Facile oxidative addition of O<sub>2</sub> and S<sub>8</sub> by an indium bis(carbene) analogue.
Desat, Marcella E.; Kretschmer, Robert; Dalton transactions (Cambridge, England : 2003) 48 (2019) 17718–17722; doi:10.1039/c9dt04481g

data_7703240
_publ_section_title
;
 Facile oxidative addition of O<sub>2</sub> and S<sub>8</sub> by an indium
 bis(carbene) analogue.
;
_journal_issue                   48
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17718
_journal_page_last               17722
_journal_paper_doi               10.1039/c9dt04481g
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C72 H104 In4 N8 O1.96'
_chemical_formula_sum            'C72 H104 In4 N8 O1.96'
_chemical_formula_weight         1572.27
_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             2019-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-21 deposited with the CCDC.	2019-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                106.288(2)
_cell_angle_beta                 110.634(2)
_cell_angle_gamma                98.668(2)
_cell_formula_units_Z            1
_cell_length_a                   11.7484(2)
_cell_length_b                   12.8340(3)
_cell_length_c                   14.8693(3)
_cell_measurement_reflns_used    26331
_cell_measurement_temperature    123.01(16)
_cell_measurement_theta_max      74.4600
_cell_measurement_theta_min      3.3460
_cell_volume                     1934.67(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      123.01(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_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    -51.00   1.00   1.00    1.00    --    0.00 121.00-130.40   52
  2  \w      6.00  33.00   1.00    1.00    --   40.00  88.00 172.49   27
  3  \w    -69.00  25.00   1.00    1.00    --  -44.81  57.00-150.00   94
  4  \w    -75.00  27.00   1.00    1.00    --  -44.81  77.00   0.00  102
  5  \w     21.00 114.00   1.00    1.00    --   44.81  57.00  90.00   93
  6  \w     21.00 114.00   1.00    1.00    --   44.81  57.00-120.00   93
  7  \w     17.00  47.00   1.00    1.00    --   48.00  79.00 118.76   30
  8  \w     16.00  46.00   1.00    1.00    --   48.00  81.00  73.53   30
  9  \w     17.00  47.00   1.00    1.00    --   48.00  79.00 -70.50   30
 10  \w     16.00  45.00   1.00    1.00    --   48.00  82.00-153.72   29
 11  \w     21.00  49.00   1.00    1.00    --   52.00  78.00  -5.07   28
 12  \w     21.00  49.00   1.00    1.00    --   52.00  78.00 170.73   28
 13  \w     31.00 131.00   1.00    1.00    --   60.00  74.00 -81.04  100
 14  \w     30.00 132.00   1.00    1.00    --   60.00  77.00   7.50  102
 15  \w     34.00 135.00   1.00    1.00    --   64.00  75.00 121.71  101
 16  \w     34.00 135.00   1.00    1.00    --   64.00  76.00  44.52  101
 17  \w     34.00 135.00   1.00    1.00    --   64.00  76.00-142.82  101
 18  \w     38.00  65.00   1.00    1.00    --   68.00  76.00 174.49   27
 19  \w     38.00  64.00   1.00    1.00    --   68.00  75.00  68.49   26
 20  \w     41.00  83.00   1.00    1.00    --   68.00  74.00  98.70   42
 21  \w     38.00  70.00   1.00    1.00    --   68.00  75.00 -58.51   32
 22  \w     43.00  69.00   1.00    1.00    --   72.00  77.00-117.79   26
 23  \w     42.00  75.00   1.00    1.00    --   72.00  77.00   1.33   33
 24  \w     43.00  68.00   1.00    1.00    --   72.00  77.00 -52.17   25
 25  \w     95.00 140.00   1.00    1.00    --   72.00  77.00-117.79   45
 26  \w     58.00  90.00   1.00    1.50    --   84.00  63.00  -0.67   32
 27  \w     56.00  82.00   1.00    1.50    --   84.00  69.00 -36.39   26
 28  \w     55.00  83.00   1.00    1.50    --   84.00  72.00 144.27   28
 29  \w     61.00 157.00   1.00    1.50    --   88.00  67.00  66.37   96
 30  \w    126.00 162.00   1.00    1.50    --   92.00  71.00-132.72   36
 31  \w     64.00  90.00   1.00    1.50    --   92.00  71.00-132.72   26
 32  \w    130.00 163.00   1.00    1.50    --   92.00  74.00-176.28   33
 33  \w     63.00  90.00   1.00    1.50    --   92.00  74.00-176.28   27
 34  \w     40.00  83.00   1.00    1.50    --  104.50 -94.00  30.00   43
 35  \w     23.00 100.00   1.00    1.50    --  104.50 -94.00 -30.00   77
 36  \w     29.00 108.00   1.00    1.50    --  104.50 -94.00 150.00   79
 37  \w     26.00 109.00   1.00    1.50    --  104.50 -94.00-120.00   83
 38  \w     76.00 170.00   1.00    1.50    --  104.50  77.00 120.00   94
 39  \w     81.00 107.00   1.00    1.50    --  104.50  61.00  90.00   26
 40  \w     74.00 162.00   1.00    1.50    --  104.50  77.00 150.00   88
 41  \w     82.00 169.00   1.00    1.50    --  104.50  61.00  30.00   87
 42  \w     74.00 143.00   1.00    1.50    --  104.50  77.00  90.00   69
 43  \w     74.00 100.00   1.00    1.50    --  104.50  77.00   0.00   26
 44  \w     79.00 147.00   1.00    1.50    --  104.50  61.00-150.00   68
 45  \w     74.00 146.00   1.00    1.50    --  104.50  77.00 -90.00   72
 46  \w     75.00 174.00   1.00    1.50    --  104.50  77.00 -60.00   99
 47  \w     36.00  84.00   1.00    1.50    --  104.50 -61.00-120.00   48
 48  \w     39.00 121.00   1.00    1.50    --  104.50-125.00 120.00   82
 49  \w    145.00 175.00   1.00    1.50    --  104.50  77.00-120.00   30
 50  \w     74.00 126.00   1.00    1.50    --  104.50  77.00-120.00   52
 51  \w     75.00 175.00   1.00    1.50    --  104.50  77.00 -30.00  100
 52  \w    137.00 163.00   1.00    1.50    --  104.50  77.00  60.00   26
 53  \w     75.00 111.00   1.00    1.50    --  104.50  77.00  60.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV-50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0852817000
_diffrn_orient_matrix_UB_12      0.0581628000
_diffrn_orient_matrix_UB_13      0.0427525000
_diffrn_orient_matrix_UB_21      -0.1183014000
_diffrn_orient_matrix_UB_22      -0.0882098000
_diffrn_orient_matrix_UB_23      -0.0902616000
_diffrn_orient_matrix_UB_31      0.0026308000
_diffrn_orient_matrix_UB_32      -0.0760477000
_diffrn_orient_matrix_UB_33      0.0641334000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41307
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.468
_diffrn_reflns_theta_min         3.405
_diffrn_source                   'microfocus X-ray tube'
_diffrn_source_type              'GV-50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.744
_exptl_absorpt_correction_T_max  0.722
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.039
_refine_diff_density_min         -0.661
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7732
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0232P)^2^+1.1648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7124
_reflns_number_total             7732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04481g2.cif
_cod_data_source_block           md47red2abs
_cod_database_code               7703240
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C72H104In4N8O2
_chemical_oxdiff_usercomment     'orange block'
_shelx_estimated_absorpt_t_max   0.611
_shelx_estimated_absorpt_t_min   0.295
_reflns_odcompleteness_completeness 99.99
_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
In \\sim In1: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001
3. Others
 Sof(In)=1-FVAR(1)
 Sof(In1)=Sof(O1)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C31(H31), C34(H34)
4.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C14(H14), C21(H21), C27(H27), C28(H28), C29(H29)
4.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C)
;
_olex2_exptl_crystal_mounting_method
'Crystal mounted in mineral oil using MiTenGen 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 2.719
_oxdiff_exptl_absorpt_empirical_full_min 0.668