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_7700751
_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 H52 Ga N3, 0.5(C7 H8)'
_chemical_formula_sum            'C51.5 H56 Ga N3'
_chemical_formula_weight         786.71
_chemical_name_common            '[GaH2(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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-30
_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                103.836(2)
_cell_angle_beta                 94.296(2)
_cell_angle_gamma                110.472(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4624(5)
_cell_length_b                   11.3645(5)
_cell_length_c                   20.0930(8)
_cell_measurement_reflns_used    9776
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.058
_cell_measurement_theta_min      2.288
_cell_volume                     2139.96(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.983
_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  0.0415
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30979
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.144
_diffrn_reflns_theta_min         2.437
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.681
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1189 before and 0.0497 after correction. The Ratio of minimum to maximum transmission is 0.9176. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       prism
_exptl_crystal_F_000             834
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         9324
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0397P)^2^+1.0745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7272
_reflns_number_total             9324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           13
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_formula_sum        'C51.50 H56 Ga N3'
_cod_database_code               7700751
_shelx_shelxl_version_number     2018/3
_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
 C49-C51 \\sim C49-C55
 with sigma of 0.04
3. Restrained planarity
 C49, C50, C55, C54, C53, C52, C51
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C55 \\sim C54 \\sim C53 \\sim C52 \\sim C51: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C49, C50, C55, C54, C53, C52, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C50(0.5) C55(0.5) H55(0.5)
 C54(0.5) H54(0.5) C53(0.5) H53(0.5) C52(0.5) H52(0.5) C51(0.5) H51(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C11(H11), C4(H4), C29(H29), C33(H33), C28(H28), C9(H9), C3(H3),
 C20(H20), C44(H44), C27(H27), C5(H5), C35(H35), C42(H42), C55(H55), C54(H54),
 C53(H53), C52(H52), C51(H51)
7.b Fitted hexagon refined as free rotating group:
 C50(C55,C54,C53,C52,C51)
7.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C14(H14A,H14B,
 H14C), C22(H22A,H22B,H22C), C48(H48A,H48B,H48C), C13(H13A,H13B,H13C), C38(H38A,
 H38B,H38C), C37(H37A,H37B,H37C), C23(H23A,H23B,H23C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              94358
_olex2_submission_special_instructions 'No special instructions were received'