43
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C43 \\sim F4A \\sim F5A \\sim F6A \\sim O3A \\sim O4A \\sim C44A \\sim F4B
\\sim F5B \\sim F6B \\sim O3B \\sim O4B \\sim C44B: within 3A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3A
O1 \\sim O2 \\sim C42: within 3A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 3A
4. Others
 Sof(F4B)=Sof(F5B)=Sof(F6B)=Sof(O3B)=Sof(O4B)=Sof(C44B)=1-FVAR(1)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O3A)=Sof(O4A)=Sof(C44A)=FVAR(1)
5.a Free rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
5.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C40(H40A,H40B)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C35(H35), C36(H36), C37(H37), C38(H38)
;
_shelx_res_checksum              74499