Kinetic stabilization of low-oxidation state and terminal hydrido main group metal complexes by a sterically demanding N,N'-bis(2,6-terphenyl)triazenide.
Leverett, Anthony R.; Diachenko, Vera; Cole, Marcus L.; McKay, Alasdair I.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13197–13204; doi:10.1039/c9dt02562f

data_7700760
_publ_section_title
;
 Kinetic stabilization of low-oxidation state and terminal hydrido main
 group metal complexes by a sterically demanding
 N,N'-bis(2,6-terphenyl)triazenide.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13197
_journal_page_last               13204
_journal_paper_doi               10.1039/c9dt02562f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C48 H50 In0.75 N3, 0.5(C7 H8)'
_chemical_formula_sum            'C51.5 H54 In0.75 N3'
_chemical_formula_weight         801.09
_chemical_name_common            '[In(N3Dmp2)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-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             2019-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-11 deposited with the CCDC.    2019-08-06 downloaded from the CCDC.
;
_cell_angle_alpha                103.975(4)
_cell_angle_beta                 95.003(4)
_cell_angle_gamma                110.046(5)
_cell_formula_units_Z            2
_cell_length_a                   10.4601(5)
_cell_length_b                   11.3940(6)
_cell_length_c                   19.9439(9)
_cell_measurement_reflns_used    3610
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.7333
_cell_measurement_theta_min      3.0029
_cell_volume                     2128.9(2)
_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      173
_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   91.00  118.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   77.0000   60.0000 27

  2 omega  -13.00  103.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   77.0000  -30.0000 116

  3 omega    4.00   37.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0069   77.0000   60.0000 33

  4 omega  -54.00   68.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1319   77.0000 -150.0000 122

  5 omega  -59.00   33.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1319   77.0000  120.0000 92

  6 omega -115.00    3.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -24.1319  -38.0000  150.0000 118
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0075452000
_diffrn_orient_matrix_UB_12      -0.0314042000
_diffrn_orient_matrix_UB_13      -0.0362666000
_diffrn_orient_matrix_UB_21      0.0494392000
_diffrn_orient_matrix_UB_22      0.0577158000
_diffrn_orient_matrix_UB_23      -0.0037739000
_diffrn_orient_matrix_UB_31      0.0538227000
_diffrn_orient_matrix_UB_32      -0.0218434000
_diffrn_orient_matrix_UB_33      0.0078774000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0986
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18249
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         3.009
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.461
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49688
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_description       block
_exptl_crystal_F_000             842
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     545
_refine_ls_number_reflns         8694
_refine_ls_number_restraints     549
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0348P)^2^+1.7033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1240
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5850
_reflns_number_total             8694
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           15
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_cell_volume        2128.86(19)
_cod_original_formula_sum        'C51.50 H54 In0.75 N3'
_cod_database_code               7700760
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.913
_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
 C50-C51 \\sim C51-C52 \\sim C52-C53 \\sim C53-C54 \\sim C54-C55 \\sim C55-C50
 with sigma of 0.02
 C50-C54 \\sim C50-C52 \\sim C55-C53 \\sim C51-C55 \\sim C52-C54 \\sim C51-C53
 with sigma of 0.04
 C49-C55 \\sim C49-C51
 with sigma of 0.04
3. Restrained planarity
 C49, C50, C51, C52, C53, C54, C55
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C49, C50, C51, C52, C53, C54, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20, In1, N3, N1, N2, C25, C1, C26, C30, C2, C6, C31, C27, C40, C29, C7, C3,
 C5, C16, C32, C36, C28, C41, C45, C8, C12, C4, C11, C21, C17, C33, C37, C35,
 C39, C42, C46, C44, C48, C13, C9, C15, C10, C24, C22, C18, C34, C43, C14, C19,
 C38, C47, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: In1(0.75) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5) C51(0.5)
 H51(0.5) C52(0.5) H52(0.5) C53(0.5) H53(0.5) C54(0.5) H54(0.5) C55(0.5)
 H55(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C42(H42), C20(H20), C44(H44), C28(H28), C27(H27), C5(H5), C33(H33),
 C9(H9), C4(H4), C11(H11), C35(H35), C3(H3), C18(H18), C51(H51), C52(H52),
 C53(H53), C54(H54), C55(H55)
7.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C38(H38A,H38B,
 H38C), C22(H22A,H22B,H22C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C14(H14A,
 H14B,H14C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C47(H47A,H47B,H47C),
 C23(H23A,H23B,H23C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              57397
_olex2_submission_special_instructions 'No special instructions were received'