Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and spectroscopic study.
Gyton, Matthew R.; Leverett, Anthony R.; Cole, Marcus L.; McKay, Alasdair I.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5653–5661; doi:10.1039/d0dt00285b

data_7703894
_publ_section_title
;
 Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and
 spectroscopic study.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5653
_journal_page_last               5661
_journal_paper_doi               10.1039/d0dt00285b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C48 H66 I In N6'
_chemical_formula_sum            'C48 H66 I In N6'
_chemical_formula_weight         968.78
_chemical_name_systematic        '[InI(N3Dipp2)2]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-14 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.19(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.375(3)
_cell_length_b                   16.586(3)
_cell_length_c                   21.259(4)
_cell_measurement_reflns_used    2450
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9851
_cell_measurement_theta_min      2.8293
_cell_volume                     4787.0(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      150.15
_diffrn_detector_area_resol_mean 8.4171
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -12.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   65.0000  169.0000 119

  2 omega  -75.00   51.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069  -77.0000  -90.0000 126

  3 omega -120.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  179.0000  -90.0000 88

  4 omega  -16.00   14.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  -77.0000  150.0000 30

  5 omega -103.00  -74.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.4444  -77.0000  150.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0293542000
_diffrn_orient_matrix_UB_12      -0.0353692000
_diffrn_orient_matrix_UB_13      0.0051572000
_diffrn_orient_matrix_UB_21      -0.0364703000
_diffrn_orient_matrix_UB_22      -0.0198619000
_diffrn_orient_matrix_UB_23      -0.0257831000
_diffrn_orient_matrix_UB_31      0.0224603000
_diffrn_orient_matrix_UB_32      0.0135710000
_diffrn_orient_matrix_UB_33      -0.0232839000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_unetI/netI     0.1553
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28650
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.878
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       cube
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.528
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         9062
_refine_ls_number_restraints     499
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1797
_refine_ls_R_factor_gt           0.0905
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+18.0010P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4430
_reflns_number_total             9062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           10
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_original_cell_volume        4786.8(19)
_cod_database_code               7703894
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 S O2'
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.891
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36A-C34 \\sim C36B-C34 \\sim C35A-C34 \\sim C35B-C34
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35B \\sim C34 \\sim C36B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C35A \\sim C34 \\sim C36A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C35B)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36B)=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=1-FVAR(1)
 Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36A)=Sof(H36A)=Sof(H36B)=
 Sof(H36C)=FVAR(1)
 Sof(C11B)=Sof(H11D)=Sof(H11E)=Sof(H11F)=1-FVAR(2)
 Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C22(H22), C31(H31), C43(H43), C46(H46)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C27(H27), C28(H28),
 C29(H29), C39(H39), C40(H40), C41(H41)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11A(H11A,H11B,H11C), C11B(H11D,H11E,H11F),
 C12(H12A,H12B,H12C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C),
 C35A(H35A,H35B,H35C), C35B(H35D,H35E,H35F), C36A(H36A,H36B,H36C), C36B(H36D,
 H36E,H36F), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              29842
_olex2_submission_special_instructions 'No special instructions were received'