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_7119244
_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 In2 N4 O0.08'
_chemical_formula_sum            'C36 H52 In2 N4 O0.08'
_chemical_formula_weight         771.73
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-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             2016-11-04
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.10.10 svn.r3347 for OlexSys, GUI svn.r5252)
;
_audit_update_record
;
2016-11-04 deposited with the CCDC.
2016-12-23 downloaded from the CCDC.
;
_cell_angle_alpha                106.4107(14)
_cell_angle_beta                 108.2254(14)
_cell_angle_gamma                99.2006(15)
_cell_formula_units_Z            2
_cell_length_a                   11.49565(18)
_cell_length_b                   12.7946(2)
_cell_length_c                   14.8078(2)
_cell_measurement_reflns_used    43241
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      74.2360
_cell_measurement_theta_min      3.3240
_cell_volume                     1909.35(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.42b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.42b (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      123.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.977
_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   -132.00 -35.00   1.00    4.00    --  -44.08-178.00  60.00   97
  2  \w     20.00 113.00   1.00    4.00    --   44.08  57.00  60.00   93
  3  \w    -25.00  68.00   1.00    4.00    --   44.08 -57.00 -90.00   93
  4  \w     36.00  98.00   1.00   16.00    --  104.50 -45.00  90.00   62
  5  \w     33.00 135.00   1.00   16.00    --  104.50 -77.00-150.00  102
  6  \w     32.00  91.00   1.00   16.00    --  104.50 -30.00 150.00   59
  7  \w     33.00 135.00   1.00   16.00    --  104.50 -77.00   0.00  102
  8  \w     33.00 123.00   1.00   16.00    --  104.50-128.00-136.00   90
  9  \w     81.00 177.00   1.00   16.00    --  104.50  30.00 -90.00   96
 10  \w     32.00  91.00   1.00   16.00    --  104.50 -30.00   0.00   59
 11  \w     27.00 141.00   1.00   16.00    --  104.50 -15.00-120.00  114
 12  \w     20.00 113.00   1.00    4.00    --   44.08  57.00 150.00   93
 13  \w     14.00 116.00   1.00    4.00    --   44.08  77.00-150.00  102
 14  \w     20.00 113.00   1.00    4.00    --   44.08  57.00 -30.00   93
 15  \w     82.00 173.00   1.00   16.00    --  104.50  45.00 150.00   91
 16  \w     81.00 177.00   1.00   16.00    --  104.50  30.00   0.00   96
 17  \w     74.00 176.00   1.00   16.00    --  104.50  77.00-180.00  102
 18  \w     82.00 173.00   1.00   16.00    --  104.50  45.00  60.00   91
 19  \w     86.00 121.00   1.00   16.00    --  104.50-125.00  30.00   35
 20  \w    131.00 172.00   1.00   16.00    --  104.50 125.00-120.00   41
 21  \w     48.00  89.00   1.00   16.00    --  104.50 -30.00-150.00   41
 22  \w     48.00  74.00   1.00   16.00    --  104.50-125.00  30.00   26
 23  \w   -124.00 -79.00   1.00    4.00    --  -44.33 -99.00 -90.00   45
 24  \w    -50.00  26.00   1.00    4.00    --  -44.33  38.00  60.00   76
 25  \w     14.00 116.00   1.00    4.00    --   44.33  77.00 150.00  102
 26  \w     14.00 116.00   1.00    4.00    --   44.33  77.00   0.00  102
 27  \w     14.00 116.00   1.00    4.00    --   44.33  77.00 -60.00  102
 28  \w     14.00 116.00   1.00    4.00    --   44.33  77.00  60.00  102
 29  \w     74.00 176.00   1.00   16.00    --  104.50  77.00  90.00  102
 30  \w     74.00 176.00   1.00   16.00    --  104.50  77.00-150.00  102
 31  \w     74.00 176.00   1.00   16.00    --  104.50  77.00 150.00  102
 32  \w     79.00 174.00   1.00   16.00    --  104.50  61.00 -90.00   95
 33  \w     74.00 176.00   1.00   16.00    --  104.50  77.00  60.00  102
 34  \w     74.00 176.00   1.00   16.00    --  104.50  77.00   0.00  102
 35  \w     74.00 176.00   1.00   16.00    --  104.50  77.00 -30.00  102
 36  \w     74.00 176.00   1.00   16.00    --  104.50  77.00-120.00  102
 37  \w     33.00 121.00   1.00   16.00    --  104.50-125.00  30.00   88
 38  \w     74.00 176.00   1.00   16.00    --  104.50  77.00  30.00  102
 39  \w     79.00 174.00   1.00   16.00    --  104.50  61.00 150.00   95
 40  \w     79.00 174.00   1.00   16.00    --  104.50  61.00 -60.00   95
 41  \w    -50.00  26.00   1.00    4.00    --  -44.33  38.00  90.00   76
 42  \w     22.00 115.00   1.00    4.00    --   44.33  38.00 -60.00   93
 43  \w     16.00 120.00   1.00    4.00    --   44.33  19.00 -90.00  104
 44  \w     22.00 115.00   1.00    4.00    --   44.33  38.00 -30.00   93
 45  \w     20.00 114.00   1.00    4.00    --   44.33  57.00 -90.00   94
 46  \w     22.00 115.00   1.00    4.00    --   44.33  38.00-180.00   93
 47  \w     74.00 176.00   1.00   16.00    --  104.50  77.00 -60.00  102
 48  \w     79.00 174.00   1.00   16.00    --  104.50  61.00-150.00   95
 49  \w     79.00 174.00   1.00   16.00    --  104.50  61.00 120.00   95
 50  \w     79.00 174.00   1.00   16.00    --  104.50  61.00  60.00   95
 51  \w     79.00 174.00   1.00   16.00    --  104.50  61.00   0.00   95
 52  \w     79.00 174.00   1.00   16.00    --  104.50  61.00-180.00   95
 53  \w     79.00 174.00   1.00   16.00    --  104.50  61.00-120.00   95
 54  \w     79.00 174.00   1.00   16.00    --  104.50  61.00  90.00   95
 55  \w     79.00 174.00   1.00   16.00    --  104.50  61.00  30.00   95
 56  \w     79.00 174.00   1.00   16.00    --  104.50  61.00 -30.00   95
 57  \w     74.00 176.00   1.00   16.00    --  104.50  77.00 120.00  102
 58  \w     74.00 176.00   1.00   16.00    --  104.50  77.00 -90.00  102
 59  \w     14.00 116.00   1.00    4.00    --   44.33  77.00  90.00  102
 60  \w    -30.00 119.00   1.00    4.00    --   44.33   0.00-180.00  149
 61  \w     20.00 114.00   1.00    4.00    --   44.33  57.00-180.00   94
 62  \w    -30.00 119.00   1.00    4.00    --   44.33   0.00-120.00  149
 63  \w    -30.00 119.00   1.00    4.00    --   44.33   0.00-150.00  149
 64  \w     14.00 116.00   1.00    4.00    --   44.33  77.00-120.00  102
 65  \w     23.00 109.00   1.00   16.00    --  104.50 -94.00  90.00   86
 66  \w     82.00 173.00   1.00   16.00    --  104.50  45.00  90.00   91
 67  \w     82.00 173.00   1.00   16.00    --  104.50  45.00 -60.00   91
 68  \w     82.00 173.00   1.00   16.00    --  104.50  45.00 -90.00   91
 69  \w     82.00 173.00   1.00   16.00    --  104.50  45.00-150.00   91
 70  \w     82.00 173.00   1.00   16.00    --  104.50  45.00-180.00   91
 71  \w     82.00 173.00   1.00   16.00    --  104.50  45.00-120.00   91
 72  \w     82.00 173.00   1.00   16.00    --  104.50  45.00 120.00   91
 73  \w     82.00 173.00   1.00   16.00    --  104.50  45.00 -30.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1220673000
_diffrn_orient_matrix_UB_12      -0.0318683000
_diffrn_orient_matrix_UB_13      0.0202009000
_diffrn_orient_matrix_UB_21      0.0787787000
_diffrn_orient_matrix_UB_22      0.0465138000
_diffrn_orient_matrix_UB_23      0.1152371000
_diffrn_orient_matrix_UB_31      -0.0199090000
_diffrn_orient_matrix_UB_32      0.1176426000
_diffrn_orient_matrix_UB_33      0.0059815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            89347
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.445
_diffrn_reflns_theta_min         3.361
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    9.845
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.42b (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_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_description       block
_exptl_crystal_F_000             789
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.074
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.961
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7726
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0333
_refine_ls_R_factor_gt           0.0291
_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^)+(0.0356P)^2^+1.5237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6956
_reflns_number_total             7726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc09488k2.cif
_cod_data_source_block           md29_abs_sq
_cod_depositor_comments
'Adding full bibliography for 7119243--7119244.cif.'
_cod_original_cell_volume        1909.34(6)
_cod_database_code               7119244
_chemical_oxdiff_formula         C36H52In2N4
_reflns_odcompleteness_completeness 100.00
_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
In4 \\sim In2 \\sim In1 \\sim In3: within 2A with sigma of 0.001 and sigma for
terminal atoms of 0.001
C12A \\sim C12 \\sim C11 \\sim C11A: within 2A with sigma of 0.001 and sigma
for terminal atoms of 0.001
3. Others
 Sof(In3)=Sof(In4)=Sof(O1)=1-FVAR(1)
 Sof(In2)=Sof(In1)=FVAR(1)
 Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(2)
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(3)
 Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=FVAR(3)
4.a Ternary CH refined with riding coordinates:
 C31(H31), C7(H7), C34(H34), C10(H10)
4.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C18(H18A,H18B)
4.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C27(H27), C29(H29), C5(H5), C28(H28), C3(H3), C15(H15), C4(H4)
4.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C36(H36A,H36B,
 H36C), C17(H17A,H17B,H17C), C32(H32A,H32B,H32C), C35(H35A,H35B,H35C), C9(H9A,
 H9B,H9C), C33(H33A,H33B,H33C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F)
;
_shelx_fab_checksum              64775
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'Crystal mounted in mineral oil using MiTeGen loops.'
_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 1.491
_oxdiff_exptl_absorpt_empirical_full_min 0.623