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_7703887
_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         'C36 H58 K N3 O6, 0.5(C7 H8)'
_chemical_formula_sum            'C39.5 H62 K N3 O6'
_chemical_formula_weight         714.02
_chemical_name_common            '[K(18-crown-6)(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                80.650(4)
_cell_angle_beta                 85.194(4)
_cell_angle_gamma                79.586(4)
_cell_formula_units_Z            2
_cell_length_a                   8.9780(6)
_cell_length_b                   10.6630(9)
_cell_length_c                   21.8772(19)
_cell_measurement_reflns_used    6321
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.898
_cell_measurement_theta_min      2.304
_cell_volume                     2029.3(3)
_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 0.997
_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  0.0628
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33912
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_min         2.048
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1407 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.8992. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             774
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         8950
_refine_ls_number_restraints     122
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0470P)^2^+0.3885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5834
_reflns_number_total             8950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           7(18c6)
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_original_formula_sum        'C39.50 H62 K N3 O6'
_cod_database_code               7703887
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.942
_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
 C38-C43 \\sim C43-C42 \\sim C42-C41 \\sim C41-C40 \\sim C40-C39 \\sim C39-C38
 with sigma of 0.02
 C38-C40 \\sim C38-C42 \\sim C39-C41 \\sim C43-C39 \\sim C42-C40 \\sim C43-C41
 with sigma of 0.04
 C37-C39 \\sim C37-C43
 with sigma of 0.04
3. Restrained planarity
 C37, C38, C43, C42, C41, C40, C39
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C43 \\sim C42 \\sim C41 \\sim C40 \\sim C39: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C37, C38, C43, C42, C41, C40, C39
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C38(0.5) C43(0.5) H43(0.5)
 C42(0.5) H42(0.5) C41(0.5) H41(0.5) C40(0.5) H40(0.5) C39(0.5) H39(0.5)
7.a Ternary CH refined with riding coordinates:
 C10(H10), C7(H7), C22(H22), C19(H19)
7.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C36(H36A,H36B), C27(H27A,H27B), C26(H26A,H26B), C29(H29A,
 H29B), C28(H28A,H28B), C35(H35A,H35B), C33(H33A,H33B), C32(H32A,H32B),
 C30(H30A,H30B), C34(H34A,H34B), C31(H31A,H31B)
7.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3), C17(H17), C15(H15), C16(H16), C43(H43), C42(H42),
 C41(H41), C40(H40), C39(H39)
7.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C9(H9A,H9B,
 H9C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C21(H21A,H21B,
 H21C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              26429
_olex2_submission_special_instructions 'No special instructions were received'