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_7700756
_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         'C48.5 H51.5 Al Cl1.5 N3, C3 H7'
_chemical_formula_sum            'C51.5 H58.5 Al Cl1.5 N3'
_chemical_formula_weight         799.66
_chemical_name_common            '[AlCl2(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             2019-02-02
_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                100.490(3)
_cell_angle_beta                 95.000(3)
_cell_angle_gamma                111.394(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7290(7)
_cell_length_b                   11.7522(8)
_cell_length_c                   19.8810(14)
_cell_measurement_reflns_used    7723
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.40
_cell_volume                     2262.5(3)
_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_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.951
_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  0.0505
_diffrn_reflns_av_unetI/netI     0.0532
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            30651
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.698
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0954 before and 0.0591 after correction.
The Ratio of minimum to maximum transmission is 0.9151.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       prism
_exptl_crystal_F_000             854
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Hexane'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0073(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         8178
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0847P)^2^+1.7180P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.1790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6024
_reflns_number_total             8178
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_formula_sum        'C51.50 H58.50 Al Cl1.50 N3'
_cod_database_code               7700756
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.954
_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
 Al1-C1A
 1.94 with sigma of 0.02
 C50A-C49 \\sim C51-C50A \\sim C51-C50 \\sim C50-C49
 with sigma of 0.02
 C50-C49 \\sim C51-C50
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C49 \\sim C50 \\sim C51: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C49 \\sim C50A \\sim C51: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C1A \\sim Cl1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C49, C50, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C50A, C51
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, Al1, Cl1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(H51C)=Sof(H51D)=Sof(H49D)=Sof(H49E)=Sof(H49F)=Sof(C50A)=Sof(H50A)=
 Sof(H50B)=1-FVAR(1)
 Sof(H51A)=Sof(H51B)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C50)=Sof(H50C)=
 Sof(H50D)=FVAR(1)
 Fixed Sof: Cl1(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C51(H51C,H51D), C51(H51A,H51B), C50A(H50A,H50B), C50(H50C,H50D)
6.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C33(H33), C27(H27), C20(H20), C35(H35), C42(H42), C28(H28), C4(H4),
 C3(H3), C18(H18), C5(H5), C9(H9), C11(H11), C44(H44)
6.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C22(H22A,H22B,H22C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C15(H15A,
 H15B,H15C), C23(H23A,H23B,H23C), C14(H14A,H14B,H14C), C47(H47A,H47B,H47C),
 C37(H37A,H37B,H37C), C49(H49D,H49E,H49F), C49(H49A,H49B,H49C), C1A(H1AA,H1AB,
 H1AC)
;
_shelx_res_checksum              33664
_olex2_submission_special_instructions 'No special instructions were received'