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_7700749
_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 Br2 In N3, C2 H5 O0.5'
_chemical_formula_sum            'C50 H55 Br2 In N3 O0.5'
_chemical_formula_weight         980.61
_chemical_name_common            '[InBr2(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     direct
_audit_creation_date             2019-01-07
_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                80.214(2)
_cell_angle_beta                 78.334(3)
_cell_angle_gamma                70.584(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0858(9)
_cell_length_b                   11.1952(9)
_cell_length_c                   19.8902(13)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.811
_cell_measurement_theta_min      2.300
_cell_volume                     2265.9(3)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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      150.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31109
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         3.018
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.323
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0630 before and 0.0492 after correction. The Ratio of minimum to maximum transmission is 0.8609. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             998
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Diethyl ether'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         9931
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0368P)^2^+1.2292P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7452
_reflns_number_total             9931
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_formula_sum        'C50 H55 Br2 In N3 O0.50'
_cod_database_code               7700749
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C50-C49A \\sim C50-C49
 with sigma of 0.02
 O1-C49 \\sim O1-C49A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim C49 \\sim C50 \\sim C49A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 O1, C49, C50, C49A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C49A)=Sof(H49C)=Sof(H49D)=1-FVAR(1)
 Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C49)=Sof(H49A)=Sof(H49B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C49A(H49C,H49D)
6.b Me refined with riding coordinates:
 C50(H50A,H50B,H50C), C50(H50D,H50E,H50F)
6.c Aromatic/amide H refined with riding coordinates:
 C44(H44), C42(H42), C18(H18), C9(H9), C35(H35), C11(H11), C3(H3), C33(H33),
 C20(H20), C5(H5), C29(H29), C4(H4), C27(H27), C28(H28)
6.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C37(H37A,
 H37B,H37C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C), C14(H14A,H14B,H14C),
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              4240
_olex2_submission_special_instructions 'No special instructions were received'