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_7703891
_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         'C54 H80 K2 N6 O1.5, 0.5(C7 H8)'
_chemical_formula_sum            'C57.5 H84 K2 N6 O1.5'
_chemical_formula_weight         961.50
_chemical_name_common            '[K(THF)1.5(N3Dipp2)]'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-27
_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                96.923(4)
_cell_angle_beta                 110.851(3)
_cell_angle_gamma                98.577(3)
_cell_formula_units_Z            2
_cell_length_a                   13.1068(9)
_cell_length_b                   14.9847(10)
_cell_length_c                   15.9757(11)
_cell_measurement_reflns_used    8313
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.21
_cell_measurement_theta_min      2.29
_cell_volume                     2847.7(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 0.974
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0617
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            42503
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.149
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.209
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6620
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1829 before and 0.0494 after correction. The Ratio of minimum to maximum transmission is 0.8873. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       plate
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         12220
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1096
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+1.4929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1501
_refine_ls_wR_factor_ref         0.1725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7559
_reflns_number_total             12220
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           7(THF)
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_original_formula_sum        'C57.50 H84 K2 N6 O1.50'
_cod_database_code               7703891
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.971
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O1-C25 = O1-C28
 1.408 with sigma of 0.02
 C26-C25 = C28-C27
 1.472 with sigma of 0.02
 C26-C27
 1.459 with sigma of 0.02
 N4-N5A = N5A-N6A
 1.318 with sigma of 0.02
 N3A-N2A = N1-N2A
 1.318 with sigma of 0.02
 O1-C26 = O1-C27
 2.315 with sigma of 0.02
 C25-C27 = C28-C26
 2.332 with sigma of 0.02
 N1-N3A = N4-N6A
 2.183 with sigma of 0.02
 C29-C30 \\sim C30-C31 \\sim C31-C32
 with sigma of 0.02
 O2-C29 \\sim O2-C32
 with sigma of 0.02
 O2-C30 \\sim O2-C31
 with sigma of 0.04
 C30-C32 \\sim C29-C31
 with sigma of 0.04
 C58-C63 \\sim C63-C62 \\sim C62-C61 \\sim C61-C60 \\sim C60-C59 \\sim C59-C58
 with sigma of 0.02
 C58-C60 \\sim C58-C62 \\sim C59-C61 \\sim C63-C59 \\sim C62-C60 \\sim C63-C61
 with sigma of 0.04
 C57-C59 \\sim C57-C63
 with sigma of 0.04
3. Restrained planarity
 C57, C58, C63, C62, C61, C60, C59
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O2 \\sim C29 \\sim C30 \\sim C31 \\sim C32: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04
C57 \\sim C58 \\sim C63 \\sim C62 \\sim C61 \\sim C60 \\sim C59: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C24A \\sim C22A \\sim C23 \\sim C18A \\sim C17 \\sim C13A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O2, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C57, C58, C63, C62, C61, C60, C59
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24A, C22A, C23, C18A, C17, C13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: N5(0.7) N6(0.7) C45(0.7) C50(0.7) H49(0.7) H49A(0.3) C54(0.7)
 H54(0.7) C55(0.7) H55A(0.7) H55B(0.7) H55C(0.7) C56(0.7) H56A(0.7) H56B(0.7)
 H56C(0.7) N2(0.8) N3(0.8) C13(0.8) H17(0.8) H17A(0.2) C18(0.8) C22(0.8)
 H22(0.8) H23A(0.8) H23B(0.8) H23C(0.8) H23D(0.2) H23E(0.2) H23F(0.2) C24(0.8)
 H24A(0.8) H24B(0.8) H24C(0.8) N5A(0.3) N6A(0.3) C45A(0.3) C50A(0.3) C54A(0.3)
 H54A(0.3) C55A(0.3) H55D(0.3) H55E(0.3) H55F(0.3) C56A(0.3) H56D(0.3)
 H56E(0.3) H56F(0.3) N2A(0.2) N3A(0.2) C13A(0.2) C18A(0.2) C22A(0.2) H22A(0.2)
 C24A(0.2) H24D(0.2) H24E(0.2) H24F(0.2) O2(0.5) C29(0.5) H29A(0.5) H29B(0.5)
 C30(0.5) H30A(0.5) H30B(0.5) C31(0.5) H31A(0.5) H31B(0.5) C32(0.5) H32A(0.5)
 H32B(0.5) C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) C58(0.5) C63(0.5) H63(0.5)
 C62(0.5) H62(0.5) C61(0.5) H61(0.5) C60(0.5) H60(0.5) C59(0.5) H59(0.5)
7.a Ternary CH refined with riding coordinates:
 C42(H42), C39(H39), C54(H54), C51(H51), C7(H7), C10(H10), C19(H19), C22(H22),
 C54A(H54A), C22A(H22A)
7.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C27(H27A,H27B), C29(H29A,
 H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B)
7.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C), C23(H23D,H23E,H23F)
7.d Aromatic/amide H refined with riding coordinates:
 C37(H37), C36(H36), C35(H35), C49(H49), C49(H49A), C48(H48), C47(H47), C3(H3),
  C4(H4), C5(H5), C15(H15), C16(H16), C17(H17), C17(H17A), C63(H63), C62(H62),
 C61(H61), C60(H60), C59(H59)
7.e Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C11(H11A,
 H11B,H11C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C),
 C55A(H55D,H55E,H55F), C56A(H56D,H56E,H56F), C24A(H24D,H24E,H24F), C57(H57A,
 H57B,H57C)
;
_shelx_res_checksum              86421
_olex2_submission_special_instructions 'No special instructions were received'