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_7710393
_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         'C28 H18 N2 O4 Re, F6 P'
_chemical_formula_sum            'C28 H18 F6 N2 O4 P Re'
_chemical_formula_weight         777.61
_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             2020-11-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                102.971(4)
_cell_angle_beta                 102.419(4)
_cell_angle_gamma                92.903(4)
_cell_formula_units_Z            2
_cell_length_a                   7.1963(3)
_cell_length_b                   12.2113(5)
_cell_length_c                   14.9263(6)
_cell_measurement_reflns_used    9027
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.4730
_cell_measurement_theta_min      3.0910
_cell_volume                     1241.53(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_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     27.00  95.80   0.80    3.50    --   43.61-125.00 -60.00   86
  2  \w     13.00  41.00   0.80    3.50    --   43.61  79.00-123.41   35
  3  \w      6.00  82.00   0.80    3.50    --   43.61 -99.00 -60.00   95
  4  \w      6.00  82.00   0.80    3.50    --   43.61 -99.00 -30.00   95
  5  \w      6.00  82.00   0.80    3.50    --   43.61 -99.00 120.00   95
  6  \w    -33.00  76.60   0.80    3.50    --   43.61 -19.00   0.00  137
  7  \w     23.00 115.00   0.80    3.50    --   43.61  37.00   0.00  115
  8  \w     38.00 131.60   0.80   12.00    --  111.00 -30.00   0.00  117
  9  \w    104.00 177.60   0.80   12.00    --  111.00 111.00-180.00   92
 10  \w    103.00 177.40   0.80   12.00    --  111.00  77.00 -60.00   93
 11  \w     41.00 133.00   0.80   12.00    --  111.00 -45.00-120.00  115
 12  \w    103.00 177.40   0.80   12.00    --  111.00  77.00-180.00   93
 13  \w     38.00 108.40   0.80   12.00    --  111.00-111.00 120.00   88
 14  \w     38.00 108.40   0.80   12.00    --  111.00-111.00   0.00   88
 15  \w    104.00 177.60   0.80   12.00    --  111.00 111.00  60.00   92
 16  \w     38.00 108.40   0.80   12.00    --  111.00-111.00-180.00   88
 17  \w     40.00 140.00   0.80   12.00    --  111.00 -77.00-150.00  125
 18  \w     38.00 108.40   0.80   12.00    --  111.00-111.00  60.00   88
 19  \w     43.00 136.60   0.80   12.00    --  111.00 -61.00  60.00  117
 20  \w     89.00 177.00   0.80   12.00    --  111.00  45.00   0.00  110
 21  \w     31.00 107.00   0.80   12.00    --  111.00 -94.00 -90.00   95
 22  \w     90.00 178.00   0.80   12.00    --  111.00  30.00 -30.00  110
 23  \w     31.00 107.00   0.80   12.00    --  111.00 -94.00-150.00   95
 24  \w     31.00 107.00   0.80   12.00    --  111.00 -94.00  30.00   95
 25  \w     38.00 108.40   0.80   12.00    --  111.00-111.00  90.00   88
 26  \w    104.00 177.60   0.80   12.00    --  111.00 111.00 -90.00   92
 27  \w     38.00 131.60   0.80   12.00    --  111.00 -30.00 150.00  117
 28  \w     14.00 114.00   0.80    3.50    --   43.61  74.00   8.44  125
 29  \w     18.00 111.60   0.80    3.50    --   43.61  57.00-180.00  117
 30  \w     18.00 111.60   0.80    3.50    --   43.61  57.00  90.00  117
 31  \w     18.00 111.60   0.80    3.50    --   43.61  57.00 -90.00  117
 32  \w     13.00  41.00   0.80    3.50    --   43.61  79.00 -70.44   35
 33  \w     13.00  41.00   0.80    3.50    --   43.61  78.00 175.90   35
 34  \w     90.00 178.00   0.80   12.00    --  111.00  30.00 150.00  110
 35  \w     85.00 169.00   0.80   12.00    --  111.00  61.00  90.00  105
 36  \w     85.00 177.00   0.80   12.00    --  111.00  61.00 -90.00  115
 37  \w     82.00 178.00   0.80   12.00    --  111.00  71.00 168.85  120
 38  \w     85.00 177.00   0.80   12.00    --  111.00  61.00-115.19  115
 39  \w     71.00 177.40   0.80   12.00    --  111.00  15.00  90.00  133
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1154303000
_diffrn_orient_matrix_UB_12      0.0563559000
_diffrn_orient_matrix_UB_13      0.1009795000
_diffrn_orient_matrix_UB_21      0.1859049000
_diffrn_orient_matrix_UB_22      -0.0023543000
_diffrn_orient_matrix_UB_23      -0.0355005000
_diffrn_orient_matrix_UB_31      -0.0263035000
_diffrn_orient_matrix_UB_32      0.1173119000
_diffrn_orient_matrix_UB_33      -0.0200646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9155
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.319
_diffrn_reflns_theta_min         3.124
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.980
_exptl_absorpt_correction_T_max  0.806
_exptl_absorpt_correction_T_min  0.481
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    2.080
_exptl_crystal_description       plate
_exptl_crystal_F_000             752
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.500
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         9155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0608P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7820
_reflns_number_total             9155
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9916\% 
around [-0.00 1.00 0.00] (reciprocal) or [0.17 0.97 0.20] (direct)
;
_cod_data_source_file            d2dt00743f2.cif
_cod_data_source_block           '[3][PF6]'
_cod_database_code               7710393
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.474
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8240(5)
 0.1760(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13),
 C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C25(H25), C26(H26),
  C27(H27), C28(H28)
;
_shelx_res_checksum              28366
_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 1.715
_oxdiff_exptl_absorpt_empirical_full_min 0.611
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2