Dinuclear indium and thallium diyls: biscarbenoids or metal cluster?
Desat, Marcella E.; Gärtner, Stefanie; Kretschmer, Robert; Chemical communications (Cambridge, England) 53 (2017) 1510–1513; doi:10.1039/c6cc09488k

data_7119243
_publ_section_title
;
 Dinuclear indium and thallium diyls: biscarbenoids or metal cluster?
;
_journal_issue                   9
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1510
_journal_page_last               1513
_journal_paper_doi               10.1039/c6cc09488k
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C36 H52 N4 Tl2'
_chemical_formula_sum            'C36 H52 N4 Tl2'
_chemical_formula_weight         949.55
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-09-15 deposited with the CCDC.
2016-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                66.579(3)
_cell_angle_beta                 78.590(3)
_cell_angle_gamma                80.819(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1313(3)
_cell_length_b                   12.0117(3)
_cell_length_c                   14.7648(4)
_cell_measurement_reflns_used    22705
_cell_measurement_temperature    123.3(6)
_cell_measurement_theta_max      74.1890
_cell_measurement_theta_min      3.9920
_cell_volume                     1768.49(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.3(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_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      6.00  33.00   1.00    1.25    --   40.00  88.00 -70.30   27
  2  \w   -114.00 -22.00   1.00    1.25    --  -45.65 -57.00 150.00   92
  3  \w    -99.00  -2.00   1.00    1.25    --  -45.65 125.00   0.00   97
  4  \w    -70.00  24.00   1.00    1.25    --  -45.65  57.00 -90.00   94
  5  \w     23.00 117.00   1.00    1.25    --   45.65  37.00-180.00   94
  6  \w     22.00 115.00   1.00    1.25    --   45.65  57.00 -60.00   93
  7  \w     23.00 117.00   1.00    1.25    --   45.65  37.00 -90.00   94
  8  \w     17.00  47.00   1.00    1.25    --   48.00  79.00 -28.62   30
  9  \w     21.00  47.00   1.00    1.25    --   52.00  79.00  10.96   26
 10  \w     21.00  47.00   1.00    1.25    --   52.00  79.00 102.51   26
 11  \w     20.00  46.00   1.00    1.25    --   52.00  81.00-151.00   26
 12  \w     21.00  47.00   1.00    1.25    --   52.00  79.00 159.94   26
 13  \w     30.00 131.00   1.00    1.25    --   60.00  76.00  44.57  101
 14  \w     34.00 135.00   1.00    1.25    --   64.00  76.00 164.10  101
 15  \w     34.00 135.00   1.00    1.25    --   64.00  76.00-115.21  101
 16  \w     39.00 139.00   1.00    1.25    --   68.00  74.00  -6.87  100
 17  \w     38.00 139.00   1.00    1.25    --   68.00  75.00  99.14  101
 18  \w     38.00 139.00   1.00    1.25    --   68.00  76.00 -56.07  101
 19  \w     38.00 140.00   1.00    1.25    --   68.00  77.00  44.03  102
 20  \w     42.00 143.00   1.00    1.25    --   72.00  76.00 -91.73  101
 21  \w     46.00 148.00   1.00    5.37    --   76.00  77.00-172.67  102
 22  \w     46.00 148.00   1.00    5.37    --   76.00  77.00 114.62  102
 23  \w     46.00 147.00   1.00    5.37    --   76.00  76.00  -6.24  101
 24  \w     51.00 142.00   1.00    5.37    --   80.00  73.00-134.33   91
 25  \w     53.00  88.00   1.00    5.37    --   80.00  71.00 -45.13   35
 26  \w     55.00  81.00   1.00    5.37    --   84.00  74.00  52.63   26
 27  \w     55.00  81.00   1.00    5.37    --   84.00  74.00 152.67   26
 28  \w     98.00 141.00   1.00    5.37    --   88.00  68.00 -73.70   43
 29  \w     64.00  89.00   1.00    5.37    --   88.00  68.00 -73.70   25
 30  \w     59.00  85.00   1.00    5.37    --   88.00  72.00  30.77   26
 31  \w     71.00 147.00   1.00    5.37    --   96.00  65.00 -52.28   76
 32  \w     97.00 148.00   1.00    5.37    --   96.00  75.00-172.46   51
 33  \w     66.00  93.00   1.00    5.37    --   96.00  75.00-172.46   27
 34  \w     36.00  85.00   1.00    5.37    --  104.50 -45.00  90.00   49
 35  \w     29.00 103.00   1.00    5.37    --  104.50 -94.00   0.00   74
 36  \w     55.00 109.00   1.00    5.37    --  104.50 -94.00  90.00   54
 37  \w     36.00 135.00   1.00    5.37    --  104.50 -77.00-150.00   99
 38  \w    123.00 168.00   1.00    5.37    --  104.50  73.00  48.11   45
 39  \w     75.00 166.00   1.00    5.37    --  104.50  77.00 150.00   91
 40  \w     75.00 102.00   1.00    5.37    --  104.50  73.00  48.11   27
 41  \w     74.00 168.00   1.00    5.37    --  104.50  77.00-120.00   94
 42  \w     80.00 172.00   1.00    5.37    --  104.50  61.00  30.00   92
 43  \w    115.00 144.00   1.00    5.37    --  104.50  77.00-150.00   29
 44  \w     75.00 112.00   1.00    5.37    --  104.50  77.00-150.00   37
 45  \w     80.00 166.00   1.00    5.37    --  104.50  61.00 120.00   86
 46  \w    111.00 137.00   1.00    5.37    --  104.50  77.00 -90.00   26
 47  \w     76.00 104.00   1.00    5.37    --  104.50  77.00 -90.00   28
 48  \w     74.00 154.00   1.00    5.37    --  104.50  77.00 -30.00   80
 49  \w     74.00 114.00   1.00    5.37    --  104.50  77.00  90.00   40
 50  \w    121.00 147.00   1.00    5.37    --  104.50  77.00  90.00   26
 51  \w     69.00 121.00   1.00    5.37    --  104.50-125.00-120.00   52
 52  \w     36.00  67.00   1.00    5.37    --  104.50-125.00-120.00   31
 53  \w    131.00 176.00   1.00    5.37    --  104.50  77.00  60.00   45
 54  \w     75.00 115.00   1.00    5.37    --  104.50  77.00  60.00   40
 55  \w     57.00 115.00   1.00    5.37    --  104.50 -45.00 -30.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0773359000
_diffrn_orient_matrix_UB_12      0.0063212000
_diffrn_orient_matrix_UB_13      -0.1004685000
_diffrn_orient_matrix_UB_21      0.0058917000
_diffrn_orient_matrix_UB_22      -0.1396639000
_diffrn_orient_matrix_UB_23      0.0353316000
_diffrn_orient_matrix_UB_31      -0.1186741000
_diffrn_orient_matrix_UB_32      0.0122678000
_diffrn_orient_matrix_UB_33      -0.0433383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43841
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         74.072
_diffrn_reflns_theta_min         3.299
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.502
_exptl_absorpt_correction_T_max  0.548
_exptl_absorpt_correction_T_min  0.230
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41h (Rigaku Oxford Diffraction, 2015)
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 light yellow'
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.054
_refine_diff_density_max         1.314
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         7001
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0321P)^2^+1.7167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0645
_refine_ls_wR_factor_ref         0.0672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6226
_reflns_number_total             7001
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09488k2.cif
_cod_data_source_block           md043redabs
_cod_depositor_comments
'Adding full bibliography for 7119243--7119244.cif.'
_cod_original_cell_volume        1768.50(10)
_cod_database_code               7119243
_chemical_oxdiff_formula         C36H52N4Tl2C7H8
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
C8: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C9 \\sim C9A \\sim C8 \\sim C8A: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.001
3. Others
 Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=
 Sof(H8AC)=1-FVAR(1)
 Sof(H7A)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C9)=Sof(H9A)=Sof(H9B)=
 Sof(H9C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C34(H34), C7(H7A), C7(H7B), C31(H31)
4.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
4.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C14(H14), C5(H5), C29(H29), C27(H27), C28(H28), C3(H3), C4(H4)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C32(H32A,H32B,H32C), C23(H23A,H23B,
 H23C), C35(H35A,H35B,H35C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C17(H17A,
 H17B,H17C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C33(H33A,H33B,H33C), C36(H36A,
 H36B,H36C), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,H8AC)
;
_shelx_res_checksum              14319
_shelx_shelxl_version_number     2014/7
_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 2.133
_oxdiff_exptl_absorpt_empirical_full_min 0.668