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_7700758
_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 Al N3, 0.5(C5 H12)'
_chemical_formula_sum            'C52.5 H62 Al N3'
_chemical_formula_weight         762.03
_chemical_name_common            '[AlMe2(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             2019-01-23
_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                98.246(2)
_cell_angle_beta                 96.521(2)
_cell_angle_gamma                111.357(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7943(5)
_cell_length_b                   11.7863(6)
_cell_length_c                   19.6677(9)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.44
_cell_volume                     2268.68(19)
_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
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.984
_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  0.0431
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45171
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.146
_diffrn_reflns_theta_min         2.441
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1219 before and 0.0548 after correction. The Ratio of minimum to maximum transmission is 0.9552. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Pentane'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9887
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0754P)^2^+1.2434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1435
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7920
_reflns_number_total             9887
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02562f2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7700747--7700761.cif.'
_cod_original_formula_sum        'C52.50 H62 Al N3'
_cod_database_code               7700758
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.964
_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
2. Restrained distances
 C51-C52 = C52-C53 = C53-C54 = C54-C55
 1.5 with sigma of 0.01
 C51-C53 \\sim C53-C55 \\sim C52-C54
 with sigma of 0.04
3. Restrained planarity
 C51, C52, C53, C54, C55
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C51, C52, C53, C54, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C51(0.5) H51A(0.5) H51B(0.5) H51C(0.5) C52(0.5) H52A(0.5)
 H52B(0.5) C53(0.5) H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C55(0.5)
 H55A(0.5) H55B(0.5) H55C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
7.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C29(H29), C33(H33), C35(H35), C20(H20), C28(H28), C18(H18), C5(H5),
 C44(H44), C9(H9), C11(H11), C3(H3), C4(H4), C42(H42)
7.c Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C38(H38A,H38B,
 H38C), C48(H48A,H48B,H48C), C15(H15A,H15B,H15C), C50(H50A,H50B,H50C), C37(H37A,
 H37B,H37C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C),
 C22(H22A,H22B,H22C), C14(H14A,H14B,H14C), C47(H47A,H47B,H47C), C51(H51A,H51B,
 H51C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              70388
_olex2_submission_special_instructions 'No special instructions were received'