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_7700761
_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         'C50 H56 Ga N3, C3 H7'
_chemical_formula_sum            'C53 H63 Ga N3'
_chemical_formula_weight         811.78
_chemical_name_common            '[GaMe2(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             2019-01-24
_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                97.282(3)
_cell_angle_beta                 96.972(3)
_cell_angle_gamma                111.686(2)
_cell_formula_units_Z            2
_cell_length_a                   10.8007(6)
_cell_length_b                   11.8461(7)
_cell_length_c                   19.6602(11)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.44
_cell_volume                     2279.6(2)
_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
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0355
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35298
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.099
_diffrn_reflns_theta_min         1.982
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6708
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1243 before and 0.0507 after correction. The Ratio of minimum to maximum transmission is 0.8998. The \I/2 correction'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       prism
_exptl_crystal_F_000             866
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9992
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.0902P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8699
_reflns_number_total             9992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_database_code               7700761
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,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
 C51A-C53 \\sim C52-C53 \\sim C51-C51A \\sim C51-C52
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C53 \\sim C52 \\sim C51: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C53 \\sim C51A \\sim C51: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 C53, C52, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C51A, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H51D)=Sof(H51E)=Sof(H51F)=Sof(H53C)=Sof(H53D)=Sof(C52)=Sof(H52A)=
 Sof(H52B)=1-FVAR(1)
 Sof(H51A)=Sof(H51B)=Sof(H51C)=Sof(H53A)=Sof(H53B)=Sof(C51A)=Sof(H51G)=
 Sof(H51H)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C53(H53C,H53D), C53(H53A,H53B), C52(H52A,H52B), C51A(H51G,H51H)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C35(H35), C4(H4), C27(H27), C3(H3), C33(H33), C29(H29), C28(H28),
 C9(H9), C18(H18), C11(H11), C20(H20), C44(H44), C42(H42)
6.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C49(H49A,H49B,H49C), C39(H39A,H39B,
 H39C), C22(H22A,H22B,H22C), C48(H48A,H48B,H48C), C15(H15A,H15B,H15C), C46(H46A,
 H46B,H46C), C13(H13A,H13B,H13C), C50(H50A,H50B,H50C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C14(H14A,H14B,H14C), C51(H51D,H51E,
 H51F), C51(H51A,H51B,H51C)
;
_shelx_res_checksum              17922
_olex2_submission_special_instructions 'No special instructions were received'