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_7703238
_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 S4, 2[C7H8], 1[C4H8O]'
_chemical_formula_sum            'C104 H144 In4 N8 O S4'
_chemical_formula_weight         2109.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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
;
2019-11-25 deposited with the CCDC.	2019-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9261(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.22393(14)
_cell_length_b                   24.1502(2)
_cell_length_c                   23.9945(2)
_cell_measurement_reflns_used    12819
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.0000
_cell_measurement_theta_min      4.0410
_cell_volume                     9230.89(14)
_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_temperature      123.01(10)
_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     17.00 121.00   0.50   10.00    --   45.40  19.00 -60.00  208
  2  \w    -24.00  69.00   0.50   10.00    --   45.40 -57.00 120.00  186
  3  \w     32.00 128.00   0.50   30.00    --  104.50 -30.00  30.00  192
  4  \w     82.00 173.00   0.50   30.00    --  104.50  45.00-150.00  182
  5  \w     82.00 173.00   0.50   30.00    --  104.50  45.00 120.00  182
  6  \w     36.00 127.00   0.50   30.00    --  104.50 -45.00-180.00  182
  7  \w     32.00 128.00   0.50   30.00    --  104.50 -30.00-180.00  192
  8  \w     36.00 101.00   0.50   30.00    --  104.50 -45.00  60.00  130
  9  \w    143.00 177.00   0.50   30.00    --  104.50  30.00-120.00   68
 10  \w     28.00  50.50   0.50   30.00    --  104.50 -94.00-180.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV-50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26078
_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         74.065
_diffrn_reflns_theta_min         3.324
_exptl_absorpt_coefficient_mu    9.144
_exptl_absorpt_correction_T_max  0.717
_exptl_absorpt_correction_T_min  0.443
_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 yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.148
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         9159
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0428P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7283
_reflns_number_total             9159
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04481g2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        9230.90(15)
_cod_database_code               7703238
_shelx_shelxl_version_number     2018/3
_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 Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C31(H31), C34(H34)
2.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C14(H14), C21(H21), C27(H27), C28(H28), C29(H29)
2.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)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 600 electrons were
found in a volume of 2416\%A^3 in 1 void per unit cell.
This is consistent with the presence of 2[C7H8] and 1[C4H8O]
per Formula Unit which account for 560 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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
;
_twin_special_details
;
Component 2 rotated by 5.1344\% 
 around [-0.00 -0.96 0.29] (reciprocal) or [0.08 -0.95 0.30] (direct)
;