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_7703888
_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         '0.5(C64 H108 N6 Na2 O8)'
_chemical_formula_sum            'C32 H54 N3 Na O4'
_chemical_formula_weight         567.77
_chemical_name_systematic        '[Na(DME)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 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 105.340(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.0231(15)
_cell_length_b                   10.9042(8)
_cell_length_c                   33.135(3)
_cell_measurement_reflns_used    1886
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.005
_cell_measurement_theta_min      2.550
_cell_volume                     6976.8(10)
_computing_cell_refinement       'SAINT V8.32B (?, 2016)'
_computing_data_reduction        'SAINT V8.32B (?, 2016)'
_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      149.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1518
_diffrn_reflns_av_unetI/netI     0.1665
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            51336
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         1.078
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1563 before and 0.0671 after correction. The Ratio of minimum to maximum transmission is 0.9018. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0017(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   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     860
_refine_ls_number_reflns         12438
_refine_ls_number_restraints     268
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2242
_refine_ls_R_factor_gt           0.0780
_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^)+(0.0970P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1772
_refine_ls_wR_factor_ref         0.2454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4571
_reflns_number_total             12438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00285b2.cif
_cod_data_source_block           6(dme)2
_cod_depositor_comments
'Adding full bibliography for 7703878--7703902.cif.'
_cod_original_cell_volume        6976.8(9)
_cod_database_code               7703888
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.986
_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
 C64A-C63A = C62A-C61A
 2.394 with sigma of 0.04
 C63A-O7A = O8A-C62A
 2.412 with sigma of 0.04
 C61-C62 = C63-C64
 2.394 with sigma of 0.04
 C62-O8 = O7-C63
 2.412 with sigma of 0.04
 C57-C58 = C59-C60
 2.394 with sigma of 0.04
 C58-O6 = O5-C59
 2.412 with sigma of 0.04
 C57A-C58A = C59A-C60A
 2.394 with sigma of 0.04
 C58A-O6A = O5A-C59A
 2.412 with sigma of 0.04
 O8A-C64A \\sim O7A-C61A \\sim O8A-C63A \\sim O7A-C62A
 with sigma of 0.02
 O7-C61 \\sim O8-C64 \\sim O7-C62 \\sim O8-C63
 with sigma of 0.02
 O5-C57 \\sim O6-C60 \\sim O5-C58 \\sim O6-C59
 with sigma of 0.02
 O5A-C57A \\sim O6A-C60A \\sim O5A-C58A \\sim O6A-C59A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C64A \\sim C63A \\sim C62A \\sim C61A \\sim O7A \\sim O8A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
C61 \\sim C62 \\sim C63 \\sim C64 \\sim O8 \\sim O7: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
C57 \\sim C58 \\sim C59 \\sim C60 \\sim O6 \\sim O5: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
C57A \\sim C58A \\sim C59A \\sim C60A \\sim O6A \\sim O5A: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C64A, C63A, C62A, C61A, O7A, O8A
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C61, C62, C63, C64, O8, O7
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C57, C58, C59, C60, O6, O5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C57A, C58A, C59A, C60A, O6A, O5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O8A)=Sof(O7A)=Sof(C64A)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C63A)=Sof(H1AA)=
 Sof(H1AB)=Sof(C62A)=Sof(H1BA)=Sof(H1BB)=Sof(C61A)=Sof(H1CA)=Sof(H1CB)=
 Sof(H1CC)=1-FVAR(1)
 Sof(O7)=Sof(O8)=Sof(C61)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(C62)=Sof(H1EA)=
 Sof(H1EB)=Sof(C63)=Sof(H1FA)=Sof(H1FB)=Sof(C64)=Sof(H1GA)=Sof(H1GB)=Sof(H1GC)=
 FVAR(1)
 Sof(O5A)=Sof(O6A)=Sof(C57A)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=Sof(C58A)=Sof(H1MA)=
 Sof(H1MB)=Sof(C59A)=Sof(H1NA)=Sof(H1NB)=Sof(C60A)=Sof(H1OA)=Sof(H1OB)=
 Sof(H1OC)=1-FVAR(2)
 Sof(O5)=Sof(O6)=Sof(C57)=Sof(H57A)=Sof(H57B)=Sof(H57C)=Sof(C58)=Sof(H58A)=
 Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(H60C)=
 FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C22(H22), C19(H19), C10(H10), C7(H7), C39(H39), C51(H51), C42(H42), C54(H54)
6.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C31(H31A,H31B), C30(H30A,H30B), C63A(H1AA,
 H1AB), C62A(H1BA,H1BB), C62(H1EA,H1EB), C63(H1FA,H1FB), C58(H58A,H58B),
 C59(H59A,H59B), C58A(H1MA,H1MB), C59A(H1NA,H1NB)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C15(H15), C5(H5), C17(H17), C16(H16), C35(H35), C47(H47),
 C37(H37), C36(H36), C49(H49), C48(H48)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C11(H11A,H11B,H11C), C24(H24A,H24B,H24C), C20(H20A,H20B,
 H20C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C12(H12A,H12B,
 H12C), C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C29(H29A,
 H29B,H29C), C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C40(H40A,H40B,H40C),
 C44(H44A,H44B,H44C), C56(H56A,H56B,H56C), C55(H55A,H55B,H55C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C64A(H0AA,H0AB,H0AC), C61A(H1CA,H1CB,H1CC),
 C61(H1DA,H1DB,H1DC), C64(H1GA,H1GB,H1GC), C57(H57A,H57B,H57C), C60(H60A,H60B,
 H60C), C57A(H1LA,H1LB,H1LC), C60A(H1OA,H1OB,H1OC)
;
_shelx_res_checksum              1031
_olex2_submission_special_instructions 'No special instructions were received'