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_7703239
_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         'C36 H52 N4 S4, C7 H8'
_chemical_formula_sum            'C43 H60 N4 S4'
_chemical_formula_weight         761.19
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2217(2)
_cell_length_b                   18.6267(5)
_cell_length_c                   24.4822(6)
_cell_measurement_reflns_used    6598
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.4430
_cell_measurement_theta_min      3.5390
_cell_volume                     4205.30(18)
_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      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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   -133.00 -35.00   1.00    4.03    --  -44.56-178.00 120.00   98
  2  \w     36.00  98.00   1.00   20.00    --  104.50 -45.00-180.00   62
  3  \w     36.00  98.00   1.00   20.00    --  104.50 -45.00 120.00   62
  4  \w     23.00 109.00   1.00   20.00    --  104.50 -94.00  90.00   86
  5  \w     36.00  98.00   1.00   20.00    --  104.50 -45.00  60.00   62
  6  \w     14.00 114.00   1.00    4.03    --   44.56  77.00-180.00  100
;
_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      -0.1646640000
_diffrn_orient_matrix_UB_12      -0.0032743000
_diffrn_orient_matrix_UB_13      0.0104814000
_diffrn_orient_matrix_UB_21      0.0139476000
_diffrn_orient_matrix_UB_22      -0.0796212000
_diffrn_orient_matrix_UB_23      0.0164027000
_diffrn_orient_matrix_UB_31      0.0250619000
_diffrn_orient_matrix_UB_32      0.0223420000
_diffrn_orient_matrix_UB_33      0.0597627000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12714
_diffrn_reflns_point_group_measured_fraction_full 0.953
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.495
_diffrn_reflns_theta_max         67.494
_diffrn_reflns_theta_min         2.981
_diffrn_source                   'microfocus X-ray tube'
_diffrn_source_type              'GV-50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.718
_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    1.202
_exptl_crystal_description       needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Flack x determined using 2618 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0461P)^2^+0.0962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.710
_reflns_Friedel_fraction_full    0.903
_reflns_Friedel_fraction_max     0.903
_reflns_number_gt                6680
_reflns_number_total             7213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04481g2.cif
_cod_data_source_block           md107redabs
_cod_database_code               7703239
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C36 H52 N4 S4'
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.583
_reflns_odcompleteness_completeness 99.32
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
S2: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C31(H31), C34(H34)
3.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C19(H19A,H19B)
3.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C3(H3A), C4(H4), C5(H5), C27(H27), C28(H28), C29(H29),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43)
3.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C21(H21A,H21B,H21C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C)
;
_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 1.624
_oxdiff_exptl_absorpt_empirical_full_min 0.760