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_7710394
_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         'C20 H16 N2 Re, F6 P, C2 H3 N'
_chemical_formula_sum            'C22 H19 F6 N3 P Re'
_chemical_formula_weight         656.57
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.1320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.61700(10)
_cell_length_b                   31.5018(3)
_cell_length_c                   8.58250(10)
_cell_measurement_reflns_used    18067
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      76.3780
_cell_measurement_theta_min      2.7790
_cell_volume                     2043.43(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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 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    -80.00  36.00   0.80    1.50    --  -42.61  19.00-180.00  145
  2  \w      6.00  82.00   0.80    1.50    --   42.61 -99.00 120.00   95
  3  \w     27.00  97.40   0.80    1.50    --   42.61-125.00-120.00   88
  4  \w    -30.00  64.40   0.80    1.50    --   42.61 -37.00 -90.00  118
  5  \w     40.00 134.40   0.80    6.00    --  111.00 -45.00  60.00  118
  6  \w     36.00 108.00   0.80    6.00    --  111.00-111.00  90.00   90
  7  \w    103.00 177.40   0.80    6.00    --  111.00  77.00  30.00   93
  8  \w     36.00 108.00   0.80    6.00    --  111.00-111.00 -90.00   90
  9  \w     36.00 108.00   0.80    6.00    --  111.00-111.00 -30.00   90
 10  \w     83.00 177.40   0.80    6.00    --  111.00  61.00-150.00  118
 11  \w     30.00 106.00   0.80    6.00    --  111.00 -94.00   0.00   95
 12  \w     87.00 177.40   0.80    6.00    --  111.00  45.00-180.00  113
 13  \w     36.00 108.00   0.80    6.00    --  111.00-111.00 150.00   90
 14  \w     30.00 106.00   0.80    6.00    --  111.00 -94.00 -30.00   95
 15  \w    104.00 177.60   0.80    6.00    --  111.00 111.00 150.00   92
 16  \w   -113.00 -17.00   0.80    1.50    --  -42.61 -57.00  30.00  120
 17  \w     16.00 112.00   0.80    1.50    --   42.61  57.00 -30.00  120
 18  \w     16.00 112.00   0.80    1.50    --   42.61  57.00-150.00  120
 19  \w     87.00 177.40   0.80    6.00    --  111.00  45.00 -90.00  113
 20  \w     66.00 178.00   0.80    6.00    --  111.00  15.00   0.00  140
 21  \w     87.00 132.60   0.80    6.00    --  111.00  45.00  60.00   57
 22  \w     87.00 177.40   0.80    6.00    --  111.00  30.00 120.00  113
;
_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      0.0640100000
_diffrn_orient_matrix_UB_12      -0.0462962000
_diffrn_orient_matrix_UB_13      -0.0056624000
_diffrn_orient_matrix_UB_21      0.1418073000
_diffrn_orient_matrix_UB_22      0.0136926000
_diffrn_orient_matrix_UB_23      -0.1030669000
_diffrn_orient_matrix_UB_31      0.1317234000
_diffrn_orient_matrix_UB_32      0.0077450000
_diffrn_orient_matrix_UB_33      0.1485764000
_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  0.0221
_diffrn_reflns_av_unetI/netI     0.0114
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            22813
_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         74.501
_diffrn_reflns_theta_min         2.805
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.032
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.129
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_description       plate
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.748
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0185
_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^)+(0.0172P)^2^+3.2769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4166
_reflns_number_total             4195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00743f2.cif
_cod_data_source_block           '[5][PF6]CH3CN'
_cod_database_code               7710394
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.111
_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.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B)
2.b 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)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              40321