Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and spectroscopic study.
Gyton, Matthew R.; Leverett, Anthony R.; Cole, Marcus L.; McKay, Alasdair I.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 5653–5661; doi:10.1039/d0dt00285b

data_7703886
_publ_section_title
;
 Bulky bis(aryl)triazenides: just aspiring amidinates? A structural and
 spectroscopic study.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5653
_journal_page_last               5661
_journal_paper_doi               10.1039/d0dt00285b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C32 H50 Li N3 O2'
_chemical_formula_sum            'C32 H50 Li N3 O2'
_chemical_formula_weight         515.69
_chemical_name_systematic        '[Li(THF)2(N3Dipp2)]'
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-14 deposited with the CCDC.	2020-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.063(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.8789(9)
_cell_length_b                   18.6075(9)
_cell_length_c                   19.5150(8)
_cell_measurement_reflns_used    8242
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.96
_cell_measurement_theta_min      2.31
_cell_volume                     6397.4(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0923
_diffrn_reflns_av_unetI/netI     0.0792
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            78234
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.139
_diffrn_reflns_theta_min         1.565
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1022 before and 0.0798 after correction. The Ratio of minimum to maximum transmission is 0.8757. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_description       block
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.0019(3)
_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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         14123
_refine_ls_number_restraints     178
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0750P)^2^+2.0450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1917
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7373
_reflns_number_total             14123
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           5(THF)2
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_database_code               7703886
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C64-C63 \\sim C63-C62 \\sim C62-C61
 with sigma of 0.02
 O4-C64 \\sim O4-C61
 with sigma of 0.02
 O4-C63 \\sim O4-C62
 with sigma of 0.04
 C63-C61 \\sim C64-C62
 with sigma of 0.04
 C64A-C63A \\sim C63A-C62A \\sim C62A-C61A
 with sigma of 0.02
 O4A-C64A \\sim O4A-C61A
 with sigma of 0.02
 O4A-C63A \\sim O4A-C62A
 with sigma of 0.04
 C63A-C61A \\sim C64A-C62A
 with sigma of 0.04
 O4-Li3 \\sim O4A-Li3
 with sigma of 0.02
 C30-C31 \\sim C30-C31A \\sim C32-C31A \\sim C32-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C64 \\sim C63 \\sim C62 \\sim C61: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O4A \\sim C64A \\sim C63A \\sim C62A \\sim C61A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C32 \\sim C31 \\sim C30: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C32 \\sim C31A \\sim C30: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Rigid body (RIGU) restrains
 O4, C64, C63, C62, C61
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O4A, C64A, C63A, C62A, C61A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C32, C31A, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O4A)=Sof(C64A)=Sof(H64C)=Sof(H64D)=Sof(C63A)=Sof(H63C)=Sof(H63D)=
 Sof(C62A)=Sof(H62C)=Sof(H62D)=Sof(C61A)=Sof(H61C)=Sof(H61D)=1-FVAR(1)
 Sof(O4)=Sof(C64)=Sof(H64A)=Sof(H64B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C62)=
 Sof(H62A)=Sof(H62B)=Sof(C61)=Sof(H61A)=Sof(H61B)=FVAR(1)
 Sof(H32C)=Sof(H32D)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31C)=Sof(H31D)=1-FVAR(2)
 Sof(H32A)=Sof(H32B)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C39(H39), C22(H22), C51(H51), C54(H54), C42(H42), C10(H10)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C57(H57A,H57B), C26(H26A,H26B), C25(H25A,H25B), C29(H29A,
 H29B), C60(H60A,H60B), C27(H27A,H27B), C32(H32A,H32B), C32(H32C,H32D),
 C30(H30A,H30B), C30(H30C,H30D), C58(H58A,H58B), C59(H59A,H59B), C31(H31A,H31B),
  C64(H64A,H64B), C63(H63A,H63B), C62(H62A,H62B), C61(H61A,H61B), C64A(H64C,
 H64D), C63A(H63C,H63D), C62A(H62C,H62D), C61A(H61C,H61D), C31A(H31C,H31D)
6.c Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C47(H47), C17(H17), C3(H3), C35(H35), C4(H4), C49(H49),
 C48(H48), C5(H5), C37(H37), C36(H36)
6.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C24(H24A,H24B,H24C), C21(H21A,H21B,H21C), C43(H43A,H43B,H43C), C44(H44A,
 H44B,H44C), C55(H55A,H55B,H55C), C41(H41A,H41B,H41C), C53(H53A,H53B,H53C),
 C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C),
  C9(H9A,H9B,H9C)
;
_shelx_res_checksum              50949
_olex2_submission_special_instructions 'No special instructions were received'